# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2002 data_global _journal_coden_Cambridge 440 _publ_requested_journal 'New Journal of Chemistry' loop_ _publ_author_name 'Lin-Pei Jin' 'Shaozhe Lu' 'Yonghong Wan' 'Kezhi Wang' 'Liping Zhang' 'Xiangjun Zheng' _publ_contact_author_name 'Prof Lin-Pei Jin' _publ_contact_author_address ; Department of Chemistry Beijing Normal University Beijing 100875 CHINA ; _publ_contact_author_email 'LPJIN@BNU.EDU.CN' _publ_section_title ; Hydrothermal sysnthesis and structural studies of novel 2-D lanthanide coordination polymers with phthalic acid ; data_JA012746I-15-344 _database_code_CSD 177915 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H28 O26 Yb4' _chemical_formula_weight 1712.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Yb' 'Yb' -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.570(4) _cell_length_b 13.780(4) _cell_length_c 15.869(5) _cell_angle_alpha 75.363(4) _cell_angle_beta 69.196(5) _cell_angle_gamma 65.697(4) _cell_volume 2323.3(12) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.448 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1608 _exptl_absorpt_coefficient_mu 8.076 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.1071 _exptl_absorpt_correction_T_max 0.6882 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9393 _diffrn_reflns_av_R_equivalents 0.0408 _diffrn_reflns_av_sigmaI/netI 0.0343 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 25.03 _reflns_number_total 7875 _reflns_number_gt 6891 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0900P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00305(19) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 7875 _refine_ls_number_parameters 704 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0477 _refine_ls_R_factor_gt 0.0423 _refine_ls_wR_factor_ref 0.1158 _refine_ls_wR_factor_gt 0.1110 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.011 _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 Yb1 Yb 0.68190(3) 0.12053(3) 0.463347(19) 0.01705(12) Uani 1 1 d . . . Yb2 Yb 0.99828(2) 0.00354(3) 0.24149(2) 0.01807(12) Uani 1 1 d . . . Yb3 Yb 0.30643(3) -0.11185(3) 1.00344(2) 0.01781(12) Uani 1 1 d . . . Yb4 Yb 0.51489(3) 0.04948(3) 0.741624(19) 0.01723(12) Uani 1 1 d . . . O1 O 0.6206(5) 0.2550(4) 0.5469(3) 0.0229(11) Uani 1 1 d . . . O2 O 0.6039(5) 0.1758(4) 0.6896(3) 0.0259(12) Uani 1 1 d . . . O3 O 0.8497(5) 0.1489(5) 0.7328(4) 0.0309(13) Uani 1 1 d . . . O4 O 0.6841(5) 0.1855(5) 0.8513(3) 0.0276(13) Uani 1 1 d . . . O5 O 0.8555(5) -0.0424(5) 0.3570(4) 0.0283(13) Uani 1 1 d . . . O6 O 0.6693(5) -0.0306(5) 0.4389(4) 0.0275(13) Uani 1 1 d . . . O7 O 0.4977(4) -0.1007(4) 0.4033(3) 0.0213(11) Uani 1 1 d . . . O8 O 0.5259(4) -0.1917(5) 0.5335(3) 0.0251(12) Uani 1 1 d . . . O9 O 0.8434(5) 0.1692(5) 0.4127(4) 0.0338(14) Uani 1 1 d . . . O10 O 1.0293(5) 0.0751(5) 0.3376(4) 0.0327(14) Uani 1 1 d . . . O11 O 1.2955(5) 0.0627(5) 0.3019(4) 0.0312(14) Uani 1 1 d . . . O12 O 1.2177(5) -0.0034(4) 0.4426(4) 0.0252(12) Uani 1 1 d . . . O13 O 0.6782(5) 0.1916(5) 0.3210(4) 0.0299(13) Uani 1 1 d . . . O14 O 0.8525(5) 0.1581(5) 0.2112(4) 0.0274(13) Uani 1 1 d . . . O15 O 0.6461(5) 0.1884(4) 0.1296(3) 0.0257(12) Uani 1 1 d . . . O16 O 0.6395(5) 0.2997(4) 0.0050(3) 0.0263(12) Uani 1 1 d . . . O17 O 0.3151(4) 0.1188(5) 0.7884(4) 0.0274(13) Uani 1 1 d . . . O18 O 0.2295(5) 0.0268(4) 0.9121(4) 0.0267(12) Uani 1 1 d . . . O19 O 0.0329(5) 0.0864(5) 0.8387(4) 0.0288(13) Uani 1 1 d . . . O20 O -0.1303(5) 0.1338(5) 0.9558(4) 0.0351(14) Uani 1 1 d . . . O21 O 0.5125(5) -0.0684(5) 0.8684(4) 0.0310(14) Uani 1 1 d . . . O22 O 0.5122(4) -0.1877(5) 0.9895(3) 0.0252(12) Uani 1 1 d . . . O23 O 0.6714(5) -0.0332(5) 0.9559(4) 0.0264(13) Uani 1 1 d . . . O24 O 0.8585(5) -0.0442(5) 0.8770(4) 0.0295(13) Uani 1 1 d . . . O25 O 0.4745(5) 0.1465(5) 0.8565(4) 0.0324(14) Uani 1 1 d . . . O26 O 0.4769(5) -0.0879(5) 0.7095(4) 0.0321(14) Uani 1 1 d . . . C1 C 0.6225(6) 0.2505(6) 0.6270(5) 0.0187(16) Uani 1 1 d . . . C2 C 0.6477(6) 0.3346(6) 0.6500(5) 0.0185(16) Uani 1 1 d . . . C3 C 0.6136(7) 0.4379(7) 0.6034(6) 0.0282(18) Uani 1 1 d . . . H3A H 0.5862 0.4498 0.5531 0.034 Uiso 1 1 calc R . . C4 C 0.6196(9) 0.5231(7) 0.6303(7) 0.041(2) Uani 1 1 d . . . H4A H 0.5917 0.5923 0.6010 0.049 Uiso 1 1 calc R . . C5 C 0.6677(9) 0.5039(8) 0.7013(7) 0.042(2) Uani 1 1 d . . . H5A H 0.6745 0.5603 0.7186 0.050 Uiso 1 1 calc R . . C6 C 0.7056(8) 0.4028(7) 0.7467(6) 0.032(2) Uani 1 1 d . . . H6A H 0.7378 0.3912 0.7944 0.038 Uiso 1 1 calc R . . C7 C 0.6963(7) 0.3176(6) 0.7220(5) 0.0195(16) Uani 1 1 d . . . C8 C 0.7467(7) 0.2075(7) 0.7723(5) 0.0213(17) Uani 1 1 d . . . C9 C 0.7714(7) -0.0822(6) 0.3907(5) 0.0196(16) Uani 1 1 d . . . C10 C 0.7931(6) -0.1899(7) 0.3744(5) 0.0220(17) Uani 1 1 d . . . C11 C 0.9100(7) -0.2575(7) 0.3341(5) 0.0287(19) Uani 1 1 d . . . H11A H 0.9751 -0.2341 0.3176 0.034 Uiso 1 1 calc R . . C12 C 0.9304(8) -0.3584(8) 0.3183(6) 0.037(2) Uani 1 1 d . . . H12A H 1.0090 -0.4026 0.2915 0.044 Uiso 1 1 calc R . . C13 C 0.8350(8) -0.3941(7) 0.3421(6) 0.033(2) Uani 1 1 d . . . H13A H 0.8485 -0.4603 0.3277 0.040 Uiso 1 1 calc R . . C14 C 0.7187(8) -0.3316(7) 0.3874(5) 0.0293(19) Uani 1 1 d . . . H14A H 0.6550 -0.3573 0.4065 0.035 Uiso 1 1 calc R . . C15 C 0.6988(7) -0.2308(7) 0.4038(5) 0.0213(16) Uani 1 1 d . . . C16 C 0.5688(6) -0.1676(6) 0.4502(5) 0.0189(16) Uani 1 1 d . . . C17 C 0.9545(7) 0.1457(6) 0.3897(5) 0.0191(16) Uani 1 1 d . . . C18 C 1.0045(7) 0.2115(6) 0.4162(5) 0.0181(15) Uani 1 1 d . . . C19 C 0.9283(8) 0.3060(8) 0.4496(6) 0.034(2) Uani 1 1 d . . . H19A H 0.8446 0.3257 0.4617 0.041 Uiso 1 1 calc R . . C20 C 0.9741(10) 0.3728(7) 0.4658(7) 0.040(2) Uani 1 1 d . . . H20A H 0.9210 0.4365 0.4897 0.049 Uiso 1 1 calc R . . C21 C 1.0979(9) 0.3459(8) 0.4467(7) 0.041(2) Uani 1 1 d . . . H21A H 1.1286 0.3922 0.4555 0.050 Uiso 1 1 calc R . . C22 C 1.1765(8) 0.2488(7) 0.4141(6) 0.032(2) Uani 1 1 d . . . H22A H 1.2602 0.2305 0.4005 0.039 Uiso 1 1 calc R . . C23 C 1.1310(7) 0.1795(7) 0.4017(5) 0.0263(18) Uani 1 1 d . . . C24 C 1.2204(6) 0.0707(7) 0.3783(5) 0.0222(17) Uani 1 1 d . . . C25 C 0.7469(7) 0.2170(7) 0.2466(5) 0.0238(18) Uani 1 1 d . . . C26 C 0.6997(7) 0.3314(7) 0.2018(5) 0.0214(16) Uani 1 1 d . . . C27 C 0.7026(7) 0.4105(7) 0.2401(6) 0.0295(19) Uani 1 1 d . . . H27A H 0.7321 0.3919 0.2903 0.035 Uiso 1 1 calc R . . C28 C 0.6612(8) 0.5177(9) 0.2028(6) 0.040(2) Uani 1 1 d . . . H28A H 0.6658 0.5702 0.2271 0.048 Uiso 1 1 calc R . . C29 C 0.6136(9) 0.5464(8) 0.1302(7) 0.039(2) Uani 1 1 d . . . H29A H 0.5842 0.6182 0.1068 0.047 Uiso 1 1 calc R . . C30 C 0.6096(8) 0.4688(7) 0.0925(6) 0.032(2) Uani 1 1 d . . . H30A H 0.5790 0.4884 0.0428 0.039 Uiso 1 1 calc R . . C31 C 0.6510(7) 0.3608(7) 0.1283(5) 0.0213(17) Uani 1 1 d . . . C32 C 0.6435(6) 0.2797(6) 0.0849(5) 0.0190(16) Uani 1 1 d . . . C33 C 0.2308(6) 0.1119(6) 0.8605(5) 0.0191(16) Uani 1 1 d . . . C34 C 0.1293(6) 0.2145(6) 0.8872(5) 0.0180(15) Uani 1 1 d . . . C35 C 0.1592(7) 0.2981(7) 0.8932(6) 0.0287(18) Uani 1 1 d . . . H35A H 0.2405 0.2916 0.8754 0.034 Uiso 1 1 calc R . . C36 C 0.0693(8) 0.3910(8) 0.9255(7) 0.041(2) Uani 1 1 d . . . H36A H 0.0903 0.4465 0.9299 0.049 Uiso 1 1 calc R . . C37 C -0.0517(9) 0.4016(9) 0.9513(7) 0.043(2) Uani 1 1 d . . . H37A H -0.1123 0.4643 0.9727 0.051 Uiso 1 1 calc R . . C38 C -0.0822(7) 0.3189(7) 0.9451(6) 0.0298(19) Uani 1 1 d . . . H38A H -0.1638 0.3266 0.9619 0.036 Uiso 1 1 calc R . . C39 C 0.0068(7) 0.2247(7) 0.9144(5) 0.0226(17) Uani 1 1 d . . . C40 C -0.0328(7) 0.1403(6) 0.9036(5) 0.0193(16) Uani 1 1 d . . . C41 C 0.5692(6) -0.1506(6) 0.9142(5) 0.0176(16) Uani 1 1 d . . . C42 C 0.7008(7) -0.2146(6) 0.8785(5) 0.0198(15) Uani 1 1 d . . . C43 C 0.7260(8) -0.3091(7) 0.8475(6) 0.033(2) Uani 1 1 d . . . H43A H 0.6624 -0.3293 0.8508 0.039 Uiso 1 1 calc R . . C44 C 0.8454(8) -0.3739(7) 0.8116(6) 0.038(2) Uani 1 1 d . . . H44A H 0.8622 -0.4362 0.7888 0.046 Uiso 1 1 calc R . . C45 C 0.9399(8) -0.3448(7) 0.8099(6) 0.037(2) Uani 1 1 d . . . H45A H 1.0202 -0.3885 0.7868 0.045 Uiso 1 1 calc R . . C46 C 0.9153(7) -0.2529(7) 0.8420(6) 0.0285(18) Uani 1 1 d . . . H46A H 0.9793 -0.2354 0.8419 0.034 Uiso 1 1 calc R . . C47 C 0.7967(6) -0.1851(7) 0.8746(5) 0.0220(16) Uani 1 1 d . . . C48 C 0.7730(7) -0.0824(6) 0.9051(5) 0.0214(16) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Yb1 0.01503(18) 0.0250(2) 0.01519(18) -0.00889(13) -0.00086(13) -0.01028(15) Yb2 0.01456(19) 0.0263(2) 0.01777(18) -0.01256(13) 0.00124(13) -0.01070(16) Yb3 0.01697(19) 0.0243(2) 0.01685(18) -0.00860(13) -0.00182(13) -0.01081(15) Yb4 0.01494(19) 0.0243(2) 0.01459(18) -0.00827(13) -0.00009(13) -0.00916(15) O1 0.028(3) 0.021(3) 0.021(3) -0.010(2) -0.004(2) -0.008(2) O2 0.039(3) 0.026(3) 0.021(3) -0.002(2) -0.010(2) -0.018(3) O3 0.019(3) 0.034(4) 0.030(3) -0.012(3) 0.002(2) -0.002(3) O4 0.032(3) 0.034(4) 0.018(3) -0.009(2) -0.003(2) -0.013(3) O5 0.026(3) 0.045(4) 0.023(3) -0.004(2) -0.002(2) -0.026(3) O6 0.018(3) 0.031(3) 0.034(3) -0.019(3) 0.007(2) -0.012(2) O7 0.017(3) 0.021(3) 0.028(3) -0.012(2) -0.005(2) -0.004(2) O8 0.018(3) 0.039(4) 0.018(3) -0.003(2) -0.002(2) -0.012(2) O9 0.019(3) 0.034(4) 0.051(4) -0.010(3) -0.006(3) -0.014(3) O10 0.026(3) 0.048(4) 0.037(3) -0.025(3) -0.007(3) -0.016(3) O11 0.016(3) 0.032(4) 0.036(3) -0.013(3) 0.007(2) -0.006(2) O12 0.027(3) 0.023(3) 0.027(3) -0.011(2) -0.010(2) -0.005(2) O13 0.026(3) 0.046(4) 0.021(3) -0.007(2) -0.004(2) -0.016(3) O14 0.016(3) 0.032(4) 0.033(3) -0.017(2) -0.001(2) -0.005(2) O15 0.033(3) 0.022(3) 0.024(3) -0.011(2) -0.001(2) -0.013(3) O16 0.035(3) 0.025(3) 0.025(3) -0.005(2) -0.012(2) -0.011(3) O17 0.014(3) 0.035(4) 0.029(3) -0.011(2) -0.001(2) -0.006(2) O18 0.029(3) 0.016(3) 0.037(3) -0.008(2) -0.009(3) -0.008(2) O19 0.031(3) 0.042(4) 0.029(3) -0.020(3) -0.005(2) -0.021(3) O20 0.023(3) 0.030(4) 0.053(4) -0.022(3) 0.008(3) -0.017(3) O21 0.032(3) 0.046(4) 0.019(3) -0.006(3) -0.005(2) -0.019(3) O22 0.016(3) 0.033(3) 0.025(3) -0.005(2) 0.002(2) -0.012(2) O23 0.024(3) 0.037(4) 0.027(3) -0.018(2) 0.000(2) -0.017(3) O24 0.024(3) 0.042(4) 0.031(3) -0.008(3) -0.003(2) -0.023(3) O25 0.032(3) 0.040(4) 0.029(3) -0.021(3) -0.005(2) -0.009(3) O26 0.044(4) 0.030(4) 0.033(3) -0.010(3) -0.010(3) -0.021(3) C1 0.017(4) 0.018(4) 0.021(4) -0.011(3) -0.003(3) -0.004(3) C2 0.017(4) 0.023(4) 0.016(3) -0.008(3) 0.001(3) -0.009(3) C3 0.030(4) 0.028(5) 0.028(4) -0.006(3) -0.010(3) -0.009(4) C4 0.060(6) 0.013(5) 0.049(6) -0.001(4) -0.015(5) -0.015(4) C5 0.059(6) 0.022(5) 0.052(6) -0.019(4) -0.012(5) -0.017(5) C6 0.044(5) 0.028(5) 0.037(5) -0.014(4) -0.015(4) -0.017(4) C7 0.022(4) 0.022(4) 0.014(3) -0.011(3) 0.000(3) -0.006(3) C8 0.019(4) 0.036(5) 0.018(4) -0.017(3) 0.000(3) -0.015(4) C9 0.025(4) 0.020(4) 0.018(3) -0.002(3) -0.009(3) -0.011(3) C10 0.018(4) 0.033(5) 0.015(3) -0.011(3) 0.000(3) -0.009(3) C11 0.021(4) 0.040(6) 0.022(4) -0.007(3) 0.001(3) -0.012(4) C12 0.027(4) 0.029(5) 0.042(5) -0.013(4) -0.002(4) -0.001(4) C13 0.035(5) 0.019(5) 0.041(5) -0.015(4) -0.006(4) -0.003(4) C14 0.036(5) 0.031(5) 0.030(4) -0.007(4) -0.007(4) -0.020(4) C15 0.020(4) 0.029(5) 0.018(3) -0.008(3) -0.005(3) -0.009(3) C16 0.019(4) 0.027(5) 0.018(4) -0.006(3) -0.003(3) -0.016(3) C17 0.018(4) 0.022(4) 0.024(4) -0.004(3) -0.004(3) -0.013(3) C18 0.023(4) 0.009(4) 0.022(4) -0.007(3) -0.003(3) -0.006(3) C19 0.031(5) 0.035(6) 0.040(5) -0.016(4) -0.012(4) -0.007(4) C20 0.061(6) 0.014(5) 0.048(6) -0.020(4) -0.021(5) -0.001(4) C21 0.056(6) 0.034(6) 0.054(6) -0.013(4) -0.022(5) -0.025(5) C22 0.034(5) 0.036(6) 0.039(5) -0.003(4) -0.017(4) -0.020(4) C23 0.026(4) 0.041(5) 0.019(4) -0.013(3) 0.000(3) -0.018(4) C24 0.010(3) 0.031(5) 0.032(4) -0.010(3) -0.008(3) -0.009(3) C25 0.023(4) 0.043(5) 0.016(4) -0.015(3) 0.001(3) -0.022(4) C26 0.022(4) 0.028(5) 0.016(3) -0.011(3) 0.006(3) -0.015(3) C27 0.033(5) 0.033(5) 0.029(4) -0.015(4) -0.005(4) -0.016(4) C28 0.042(5) 0.050(7) 0.041(5) -0.025(5) 0.000(4) -0.027(5) C29 0.048(6) 0.021(5) 0.046(5) -0.014(4) -0.007(4) -0.011(4) C30 0.033(5) 0.035(6) 0.032(5) -0.011(4) -0.007(4) -0.014(4) C31 0.022(4) 0.027(5) 0.019(4) -0.012(3) 0.003(3) -0.014(3) C32 0.018(4) 0.020(4) 0.019(4) -0.009(3) -0.002(3) -0.006(3) C33 0.010(3) 0.026(5) 0.025(4) -0.016(3) 0.001(3) -0.008(3) C34 0.022(4) 0.022(4) 0.014(3) -0.006(3) 0.001(3) -0.015(3) C35 0.025(4) 0.030(5) 0.039(5) -0.012(4) -0.008(4) -0.014(4) C36 0.041(5) 0.035(6) 0.057(6) -0.020(4) -0.005(4) -0.022(5) C37 0.034(5) 0.042(6) 0.056(6) -0.025(5) -0.006(5) -0.013(5) C38 0.023(4) 0.039(5) 0.034(4) -0.018(4) -0.002(3) -0.015(4) C39 0.029(4) 0.024(5) 0.021(4) -0.008(3) 0.000(3) -0.018(4) C40 0.020(4) 0.018(4) 0.026(4) -0.010(3) -0.007(3) -0.009(3) C41 0.016(4) 0.029(5) 0.014(3) -0.011(3) -0.004(3) -0.011(3) C42 0.021(4) 0.014(4) 0.024(4) -0.006(3) -0.003(3) -0.007(3) C43 0.031(5) 0.034(5) 0.043(5) -0.013(4) -0.007(4) -0.019(4) C44 0.043(5) 0.022(5) 0.043(5) -0.018(4) -0.001(4) -0.007(4) C45 0.024(4) 0.022(5) 0.050(5) -0.012(4) 0.000(4) 0.002(4) C46 0.019(4) 0.023(5) 0.039(5) -0.007(4) -0.005(3) -0.004(3) C47 0.014(4) 0.028(5) 0.019(4) -0.008(3) 0.001(3) -0.005(3) C48 0.023(4) 0.026(5) 0.017(3) -0.009(3) -0.007(3) -0.006(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Yb1 O12 2.206(5) 2_756 ? Yb1 O9 2.215(5) . ? Yb1 O13 2.233(5) . ? Yb1 O1 2.264(5) . ? Yb1 O6 2.288(5) . ? Yb1 O8 2.369(5) 2_656 ? Yb1 O7 2.544(5) 2_656 ? Yb1 O5 2.814(6) . ? Yb1 C16 2.816(7) 2_656 ? Yb1 C9 2.918(8) . ? Yb1 Yb4 4.2176(12) . ? Yb1 Yb2 4.2959(10) . ? Yb2 O19 2.205(5) 2_656 ? Yb2 O10 2.224(5) . ? Yb2 O24 2.232(5) 2_756 ? Yb2 O5 2.234(5) . ? Yb2 O14 2.241(6) . ? Yb2 O3 2.247(6) 2_756 ? Yb2 C17 3.193(8) . ? Yb3 O18 2.183(6) . ? Yb3 O20 2.202(5) 2_557 ? Yb3 O4 2.295(5) 2_657 ? Yb3 O22 2.306(5) . ? Yb3 O15 2.375(5) 2_656 ? Yb3 O23 2.393(5) 2_657 ? Yb3 O16 2.418(6) 2_656 ? Yb3 C32 2.743(8) 2_656 ? Yb3 O24 2.850(6) 2_657 ? Yb3 O21 2.889(5) . ? Yb3 C41 2.968(7) . ? Yb3 C48 3.000(8) 2_657 ? Yb4 O17 2.198(5) . ? Yb4 O11 2.210(5) 2_756 ? Yb4 O21 2.243(6) . ? Yb4 O7 2.272(5) 2_656 ? Yb4 O2 2.277(5) . ? Yb4 O25 2.320(5) . ? Yb4 O26 2.340(6) . ? Yb4 C24 3.161(7) 2_756 ? O1 C1 1.265(9) . ? O2 C1 1.271(9) . ? O3 C8 1.241(9) . ? O3 Yb2 2.247(6) 2_756 ? O4 C8 1.260(9) . ? O4 Yb3 2.295(5) 2_657 ? O5 C9 1.277(9) . ? O6 C9 1.251(9) . ? O7 C16 1.284(9) . ? O7 Yb4 2.272(5) 2_656 ? O7 Yb1 2.544(5) 2_656 ? O8 C16 1.253(9) . ? O8 Yb1 2.369(5) 2_656 ? O9 C17 1.231(9) . ? O10 C17 1.271(10) . ? O11 C24 1.242(9) . ? O11 Yb4 2.210(5) 2_756 ? O12 C24 1.250(9) . ? O12 Yb1 2.206(5) 2_756 ? O13 C25 1.257(9) . ? O14 C25 1.245(9) . ? O15 C32 1.271(9) . ? O15 Yb3 2.375(5) 2_656 ? O16 C32 1.243(9) . ? O16 Yb3 2.418(6) 2_656 ? O17 C33 1.268(9) . ? O18 C33 1.251(9) . ? O19 C40 1.254(9) . ? O19 Yb2 2.205(5) 2_656 ? O20 C40 1.236(9) . ? O20 Yb3 2.202(5) 2_557 ? O21 C41 1.267(9) . ? O22 C41 1.260(9) . ? O23 C48 1.255(9) . ? O23 Yb3 2.393(5) 2_657 ? O24 C48 1.279(9) . ? O24 Yb2 2.232(5) 2_756 ? O24 Yb3 2.850(6) 2_657 ? C1 C2 1.475(11) . ? C2 C3 1.395(11) . ? C2 C7 1.406(10) . ? C3 C4 1.385(12) . ? C4 C5 1.380(14) . ? C5 C6 1.370(13) . ? C6 C7 1.387(11) . ? C7 C8 1.515(11) . ? C9 C10 1.469(11) . ? C10 C11 1.393(11) . ? C10 C15 1.401(10) . ? C11 C12 1.379(13) . ? C12 C13 1.375(13) . ? C13 C14 1.387(12) . ? C14 C15 1.383(12) . ? C15 C16 1.506(10) . ? C16 Yb1 2.816(7) 2_656 ? C17 C18 1.498(10) . ? C18 C19 1.363(12) . ? C18 C23 1.411(10) . ? C19 C20 1.381(13) . ? C20 C21 1.377(13) . ? C21 C22 1.390(13) . ? C22 C23 1.379(11) . ? C23 C24 1.499(12) . ? C24 Yb4 3.161(7) 2_756 ? C25 C26 1.517(12) . ? C26 C27 1.394(11) . ? C26 C31 1.402(11) . ? C27 C28 1.395(13) . ? C28 C29 1.381(14) . ? C29 C30 1.375(12) . ? C30 C31 1.397(12) . ? C31 C32 1.502(10) . ? C32 Yb3 2.743(8) 2_656 ? C33 C34 1.497(10) . ? C34 C35 1.383(11) . ? C34 C39 1.400(10) . ? C35 C36 1.382(13) . ? C36 C37 1.381(13) . ? C37 C38 1.378(13) . ? C38 C39 1.384(12) . ? C39 C40 1.506(10) . ? C41 C42 1.490(10) . ? C42 C43 1.384(11) . ? C42 C47 1.399(10) . ? C43 C44 1.386(12) . ? C44 C45 1.391(13) . ? C45 C46 1.361(12) . ? C46 C47 1.384(11) . ? C47 C48 1.491(11) . ? C48 Yb3 3.000(8) 2_657 ? 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 O12 Yb1 O9 83.2(2) 2_756 . ? O12 Yb1 O13 148.9(2) 2_756 . ? O9 Yb1 O13 78.5(2) . . ? O12 Yb1 O1 91.89(19) 2_756 . ? O9 Yb1 O1 78.8(2) . . ? O13 Yb1 O1 108.8(2) . . ? O12 Yb1 O6 81.8(2) 2_756 . ? O9 Yb1 O6 127.3(2) . . ? O13 Yb1 O6 89.4(2) . . ? O1 Yb1 O6 151.64(18) . . ? O12 Yb1 O8 133.14(18) 2_756 2_656 ? O9 Yb1 O8 139.6(2) . 2_656 ? O13 Yb1 O8 74.13(18) . 2_656 ? O1 Yb1 O8 82.48(19) . 2_656 ? O6 Yb1 O8 81.9(2) . 2_656 ? O12 Yb1 O7 80.86(18) 2_756 2_656 ? O9 Yb1 O7 147.2(2) . 2_656 ? O13 Yb1 O7 126.65(18) . 2_656 ? O1 Yb1 O7 73.22(18) . 2_656 ? O6 Yb1 O7 78.48(17) . 2_656 ? O8 Yb1 O7 52.89(16) 2_656 2_656 ? O12 Yb1 O5 76.16(18) 2_756 . ? O9 Yb1 O5 77.62(19) . . ? O13 Yb1 O5 75.46(19) . . ? O1 Yb1 O5 154.64(16) . . ? O6 Yb1 O5 49.71(16) . . ? O8 Yb1 O5 122.02(17) 2_656 . ? O7 Yb1 O5 125.29(17) 2_656 . ? O12 Yb1 C16 108.0(2) 2_756 2_656 ? O9 Yb1 C16 150.0(2) . 2_656 ? O13 Yb1 C16 100.3(2) . 2_656 ? O1 Yb1 C16 73.2(2) . 2_656 ? O6 Yb1 C16 82.5(2) . 2_656 ? O8 Yb1 C16 26.18(19) 2_656 2_656 ? O7 Yb1 C16 27.11(19) 2_656 2_656 ? O5 Yb1 C16 131.56(18) . 2_656 ? O12 Yb1 C9 76.47(19) 2_756 . ? O9 Yb1 C9 103.1(2) . . ? O13 Yb1 C9 83.4(2) . . ? O1 Yb1 C9 167.77(19) . . ? O6 Yb1 C9 24.14(19) . . ? O8 Yb1 C9 102.6(2) 2_656 . ? O7 Yb1 C9 100.82(18) 2_656 . ? O5 Yb1 C9 25.65(18) . . ? C16 Yb1 C9 106.5(2) 2_656 . ? O12 Yb1 Yb4 56.75(14) 2_756 . ? O9 Yb1 Yb4 123.33(16) . . ? O13 Yb1 Yb4 153.16(14) . . ? O1 Yb1 Yb4 65.80(13) . . ? O6 Yb1 Yb4 88.03(14) . . ? O8 Yb1 Yb4 79.06(12) 2_656 . ? O7 Yb1 Yb4 27.12(11) 2_656 . ? O5 Yb1 Yb4 121.40(11) . . ? C16 Yb1 Yb4 52.87(14) 2_656 . ? C9 Yb1 Yb4 103.95(14) . . ? O12 Yb1 Yb2 88.51(14) 2_756 . ? O9 Yb1 Yb2 53.74(16) . . ? O13 Yb1 Yb2 60.39(15) . . ? O1 Yb1 Yb2 132.17(13) . . ? O6 Yb1 Yb2 75.55(13) . . ? O8 Yb1 Yb2 128.70(12) 2_656 . ? O7 Yb1 Yb2 153.09(12) 2_656 . ? O5 Yb1 Yb2 27.83(11) . . ? C16 Yb1 Yb2 150.35(14) 2_656 . ? C9 Yb1 Yb2 52.46(14) . . ? Yb4 Yb1 Yb2 143.649(13) . . ? O19 Yb2 O10 172.0(2) 2_656 . ? O19 Yb2 O24 91.9(2) 2_656 2_756 ? O10 Yb2 O24 93.8(2) . 2_756 ? O19 Yb2 O5 85.8(2) 2_656 . ? O10 Yb2 O5 88.4(2) . . ? O24 Yb2 O5 177.60(19) 2_756 . ? O19 Yb2 O14 94.2(2) 2_656 . ? O10 Yb2 O14 91.2(2) . . ? O24 Yb2 O14 92.4(2) 2_756 . ? O5 Yb2 O14 88.4(2) . . ? O19 Yb2 O3 86.2(2) 2_656 2_756 ? O10 Yb2 O3 88.6(2) . 2_756 ? O24 Yb2 O3 85.2(2) 2_756 2_756 ? O5 Yb2 O3 94.0(2) . 2_756 ? O14 Yb2 O3 177.57(19) . 2_756 ? O19 Yb2 C17 161.76(19) 2_656 . ? O10 Yb2 C17 17.77(19) . . ? O24 Yb2 C17 103.93(19) 2_756 . ? O5 Yb2 C17 78.46(19) . . ? O14 Yb2 C17 76.4(2) . . ? O3 Yb2 C17 103.9(2) 2_756 . ? O19 Yb2 Yb1 111.44(14) 2_656 . ? O10 Yb2 Yb1 66.01(14) . . ? O24 Yb2 Yb1 146.08(16) 2_756 . ? O5 Yb2 Yb1 36.01(16) . . ? O14 Yb2 Yb1 62.72(14) . . ? O3 Yb2 Yb1 119.35(14) 2_756 . ? C17 Yb2 Yb1 50.38(12) . . ? O18 Yb3 O20 85.9(2) . 2_557 ? O18 Yb3 O4 148.4(2) . 2_657 ? O20 Yb3 O4 86.4(2) 2_557 2_657 ? O18 Yb3 O22 122.54(19) . . ? O20 Yb3 O22 148.1(2) 2_557 . ? O4 Yb3 O22 75.98(19) 2_657 . ? O18 Yb3 O15 77.3(2) . 2_656 ? O20 Yb3 O15 86.7(2) 2_557 2_656 ? O4 Yb3 O15 132.7(2) 2_657 2_656 ? O22 Yb3 O15 86.17(19) . 2_656 ? O18 Yb3 O23 76.1(2) . 2_657 ? O20 Yb3 O23 122.4(2) 2_557 2_657 ? O4 Yb3 O23 82.4(2) 2_657 2_657 ? O22 Yb3 O23 81.82(19) . 2_657 ? O15 Yb3 O23 138.33(18) 2_656 2_657 ? O18 Yb3 O16 128.24(19) . 2_656 ? O20 Yb3 O16 75.7(2) 2_557 2_656 ? O4 Yb3 O16 78.92(19) 2_657 2_656 ? O22 Yb3 O16 74.92(19) . 2_656 ? O15 Yb3 O16 54.09(18) 2_656 2_656 ? O23 Yb3 O16 153.03(18) 2_657 2_656 ? O18 Yb3 C32 102.1(2) . 2_656 ? O20 Yb3 C32 76.6(2) 2_557 2_656 ? O4 Yb3 C32 105.8(2) 2_657 2_656 ? O22 Yb3 C32 82.9(2) . 2_656 ? O15 Yb3 C32 27.6(2) 2_656 2_656 ? O23 Yb3 C32 160.25(19) 2_657 2_656 ? O16 Yb3 C32 26.9(2) 2_656 2_656 ? O18 Yb3 O24 76.81(19) . 2_657 ? O20 Yb3 O24 74.23(18) 2_557 2_657 ? O4 Yb3 O24 71.59(18) 2_657 2_657 ? O22 Yb3 O24 122.86(17) . 2_657 ? O15 Yb3 O24 148.68(18) 2_656 2_657 ? O23 Yb3 O24 48.63(16) 2_657 2_657 ? O16 Yb3 O24 138.71(17) 2_656 2_657 ? C32 Yb3 O24 150.79(18) 2_656 2_657 ? O18 Yb3 O21 74.41(18) . . ? O20 Yb3 O21 152.2(2) 2_557 . ? O4 Yb3 O21 120.49(17) 2_657 . ? O22 Yb3 O21 48.30(17) . . ? O15 Yb3 O21 70.26(17) 2_656 . ? O23 Yb3 O21 72.04(17) 2_657 . ? O16 Yb3 O21 101.17(18) 2_656 . ? C32 Yb3 O21 88.45(19) 2_656 . ? O24 Yb3 O21 118.45(17) 2_657 . ? O18 Yb3 C41 99.3(2) . . ? O20 Yb3 C41 159.0(2) 2_557 . ? O4 Yb3 C41 98.78(19) 2_657 . ? O22 Yb3 C41 23.65(19) . . ? O15 Yb3 C41 74.82(18) 2_656 . ? O23 Yb3 C41 78.54(19) 2_657 . ? O16 Yb3 C41 85.26(19) 2_656 . ? C32 Yb3 C41 82.4(2) 2_656 . ? O24 Yb3 C41 126.75(17) 2_657 . ? O21 Yb3 C41 24.95(18) . . ? O18 Yb3 C48 73.5(2) . 2_657 ? O20 Yb3 C48 98.9(2) 2_557 2_657 ? O4 Yb3 C48 77.5(2) 2_657 2_657 ? O22 Yb3 C48 102.9(2) . 2_657 ? O15 Yb3 C48 149.70(19) 2_656 2_657 ? O23 Yb3 C48 23.64(19) 2_657 2_657 ? O16 Yb3 C48 156.11(18) 2_656 2_657 ? C32 Yb3 C48 174.0(2) 2_656 2_657 ? O24 Yb3 C48 25.09(18) 2_657 2_657 ? O21 Yb3 C48 94.12(18) . 2_657 ? C41 Yb3 C48 102.2(2) . 2_657 ? O17 Yb4 O11 163.3(2) . 2_756 ? O17 Yb4 O21 89.3(2) . . ? O11 Yb4 O21 82.1(2) 2_756 . ? O17 Yb4 O7 88.16(19) . 2_656 ? O11 Yb4 O7 92.5(2) 2_756 2_656 ? O21 Yb4 O7 151.0(2) . 2_656 ? O17 Yb4 O2 113.1(2) . . ? O11 Yb4 O2 83.3(2) 2_756 . ? O21 Yb4 O2 129.68(19) . . ? O7 Yb4 O2 77.30(18) 2_656 . ? O17 Yb4 O25 75.8(2) . . ? O11 Yb4 O25 115.1(2) 2_756 . ? O21 Yb4 O25 74.6(2) . . ? O7 Yb4 O25 132.2(2) 2_656 . ? O2 Yb4 O25 68.9(2) . . ? O17 Yb4 O26 83.0(2) . . ? O11 Yb4 O26 81.1(2) 2_756 . ? O21 Yb4 O26 75.4(2) . . ? O7 Yb4 O26 75.58(19) 2_656 . ? O2 Yb4 O26 147.91(19) . . ? O25 Yb4 O26 143.2(2) . . ? O17 Yb4 C24 159.94(19) . 2_756 ? O11 Yb4 C24 17.4(2) 2_756 2_756 ? O21 Yb4 C24 99.0(2) . 2_756 ? O7 Yb4 C24 75.75(18) 2_656 2_756 ? O2 Yb4 C24 75.4(2) . 2_756 ? O25 Yb4 C24 124.01(19) . 2_756 ? O26 Yb4 C24 81.5(2) . 2_756 ? O17 Yb4 Yb1 116.89(14) . . ? O11 Yb4 Yb1 68.18(15) 2_756 . ? O21 Yb4 Yb1 148.82(15) . . ? O7 Yb4 Yb1 30.69(12) 2_656 . ? O2 Yb4 Yb1 57.66(13) . . ? O25 Yb4 Yb1 125.93(16) . . ? O26 Yb4 Yb1 90.45(14) . . ? C24 Yb4 Yb1 50.85(14) 2_756 . ? C1 O1 Yb1 129.7(5) . . ? C1 O2 Yb4 146.0(5) . . ? C8 O3 Yb2 141.1(5) . 2_756 ? C8 O4 Yb3 143.6(5) . 2_657 ? C9 O5 Yb2 152.8(5) . . ? C9 O5 Yb1 81.7(4) . . ? Yb2 O5 Yb1 116.2(2) . . ? C9 O6 Yb1 107.4(4) . . ? C16 O7 Yb4 141.6(5) . 2_656 ? C16 O7 Yb1 88.4(4) . 2_656 ? Yb4 O7 Yb1 122.2(2) 2_656 2_656 ? C16 O8 Yb1 97.3(4) . 2_656 ? C17 O9 Yb1 150.3(6) . . ? C17 O10 Yb2 129.9(5) . . ? C24 O11 Yb4 130.5(5) . 2_756 ? C24 O12 Yb1 145.0(5) . 2_756 ? C25 O13 Yb1 139.9(5) . . ? C25 O14 Yb2 141.4(5) . . ? C32 O15 Yb3 92.6(4) . 2_656 ? C32 O16 Yb3 91.3(5) . 2_656 ? C33 O17 Yb4 137.7(5) . . ? C33 O18 Yb3 151.7(5) . . ? C40 O19 Yb2 134.4(5) . 2_656 ? C40 O20 Yb3 156.7(6) . 2_557 ? C41 O21 Yb4 149.3(5) . . ? C41 O21 Yb3 81.0(4) . . ? Yb4 O21 Yb3 128.6(2) . . ? C41 O22 Yb3 109.1(5) . . ? C48 O23 Yb3 106.4(5) . 2_657 ? C48 O24 Yb2 146.8(5) . 2_756 ? C48 O24 Yb3 84.0(4) . 2_657 ? Yb2 O24 Yb3 119.5(2) 2_756 2_657 ? O2 C1 O1 122.9(7) . . ? O2 C1 C2 117.8(6) . . ? O1 C1 C2 119.4(7) . . ? C3 C2 C7 118.0(7) . . ? C3 C2 C1 119.2(7) . . ? C7 C2 C1 122.7(7) . . ? C4 C3 C2 121.5(8) . . ? C5 C4 C3 119.0(8) . . ? C6 C5 C4 120.8(8) . . ? C5 C6 C7 120.5(8) . . ? C6 C7 C2 120.0(7) . . ? C6 C7 C8 117.0(7) . . ? C2 C7 C8 122.9(7) . . ? O3 C8 O4 125.9(8) . . ? O3 C8 C7 116.1(6) . . ? O4 C8 C7 117.9(7) . . ? O6 C9 O5 120.7(7) . . ? O6 C9 C10 118.6(6) . . ? O5 C9 C10 120.6(7) . . ? O6 C9 Yb1 48.4(4) . . ? O5 C9 Yb1 72.6(4) . . ? C10 C9 Yb1 165.6(5) . . ? C11 C10 C15 117.7(8) . . ? C11 C10 C9 120.9(7) . . ? C15 C10 C9 121.3(7) . . ? C12 C11 C10 121.0(8) . . ? C11 C12 C13 120.2(8) . . ? C12 C13 C14 120.3(8) . . ? C15 C14 C13 119.1(7) . . ? C14 C15 C10 121.4(7) . . ? C14 C15 C16 115.1(7) . . ? C10 C15 C16 123.4(7) . . ? O8 C16 O7 119.7(7) . . ? O8 C16 C15 119.0(7) . . ? O7 C16 C15 120.5(6) . . ? O8 C16 Yb1 56.5(4) . 2_656 ? O7 C16 Yb1 64.5(4) . 2_656 ? C15 C16 Yb1 159.1(5) . 2_656 ? O9 C17 O10 123.9(7) . . ? O9 C17 C18 118.4(7) . . ? O10 C17 C18 117.4(6) . . ? O9 C17 Yb2 92.9(5) . . ? O10 C17 Yb2 32.3(3) . . ? C18 C17 Yb2 144.8(5) . . ? C19 C18 C23 119.6(7) . . ? C19 C18 C17 119.9(7) . . ? C23 C18 C17 120.4(7) . . ? C18 C19 C20 120.6(8) . . ? C21 C20 C19 120.4(8) . . ? C20 C21 C22 119.5(8) . . ? C23 C22 C21 120.3(8) . . ? C22 C23 C18 119.3(8) . . ? C22 C23 C24 116.9(7) . . ? C18 C23 C24 123.7(7) . . ? O11 C24 O12 126.0(8) . . ? O11 C24 C23 119.0(7) . . ? O12 C24 C23 114.7(7) . . ? O11 C24 Yb4 32.1(4) . 2_756 ? O12 C24 Yb4 96.5(5) . 2_756 ? C23 C24 Yb4 143.0(5) . 2_756 ? O14 C25 O13 124.7(8) . . ? O14 C25 C26 118.6(7) . . ? O13 C25 C26 116.5(7) . . ? C27 C26 C31 119.5(8) . . ? C27 C26 C25 116.1(7) . . ? C31 C26 C25 124.3(7) . . ? C28 C27 C26 119.7(8) . . ? C29 C28 C27 120.5(8) . . ? C30 C29 C28 120.1(9) . . ? C29 C30 C31 120.6(8) . . ? C30 C31 C26 119.5(7) . . ? C30 C31 C32 118.3(7) . . ? C26 C31 C32 122.2(7) . . ? O16 C32 O15 120.1(7) . . ? O16 C32 C31 120.5(7) . . ? O15 C32 C31 119.4(6) . . ? O16 C32 Yb3 61.8(4) . 2_656 ? O15 C32 Yb3 59.9(4) . 2_656 ? C31 C32 Yb3 165.2(5) . 2_656 ? O18 C33 O17 124.7(7) . . ? O18 C33 C34 118.5(6) . . ? O17 C33 C34 116.7(7) . . ? C35 C34 C39 119.4(7) . . ? C35 C34 C33 118.1(7) . . ? C39 C34 C33 122.2(7) . . ? C36 C35 C34 120.6(8) . . ? C35 C36 C37 120.1(8) . . ? C38 C37 C36 119.7(9) . . ? C37 C38 C39 120.9(8) . . ? C38 C39 C34 119.3(7) . . ? C38 C39 C40 118.2(7) . . ? C34 C39 C40 122.2(7) . . ? O20 C40 O19 125.4(7) . . ? O20 C40 C39 117.7(7) . . ? O19 C40 C39 116.8(7) . . ? O22 C41 O21 120.2(7) . . ? O22 C41 C42 116.8(7) . . ? O21 C41 C42 122.7(6) . . ? O22 C41 Yb3 47.2(3) . . ? O21 C41 Yb3 74.0(4) . . ? C42 C41 Yb3 157.0(5) . . ? C43 C42 C47 119.7(7) . . ? C43 C42 C41 115.6(7) . . ? C47 C42 C41 124.7(7) . . ? C42 C43 C44 120.4(8) . . ? C43 C44 C45 119.3(8) . . ? C46 C45 C44 120.4(8) . . ? C45 C46 C47 121.0(8) . . ? C46 C47 C42 119.2(8) . . ? C46 C47 C48 119.6(7) . . ? C42 C47 C48 121.2(6) . . ? O23 C48 O24 120.4(7) . . ? O23 C48 C47 121.2(7) . . ? O24 C48 C47 118.4(7) . . ? O23 C48 Yb3 49.9(4) . 2_657 ? O24 C48 Yb3 70.9(4) . 2_657 ? C47 C48 Yb3 169.6(5) . 2_657 ? 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 O12 Yb1 Yb2 O19 110.0(2) 2_756 . . 2_656 ? O9 Yb1 Yb2 O19 -167.3(3) . . . 2_656 ? O13 Yb1 Yb2 O19 -69.7(2) . . . 2_656 ? O1 Yb1 Yb2 O19 -158.8(2) . . . 2_656 ? O6 Yb1 Yb2 O19 28.1(2) . . . 2_656 ? O8 Yb1 Yb2 O19 -38.8(2) 2_656 . . 2_656 ? O7 Yb1 Yb2 O19 43.7(3) 2_656 . . 2_656 ? O5 Yb1 Yb2 O19 47.6(3) . . . 2_656 ? C16 Yb1 Yb2 O19 -15.3(4) 2_656 . . 2_656 ? C9 Yb1 Yb2 O19 36.0(2) . . . 2_656 ? Yb4 Yb1 Yb2 O19 93.88(17) . . . 2_656 ? O12 Yb1 Yb2 O10 -61.8(2) 2_756 . . . ? O9 Yb1 Yb2 O10 20.9(3) . . . . ? O13 Yb1 Yb2 O10 118.5(3) . . . . ? O1 Yb1 Yb2 O10 29.4(3) . . . . ? O6 Yb1 Yb2 O10 -143.7(2) . . . . ? O8 Yb1 Yb2 O10 149.4(3) 2_656 . . . ? O7 Yb1 Yb2 O10 -128.1(3) 2_656 . . . ? O5 Yb1 Yb2 O10 -124.2(3) . . . . ? C16 Yb1 Yb2 O10 172.9(4) 2_656 . . . ? C9 Yb1 Yb2 O10 -135.8(3) . . . . ? Yb4 Yb1 Yb2 O10 -77.90(19) . . . . ? O12 Yb1 Yb2 O24 -119.6(3) 2_756 . . 2_756 ? O9 Yb1 Yb2 O24 -36.9(3) . . . 2_756 ? O13 Yb1 Yb2 O24 60.7(3) . . . 2_756 ? O1 Yb1 Yb2 O24 -28.4(3) . . . 2_756 ? O6 Yb1 Yb2 O24 158.4(3) . . . 2_756 ? O8 Yb1 Yb2 O24 91.5(3) 2_656 . . 2_756 ? O7 Yb1 Yb2 O24 174.1(3) 2_656 . . 2_756 ? O5 Yb1 Yb2 O24 178.0(3) . . . 2_756 ? C16 Yb1 Yb2 O24 115.1(4) 2_656 . . 2_756 ? C9 Yb1 Yb2 O24 166.3(3) . . . 2_756 ? Yb4 Yb1 Yb2 O24 -135.8(3) . . . 2_756 ? O12 Yb1 Yb2 O5 62.4(3) 2_756 . . . ? O9 Yb1 Yb2 O5 145.1(3) . . . . ? O13 Yb1 Yb2 O5 -117.3(3) . . . . ? O1 Yb1 Yb2 O5 153.6(3) . . . . ? O6 Yb1 Yb2 O5 -19.5(3) . . . . ? O8 Yb1 Yb2 O5 -86.4(3) 2_656 . . . ? O7 Yb1 Yb2 O5 -3.9(3) 2_656 . . . ? C16 Yb1 Yb2 O5 -62.9(4) 2_656 . . . ? C9 Yb1 Yb2 O5 -11.6(3) . . . . ? Yb4 Yb1 Yb2 O5 46.3(2) . . . . ? O12 Yb1 Yb2 O14 -166.6(2) 2_756 . . . ? O9 Yb1 Yb2 O14 -83.9(3) . . . . ? O13 Yb1 Yb2 O14 13.7(2) . . . . ? O1 Yb1 Yb2 O14 -75.4(2) . . . . ? O6 Yb1 Yb2 O14 111.5(2) . . . . ? O8 Yb1 Yb2 O14 44.6(2) 2_656 . . . ? O7 Yb1 Yb2 O14 127.1(3) 2_656 . . . ? O5 Yb1 Yb2 O14 131.0(3) . . . . ? C16 Yb1 Yb2 O14 68.1(4) 2_656 . . . ? C9 Yb1 Yb2 O14 119.4(2) . . . . ? Yb4 Yb1 Yb2 O14 177.29(16) . . . . ? O12 Yb1 Yb2 O3 12.0(2) 2_756 . . 2_756 ? O9 Yb1 Yb2 O3 94.7(3) . . . 2_756 ? O13 Yb1 Yb2 O3 -167.7(2) . . . 2_756 ? O1 Yb1 Yb2 O3 103.2(3) . . . 2_756 ? O6 Yb1 Yb2 O3 -70.0(2) . . . 2_756 ? O8 Yb1 Yb2 O3 -136.9(3) 2_656 . . 2_756 ? O7 Yb1 Yb2 O3 -54.3(3) 2_656 . . 2_756 ? O5 Yb1 Yb2 O3 -50.4(3) . . . 2_756 ? C16 Yb1 Yb2 O3 -113.3(4) 2_656 . . 2_756 ? C9 Yb1 Yb2 O3 -62.1(2) . . . 2_756 ? Yb4 Yb1 Yb2 O3 -4.16(18) . . . 2_756 ? O12 Yb1 Yb2 C17 -71.8(2) 2_756 . . . ? O9 Yb1 Yb2 C17 10.9(3) . . . . ? O13 Yb1 Yb2 C17 108.5(2) . . . . ? O1 Yb1 Yb2 C17 19.4(3) . . . . ? O6 Yb1 Yb2 C17 -153.7(2) . . . . ? O8 Yb1 Yb2 C17 139.4(3) 2_656 . . . ? O7 Yb1 Yb2 C17 -138.1(3) 2_656 . . . ? O5 Yb1 Yb2 C17 -134.2(3) . . . . ? C16 Yb1 Yb2 C17 162.9(4) 2_656 . . . ? C9 Yb1 Yb2 C17 -145.8(2) . . . . ? Yb4 Yb1 Yb2 C17 -87.91(18) . . . . ? O12 Yb1 Yb4 O17 -172.1(2) 2_756 . . . ? O9 Yb1 Yb4 O17 134.8(3) . . . . ? O13 Yb1 Yb4 O17 -5.7(4) . . . . ? O1 Yb1 Yb4 O17 78.1(2) . . . . ? O6 Yb1 Yb4 O17 -90.6(2) . . . . ? O8 Yb1 Yb4 O17 -8.5(2) 2_656 . . . ? O7 Yb1 Yb4 O17 -22.4(3) 2_656 . . . ? O5 Yb1 Yb4 O17 -129.4(2) . . . . ? C16 Yb1 Yb4 O17 -8.6(3) 2_656 . . . ? C9 Yb1 Yb4 O17 -108.9(2) . . . . ? Yb2 Yb1 Yb4 O17 -152.71(17) . . . . ? O12 Yb1 Yb4 O11 -9.6(2) 2_756 . . 2_756 ? O9 Yb1 Yb4 O11 -62.7(3) . . . 2_756 ? O13 Yb1 Yb4 O11 156.8(4) . . . 2_756 ? O1 Yb1 Yb4 O11 -119.3(2) . . . 2_756 ? O6 Yb1 Yb4 O11 71.9(2) . . . 2_756 ? O8 Yb1 Yb4 O11 154.1(2) 2_656 . . 2_756 ? O7 Yb1 Yb4 O11 140.1(3) 2_656 . . 2_756 ? O5 Yb1 Yb4 O11 33.1(2) . . . 2_756 ? C16 Yb1 Yb4 O11 153.9(2) 2_656 . . 2_756 ? C9 Yb1 Yb4 O11 53.6(2) . . . 2_756 ? Yb2 Yb1 Yb4 O11 9.81(17) . . . 2_756 ? O12 Yb1 Yb4 O21 -28.0(3) 2_756 . . . ? O9 Yb1 Yb4 O21 -81.1(3) . . . . ? O13 Yb1 Yb4 O21 138.4(5) . . . . ? O1 Yb1 Yb4 O21 -137.7(3) . . . . ? O6 Yb1 Yb4 O21 53.5(3) . . . . ? O8 Yb1 Yb4 O21 135.7(3) 2_656 . . . ? O7 Yb1 Yb4 O21 121.7(4) 2_656 . . . ? O5 Yb1 Yb4 O21 14.7(3) . . . . ? C16 Yb1 Yb4 O21 135.5(3) 2_656 . . . ? C9 Yb1 Yb4 O21 35.2(3) . . . . ? Yb2 Yb1 Yb4 O21 -8.6(3) . . . . ? O12 Yb1 Yb4 O7 -149.7(3) 2_756 . . 2_656 ? O9 Yb1 Yb4 O7 157.2(3) . . . 2_656 ? O13 Yb1 Yb4 O7 16.7(4) . . . 2_656 ? O1 Yb1 Yb4 O7 100.5(3) . . . 2_656 ? O6 Yb1 Yb4 O7 -68.2(3) . . . 2_656 ? O8 Yb1 Yb4 O7 13.9(3) 2_656 . . 2_656 ? O5 Yb1 Yb4 O7 -107.0(3) . . . 2_656 ? C16 Yb1 Yb4 O7 13.8(3) 2_656 . . 2_656 ? C9 Yb1 Yb4 O7 -86.5(3) . . . 2_656 ? Yb2 Yb1 Yb4 O7 -130.3(3) . . . 2_656 ? O12 Yb1 Yb4 O2 86.4(2) 2_756 . . . ? O9 Yb1 Yb4 O2 33.3(3) . . . . ? O13 Yb1 Yb4 O2 -107.2(4) . . . . ? O1 Yb1 Yb4 O2 -23.3(2) . . . . ? O6 Yb1 Yb4 O2 167.9(2) . . . . ? O8 Yb1 Yb4 O2 -109.9(2) 2_656 . . . ? O7 Yb1 Yb4 O2 -123.9(3) 2_656 . . . ? O5 Yb1 Yb4 O2 129.1(2) . . . . ? C16 Yb1 Yb4 O2 -110.1(3) 2_656 . . . ? C9 Yb1 Yb4 O2 149.6(2) . . . . ? Yb2 Yb1 Yb4 O2 105.82(17) . . . . ? O12 Yb1 Yb4 O25 96.4(2) 2_756 . . . ? O9 Yb1 Yb4 O25 43.2(3) . . . . ? O13 Yb1 Yb4 O25 -97.3(4) . . . . ? O1 Yb1 Yb4 O25 -13.4(2) . . . . ? O6 Yb1 Yb4 O25 177.9(2) . . . . ? O8 Yb1 Yb4 O25 -100.0(2) 2_656 . . . ? O7 Yb1 Yb4 O25 -113.9(3) 2_656 . . . ? O5 Yb1 Yb4 O25 139.0(2) . . . . ? C16 Yb1 Yb4 O25 -100.1(3) 2_656 . . . ? C9 Yb1 Yb4 O25 159.5(2) . . . . ? Yb2 Yb1 Yb4 O25 115.75(18) . . . . ? O12 Yb1 Yb4 O26 -89.8(2) 2_756 . . . ? O9 Yb1 Yb4 O26 -142.9(2) . . . . ? O13 Yb1 Yb4 O26 76.6(4) . . . . ? O1 Yb1 Yb4 O26 160.5(2) . . . . ? O6 Yb1 Yb4 O26 -8.3(2) . . . . ? O8 Yb1 Yb4 O26 73.9(2) 2_656 . . . ? O7 Yb1 Yb4 O26 59.9(3) 2_656 . . . ? O5 Yb1 Yb4 O26 -47.11(19) . . . . ? C16 Yb1 Yb4 O26 73.7(2) 2_656 . . . ? C9 Yb1 Yb4 O26 -26.6(2) . . . . ? Yb2 Yb1 Yb4 O26 -70.39(15) . . . . ? O12 Yb1 Yb4 C24 -11.1(2) 2_756 . . 2_756 ? O9 Yb1 Yb4 C24 -64.3(3) . . . 2_756 ? O13 Yb1 Yb4 C24 155.2(4) . . . 2_756 ? O1 Yb1 Yb4 C24 -120.9(2) . . . 2_756 ? O6 Yb1 Yb4 C24 70.4(2) . . . 2_756 ? O8 Yb1 Yb4 C24 152.5(2) 2_656 . . 2_756 ? O7 Yb1 Yb4 C24 138.6(3) 2_656 . . 2_756 ? O5 Yb1 Yb4 C24 31.5(2) . . . 2_756 ? C16 Yb1 Yb4 C24 152.4(3) 2_656 . . 2_756 ? C9 Yb1 Yb4 C24 52.0(2) . . . 2_756 ? Yb2 Yb1 Yb4 C24 8.25(17) . . . 2_756 ? O12 Yb1 O1 C1 -14.6(6) 2_756 . . . ? O9 Yb1 O1 C1 -97.3(6) . . . . ? O13 Yb1 O1 C1 -170.9(6) . . . . ? O6 Yb1 O1 C1 61.6(8) . . . . ? O8 Yb1 O1 C1 118.7(6) 2_656 . . . ? O7 Yb1 O1 C1 65.3(6) 2_656 . . . ? O5 Yb1 O1 C1 -75.3(7) . . . . ? C16 Yb1 O1 C1 93.6(6) 2_656 . . . ? C9 Yb1 O1 C1 3.1(13) . . . . ? Yb4 Yb1 O1 C1 37.4(6) . . . . ? Yb2 Yb1 O1 C1 -104.3(6) . . . . ? O17 Yb4 O2 C1 -69.9(9) . . . . ? O11 Yb4 O2 C1 106.7(9) 2_756 . . . ? O21 Yb4 O2 C1 -179.5(8) . . . . ? O7 Yb4 O2 C1 12.6(9) 2_656 . . . ? O25 Yb4 O2 C1 -133.1(9) . . . . ? O26 Yb4 O2 C1 45.5(11) . . . . ? C24 Yb4 O2 C1 90.9(9) 2_756 . . . ? Yb1 Yb4 O2 C1 38.3(8) . . . . ? O19 Yb2 O5 C9 -9.3(12) 2_656 . . . ? O10 Yb2 O5 C9 176.2(12) . . . . ? O24 Yb2 O5 C9 -25(5) 2_756 . . . ? O14 Yb2 O5 C9 85.0(12) . . . . ? O3 Yb2 O5 C9 -95.2(12) 2_756 . . . ? C17 Yb2 O5 C9 161.4(12) . . . . ? Yb1 Yb2 O5 C9 127.1(13) . . . . ? O19 Yb2 O5 Yb1 -136.4(3) 2_656 . . . ? O10 Yb2 O5 Yb1 49.1(2) . . . . ? O24 Yb2 O5 Yb1 -152(5) 2_756 . . . ? O14 Yb2 O5 Yb1 -42.1(2) . . . . ? O3 Yb2 O5 Yb1 137.7(2) 2_756 . . . ? C17 Yb2 O5 Yb1 34.3(2) . . . . ? O12 Yb1 O5 C9 87.5(4) 2_756 . . . ? O9 Yb1 O5 C9 173.5(4) . . . . ? O13 Yb1 O5 C9 -105.4(4) . . . . ? O1 Yb1 O5 C9 151.4(4) . . . . ? O6 Yb1 O5 C9 -3.5(4) . . . . ? O8 Yb1 O5 C9 -45.1(4) 2_656 . . . ? O7 Yb1 O5 C9 19.5(5) 2_656 . . . ? C16 Yb1 O5 C9 -14.4(5) 2_656 . . . ? Yb4 Yb1 O5 C9 51.8(4) . . . . ? Yb2 Yb1 O5 C9 -158.3(5) . . . . ? O12 Yb1 O5 Yb2 -114.2(3) 2_756 . . . ? O9 Yb1 O5 Yb2 -28.2(2) . . . . ? O13 Yb1 O5 Yb2 53.0(2) . . . . ? O1 Yb1 O5 Yb2 -50.3(5) . . . . ? O6 Yb1 O5 Yb2 154.9(4) . . . . ? O8 Yb1 O5 Yb2 113.3(2) 2_656 . . . ? O7 Yb1 O5 Yb2 177.85(17) 2_656 . . . ? C16 Yb1 O5 Yb2 143.9(2) 2_656 . . . ? C9 Yb1 O5 Yb2 158.3(5) . . . . ? Yb4 Yb1 O5 Yb2 -149.88(15) . . . . ? O12 Yb1 O6 C9 -75.1(5) 2_756 . . . ? O9 Yb1 O6 C9 -0.1(6) . . . . ? O13 Yb1 O6 C9 74.9(5) . . . . ? O1 Yb1 O6 C9 -153.8(5) . . . . ? O8 Yb1 O6 C9 149.0(5) 2_656 . . . ? O7 Yb1 O6 C9 -157.4(5) 2_656 . . . ? O5 Yb1 O6 C9 3.7(4) . . . . ? C16 Yb1 O6 C9 175.4(5) 2_656 . . . ? Yb4 Yb1 O6 C9 -131.8(5) . . . . ? Yb2 Yb1 O6 C9 15.5(4) . . . . ? O12 Yb1 O9 C17 43.4(11) 2_756 . . . ? O13 Yb1 O9 C17 -111.3(11) . . . . ? O1 Yb1 O9 C17 136.7(11) . . . . ? O6 Yb1 O9 C17 -30.9(12) . . . . ? O8 Yb1 O9 C17 -159.3(10) 2_656 . . . ? O7 Yb1 O9 C17 104.8(11) 2_656 . . . ? O5 Yb1 O9 C17 -33.8(11) . . . . ? C16 Yb1 O9 C17 158.0(10) 2_656 . . . ? C9 Yb1 O9 C17 -30.9(11) . . . . ? Yb4 Yb1 O9 C17 85.8(11) . . . . ? Yb2 Yb1 O9 C17 -49.7(10) . . . . ? O19 Yb2 O10 C17 -99.1(15) 2_656 . . . ? O24 Yb2 O10 C17 125.7(7) 2_756 . . . ? O5 Yb2 O10 C17 -55.1(7) . . . . ? O14 Yb2 O10 C17 33.2(7) . . . . ? O3 Yb2 O10 C17 -149.2(7) 2_756 . . . ? Yb1 Yb2 O10 C17 -26.0(6) . . . . ? O12 Yb1 O13 C25 -37.8(11) 2_756 . . . ? O9 Yb1 O13 C25 17.5(9) . . . . ? O1 Yb1 O13 C25 91.3(9) . . . . ? O6 Yb1 O13 C25 -110.8(9) . . . . ? O8 Yb1 O13 C25 167.4(9) 2_656 . . . ? O7 Yb1 O13 C25 174.0(8) 2_656 . . . ? O5 Yb1 O13 C25 -62.5(9) . . . . ? C16 Yb1 O13 C25 167.0(9) 2_656 . . . ? C9 Yb1 O13 C25 -87.4(9) . . . . ? Yb4 Yb1 O13 C25 164.6(7) . . . . ? Yb2 Yb1 O13 C25 -37.2(8) . . . . ? O19 Yb2 O14 C25 104.0(8) 2_656 . . . ? O10 Yb2 O14 C25 -70.0(8) . . . . ? O24 Yb2 O14 C25 -163.9(8) 2_756 . . . ? O5 Yb2 O14 C25 18.4(8) . . . . ? O3 Yb2 O14 C25 -157(4) 2_756 . . . ? C17 Yb2 O14 C25 -60.1(8) . . . . ? Yb1 Yb2 O14 C25 -8.0(7) . . . . ? O11 Yb4 O17 C33 69.0(11) 2_756 . . . ? O21 Yb4 O17 C33 10.5(8) . . . . ? O7 Yb4 O17 C33 161.6(8) 2_656 . . . ? O2 Yb4 O17 C33 -123.0(7) . . . . ? O25 Yb4 O17 C33 -63.8(7) . . . . ? O26 Yb4 O17 C33 85.9(8) . . . . ? C24 Yb4 O17 C33 125.3(8) 2_756 . . . ? Yb1 Yb4 O17 C33 172.8(7) . . . . ? O20 Yb3 O18 C33 166.0(11) 2_557 . . . ? O4 Yb3 O18 C33 89.8(11) 2_657 . . . ? O22 Yb3 O18 C33 -29.5(12) . . . . ? O15 Yb3 O18 C33 -106.5(11) 2_656 . . . ? O23 Yb3 O18 C33 41.2(11) 2_657 . . . ? O16 Yb3 O18 C33 -125.8(10) 2_656 . . . ? C32 Yb3 O18 C33 -118.7(11) 2_656 . . . ? O24 Yb3 O18 C33 91.3(11) 2_657 . . . ? O21 Yb3 O18 C33 -33.7(11) . . . . ? C41 Yb3 O18 C33 -34.5(11) . . . . ? C48 Yb3 O18 C33 65.5(11) 2_657 . . . ? O17 Yb4 O21 C41 172.8(10) . . . . ? O11 Yb4 O21 C41 7.1(10) 2_756 . . . ? O7 Yb4 O21 C41 87.9(10) 2_656 . . . ? O2 Yb4 O21 C41 -67.4(11) . . . . ? O25 Yb4 O21 C41 -111.8(10) . . . . ? O26 Yb4 O21 C41 89.8(10) . . . . ? C24 Yb4 O21 C41 11.1(10) 2_756 . . . ? Yb1 Yb4 O21 C41 24.3(12) . . . . ? O17 Yb4 O21 Yb3 10.1(3) . . . . ? O11 Yb4 O21 Yb3 -155.6(3) 2_756 . . . ? O7 Yb4 O21 Yb3 -74.8(5) 2_656 . . . ? O2 Yb4 O21 Yb3 130.0(3) . . . . ? O25 Yb4 O21 Yb3 85.5(3) . . . . ? O26 Yb4 O21 Yb3 -72.8(3) . . . . ? C24 Yb4 O21 Yb3 -151.6(3) 2_756 . . . ? Yb1 Yb4 O21 Yb3 -138.41(19) . . . . ? O18 Yb3 O21 C41 -178.2(5) . . . . ? O20 Yb3 O21 C41 -131.9(5) 2_557 . . . ? O4 Yb3 O21 C41 32.3(5) 2_657 . . . ? O22 Yb3 O21 C41 6.6(4) . . . . ? O15 Yb3 O21 C41 -96.4(4) 2_656 . . . ? O23 Yb3 O21 C41 101.6(4) 2_657 . . . ? O16 Yb3 O21 C41 -51.4(4) 2_656 . . . ? C32 Yb3 O21 C41 -75.2(4) 2_656 . . . ? O24 Yb3 O21 C41 116.7(4) 2_657 . . . ? C48 Yb3 O21 C41 110.2(4) 2_657 . . . ? O18 Yb3 O21 Yb4 -7.1(3) . . . . ? O20 Yb3 O21 Yb4 39.3(6) 2_557 . . . ? O4 Yb3 O21 Yb4 -156.6(3) 2_657 . . . ? O22 Yb3 O21 Yb4 177.7(4) . . . . ? O15 Yb3 O21 Yb4 74.7(3) 2_656 . . . ? O23 Yb3 O21 Yb4 -87.2(3) 2_657 . . . ? O16 Yb3 O21 Yb4 119.8(3) 2_656 . . . ? C32 Yb3 O21 Yb4 95.9(3) 2_656 . . . ? O24 Yb3 O21 Yb4 -72.2(3) 2_657 . . . ? C41 Yb3 O21 Yb4 171.2(6) . . . . ? C48 Yb3 O21 Yb4 -78.6(3) 2_657 . . . ? O18 Yb3 O22 C41 -12.4(6) . . . . ? O20 Yb3 O22 C41 137.3(5) 2_557 . . . ? O4 Yb3 O22 C41 -164.2(5) 2_657 . . . ? O15 Yb3 O22 C41 59.9(5) 2_656 . . . ? O23 Yb3 O22 C41 -80.1(5) 2_657 . . . ? O16 Yb3 O22 C41 113.7(5) 2_656 . . . ? C32 Yb3 O22 C41 87.4(5) 2_656 . . . ? O24 Yb3 O22 C41 -107.5(5) 2_657 . . . ? O21 Yb3 O22 C41 -6.9(4) . . . . ? C48 Yb3 O22 C41 -90.8(5) 2_657 . . . ? Yb4 O2 C1 O1 -25.2(14) . . . . ? Yb4 O2 C1 C2 155.0(6) . . . . ? Yb1 O1 C1 O2 -35.3(10) . . . . ? Yb1 O1 C1 C2 144.5(5) . . . . ? O2 C1 C2 C3 -150.4(7) . . . . ? O1 C1 C2 C3 29.8(10) . . . . ? O2 C1 C2 C7 24.5(11) . . . . ? O1 C1 C2 C7 -155.3(7) . . . . ? C7 C2 C3 C4 -4.1(12) . . . . ? C1 C2 C3 C4 171.0(8) . . . . ? C2 C3 C4 C5 4.2(14) . . . . ? C3 C4 C5 C6 -2.0(15) . . . . ? C4 C5 C6 C7 0.0(15) . . . . ? C5 C6 C7 C2 0.0(13) . . . . ? C5 C6 C7 C8 176.7(8) . . . . ? C3 C2 C7 C6 2.0(11) . . . . ? C1 C2 C7 C6 -172.9(7) . . . . ? C3 C2 C7 C8 -174.5(7) . . . . ? C1 C2 C7 C8 10.5(11) . . . . ? Yb2 O3 C8 O4 -9.5(13) 2_756 . . . ? Yb2 O3 C8 C7 166.9(6) 2_756 . . . ? Yb3 O4 C8 O3 42.1(13) 2_657 . . . ? Yb3 O4 C8 C7 -134.2(7) 2_657 . . . ? C6 C7 C8 O3 -99.4(8) . . . . ? C2 C7 C8 O3 77.2(9) . . . . ? C6 C7 C8 O4 77.3(9) . . . . ? C2 C7 C8 O4 -106.1(8) . . . . ? Yb1 O6 C9 O5 -7.2(8) . . . . ? Yb1 O6 C9 C10 172.3(5) . . . . ? Yb2 O5 C9 O6 -128.1(10) . . . . ? Yb1 O5 C9 O6 5.6(6) . . . . ? Yb2 O5 C9 C10 52.5(15) . . . . ? Yb1 O5 C9 C10 -173.9(6) . . . . ? Yb2 O5 C9 Yb1 -133.7(11) . . . . ? O12 Yb1 C9 O6 100.3(5) 2_756 . . . ? O9 Yb1 C9 O6 179.9(5) . . . . ? O13 Yb1 C9 O6 -103.6(5) . . . . ? O1 Yb1 C9 O6 82.1(10) . . . . ? O8 Yb1 C9 O6 -31.5(5) 2_656 . . . ? O7 Yb1 C9 O6 22.6(5) 2_656 . . . ? O5 Yb1 C9 O6 -173.6(7) . . . . ? C16 Yb1 C9 O6 -4.7(5) 2_656 . . . ? Yb4 Yb1 C9 O6 50.2(5) . . . . ? Yb2 Yb1 C9 O6 -161.0(5) . . . . ? O12 Yb1 C9 O5 -86.2(4) 2_756 . . . ? O9 Yb1 C9 O5 -6.6(4) . . . . ? O13 Yb1 C9 O5 70.0(4) . . . . ? O1 Yb1 C9 O5 -104.3(9) . . . . ? O6 Yb1 C9 O5 173.6(7) . . . . ? O8 Yb1 C9 O5 142.0(4) 2_656 . . . ? O7 Yb1 C9 O5 -163.9(4) 2_656 . . . ? C16 Yb1 C9 O5 168.8(4) 2_656 . . . ? Yb4 Yb1 C9 O5 -136.3(4) . . . . ? Yb2 Yb1 C9 O5 12.5(3) . . . . ? O12 Yb1 C9 C10 72(2) 2_756 . . . ? O9 Yb1 C9 C10 152(2) . . . . ? O13 Yb1 C9 C10 -132(2) . . . . ? O1 Yb1 C9 C10 54(2) . . . . ? O6 Yb1 C9 C10 -28.2(18) . . . . ? O8 Yb1 C9 C10 -60(2) 2_656 . . . ? O7 Yb1 C9 C10 -6(2) 2_656 . . . ? O5 Yb1 C9 C10 158(2) . . . . ? C16 Yb1 C9 C10 -33(2) 2_656 . . . ? Yb4 Yb1 C9 C10 22(2) . . . . ? Yb2 Yb1 C9 C10 171(2) . . . . ? O6 C9 C10 C11 -169.5(7) . . . . ? O5 C9 C10 C11 10.0(11) . . . . ? Yb1 C9 C10 C11 -145.7(17) . . . . ? O6 C9 C10 C15 6.4(10) . . . . ? O5 C9 C10 C15 -174.1(7) . . . . ? Yb1 C9 C10 C15 30(2) . . . . ? C15 C10 C11 C12 4.3(11) . . . . ? C9 C10 C11 C12 -179.7(7) . . . . ? C10 C11 C12 C13 0.2(13) . . . . ? C11 C12 C13 C14 -4.2(14) . . . . ? C12 C13 C14 C15 3.6(13) . . . . ? C13 C14 C15 C10 1.0(12) . . . . ? C13 C14 C15 C16 177.8(7) . . . . ? C11 C10 C15 C14 -4.9(11) . . . . ? C9 C10 C15 C14 179.1(7) . . . . ? C11 C10 C15 C16 178.7(7) . . . . ? C9 C10 C15 C16 2.7(11) . . . . ? Yb1 O8 C16 O7 14.1(7) 2_656 . . . ? Yb1 O8 C16 C15 -156.0(6) 2_656 . . . ? Yb4 O7 C16 O8 -158.3(5) 2_656 . . . ? Yb1 O7 C16 O8 -13.0(7) 2_656 . . . ? Yb4 O7 C16 C15 11.6(12) 2_656 . . . ? Yb1 O7 C16 C15 156.9(6) 2_656 . . . ? Yb4 O7 C16 Yb1 -145.3(7) 2_656 . . 2_656 ? C14 C15 C16 O8 75.7(9) . . . . ? C10 C15 C16 O8 -107.7(8) . . . . ? C14 C15 C16 O7 -94.3(9) . . . . ? C10 C15 C16 O7 82.3(9) . . . . ? C14 C15 C16 Yb1 3.9(17) . . . 2_656 ? C10 C15 C16 Yb1 -179.4(10) . . . 2_656 ? Yb1 O9 C17 O10 46.1(15) . . . . ? Yb1 O9 C17 C18 -140.7(9) . . . . ? Yb1 O9 C17 Yb2 56.0(11) . . . . ? Yb2 O10 C17 O9 18.6(12) . . . . ? Yb2 O10 C17 C18 -154.6(5) . . . . ? O19 Yb2 C17 O9 -10.6(10) 2_656 . . . ? O10 Yb2 C17 O9 -164.6(10) . . . . ? O24 Yb2 C17 O9 138.8(5) 2_756 . . . ? O5 Yb2 C17 O9 -41.4(5) . . . . ? O14 Yb2 C17 O9 49.7(5) . . . . ? O3 Yb2 C17 O9 -132.8(5) 2_756 . . . ? Yb1 Yb2 C17 O9 -16.0(4) . . . . ? O19 Yb2 C17 O10 154.0(7) 2_656 . . . ? O24 Yb2 C17 O10 -56.6(7) 2_756 . . . ? O5 Yb2 C17 O10 123.1(7) . . . . ? O14 Yb2 C17 O10 -145.7(7) . . . . ? O3 Yb2 C17 O10 31.8(7) 2_756 . . . ? Yb1 Yb2 C17 O10 148.6(7) . . . . ? O19 Yb2 C17 C18 -164.7(8) 2_656 . . . ? O10 Yb2 C17 C18 41.4(9) . . . . ? O24 Yb2 C17 C18 -15.2(9) 2_756 . . . ? O5 Yb2 C17 C18 164.5(9) . . . . ? O14 Yb2 C17 C18 -104.3(9) . . . . ? O3 Yb2 C17 C18 73.2(9) 2_756 . . . ? Yb1 Yb2 C17 C18 -170.0(10) . . . . ? O9 C17 C18 C19 -12.0(11) . . . . ? O10 C17 C18 C19 161.7(8) . . . . ? Yb2 C17 C18 C19 138.2(8) . . . . ? O9 C17 C18 C23 171.8(7) . . . . ? O10 C17 C18 C23 -14.5(11) . . . . ? Yb2 C17 C18 C23 -38.0(12) . . . . ? C23 C18 C19 C20 2.8(13) . . . . ? C17 C18 C19 C20 -173.5(8) . . . . ? C18 C19 C20 C21 1.3(15) . . . . ? C19 C20 C21 C22 -2.4(15) . . . . ? C20 C21 C22 C23 -0.6(14) . . . . ? C21 C22 C23 C18 4.5(13) . . . . ? C21 C22 C23 C24 -172.1(8) . . . . ? C19 C18 C23 C22 -5.6(12) . . . . ? C17 C18 C23 C22 170.6(7) . . . . ? C19 C18 C23 C24 170.7(8) . . . . ? C17 C18 C23 C24 -13.1(11) . . . . ? Yb4 O11 C24 O12 -26.8(11) 2_756 . . . ? Yb4 O11 C24 C23 146.6(5) 2_756 . . . ? Yb1 O12 C24 O11 61.7(13) 2_756 . . . ? Yb1 O12 C24 C23 -111.9(8) 2_756 . . . ? Yb1 O12 C24 Yb4 47.8(9) 2_756 . . 2_756 ? C22 C23 C24 O11 -70.8(10) . . . . ? C18 C23 C24 O11 112.7(8) . . . . ? C22 C23 C24 O12 103.3(8) . . . . ? C18 C23 C24 O12 -73.2(9) . . . . ? C22 C23 C24 Yb4 -41.7(12) . . . 2_756 ? C18 C23 C24 Yb4 141.9(7) . . . 2_756 ? Yb2 O14 C25 O13 -10.2(13) . . . . ? Yb2 O14 C25 C26 164.5(5) . . . . ? Yb1 O13 C25 O14 48.2(12) . . . . ? Yb1 O13 C25 C26 -126.5(7) . . . . ? O14 C25 C26 C27 -99.6(8) . . . . ? O13 C25 C26 C27 75.5(9) . . . . ? O14 C25 C26 C31 82.5(9) . . . . ? O13 C25 C26 C31 -102.4(9) . . . . ? C31 C26 C27 C28 -2.3(12) . . . . ? C25 C26 C27 C28 179.8(7) . . . . ? C26 C27 C28 C29 2.2(13) . . . . ? C27 C28 C29 C30 -1.7(14) . . . . ? C28 C29 C30 C31 1.4(14) . . . . ? C29 C30 C31 C26 -1.5(12) . . . . ? C29 C30 C31 C32 179.5(8) . . . . ? C27 C26 C31 C30 1.9(11) . . . . ? C25 C26 C31 C30 179.7(7) . . . . ? C27 C26 C31 C32 -179.0(7) . . . . ? C25 C26 C31 C32 -1.3(11) . . . . ? Yb3 O16 C32 O15 -14.0(7) 2_656 . . . ? Yb3 O16 C32 C31 163.2(6) 2_656 . . . ? Yb3 O15 C32 O16 14.2(7) 2_656 . . . ? Yb3 O15 C32 C31 -163.0(6) 2_656 . . . ? C30 C31 C32 O16 23.1(11) . . . . ? C26 C31 C32 O16 -155.9(7) . . . . ? C30 C31 C32 O15 -159.7(7) . . . . ? C26 C31 C32 O15 21.3(11) . . . . ? C30 C31 C32 Yb3 118(2) . . . 2_656 ? C26 C31 C32 Yb3 -61(2) . . . 2_656 ? Yb3 O18 C33 O17 61.3(14) . . . . ? Yb3 O18 C33 C34 -115.4(10) . . . . ? Yb4 O17 C33 O18 -39.1(12) . . . . ? Yb4 O17 C33 C34 137.7(6) . . . . ? O18 C33 C34 C35 124.4(8) . . . . ? O17 C33 C34 C35 -52.6(10) . . . . ? O18 C33 C34 C39 -49.2(10) . . . . ? O17 C33 C34 C39 133.8(7) . . . . ? C39 C34 C35 C36 -0.2(12) . . . . ? C33 C34 C35 C36 -174.0(8) . . . . ? C34 C35 C36 C37 -0.6(14) . . . . ? C35 C36 C37 C38 0.4(15) . . . . ? C36 C37 C38 C39 0.7(15) . . . . ? C37 C38 C39 C34 -1.5(13) . . . . ? C37 C38 C39 C40 -176.1(8) . . . . ? C35 C34 C39 C38 1.3(11) . . . . ? C33 C34 C39 C38 174.8(7) . . . . ? C35 C34 C39 C40 175.6(7) . . . . ? C33 C34 C39 C40 -10.8(11) . . . . ? Yb3 O20 C40 O19 -36(2) 2_557 . . . ? Yb3 O20 C40 C39 140.2(11) 2_557 . . . ? Yb2 O19 C40 O20 20.2(13) 2_656 . . . ? Yb2 O19 C40 C39 -155.5(6) 2_656 . . . ? C38 C39 C40 O20 -31.2(11) . . . . ? C34 C39 C40 O20 154.3(7) . . . . ? C38 C39 C40 O19 144.9(8) . . . . ? C34 C39 C40 O19 -29.6(11) . . . . ? Yb3 O22 C41 O21 13.7(8) . . . . ? Yb3 O22 C41 C42 -159.6(5) . . . . ? Yb4 O21 C41 O22 -176.8(7) . . . . ? Yb3 O21 C41 O22 -10.4(6) . . . . ? Yb4 O21 C41 C42 -3.9(14) . . . . ? Yb3 O21 C41 C42 162.5(7) . . . . ? Yb4 O21 C41 Yb3 -166.4(10) . . . . ? O18 Yb3 C41 O22 169.5(5) . . . . ? O20 Yb3 C41 O22 -87.5(8) 2_557 . . . ? O4 Yb3 C41 O22 15.5(5) 2_657 . . . ? O15 Yb3 C41 O22 -116.6(5) 2_656 . . . ? O23 Yb3 C41 O22 95.8(5) 2_657 . . . ? O16 Yb3 C41 O22 -62.5(5) 2_656 . . . ? C32 Yb3 C41 O22 -89.5(5) 2_656 . . . ? O24 Yb3 C41 O22 89.0(5) 2_657 . . . ? O21 Yb3 C41 O22 167.7(7) . . . . ? C48 Yb3 C41 O22 94.5(5) 2_657 . . . ? O18 Yb3 C41 O21 1.7(4) . . . . ? O20 Yb3 C41 O21 104.8(7) 2_557 . . . ? O4 Yb3 C41 O21 -152.3(4) 2_657 . . . ? O22 Yb3 C41 O21 -167.7(7) . . . . ? O15 Yb3 C41 O21 75.7(4) 2_656 . . . ? O23 Yb3 C41 O21 -71.9(4) 2_657 . . . ? O16 Yb3 C41 O21 129.7(4) 2_656 . . . ? C32 Yb3 C41 O21 102.8(4) 2_656 . . . ? O24 Yb3 C41 O21 -78.7(4) 2_657 . . . ? C48 Yb3 C41 O21 -73.2(4) 2_657 . . . ? O18 Yb3 C41 C42 -137.9(12) . . . . ? O20 Yb3 C41 C42 -34.9(15) 2_557 . . . ? O4 Yb3 C41 C42 68.1(12) 2_657 . . . ? O22 Yb3 C41 C42 52.6(12) . . . . ? O15 Yb3 C41 C42 -64.0(12) 2_656 . . . ? O23 Yb3 C41 C42 148.4(12) 2_657 . . . ? O16 Yb3 C41 C42 -9.9(12) 2_656 . . . ? C32 Yb3 C41 C42 -36.9(12) 2_656 . . . ? O24 Yb3 C41 C42 141.6(11) 2_657 . . . ? O21 Yb3 C41 C42 -139.7(14) . . . . ? C48 Yb3 C41 C42 147.1(12) 2_657 . . . ? O22 C41 C42 C43 71.7(9) . . . . ? O21 C41 C42 C43 -101.4(9) . . . . ? Yb3 C41 C42 C43 31.0(16) . . . . ? O22 C41 C42 C47 -108.4(8) . . . . ? O21 C41 C42 C47 78.5(10) . . . . ? Yb3 C41 C42 C47 -149.2(9) . . . . ? C47 C42 C43 C44 -0.9(13) . . . . ? C41 C42 C43 C44 179.0(8) . . . . ? C42 C43 C44 C45 2.2(14) . . . . ? C43 C44 C45 C46 -1.0(14) . . . . ? C44 C45 C46 C47 -1.7(14) . . . . ? C45 C46 C47 C42 3.1(12) . . . . ? C45 C46 C47 C48 -177.1(8) . . . . ? C43 C42 C47 C46 -1.8(11) . . . . ? C41 C42 C47 C46 178.4(7) . . . . ? C43 C42 C47 C48 178.4(7) . . . . ? C41 C42 C47 C48 -1.4(11) . . . . ? Yb3 O23 C48 O24 -7.9(8) 2_657 . . . ? Yb3 O23 C48 C47 173.4(5) 2_657 . . . ? Yb2 O24 C48 O23 -131.8(8) 2_756 . . . ? Yb3 O24 C48 O23 6.4(7) 2_657 . . . ? Yb2 O24 C48 C47 46.9(13) 2_756 . . . ? Yb3 O24 C48 C47 -174.8(6) 2_657 . . . ? Yb2 O24 C48 Yb3 -138.3(9) 2_756 . . 2_657 ? C46 C47 C48 O23 -161.2(7) . . . . ? C42 C47 C48 O23 18.6(11) . . . . ? C46 C47 C48 O24 20.1(11) . . . . ? C42 C47 C48 O24 -160.1(7) . . . . ? C46 C47 C48 Yb3 -132(3) . . . 2_657 ? C42 C47 C48 Yb3 48(3) . . . 2_657 ? _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 2.920 _refine_diff_density_min -2.455 _refine_diff_density_rms 0.257 data_complex1 _database_code_CSD 184845 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H14 La2 O13' _chemical_formula_weight 788.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'La' 'La' -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.638(3) _cell_length_b 10.625(3) _cell_length_c 14.376(4) _cell_angle_alpha 96.975(5) _cell_angle_beta 102.110(4) _cell_angle_gamma 104.372(4) _cell_volume 1228.6(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.130 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 752 _exptl_absorpt_coefficient_mu 3.501 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.3738 _exptl_absorpt_correction_T_max 0.7209 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5014 _diffrn_reflns_av_R_equivalents 0.0260 _diffrn_reflns_av_sigmaI/netI 0.0223 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 25.03 _reflns_number_total 4208 _reflns_number_gt 3791 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0723P)^2^+1.7642P] 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 4208 _refine_ls_number_parameters 360 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0384 _refine_ls_R_factor_gt 0.0348 _refine_ls_wR_factor_ref 0.0970 _refine_ls_wR_factor_gt 0.0921 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.006 _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 1.19609(3) 0.84651(2) 0.497145(19) 0.01967(11) Uani 1 1 d . . . La2 La 0.66931(3) 0.72478(2) 0.510569(19) 0.02075(11) Uani 1 1 d . . . O1 O 0.4982(4) 0.3240(4) 0.3707(3) 0.0351(9) Uani 1 1 d . . . O2 O 0.7595(4) 0.3212(4) 0.4087(3) 0.0349(9) Uani 1 1 d . . . O3 O 1.0693(4) 0.6228(3) 0.3851(3) 0.0317(8) Uani 1 1 d . . . O4 O 0.8454(5) 0.6181(4) 0.4367(3) 0.0347(9) Uani 1 1 d . . . O5 O 1.2160(4) 1.0878(3) 0.5803(3) 0.0259(7) Uani 1 1 d . . . O6 O 1.0210(4) 1.1422(3) 0.6409(3) 0.0285(8) Uani 1 1 d . . . O7 O 0.9807(4) 0.8449(3) 0.5880(3) 0.0259(7) Uani 1 1 d . . . O8 O 0.8572(5) 0.7604(4) 0.6926(3) 0.0435(10) Uani 1 1 d . . . O9 O 0.5481(4) 1.0575(3) 0.3693(3) 0.0279(8) Uani 1 1 d . . . O10 O 0.3126(4) 1.0416(3) 0.4124(2) 0.0246(7) Uani 1 1 d . . . O11 O 0.4149(4) 0.7906(3) 0.4208(2) 0.0222(7) Uani 1 1 d . . . O12 O 0.5092(4) 0.6679(4) 0.3255(3) 0.0337(8) Uani 1 1 d . . . O13 O 0.6624(5) 0.4998(4) 0.5658(3) 0.0401(9) Uani 1 1 d D . . C1 C 0.6379(6) 0.3455(4) 0.3557(4) 0.0244(10) Uani 1 1 d . . . C2 C 0.6682(6) 0.4057(5) 0.2706(4) 0.0268(10) Uani 1 1 d . . . C3 C 0.5592(8) 0.3540(6) 0.1806(5) 0.0489(16) Uani 1 1 d . . . H3A H 0.4647 0.2856 0.1752 0.059 Uiso 1 1 calc R . . C4 C 0.5878(10) 0.4015(8) 0.0997(5) 0.063(2) Uani 1 1 d . . . H4A H 0.5137 0.3645 0.0399 0.076 Uiso 1 1 calc R . . C5 C 0.7268(10) 0.5046(7) 0.1062(5) 0.063(2) Uani 1 1 d . . . H5A H 0.7457 0.5378 0.0514 0.076 Uiso 1 1 calc R . . C6 C 0.8372(8) 0.5575(6) 0.1958(5) 0.0450(14) Uani 1 1 d . . . H6A H 0.9322 0.6252 0.2008 0.054 Uiso 1 1 calc R . . C7 C 0.8070(6) 0.5102(5) 0.2779(4) 0.0275(10) Uani 1 1 d . . . C8 C 0.9160(6) 0.5864(4) 0.3742(4) 0.0242(10) Uani 1 1 d . . . C9 C 1.1406(5) 1.0957(4) 0.6461(3) 0.0214(9) Uani 1 1 d . . . C10 C 1.1971(6) 1.0482(5) 0.7388(4) 0.0245(10) Uani 1 1 d . . . C11 C 1.3221(7) 1.1337(6) 0.8135(4) 0.0369(12) Uani 1 1 d . . . H11A H 1.3725 1.2187 0.8059 0.044 Uiso 1 1 calc R . . C12 C 1.3697(8) 1.0914(7) 0.8980(4) 0.0515(16) Uani 1 1 d . . . H12A H 1.4553 1.1480 0.9472 0.062 Uiso 1 1 calc R . . C13 C 1.2957(9) 0.9690(8) 0.9126(5) 0.0596(19) Uani 1 1 d . . . H13A H 1.3314 0.9427 0.9708 0.071 Uiso 1 1 calc R . . C14 C 1.1666(7) 0.8833(7) 0.8402(5) 0.0483(16) Uani 1 1 d . . . H14A H 1.1136 0.8004 0.8502 0.058 Uiso 1 1 calc R . . C15 C 1.1178(6) 0.9231(5) 0.7528(4) 0.0308(11) Uani 1 1 d . . . C16 C 0.9765(6) 0.8341(5) 0.6746(4) 0.0284(11) Uani 1 1 d . . . C17 C 0.4220(6) 0.7447(4) 0.3360(4) 0.0237(10) Uani 1 1 d . . . C18 C 0.3283(6) 0.7867(5) 0.2526(4) 0.0268(10) Uani 1 1 d . . . C19 C 0.2549(7) 0.6993(6) 0.1651(4) 0.0389(13) Uani 1 1 d . . . H19A H 0.2721 0.6161 0.1570 0.047 Uiso 1 1 calc R . . C20 C 0.1564(8) 0.7358(7) 0.0903(5) 0.0490(16) Uani 1 1 d . . . H20A H 0.1066 0.6771 0.0319 0.059 Uiso 1 1 calc R . . C21 C 0.1326(8) 0.8600(7) 0.1028(4) 0.0479(16) Uani 1 1 d . . . H21A H 0.0648 0.8841 0.0529 0.057 Uiso 1 1 calc R . . C22 C 0.2080(7) 0.9489(6) 0.1883(4) 0.0369(12) Uani 1 1 d . . . H22A H 0.1927 1.0328 0.1953 0.044 Uiso 1 1 calc R . . C23 C 0.3068(6) 0.9130(5) 0.2640(4) 0.0272(10) Uani 1 1 d . . . C24 C 0.3980(6) 1.0117(4) 0.3547(3) 0.0209(9) Uani 1 1 d . . . H1 H 0.747(6) 0.464(6) 0.569(5) 0.053(19) Uiso 1 1 d D . . H2 H 0.671(10) 0.487(8) 0.627(2) 0.07(3) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 La1 0.01762(16) 0.01539(17) 0.03079(19) 0.00751(12) 0.01097(12) 0.00758(11) La2 0.01832(16) 0.01429(16) 0.03417(19) 0.00763(12) 0.01184(12) 0.00679(11) O1 0.0270(19) 0.0315(19) 0.051(2) 0.0131(17) 0.0175(17) 0.0070(15) O2 0.0281(18) 0.0309(19) 0.050(2) 0.0223(17) 0.0092(16) 0.0090(15) O3 0.0249(18) 0.0199(16) 0.050(2) 0.0048(15) 0.0114(16) 0.0049(14) O4 0.043(2) 0.0293(19) 0.041(2) 0.0048(16) 0.0185(18) 0.0212(17) O5 0.0300(18) 0.0221(16) 0.0333(19) 0.0114(14) 0.0159(15) 0.0116(14) O6 0.0254(17) 0.0288(18) 0.036(2) 0.0098(15) 0.0074(14) 0.0137(15) O7 0.0213(16) 0.0252(17) 0.035(2) 0.0105(14) 0.0107(14) 0.0069(13) O8 0.030(2) 0.051(2) 0.047(2) 0.023(2) 0.0134(17) -0.0032(18) O9 0.0210(17) 0.0236(17) 0.041(2) 0.0051(15) 0.0123(15) 0.0061(14) O10 0.0253(17) 0.0189(16) 0.0331(19) 0.0066(14) 0.0134(14) 0.0065(13) O11 0.0216(16) 0.0159(15) 0.0310(18) 0.0044(13) 0.0106(13) 0.0054(12) O12 0.0342(19) 0.0299(19) 0.041(2) -0.0002(16) 0.0138(16) 0.0151(16) O13 0.049(2) 0.029(2) 0.056(3) 0.0162(19) 0.022(2) 0.0226(18) C1 0.024(2) 0.014(2) 0.037(3) 0.0084(19) 0.011(2) 0.0044(18) C2 0.020(2) 0.024(2) 0.037(3) 0.007(2) 0.008(2) 0.0039(19) C3 0.046(3) 0.043(3) 0.044(4) 0.013(3) -0.003(3) -0.002(3) C4 0.070(5) 0.063(4) 0.037(4) 0.014(3) -0.003(3) -0.005(4) C5 0.089(6) 0.063(4) 0.037(4) 0.020(3) 0.024(4) 0.007(4) C6 0.047(3) 0.042(3) 0.047(4) 0.014(3) 0.022(3) 0.003(3) C7 0.025(2) 0.025(2) 0.036(3) 0.009(2) 0.013(2) 0.008(2) C8 0.025(2) 0.015(2) 0.036(3) 0.0068(19) 0.010(2) 0.0087(18) C9 0.019(2) 0.016(2) 0.029(3) 0.0043(18) 0.0075(18) 0.0026(17) C10 0.022(2) 0.027(2) 0.029(3) 0.006(2) 0.0086(19) 0.0123(19) C11 0.028(3) 0.047(3) 0.035(3) 0.007(2) 0.008(2) 0.011(2) C12 0.041(3) 0.069(4) 0.031(3) 0.004(3) -0.005(2) 0.005(3) C13 0.049(4) 0.088(5) 0.038(4) 0.033(4) 0.002(3) 0.011(4) C14 0.037(3) 0.063(4) 0.046(4) 0.033(3) 0.008(3) 0.007(3) C15 0.021(2) 0.038(3) 0.036(3) 0.013(2) 0.012(2) 0.006(2) C16 0.026(2) 0.029(3) 0.036(3) 0.016(2) 0.009(2) 0.012(2) C17 0.023(2) 0.016(2) 0.033(3) 0.0013(19) 0.0131(19) 0.0024(18) C18 0.020(2) 0.025(2) 0.035(3) 0.002(2) 0.012(2) 0.0031(19) C19 0.043(3) 0.034(3) 0.036(3) -0.001(2) 0.014(2) 0.005(2) C20 0.045(3) 0.062(4) 0.034(3) -0.002(3) 0.009(3) 0.009(3) C21 0.043(3) 0.075(5) 0.026(3) 0.016(3) 0.004(2) 0.017(3) C22 0.033(3) 0.043(3) 0.040(3) 0.012(3) 0.014(2) 0.014(2) C23 0.025(2) 0.032(3) 0.028(3) 0.007(2) 0.012(2) 0.009(2) C24 0.024(2) 0.016(2) 0.027(2) 0.0097(18) 0.0109(19) 0.0076(18) _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 O2 2.422(3) 2_766 ? La1 O6 2.465(3) 2_776 ? La1 O7 2.485(3) . ? La1 O9 2.497(4) 2_776 ? La1 O11 2.530(3) 1_655 ? La1 O3 2.546(3) . ? La1 O10 2.624(3) 1_655 ? La1 O5 2.642(3) . ? La2 O4 2.443(4) . ? La2 O1 2.482(4) 2_666 ? La2 O10 2.546(3) 2_676 ? La2 O13 2.600(4) . ? La2 O11 2.603(3) . ? La2 O7 2.607(3) . ? La2 O5 2.617(3) 2_776 ? La2 O12 2.647(4) . ? La2 O8 2.702(4) . ? La2 C17 3.002(5) . ? La2 C16 3.021(5) . ? O1 C1 1.240(6) . ? O1 La2 2.482(4) 2_666 ? O2 C1 1.263(6) . ? O2 La1 2.422(3) 2_766 ? O3 C8 1.253(6) . ? O4 C8 1.247(6) . ? O5 C9 1.262(6) . ? O5 La2 2.617(3) 2_776 ? O6 C9 1.244(6) . ? O6 La1 2.465(3) 2_776 ? O7 C16 1.271(6) . ? O8 C16 1.226(6) . ? O9 C24 1.229(6) . ? O9 La1 2.497(3) 2_776 ? O10 C24 1.282(6) . ? O10 La2 2.546(3) 2_676 ? O10 La1 2.624(3) 1_455 ? O11 C17 1.277(6) . ? O11 La1 2.530(3) 1_455 ? O12 C17 1.256(6) . ? C1 C2 1.488(7) . ? C2 C3 1.386(8) . ? C2 C7 1.392(7) . ? C3 C4 1.368(9) . ? C4 C5 1.388(10) . ? C5 C6 1.388(10) . ? C6 C7 1.387(8) . ? C7 C8 1.504(7) . ? C9 C10 1.510(7) . ? C10 C11 1.390(7) . ? C10 C15 1.396(7) . ? C11 C12 1.365(9) . ? C12 C13 1.362(10) . ? C13 C14 1.390(10) . ? C14 C15 1.389(8) . ? C15 C16 1.497(7) . ? C17 C18 1.481(7) . ? C18 C19 1.391(7) . ? C18 C23 1.395(7) . ? C19 C20 1.383(9) . ? C20 C21 1.383(10) . ? C21 C22 1.380(9) . ? C22 C23 1.389(8) . ? C23 C24 1.499(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 La1 O6 134.97(12) 2_766 2_776 ? O2 La1 O7 80.72(12) 2_766 . ? O6 La1 O7 83.82(12) 2_776 . ? O2 La1 O9 70.93(12) 2_766 2_776 ? O6 La1 O9 153.92(12) 2_776 2_776 ? O7 La1 O9 100.71(11) . 2_776 ? O2 La1 O11 84.34(12) 2_766 1_655 ? O6 La1 O11 104.32(11) 2_776 1_655 ? O7 La1 O11 164.57(10) . 1_655 ? O9 La1 O11 77.84(11) 2_776 1_655 ? O2 La1 O3 72.44(13) 2_766 . ? O6 La1 O3 68.97(12) 2_776 . ? O7 La1 O3 99.85(11) . . ? O9 La1 O3 134.01(11) 2_776 . ? O11 La1 O3 71.75(10) 1_655 . ? O2 La1 O10 149.96(11) 2_766 1_655 ? O6 La1 O10 70.39(11) 2_776 1_655 ? O7 La1 O10 123.72(10) . 1_655 ? O9 La1 O10 86.20(11) 2_776 1_655 ? O11 La1 O10 71.68(10) 1_655 1_655 ? O3 La1 O10 114.74(11) . 1_655 ? O2 La1 O5 121.68(13) 2_766 . ? O6 La1 O5 90.50(11) 2_776 . ? O7 La1 O5 68.59(10) . . ? O9 La1 O5 67.98(11) 2_776 . ? O11 La1 O5 123.55(10) 1_655 . ? O3 La1 O5 157.84(11) . . ? O10 La1 O5 62.78(11) 1_655 . ? O4 La2 O1 135.68(13) . 2_666 ? O4 La2 O10 136.25(12) . 2_676 ? O1 La2 O10 79.73(11) 2_666 2_676 ? O4 La2 O13 69.77(13) . . ? O1 La2 O13 66.01(13) 2_666 . ? O10 La2 O13 137.31(13) 2_676 . ? O4 La2 O11 126.85(12) . . ? O1 La2 O11 83.30(11) 2_666 . ? O10 La2 O11 71.17(11) 2_676 . ? O13 La2 O11 125.71(12) . . ? O4 La2 O7 68.82(12) . . ? O1 La2 O7 114.38(12) 2_666 . ? O10 La2 O7 72.97(11) 2_676 . ? O13 La2 O7 98.03(12) . . ? O11 La2 O7 135.97(10) . . ? O4 La2 O5 82.13(12) . 2_776 ? O1 La2 O5 141.73(11) 2_666 2_776 ? O10 La2 O5 64.16(11) 2_676 2_776 ? O13 La2 O5 151.75(12) . 2_776 ? O11 La2 O5 73.76(10) . 2_776 ? O7 La2 O5 68.07(11) . 2_776 ? O4 La2 O12 78.04(12) . . ? O1 La2 O12 116.95(12) 2_666 . ? O10 La2 O12 111.72(11) 2_676 . ? O13 La2 O12 106.31(13) . . ? O11 La2 O12 49.32(10) . . ? O7 La2 O12 128.46(11) . . ? O5 La2 O12 69.24(11) 2_776 . ? O4 La2 O8 94.26(14) . . ? O1 La2 O8 67.48(12) 2_666 . ? O10 La2 O8 75.05(13) 2_676 . ? O13 La2 O8 68.88(14) . . ? O11 La2 O8 138.55(12) . . ? O7 La2 O8 48.35(11) . . ? O5 La2 O8 111.79(11) 2_776 . ? O12 La2 O8 172.10(12) . . ? O4 La2 C17 101.80(13) . . ? O1 La2 C17 103.20(13) 2_666 . ? O10 La2 C17 89.79(12) 2_676 . ? O13 La2 C17 121.36(13) . . ? O11 La2 C17 25.06(11) . . ? O7 La2 C17 134.21(11) . . ? O5 La2 C17 66.24(11) 2_776 . ? O12 La2 C17 24.68(12) . . ? O8 La2 C17 163.21(13) . . ? O4 La2 C16 83.47(14) . . ? O1 La2 C16 89.89(13) 2_666 . ? O10 La2 C16 69.71(12) 2_676 . ? O13 La2 C16 84.97(14) . . ? O11 La2 C16 140.88(12) . . ? O7 La2 C16 24.73(12) . . ? O5 La2 C16 89.16(12) 2_776 . ? O12 La2 C16 153.13(12) . . ? O8 La2 C16 23.91(12) . . ? C17 La2 C16 153.49(13) . . ? C1 O1 La2 146.1(4) . 2_666 ? C1 O2 La1 136.8(3) . 2_766 ? C8 O3 La1 110.8(3) . . ? C8 O4 La2 157.8(3) . . ? C9 O5 La2 127.3(3) . 2_776 ? C9 O5 La1 116.1(3) . . ? La2 O5 La1 114.94(12) 2_776 . ? C9 O6 La1 132.4(3) . 2_776 ? C16 O7 La1 133.1(3) . . ? C16 O7 La2 96.2(3) . . ? La1 O7 La2 122.45(14) . . ? C16 O8 La2 92.8(3) . . ? C24 O9 La1 141.7(3) . 2_776 ? C24 O10 La2 125.3(3) . 2_676 ? C24 O10 La1 113.1(3) . 1_455 ? La2 O10 La1 118.12(13) 2_676 1_455 ? C17 O11 La1 136.1(3) . 1_455 ? C17 O11 La2 95.3(3) . . ? La1 O11 La2 125.24(13) 1_455 . ? C17 O12 La2 93.7(3) . . ? O1 C1 O2 124.5(5) . . ? O1 C1 C2 118.9(4) . . ? O2 C1 C2 116.6(4) . . ? C3 C2 C7 118.6(5) . . ? C3 C2 C1 119.5(4) . . ? C7 C2 C1 121.8(4) . . ? C4 C3 C2 121.3(6) . . ? C3 C4 C5 120.4(6) . . ? C4 C5 C6 119.1(6) . . ? C7 C6 C5 120.4(6) . . ? C6 C7 C2 120.2(5) . . ? C6 C7 C8 117.4(5) . . ? C2 C7 C8 121.9(4) . . ? O4 C8 O3 123.7(5) . . ? O4 C8 C7 116.7(4) . . ? O3 C8 C7 119.4(4) . . ? O6 C9 O5 124.3(5) . . ? O6 C9 C10 116.2(4) . . ? O5 C9 C10 119.5(4) . . ? C11 C10 C15 119.7(5) . . ? C11 C10 C9 119.4(5) . . ? C15 C10 C9 120.8(4) . . ? C12 C11 C10 119.1(6) . . ? C13 C12 C11 122.0(6) . . ? C12 C13 C14 119.9(6) . . ? C15 C14 C13 119.2(6) . . ? C14 C15 C10 120.0(5) . . ? C14 C15 C16 120.3(5) . . ? C10 C15 C16 119.7(5) . . ? O8 C16 O7 121.2(5) . . ? O8 C16 C15 122.0(5) . . ? O7 C16 C15 116.7(4) . . ? O8 C16 La2 63.3(3) . . ? O7 C16 La2 59.1(2) . . ? C15 C16 La2 164.3(3) . . ? O12 C17 O11 119.7(5) . . ? O12 C17 C18 122.1(4) . . ? O11 C17 C18 118.2(4) . . ? O12 C17 La2 61.6(3) . . ? O11 C17 La2 59.7(2) . . ? C18 C17 La2 166.1(3) . . ? C19 C18 C23 120.0(5) . . ? C19 C18 C17 120.7(5) . . ? C23 C18 C17 119.3(4) . . ? C20 C19 C18 120.2(6) . . ? C21 C20 C19 119.5(6) . . ? C22 C21 C20 120.9(6) . . ? C21 C22 C23 120.0(6) . . ? C22 C23 C18 119.4(5) . . ? C22 C23 C24 120.3(5) . . ? C18 C23 C24 120.2(4) . . ? O9 C24 O10 124.5(5) . . ? O9 C24 C23 118.5(4) . . ? O10 C24 C23 117.0(4) . . ? 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 O2 La1 O3 C8 100.3(3) 2_766 . . . ? O6 La1 O3 C8 -56.0(3) 2_776 . . . ? O7 La1 O3 C8 23.4(3) . . . . ? O9 La1 O3 C8 138.9(3) 2_776 . . . ? O11 La1 O3 C8 -169.9(4) 1_655 . . . ? O10 La1 O3 C8 -111.0(3) 1_655 . . . ? O5 La1 O3 C8 -32.8(5) . . . . ? O1 La2 O4 C8 151.4(9) 2_666 . . . ? O10 La2 O4 C8 -74.1(10) 2_676 . . . ? O13 La2 O4 C8 147.5(10) . . . . ? O11 La2 O4 C8 27.4(10) . . . . ? O7 La2 O4 C8 -104.9(9) . . . . ? O5 La2 O4 C8 -35.5(9) 2_776 . . . ? O12 La2 O4 C8 34.9(9) . . . . ? O8 La2 O4 C8 -146.9(9) . . . . ? C17 La2 O4 C8 28.1(9) . . . . ? C16 La2 O4 C8 -125.5(9) . . . . ? O2 La1 O5 C9 -47.1(4) 2_766 . . . ? O6 La1 O5 C9 99.6(3) 2_776 . . . ? O7 La1 O5 C9 16.5(3) . . . . ? O9 La1 O5 C9 -95.5(3) 2_776 . . . ? O11 La1 O5 C9 -152.7(3) 1_655 . . . ? O3 La1 O5 C9 78.1(4) . . . . ? O10 La1 O5 C9 167.2(4) 1_655 . . . ? O2 La1 O5 La2 146.38(13) 2_766 . . 2_776 ? O6 La1 O5 La2 -66.91(15) 2_776 . . 2_776 ? O7 La1 O5 La2 -150.08(17) . . . 2_776 ? O9 La1 O5 La2 97.96(15) 2_776 . . 2_776 ? O11 La1 O5 La2 40.70(18) 1_655 . . 2_776 ? O3 La1 O5 La2 -88.5(3) . . . 2_776 ? O10 La1 O5 La2 0.63(10) 1_655 . . 2_776 ? O2 La1 O7 C16 38.8(4) 2_766 . . . ? O6 La1 O7 C16 176.3(4) 2_776 . . . ? O9 La1 O7 C16 -29.7(4) 2_776 . . . ? O11 La1 O7 C16 53.4(6) 1_655 . . . ? O3 La1 O7 C16 109.0(4) . . . . ? O10 La1 O7 C16 -122.2(4) 1_655 . . . ? O5 La1 O7 C16 -90.7(4) . . . . ? O2 La1 O7 La2 -101.59(17) 2_766 . . . ? O6 La1 O7 La2 35.97(15) 2_776 . . . ? O9 La1 O7 La2 -170.01(14) 2_776 . . . ? O11 La1 O7 La2 -86.9(4) 1_655 . . . ? O3 La1 O7 La2 -31.38(17) . . . . ? O10 La1 O7 La2 97.41(17) 1_655 . . . ? O5 La1 O7 La2 128.94(18) . . . . ? O4 La2 O7 C16 -123.4(3) . . . . ? O1 La2 O7 C16 8.5(3) 2_666 . . . ? O10 La2 O7 C16 78.4(3) 2_676 . . . ? O13 La2 O7 C16 -58.8(3) . . . . ? O11 La2 O7 C16 115.0(3) . . . . ? O5 La2 O7 C16 146.8(3) 2_776 . . . ? O12 La2 O7 C16 -177.1(3) . . . . ? O8 La2 O7 C16 -6.5(3) . . . . ? C17 La2 O7 C16 150.7(3) . . . . ? O4 La2 O7 La1 28.69(15) . . . . ? O1 La2 O7 La1 160.51(15) 2_666 . . . ? O10 La2 O7 La1 -129.58(17) 2_676 . . . ? O13 La2 O7 La1 93.27(17) . . . . ? O11 La2 O7 La1 -92.95(18) . . . . ? O5 La2 O7 La1 -61.18(15) 2_776 . . . ? O12 La2 O7 La1 -25.0(2) . . . . ? O8 La2 O7 La1 145.5(2) . . . . ? C17 La2 O7 La1 -57.2(2) . . . . ? C16 La2 O7 La1 152.0(4) . . . . ? O4 La2 O8 C16 63.3(3) . . . . ? O1 La2 O8 C16 -158.4(4) 2_666 . . . ? O10 La2 O8 C16 -73.6(3) 2_676 . . . ? O13 La2 O8 C16 129.7(4) . . . . ? O11 La2 O8 C16 -109.8(3) . . . . ? O7 La2 O8 C16 6.8(3) . . . . ? O5 La2 O8 C16 -19.9(4) 2_776 . . . ? O12 La2 O8 C16 76.0(9) . . . . ? C17 La2 O8 C16 -99.7(5) . . . . ? O4 La2 O11 C17 1.8(3) . . . . ? O1 La2 O11 C17 -142.5(3) 2_666 . . . ? O10 La2 O11 C17 136.1(3) 2_676 . . . ? O13 La2 O11 C17 -88.6(3) . . . . ? O7 La2 O11 C17 99.0(3) . . . . ? O5 La2 O11 C17 68.4(3) 2_776 . . . ? O12 La2 O11 C17 -7.9(2) . . . . ? O8 La2 O11 C17 173.1(2) . . . . ? C16 La2 O11 C17 135.9(3) . . . . ? O4 La2 O11 La1 163.63(14) . . . 1_455 ? O1 La2 O11 La1 19.31(15) 2_666 . . 1_455 ? O10 La2 O11 La1 -62.09(14) 2_676 . . 1_455 ? O13 La2 O11 La1 73.26(19) . . . 1_455 ? O7 La2 O11 La1 -99.15(17) . . . 1_455 ? O5 La2 O11 La1 -129.73(16) 2_776 . . 1_455 ? O12 La2 O11 La1 153.9(2) . . . 1_455 ? O8 La2 O11 La1 -25.0(2) . . . 1_455 ? C17 La2 O11 La1 161.9(3) . . . 1_455 ? C16 La2 O11 La1 -62.2(2) . . . 1_455 ? O4 La2 O12 C17 -164.1(3) . . . . ? O1 La2 O12 C17 60.5(3) 2_666 . . . ? O10 La2 O12 C17 -28.8(3) 2_676 . . . ? O13 La2 O12 C17 131.4(3) . . . . ? O11 La2 O12 C17 8.0(2) . . . . ? O7 La2 O12 C17 -113.8(3) . . . . ? O5 La2 O12 C17 -78.0(3) 2_776 . . . ? O8 La2 O12 C17 -177.0(7) . . . . ? C16 La2 O12 C17 -116.5(3) . . . . ? La2 O1 C1 O2 15.7(9) 2_666 . . . ? La2 O1 C1 C2 -163.4(4) 2_666 . . . ? La1 O2 C1 O1 35.7(8) 2_766 . . . ? La1 O2 C1 C2 -145.2(4) 2_766 . . . ? O1 C1 C2 C3 -48.5(7) . . . . ? O2 C1 C2 C3 132.3(6) . . . . ? O1 C1 C2 C7 133.9(5) . . . . ? O2 C1 C2 C7 -45.2(7) . . . . ? C7 C2 C3 C4 1.5(10) . . . . ? C1 C2 C3 C4 -176.1(6) . . . . ? C2 C3 C4 C5 -0.8(12) . . . . ? C3 C4 C5 C6 0.8(13) . . . . ? C4 C5 C6 C7 -1.6(11) . . . . ? C5 C6 C7 C2 2.3(9) . . . . ? C5 C6 C7 C8 -170.1(6) . . . . ? C3 C2 C7 C6 -2.2(8) . . . . ? C1 C2 C7 C6 175.3(5) . . . . ? C3 C2 C7 C8 169.8(5) . . . . ? C1 C2 C7 C8 -12.6(7) . . . . ? La2 O4 C8 O3 113.2(9) . . . . ? La2 O4 C8 C7 -61.3(10) . . . . ? La1 O3 C8 O4 -29.5(6) . . . . ? La1 O3 C8 C7 144.8(3) . . . . ? C6 C7 C8 O4 128.1(5) . . . . ? C2 C7 C8 O4 -44.1(7) . . . . ? C6 C7 C8 O3 -46.6(7) . . . . ? C2 C7 C8 O3 141.2(5) . . . . ? La1 O6 C9 O5 29.0(7) 2_776 . . . ? La1 O6 C9 C10 -151.8(3) 2_776 . . . ? La2 O5 C9 O6 49.5(6) 2_776 . . . ? La1 O5 C9 O6 -115.1(4) . . . . ? La2 O5 C9 C10 -129.6(4) 2_776 . . . ? La1 O5 C9 C10 65.7(5) . . . . ? O6 C9 C10 C11 -93.3(5) . . . . ? O5 C9 C10 C11 86.0(6) . . . . ? O6 C9 C10 C15 82.2(6) . . . . ? O5 C9 C10 C15 -98.5(5) . . . . ? C15 C10 C11 C12 2.8(8) . . . . ? C9 C10 C11 C12 178.3(5) . . . . ? C10 C11 C12 C13 -1.7(10) . . . . ? C11 C12 C13 C14 -0.5(12) . . . . ? C12 C13 C14 C15 1.6(11) . . . . ? C13 C14 C15 C10 -0.5(9) . . . . ? C13 C14 C15 C16 -178.5(6) . . . . ? C11 C10 C15 C14 -1.6(8) . . . . ? C9 C10 C15 C14 -177.1(5) . . . . ? C11 C10 C15 C16 176.4(5) . . . . ? C9 C10 C15 C16 0.9(7) . . . . ? La2 O8 C16 O7 -12.2(5) . . . . ? La2 O8 C16 C15 163.0(4) . . . . ? La1 O7 C16 O8 -134.5(4) . . . . ? La2 O7 C16 O8 12.7(5) . . . . ? La1 O7 C16 C15 50.1(6) . . . . ? La2 O7 C16 C15 -162.7(4) . . . . ? La1 O7 C16 La2 -147.2(4) . . . . ? C14 C15 C16 O8 34.1(8) . . . . ? C10 C15 C16 O8 -143.9(5) . . . . ? C14 C15 C16 O7 -150.5(5) . . . . ? C10 C15 C16 O7 31.5(7) . . . . ? C14 C15 C16 La2 139.3(11) . . . . ? C10 C15 C16 La2 -38.8(15) . . . . ? O4 La2 C16 O8 -116.2(3) . . . . ? O1 La2 C16 O8 19.8(3) 2_666 . . . ? O10 La2 C16 O8 98.9(3) 2_676 . . . ? O13 La2 C16 O8 -46.1(3) . . . . ? O11 La2 C16 O8 99.1(3) . . . . ? O7 La2 C16 O8 -167.9(5) . . . . ? O5 La2 C16 O8 161.6(3) 2_776 . . . ? O12 La2 C16 O8 -162.8(3) . . . . ? C17 La2 C16 O8 140.4(3) . . . . ? O4 La2 C16 O7 51.6(3) . . . . ? O1 La2 C16 O7 -172.3(3) 2_666 . . . ? O10 La2 C16 O7 -93.2(3) 2_676 . . . ? O13 La2 C16 O7 121.8(3) . . . . ? O11 La2 C16 O7 -93.1(3) . . . . ? O5 La2 C16 O7 -30.6(3) 2_776 . . . ? O12 La2 C16 O7 5.0(5) . . . . ? O8 La2 C16 O7 167.9(5) . . . . ? C17 La2 C16 O7 -51.8(4) . . . . ? O4 La2 C16 C15 130.2(13) . . . . ? O1 La2 C16 C15 -93.7(13) 2_666 . . . ? O10 La2 C16 C15 -14.6(12) 2_676 . . . ? O13 La2 C16 C15 -159.6(13) . . . . ? O11 La2 C16 C15 -14.5(14) . . . . ? O7 La2 C16 C15 78.6(13) . . . . ? O5 La2 C16 C15 48.0(13) 2_776 . . . ? O12 La2 C16 C15 83.6(13) . . . . ? O8 La2 C16 C15 -113.5(14) . . . . ? C17 La2 C16 C15 26.8(14) . . . . ? La2 O12 C17 O11 -14.4(4) . . . . ? La2 O12 C17 C18 164.4(4) . . . . ? La1 O11 C17 O12 -143.8(3) 1_455 . . . ? La2 O11 C17 O12 14.7(4) . . . . ? La1 O11 C17 C18 37.3(6) 1_455 . . . ? La2 O11 C17 C18 -164.2(3) . . . . ? La1 O11 C17 La2 -158.5(4) 1_455 . . . ? O4 La2 C17 O12 15.9(3) . . . . ? O1 La2 C17 O12 -127.2(3) 2_666 . . . ? O10 La2 C17 O12 153.4(3) 2_676 . . . ? O13 La2 C17 O12 -57.4(3) . . . . ? O11 La2 C17 O12 -165.5(4) . . . . ? O7 La2 C17 O12 87.8(3) . . . . ? O5 La2 C17 O12 91.8(3) 2_776 . . . ? O8 La2 C17 O12 178.6(3) . . . . ? C16 La2 C17 O12 115.1(4) . . . . ? O4 La2 C17 O11 -178.5(2) . . . . ? O1 La2 C17 O11 38.3(3) 2_666 . . . ? O10 La2 C17 O11 -41.1(3) 2_676 . . . ? O13 La2 C17 O11 108.1(3) . . . . ? O7 La2 C17 O11 -106.7(3) . . . . ? O5 La2 C17 O11 -102.7(3) 2_776 . . . ? O12 La2 C17 O11 165.5(4) . . . . ? O8 La2 C17 O11 -15.9(5) . . . . ? C16 La2 C17 O11 -79.4(4) . . . . ? O4 La2 C17 C18 -93.3(13) . . . . ? O1 La2 C17 C18 123.6(13) 2_666 . . . ? O10 La2 C17 C18 44.2(13) 2_676 . . . ? O13 La2 C17 C18 -166.6(13) . . . . ? O11 La2 C17 C18 85.3(14) . . . . ? O7 La2 C17 C18 -21.4(14) . . . . ? O5 La2 C17 C18 -17.4(13) 2_776 . . . ? O12 La2 C17 C18 -109.2(14) . . . . ? O8 La2 C17 C18 69.4(15) . . . . ? C16 La2 C17 C18 5.9(15) . . . . ? O12 C17 C18 C19 36.5(7) . . . . ? O11 C17 C18 C19 -144.7(5) . . . . ? La2 C17 C18 C19 137.8(12) . . . . ? O12 C17 C18 C23 -146.8(5) . . . . ? O11 C17 C18 C23 32.0(6) . . . . ? La2 C17 C18 C23 -45.5(15) . . . . ? C23 C18 C19 C20 -2.0(8) . . . . ? C17 C18 C19 C20 174.7(5) . . . . ? C18 C19 C20 C21 0.5(9) . . . . ? C19 C20 C21 C22 1.1(9) . . . . ? C20 C21 C22 C23 -1.3(9) . . . . ? C21 C22 C23 C18 -0.2(8) . . . . ? C21 C22 C23 C24 176.0(5) . . . . ? C19 C18 C23 C22 1.8(7) . . . . ? C17 C18 C23 C22 -174.9(4) . . . . ? C19 C18 C23 C24 -174.4(4) . . . . ? C17 C18 C23 C24 8.9(6) . . . . ? La1 O9 C24 O10 26.7(8) 2_776 . . . ? La1 O9 C24 C23 -152.7(4) 2_776 . . . ? La2 O10 C24 O9 47.9(6) 2_676 . . . ? La1 O10 C24 O9 -110.6(4) 1_455 . . . ? La2 O10 C24 C23 -132.7(4) 2_676 . . . ? La1 O10 C24 C23 68.8(4) 1_455 . . . ? C22 C23 C24 O9 -106.6(6) . . . . ? C18 C23 C24 O9 69.5(6) . . . . ? C22 C23 C24 O10 74.0(6) . . . . ? C18 C23 C24 O10 -109.8(5) . . . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 1.825 _refine_diff_density_min -1.073 _refine_diff_density_rms 0.155 #===END data_complex2 _database_code_CSD 184846 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H14 Eu2 O13' _chemical_formula_weight 814.27 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.998(3) _cell_length_b 26.397(9) _cell_length_c 11.677(4) _cell_angle_alpha 90.00 _cell_angle_beta 107.226(4) _cell_angle_gamma 90.00 _cell_volume 2354.6(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.297 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1552 _exptl_absorpt_coefficient_mu 5.352 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.2966 _exptl_absorpt_correction_T_max 0.6166 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7876 _diffrn_reflns_av_R_equivalents 0.0356 _diffrn_reflns_av_sigmaI/netI 0.0349 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 23.28 _reflns_number_total 3327 _reflns_number_gt 3049 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0393P)^2^+9.0006P] 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 3327 _refine_ls_number_parameters 350 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0337 _refine_ls_R_factor_gt 0.0300 _refine_ls_wR_factor_ref 0.0721 _refine_ls_wR_factor_gt 0.0703 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.211 _refine_ls_shift/su_mean 0.005 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 0.41674(4) 0.225655(12) 0.83761(2) 0.01482(11) Uani 1 1 d . . . Eu2 Eu 0.09725(4) 0.194978(12) 1.01073(2) 0.01619(12) Uani 1 1 d . . . O1 O 0.4363(5) 0.17712(17) 1.0282(3) 0.0197(9) Uani 1 1 d . . . O2 O 0.2605(5) 0.11573(18) 1.0479(4) 0.0244(10) Uani 1 1 d . . . O3 O 0.5849(5) 0.15427(17) 0.8517(4) 0.0231(10) Uani 1 1 d . . . O4 O 0.8694(5) 0.14079(18) 0.9267(4) 0.0260(10) Uani 1 1 d . . . O5 O 0.3050(6) 0.20137(19) 0.6352(4) 0.0298(11) Uani 1 1 d . . . O6 O 0.2405(5) 0.23291(16) 0.4524(3) 0.0176(9) Uani 1 1 d . . . O7 O 0.2643(5) 0.20142(17) 0.2317(3) 0.0219(10) Uani 1 1 d . . . O8 O 0.0176(6) 0.15974(19) 0.1826(4) 0.0298(11) Uani 1 1 d . . . O9 O 0.6119(5) 0.27365(17) 0.9829(4) 0.0244(11) Uani 1 1 d . . . O10 O 0.8878(6) 0.25203(19) 1.0155(4) 0.0288(11) Uani 1 1 d . . . O11 O 0.9209(6) 0.28043(18) 1.2650(4) 0.0268(11) Uani 1 1 d . . . O12 O 1.1623(5) 0.32532(18) 1.3239(3) 0.0200(10) Uani 1 1 d . . . O13 O 0.6103(6) 0.2641(2) 0.7389(4) 0.0274(11) Uani 1 1 d D . . C1 C 0.4075(8) 0.1303(3) 1.0415(5) 0.0187(14) Uani 1 1 d . . . C2 C 0.5452(8) 0.0907(2) 1.0562(5) 0.0173(13) Uani 1 1 d . . . C3 C 0.5346(9) 0.0501(3) 1.1285(6) 0.0328(17) Uani 1 1 d . . . H3A H 0.4432 0.0489 1.1625 0.039 Uiso 1 1 calc R . . C4 C 0.6549(10) 0.0117(3) 1.1515(7) 0.0395(19) Uani 1 1 d . . . H4A H 0.6440 -0.0151 1.2003 0.047 Uiso 1 1 calc R . . C5 C 0.7931(10) 0.0127(3) 1.1025(7) 0.0404(19) Uani 1 1 d . . . H5A H 0.8747 -0.0135 1.1171 0.049 Uiso 1 1 calc R . . C6 C 0.8065(9) 0.0530(3) 1.0321(6) 0.0335(17) Uani 1 1 d . . . H6A H 0.8999 0.0542 1.0000 0.040 Uiso 1 1 calc R . . C7 C 0.6867(8) 0.0920(3) 1.0071(5) 0.0222(15) Uani 1 1 d . . . C8 C 0.7136(8) 0.1325(2) 0.9235(5) 0.0200(14) Uani 1 1 d . . . C9 C 0.2831(7) 0.1955(2) 0.5252(5) 0.0174(14) Uani 1 1 d . . . C10 C 0.2984(8) 0.1443(2) 0.4793(5) 0.0212(14) Uani 1 1 d . . . C11 C 0.3674(9) 0.1064(3) 0.5622(6) 0.0310(17) Uani 1 1 d . . . H11A H 0.4108 0.1144 0.6431 0.037 Uiso 1 1 calc R . . C12 C 0.3719(12) 0.0565(3) 0.5249(7) 0.049(2) Uani 1 1 d . . . H12A H 0.4219 0.0314 0.5804 0.059 Uiso 1 1 calc R . . C13 C 0.3019(11) 0.0444(3) 0.4055(7) 0.044(2) Uani 1 1 d . . . H13A H 0.3017 0.0110 0.3802 0.053 Uiso 1 1 calc R . . C14 C 0.2320(10) 0.0823(3) 0.3235(6) 0.0342(17) Uani 1 1 d . . . H14A H 0.1835 0.0738 0.2432 0.041 Uiso 1 1 calc R . . C15 C 0.2326(8) 0.1318(2) 0.3575(5) 0.0186(14) Uani 1 1 d . . . C16 C 0.1636(8) 0.1678(2) 0.2548(5) 0.0190(14) Uani 1 1 d . . . C17 C 0.7727(8) 0.2842(3) 1.0130(5) 0.0180(14) Uani 1 1 d . . . C18 C 0.8269(8) 0.3379(3) 1.0381(5) 0.0192(14) Uani 1 1 d . . . C19 C 0.7666(10) 0.3731(3) 0.9472(6) 0.0395(19) Uani 1 1 d . . . H19A H 0.6868 0.3636 0.8748 0.047 Uiso 1 1 calc R . . C20 C 0.8265(11) 0.4224(4) 0.9653(7) 0.049(2) Uiso 1 1 d . . . H20A H 0.7846 0.4463 0.9052 0.058 Uiso 1 1 calc R . . C21 C 0.9469(10) 0.4364(3) 1.0707(7) 0.0411(19) Uani 1 1 d . . . H21A H 0.9886 0.4695 1.0809 0.049 Uiso 1 1 calc R . . C22 C 1.0063(9) 0.4017(3) 1.1615(6) 0.0306(16) Uiso 1 1 d . . . H22A H 1.0860 0.4115 1.2336 0.037 Uiso 1 1 calc R . . C23 C 0.9479(8) 0.3521(2) 1.1460(5) 0.0186(14) Uani 1 1 d . . . C24 C 1.0100(8) 0.3160(3) 1.2472(5) 0.0184(14) Uani 1 1 d . . . H1 H 0.713(5) 0.246(2) 0.745(5) 0.022(17) Uiso 1 1 d D . . H2 H 0.577(11) 0.285(3) 0.673(5) 0.07(3) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Eu1 0.01216(18) 0.0199(2) 0.01263(17) 0.00049(12) 0.00402(12) 0.00074(13) Eu2 0.01257(18) 0.0209(2) 0.01665(17) -0.00015(12) 0.00665(12) -0.00072(13) O1 0.016(2) 0.024(3) 0.017(2) -0.0004(18) 0.0027(16) -0.002(2) O2 0.020(2) 0.025(3) 0.032(2) 0.007(2) 0.0135(19) 0.006(2) O3 0.021(2) 0.024(3) 0.024(2) 0.0057(19) 0.0068(19) 0.009(2) O4 0.016(2) 0.035(3) 0.027(2) -0.002(2) 0.0068(18) -0.002(2) O5 0.039(3) 0.039(3) 0.013(2) -0.0026(19) 0.0094(19) -0.004(2) O6 0.018(2) 0.016(2) 0.021(2) 0.0016(18) 0.0086(17) 0.0052(19) O7 0.023(2) 0.025(3) 0.018(2) -0.0049(18) 0.0070(18) -0.007(2) O8 0.023(3) 0.044(3) 0.021(2) -0.002(2) 0.004(2) -0.011(2) O9 0.017(3) 0.033(3) 0.021(2) -0.0043(19) 0.0016(18) -0.007(2) O10 0.027(3) 0.030(3) 0.031(2) -0.003(2) 0.010(2) 0.002(2) O11 0.023(2) 0.024(3) 0.035(3) 0.006(2) 0.011(2) -0.006(2) O12 0.012(2) 0.035(3) 0.0102(19) 0.0010(18) -0.0016(16) 0.000(2) O13 0.016(2) 0.041(3) 0.026(2) 0.007(2) 0.0075(19) 0.007(2) C1 0.016(3) 0.027(4) 0.014(3) 0.001(3) 0.005(2) -0.003(3) C2 0.022(3) 0.008(3) 0.021(3) 0.002(2) 0.004(2) -0.002(3) C3 0.032(4) 0.035(5) 0.036(4) 0.007(3) 0.017(3) 0.004(4) C4 0.043(5) 0.037(5) 0.044(4) 0.013(4) 0.021(4) 0.014(4) C5 0.038(4) 0.030(5) 0.055(5) 0.016(4) 0.015(4) 0.017(4) C6 0.023(4) 0.033(5) 0.048(4) 0.009(3) 0.016(3) 0.010(3) C7 0.016(3) 0.026(4) 0.025(3) -0.001(3) 0.006(3) 0.002(3) C8 0.014(3) 0.021(4) 0.024(3) -0.008(3) 0.005(3) -0.005(3) C9 0.009(3) 0.026(4) 0.017(3) -0.002(3) 0.002(2) -0.002(3) C10 0.025(3) 0.020(4) 0.020(3) 0.003(3) 0.008(3) -0.003(3) C11 0.038(4) 0.027(4) 0.027(4) 0.006(3) 0.008(3) 0.008(3) C12 0.073(6) 0.035(5) 0.046(5) 0.015(4) 0.029(4) 0.022(5) C13 0.063(5) 0.018(4) 0.058(5) -0.005(4) 0.030(4) 0.004(4) C14 0.048(5) 0.029(4) 0.030(4) -0.006(3) 0.018(3) -0.002(4) C15 0.022(3) 0.016(4) 0.021(3) -0.001(3) 0.012(3) 0.000(3) C16 0.027(4) 0.018(4) 0.016(3) -0.001(3) 0.012(3) -0.001(3) C17 0.013(3) 0.031(4) 0.010(3) -0.004(3) 0.004(2) 0.003(3) C18 0.013(3) 0.023(4) 0.020(3) -0.001(3) 0.004(2) 0.004(3) C19 0.042(5) 0.035(5) 0.028(4) 0.001(3) -0.011(3) 0.001(4) C21 0.046(5) 0.015(4) 0.053(5) 0.008(3) -0.001(4) -0.009(4) C23 0.016(3) 0.020(4) 0.019(3) -0.001(3) 0.005(2) -0.001(3) C24 0.017(3) 0.026(4) 0.016(3) 0.001(3) 0.011(3) 0.006(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu1 O3 2.293(4) . ? Eu1 O9 2.313(4) . ? Eu1 O5 2.354(4) . ? Eu1 O12 2.405(4) 4_465 ? Eu1 O7 2.414(4) 4_566 ? Eu1 O13 2.411(4) . ? Eu1 O6 2.470(4) 4_566 ? Eu1 O1 2.532(4) . ? Eu1 Eu2 3.7857(9) . ? Eu1 Eu2 4.4396(10) 4_565 ? Eu2 O10 2.265(5) 1_455 ? Eu2 O4 2.296(4) 1_455 ? Eu2 O6 2.421(4) 4_566 ? Eu2 O2 2.436(4) . ? Eu2 O12 2.447(4) 4_465 ? Eu2 O8 2.461(4) 1_556 ? Eu2 O7 2.536(4) 1_556 ? Eu2 O1 2.700(4) . ? Eu2 C16 2.832(6) 1_556 ? Eu2 O11 2.872(4) 4_465 ? Eu2 C1 2.945(6) . ? Eu2 C24 2.961(6) 4_465 ? O1 C1 1.275(8) . ? O2 C1 1.260(7) . ? O3 C8 1.257(7) . ? O4 C8 1.255(7) . ? O4 Eu2 2.296(4) 1_655 ? O5 C9 1.254(7) . ? O6 C9 1.281(7) . ? O6 Eu2 2.421(4) 4_565 ? O6 Eu1 2.470(4) 4_565 ? O7 C16 1.279(7) . ? O7 Eu1 2.414(4) 4_565 ? O7 Eu2 2.536(4) 1_554 ? O8 C16 1.240(7) . ? O8 Eu2 2.461(4) 1_554 ? O9 C17 1.260(7) . ? O10 C17 1.247(8) . ? O10 Eu2 2.265(5) 1_655 ? O11 C24 1.233(8) . ? O11 Eu2 2.872(4) 4_666 ? O12 C24 1.304(7) . ? O12 Eu1 2.405(4) 4_666 ? O12 Eu2 2.447(4) 4_666 ? O13 H1 0.926(11) . ? O13 H2 0.925(11) . ? C1 C2 1.490(9) . ? C2 C3 1.383(9) . ? C2 C7 1.412(9) . ? C3 C4 1.368(10) . ? C3 H3A 0.9300 . ? C4 C5 1.387(10) . ? C4 H4A 0.9300 . ? C5 C6 1.369(10) . ? C5 H5A 0.9300 . ? C6 C7 1.378(9) . ? C6 H6A 0.9300 . ? C7 C8 1.506(9) . ? C9 C10 1.472(9) . ? C9 Eu2 3.232(6) 4_565 ? C10 C11 1.389(9) . ? C10 C15 1.401(8) . ? C11 C12 1.390(11) . ? C11 H11A 0.9300 . ? C12 C13 1.378(11) . ? C12 H12A 0.9300 . ? C13 C14 1.382(11) . ? C13 H13A 0.9300 . ? C14 C15 1.366(9) . ? C14 H14A 0.9300 . ? C15 C16 1.503(9) . ? C16 Eu2 2.832(6) 1_554 ? C17 C18 1.486(9) . ? C18 C19 1.385(10) . ? C18 C23 1.393(8) . ? C19 C20 1.381(12) . ? C19 H19A 0.9300 . ? C20 C21 1.371(11) . ? C20 H20A 0.9300 . ? C21 C22 1.376(10) . ? C21 H21A 0.9300 . ? C22 C23 1.384(10) . ? C22 H22A 0.9300 . ? C23 C24 1.484(9) . ? C24 Eu2 2.961(6) 4_666 ? 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 O3 Eu1 O9 98.26(16) . . ? O3 Eu1 O5 83.58(16) . . ? O9 Eu1 O5 149.13(16) . . ? O3 Eu1 O12 90.67(16) . 4_465 ? O9 Eu1 O12 136.81(14) . 4_465 ? O5 Eu1 O12 73.66(14) . 4_465 ? O3 Eu1 O7 152.71(14) . 4_566 ? O9 Eu1 O7 93.88(15) . 4_566 ? O5 Eu1 O7 73.68(16) . 4_566 ? O12 Eu1 O7 97.06(15) 4_465 4_566 ? O3 Eu1 O13 86.22(16) . . ? O9 Eu1 O13 74.37(15) . . ? O5 Eu1 O13 75.01(16) . . ? O12 Eu1 O13 148.67(14) 4_465 . ? O7 Eu1 O13 73.63(15) 4_566 . ? O3 Eu1 O6 137.91(14) . 4_566 ? O9 Eu1 O6 74.27(14) . 4_566 ? O5 Eu1 O6 123.89(15) . 4_566 ? O12 Eu1 O6 71.11(14) 4_465 4_566 ? O7 Eu1 O6 69.03(13) 4_566 4_566 ? O13 Eu1 O6 128.59(16) . 4_566 ? O3 Eu1 O1 68.84(14) . . ? O9 Eu1 O1 77.30(15) . . ? O5 Eu1 O1 130.58(16) . . ? O12 Eu1 O1 66.80(13) 4_465 . ? O7 Eu1 O1 138.06(13) 4_566 . ? O13 Eu1 O1 138.75(14) . . ? O6 Eu1 O1 69.11(13) 4_566 . ? O3 Eu1 Eu2 105.09(11) . . ? O9 Eu1 Eu2 98.12(11) . . ? O5 Eu1 Eu2 111.23(12) . . ? O12 Eu1 Eu2 39.12(9) 4_465 . ? O7 Eu1 Eu2 97.21(10) 4_566 . ? O13 Eu1 Eu2 167.41(12) . . ? O6 Eu1 Eu2 38.82(10) 4_566 . ? O1 Eu1 Eu2 45.43(9) . . ? O3 Eu1 Eu2 128.72(10) . 4_565 ? O9 Eu1 Eu2 117.62(11) . 4_565 ? O5 Eu1 Eu2 46.75(12) . 4_565 ? O12 Eu1 Eu2 86.94(9) 4_465 4_565 ? O7 Eu1 Eu2 26.95(10) 4_566 4_565 ? O13 Eu1 Eu2 71.22(11) . 4_565 ? O6 Eu1 Eu2 88.98(10) 4_566 4_565 ? O1 Eu1 Eu2 149.80(9) . 4_565 ? Eu2 Eu1 Eu2 104.62(2) . 4_565 ? O10 Eu2 O4 85.74(17) 1_455 1_455 ? O10 Eu2 O6 84.23(16) 1_455 4_566 ? O4 Eu2 O6 138.73(14) 1_455 4_566 ? O10 Eu2 O2 158.08(15) 1_455 . ? O4 Eu2 O2 81.78(16) 1_455 . ? O6 Eu2 O2 116.86(14) 4_566 . ? O10 Eu2 O12 121.44(14) 1_455 4_465 ? O4 Eu2 O12 80.44(14) 1_455 4_465 ? O6 Eu2 O12 71.23(14) 4_566 4_465 ? O2 Eu2 O12 74.13(14) . 4_465 ? O10 Eu2 O8 81.90(16) 1_455 1_556 ? O4 Eu2 O8 75.45(15) 1_455 1_556 ? O6 Eu2 O8 141.70(14) 4_566 1_556 ? O2 Eu2 O8 77.57(15) . 1_556 ? O12 Eu2 O8 144.98(16) 4_465 1_556 ? O10 Eu2 O7 95.78(15) 1_455 1_556 ? O4 Eu2 O7 126.09(15) 1_455 1_556 ? O6 Eu2 O7 94.75(14) 4_566 1_556 ? O2 Eu2 O7 77.47(14) . 1_556 ? O12 Eu2 O7 137.29(13) 4_465 1_556 ? O8 Eu2 O7 51.76(14) 1_556 1_556 ? O10 Eu2 O1 147.95(16) 1_455 . ? O4 Eu2 O1 125.15(15) 1_455 . ? O6 Eu2 O1 67.05(14) 4_566 . ? O2 Eu2 O1 50.44(14) . . ? O12 Eu2 O1 63.58(12) 4_465 . ? O8 Eu2 O1 111.67(14) 1_556 . ? O7 Eu2 O1 73.76(12) 1_556 . ? O10 Eu2 C16 93.61(16) 1_455 1_556 ? O4 Eu2 C16 99.26(17) 1_455 1_556 ? O6 Eu2 C16 121.24(16) 4_566 1_556 ? O2 Eu2 C16 70.88(16) . 1_556 ? O12 Eu2 C16 144.65(16) 4_465 1_556 ? O8 Eu2 C16 25.89(16) 1_556 1_556 ? O7 Eu2 C16 26.85(16) 1_556 1_556 ? O1 Eu2 C16 89.72(15) . 1_556 ? O10 Eu2 O11 74.13(14) 1_455 4_465 ? O4 Eu2 O11 67.72(14) 1_455 4_465 ? O6 Eu2 O11 71.02(13) 4_566 4_465 ? O2 Eu2 O11 116.81(13) . 4_465 ? O12 Eu2 O11 47.93(13) 4_465 4_465 ? O8 Eu2 O11 136.98(14) 1_556 4_465 ? O7 Eu2 O11 163.02(14) 1_556 4_465 ? O1 Eu2 O11 107.45(12) . 4_465 ? C16 Eu2 O11 162.33(16) 1_556 4_465 ? O10 Eu2 C1 170.00(16) 1_455 . ? O4 Eu2 C1 102.96(17) 1_455 . ? O6 Eu2 C1 92.19(16) 4_566 . ? O2 Eu2 C1 24.85(16) . . ? O12 Eu2 C1 65.66(14) 4_465 . ? O8 Eu2 C1 95.38(16) 1_556 . ? O7 Eu2 C1 75.17(15) 1_556 . ? O1 Eu2 C1 25.64(15) . . ? C16 Eu2 C1 80.25(16) 1_556 . ? O11 Eu2 C1 113.55(14) 4_465 . ? O10 Eu2 C24 98.19(17) 1_455 4_465 ? O4 Eu2 C24 65.29(16) 1_455 4_465 ? O6 Eu2 C24 76.72(15) 4_566 4_465 ? O2 Eu2 C24 92.87(16) . 4_465 ? O12 Eu2 C24 25.72(15) 4_465 4_465 ? O8 Eu2 C24 140.56(16) 1_556 4_465 ? O7 Eu2 C24 162.75(15) 1_556 4_465 ? O1 Eu2 C24 89.06(14) . 4_465 ? C16 Eu2 C24 159.59(19) 1_556 4_465 ? O11 Eu2 C24 24.35(15) 4_465 4_465 ? C1 Eu2 C24 90.03(17) . 4_465 ? C1 O1 Eu1 129.1(3) . . ? C1 O1 Eu2 88.0(3) . . ? Eu1 O1 Eu2 92.65(13) . . ? C1 O2 Eu2 100.8(4) . . ? C8 O3 Eu1 140.3(4) . . ? C8 O4 Eu2 140.9(4) . 1_655 ? C9 O5 Eu1 163.4(4) . . ? C9 O6 Eu2 118.3(4) . 4_565 ? C9 O6 Eu1 128.2(4) . 4_565 ? Eu2 O6 Eu1 101.43(15) 4_565 4_565 ? C16 O7 Eu1 134.4(4) . 4_565 ? C16 O7 Eu2 89.6(3) . 1_554 ? Eu1 O7 Eu2 127.49(18) 4_565 1_554 ? C16 O8 Eu2 94.0(4) . 1_554 ? C17 O9 Eu1 137.5(4) . . ? C17 O10 Eu2 177.1(4) . 1_655 ? C24 O11 Eu2 81.9(3) . 4_666 ? C24 O12 Eu1 122.7(4) . 4_666 ? C24 O12 Eu2 99.7(3) . 4_666 ? Eu1 O12 Eu2 102.55(15) 4_666 4_666 ? Eu1 O13 H1 116(4) . . ? Eu1 O13 H2 126(5) . . ? H1 O13 H2 113(7) . . ? O2 C1 O1 120.6(6) . . ? O2 C1 C2 116.7(6) . . ? O1 C1 C2 122.6(5) . . ? O2 C1 Eu2 54.3(3) . . ? O1 C1 Eu2 66.4(3) . . ? C2 C1 Eu2 170.9(4) . . ? C3 C2 C7 117.9(6) . . ? C3 C2 C1 115.9(5) . . ? C7 C2 C1 126.2(5) . . ? C4 C3 C2 121.8(6) . . ? C4 C3 H3A 119.1 . . ? C2 C3 H3A 119.1 . . ? C3 C4 C5 120.4(7) . . ? C3 C4 H4A 119.8 . . ? C5 C4 H4A 119.8 . . ? C6 C5 C4 118.4(7) . . ? C6 C5 H5A 120.8 . . ? C4 C5 H5A 120.8 . . ? C5 C6 C7 122.4(6) . . ? C5 C6 H6A 118.8 . . ? C7 C6 H6A 118.8 . . ? C6 C7 C2 119.1(6) . . ? C6 C7 C8 116.4(5) . . ? C2 C7 C8 124.5(6) . . ? O4 C8 O3 123.4(6) . . ? O4 C8 C7 115.8(6) . . ? O3 C8 C7 120.7(5) . . ? O5 C9 O6 120.9(6) . . ? O5 C9 C10 119.0(6) . . ? O6 C9 C10 120.0(5) . . ? O5 C9 Eu2 82.3(4) . 4_565 ? O6 C9 Eu2 41.2(3) . 4_565 ? C10 C9 Eu2 152.7(4) . 4_565 ? C11 C10 C15 119.3(6) . . ? C11 C10 C9 117.8(6) . . ? C15 C10 C9 122.7(6) . . ? C10 C11 C12 120.4(6) . . ? C10 C11 H11A 119.8 . . ? C12 C11 H11A 119.8 . . ? C13 C12 C11 119.7(7) . . ? C13 C12 H12A 120.1 . . ? C11 C12 H12A 120.1 . . ? C12 C13 C14 119.6(7) . . ? C12 C13 H13A 120.2 . . ? C14 C13 H13A 120.2 . . ? C15 C14 C13 121.6(7) . . ? C15 C14 H14A 119.2 . . ? C13 C14 H14A 119.2 . . ? C14 C15 C10 119.3(6) . . ? C14 C15 C16 113.9(5) . . ? C10 C15 C16 126.8(6) . . ? O8 C16 O7 120.1(5) . . ? O8 C16 C15 118.9(6) . . ? O7 C16 C15 120.1(5) . . ? O8 C16 Eu2 60.1(3) . 1_554 ? O7 C16 Eu2 63.6(3) . 1_554 ? C15 C16 Eu2 151.5(4) . 1_554 ? O10 C17 O9 122.7(6) . . ? O10 C17 C18 118.4(5) . . ? O9 C17 C18 118.7(6) . . ? C19 C18 C23 120.3(6) . . ? C19 C18 C17 118.2(6) . . ? C23 C18 C17 121.2(6) . . ? C20 C19 C18 119.2(7) . . ? C20 C19 H19A 120.4 . . ? C18 C19 H19A 120.4 . . ? C21 C20 C19 120.8(8) . . ? C21 C20 H20A 119.6 . . ? C19 C20 H20A 119.6 . . ? C20 C21 C22 120.2(8) . . ? C20 C21 H21A 119.9 . . ? C22 C21 H21A 119.9 . . ? C21 C22 C23 120.2(6) . . ? C21 C22 H22A 119.9 . . ? C23 C22 H22A 119.9 . . ? C22 C23 C18 119.3(6) . . ? C22 C23 C24 118.8(6) . . ? C18 C23 C24 121.8(6) . . ? O11 C24 O12 119.8(6) . . ? O11 C24 C23 123.3(6) . . ? O12 C24 C23 116.8(6) . . ? O11 C24 Eu2 73.8(3) . 4_666 ? O12 C24 Eu2 54.6(3) . 4_666 ? C23 C24 Eu2 144.2(4) . 4_666 ? 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 Eu1 O1 C1 -51.1(5) . . . . ? O9 Eu1 O1 C1 -155.3(5) . . . . ? O5 Eu1 O1 C1 9.6(5) . . . . ? O12 Eu1 O1 C1 49.3(5) 4_465 . . . ? O7 Eu1 O1 C1 123.2(5) 4_566 . . . ? O13 Eu1 O1 C1 -107.8(5) . . . . ? O6 Eu1 O1 C1 126.9(5) 4_566 . . . ? Eu2 Eu1 O1 C1 89.6(5) . . . . ? Eu2 Eu1 O1 C1 80.9(5) 4_565 . . . ? O3 Eu1 O1 Eu2 -140.65(17) . . . . ? O9 Eu1 O1 Eu2 115.17(16) . . . . ? O5 Eu1 O1 Eu2 -79.9(2) . . . . ? O12 Eu1 O1 Eu2 -40.30(13) 4_465 . . . ? O7 Eu1 O1 Eu2 33.6(2) 4_566 . . . ? O13 Eu1 O1 Eu2 162.64(19) . . . . ? O6 Eu1 O1 Eu2 37.37(12) 4_566 . . . ? Eu2 Eu1 O1 Eu2 -8.7(3) 4_565 . . . ? O10 Eu2 O1 C1 163.9(3) 1_455 . . . ? O4 Eu2 O1 C1 -33.6(4) 1_455 . . . ? O6 Eu2 O1 C1 -168.0(3) 4_566 . . . ? O2 Eu2 O1 C1 2.5(3) . . . . ? O12 Eu2 O1 C1 -88.4(3) 4_465 . . . ? O8 Eu2 O1 C1 53.5(3) 1_556 . . . ? O7 Eu2 O1 C1 89.5(3) 1_556 . . . ? C16 Eu2 O1 C1 67.6(3) 1_556 . . . ? O11 Eu2 O1 C1 -108.2(3) 4_465 . . . ? C24 Eu2 O1 C1 -92.0(3) 4_465 . . . ? O10 Eu2 O1 Eu1 -67.0(3) 1_455 . . . ? O4 Eu2 O1 Eu1 95.51(18) 1_455 . . . ? O6 Eu2 O1 Eu1 -38.92(13) 4_566 . . . ? O2 Eu2 O1 Eu1 131.6(2) . . . . ? O12 Eu2 O1 Eu1 40.73(14) 4_465 . . . ? O8 Eu2 O1 Eu1 -177.41(13) 1_556 . . . ? O7 Eu2 O1 Eu1 -141.45(17) 1_556 . . . ? C16 Eu2 O1 Eu1 -163.34(17) 1_556 . . . ? O11 Eu2 O1 Eu1 20.85(16) 4_465 . . . ? C1 Eu2 O1 Eu1 129.1(3) . . . . ? C24 Eu2 O1 Eu1 37.04(16) 4_465 . . . ? O10 Eu2 O2 C1 -155.7(4) 1_455 . . . ? O4 Eu2 O2 C1 148.4(4) 1_455 . . . ? O6 Eu2 O2 C1 7.3(4) 4_566 . . . ? O12 Eu2 O2 C1 66.0(3) 4_465 . . . ? O8 Eu2 O2 C1 -134.8(4) 1_556 . . . ? O7 Eu2 O2 C1 -81.7(3) 1_556 . . . ? O1 Eu2 O2 C1 -2.5(3) . . . . ? C16 Eu2 O2 C1 -108.8(4) 1_556 . . . ? O11 Eu2 O2 C1 88.5(4) 4_465 . . . ? C24 Eu2 O2 C1 83.9(4) 4_465 . . . ? O9 Eu1 O3 C8 20.6(6) . . . . ? O5 Eu1 O3 C8 169.5(6) . . . . ? O12 Eu1 O3 C8 -117.0(6) 4_465 . . . ? O7 Eu1 O3 C8 136.1(6) 4_566 . . . ? O13 Eu1 O3 C8 94.2(6) . . . . ? O6 Eu1 O3 C8 -55.0(7) 4_566 . . . ? O1 Eu1 O3 C8 -52.3(6) . . . . ? Eu2 Eu1 O3 C8 -80.2(6) . . . . ? Eu2 Eu1 O3 C8 156.4(6) 4_565 . . . ? O3 Eu1 O5 C9 -86.0(16) . . . . ? O9 Eu1 O5 C9 9.4(17) . . . . ? O12 Eu1 O5 C9 -178.6(16) 4_465 . . . ? O7 Eu1 O5 C9 78.8(16) 4_566 . . . ? O13 Eu1 O5 C9 1.8(15) . . . . ? O6 Eu1 O5 C9 128.5(15) 4_566 . . . ? O1 Eu1 O5 C9 -140.9(15) . . . . ? Eu2 Eu1 O5 C9 170.3(15) . . . . ? Eu2 Eu1 O5 C9 79.9(15) 4_565 . . . ? O3 Eu1 O9 C17 45.0(6) . . . . ? O5 Eu1 O9 C17 -46.2(8) . . . . ? O12 Eu1 O9 C17 144.9(6) 4_465 . . . ? O7 Eu1 O9 C17 -110.4(6) 4_566 . . . ? O13 Eu1 O9 C17 -38.6(6) . . . . ? O6 Eu1 O9 C17 -177.4(6) 4_566 . . . ? O1 Eu1 O9 C17 111.1(6) . . . . ? Eu2 Eu1 O9 C17 151.7(6) . . . . ? Eu2 Eu1 O9 C17 -97.1(6) 4_565 . . . ? Eu2 O2 C1 O1 4.8(6) . . . . ? Eu2 O2 C1 C2 -178.1(4) . . . . ? Eu1 O1 C1 O2 -96.1(6) . . . . ? Eu2 O1 C1 O2 -4.3(5) . . . . ? Eu1 O1 C1 C2 87.1(6) . . . . ? Eu2 O1 C1 C2 178.8(5) . . . . ? Eu1 O1 C1 Eu2 -91.8(4) . . . . ? O10 Eu2 C1 O2 117.8(9) 1_455 . . . ? O4 Eu2 C1 O2 -32.2(4) 1_455 . . . ? O6 Eu2 C1 O2 -173.5(3) 4_566 . . . ? O12 Eu2 C1 O2 -105.2(4) 4_465 . . . ? O8 Eu2 C1 O2 44.1(4) 1_556 . . . ? O7 Eu2 C1 O2 92.2(3) 1_556 . . . ? O1 Eu2 C1 O2 175.5(5) . . . . ? C16 Eu2 C1 O2 65.2(3) 1_556 . . . ? O11 Eu2 C1 O2 -103.3(3) 4_465 . . . ? C24 Eu2 C1 O2 -96.8(4) 4_465 . . . ? O10 Eu2 C1 O1 -57.7(11) 1_455 . . . ? O4 Eu2 C1 O1 152.4(3) 1_455 . . . ? O6 Eu2 C1 O1 11.0(3) 4_566 . . . ? O2 Eu2 C1 O1 -175.5(5) . . . . ? O12 Eu2 C1 O1 79.3(3) 4_465 . . . ? O8 Eu2 C1 O1 -131.4(3) 1_556 . . . ? O7 Eu2 C1 O1 -83.3(3) 1_556 . . . ? C16 Eu2 C1 O1 -110.3(3) 1_556 . . . ? O11 Eu2 C1 O1 81.3(3) 4_465 . . . ? C24 Eu2 C1 O1 87.7(3) 4_465 . . . ? O10 Eu2 C1 C2 129(2) 1_455 . . . ? O4 Eu2 C1 C2 -21(2) 1_455 . . . ? O6 Eu2 C1 C2 -163(2) 4_566 . . . ? O2 Eu2 C1 C2 11(2) . . . . ? O12 Eu2 C1 C2 -95(2) 4_465 . . . ? O8 Eu2 C1 C2 55(2) 1_556 . . . ? O7 Eu2 C1 C2 103(2) 1_556 . . . ? O1 Eu2 C1 C2 -174(3) . . . . ? C16 Eu2 C1 C2 76(2) 1_556 . . . ? O11 Eu2 C1 C2 -93(2) 4_465 . . . ? C24 Eu2 C1 C2 -86(2) 4_465 . . . ? O2 C1 C2 C3 -29.9(8) . . . . ? O1 C1 C2 C3 147.1(6) . . . . ? Eu2 C1 C2 C3 -40(3) . . . . ? O2 C1 C2 C7 152.6(6) . . . . ? O1 C1 C2 C7 -30.4(9) . . . . ? Eu2 C1 C2 C7 143(2) . . . . ? C7 C2 C3 C4 -0.8(10) . . . . ? C1 C2 C3 C4 -178.6(7) . . . . ? C2 C3 C4 C5 0.3(12) . . . . ? C3 C4 C5 C6 0.7(12) . . . . ? C4 C5 C6 C7 -1.0(12) . . . . ? C5 C6 C7 C2 0.4(11) . . . . ? C5 C6 C7 C8 -177.1(7) . . . . ? C3 C2 C7 C6 0.5(9) . . . . ? C1 C2 C7 C6 178.0(6) . . . . ? C3 C2 C7 C8 177.8(6) . . . . ? C1 C2 C7 C8 -4.6(10) . . . . ? Eu2 O4 C8 O3 85.9(8) 1_655 . . . ? Eu2 O4 C8 C7 -97.6(7) 1_655 . . . ? Eu1 O3 C8 O4 -89.1(8) . . . . ? Eu1 O3 C8 C7 94.6(7) . . . . ? C6 C7 C8 O4 -30.8(8) . . . . ? C2 C7 C8 O4 151.7(6) . . . . ? C6 C7 C8 O3 145.7(6) . . . . ? C2 C7 C8 O3 -31.7(9) . . . . ? Eu1 O5 C9 O6 -68.6(17) . . . . ? Eu1 O5 C9 C10 114.4(15) . . . . ? Eu1 O5 C9 Eu2 -83.8(15) . . . 4_565 ? Eu2 O6 C9 O5 -23.2(7) 4_565 . . . ? Eu1 O6 C9 O5 112.2(5) 4_565 . . . ? Eu2 O6 C9 C10 153.8(4) 4_565 . . . ? Eu1 O6 C9 C10 -70.8(7) 4_565 . . . ? Eu1 O6 C9 Eu2 135.4(6) 4_565 . . 4_565 ? O5 C9 C10 C11 -11.5(9) . . . . ? O6 C9 C10 C11 171.5(6) . . . . ? Eu2 C9 C10 C11 -149.1(7) 4_565 . . . ? O5 C9 C10 C15 162.8(6) . . . . ? O6 C9 C10 C15 -14.2(9) . . . . ? Eu2 C9 C10 C15 25.1(12) 4_565 . . . ? C15 C10 C11 C12 0.3(11) . . . . ? C9 C10 C11 C12 174.7(7) . . . . ? C10 C11 C12 C13 -2.3(12) . . . . ? C11 C12 C13 C14 1.7(12) . . . . ? C12 C13 C14 C15 0.9(12) . . . . ? C13 C14 C15 C10 -2.9(10) . . . . ? C13 C14 C15 C16 175.5(7) . . . . ? C11 C10 C15 C14 2.3(10) . . . . ? C9 C10 C15 C14 -171.9(6) . . . . ? C11 C10 C15 C16 -175.9(6) . . . . ? C9 C10 C15 C16 9.9(10) . . . . ? Eu2 O8 C16 O7 22.0(6) 1_554 . . . ? Eu2 O8 C16 C15 -147.2(5) 1_554 . . . ? Eu1 O7 C16 O8 126.3(5) 4_565 . . . ? Eu2 O7 C16 O8 -21.3(6) 1_554 . . . ? Eu1 O7 C16 C15 -64.6(8) 4_565 . . . ? Eu2 O7 C16 C15 147.8(5) 1_554 . . . ? Eu1 O7 C16 Eu2 147.6(5) 4_565 . . 1_554 ? C14 C15 C16 O8 53.3(8) . . . . ? C10 C15 C16 O8 -128.5(7) . . . . ? C14 C15 C16 O7 -116.0(7) . . . . ? C10 C15 C16 O7 62.3(9) . . . . ? C14 C15 C16 Eu2 -26.6(12) . . . 1_554 ? C10 C15 C16 Eu2 151.7(7) . . . 1_554 ? Eu2 O10 C17 O9 99(9) 1_655 . . . ? Eu2 O10 C17 C18 -77(9) 1_655 . . . ? Eu1 O9 C17 O10 -42.0(9) . . . . ? Eu1 O9 C17 C18 133.4(5) . . . . ? O10 C17 C18 C19 115.7(7) . . . . ? O9 C17 C18 C19 -59.9(8) . . . . ? O10 C17 C18 C23 -58.3(8) . . . . ? O9 C17 C18 C23 126.1(6) . . . . ? C23 C18 C19 C20 -0.7(11) . . . . ? C17 C18 C19 C20 -174.8(7) . . . . ? C18 C19 C20 C21 1.4(12) . . . . ? C19 C20 C21 C22 -1.8(13) . . . . ? C20 C21 C22 C23 1.5(12) . . . . ? C21 C22 C23 C18 -0.8(10) . . . . ? C21 C22 C23 C24 -178.0(6) . . . . ? C19 C18 C23 C22 0.5(9) . . . . ? C17 C18 C23 C22 174.4(6) . . . . ? C19 C18 C23 C24 177.5(6) . . . . ? C17 C18 C23 C24 -8.6(9) . . . . ? Eu2 O11 C24 O12 30.4(5) 4_666 . . . ? Eu2 O11 C24 C23 -145.0(6) 4_666 . . . ? Eu1 O12 C24 O11 75.3(6) 4_666 . . . ? Eu2 O12 C24 O11 -36.6(6) 4_666 . . . ? Eu1 O12 C24 C23 -109.1(5) 4_666 . . . ? Eu2 O12 C24 C23 139.1(4) 4_666 . . . ? Eu1 O12 C24 Eu2 111.8(4) 4_666 . . 4_666 ? C22 C23 C24 O11 148.3(6) . . . . ? C18 C23 C24 O11 -28.7(9) . . . . ? C22 C23 C24 O12 -27.1(8) . . . . ? C18 C23 C24 O12 155.8(6) . . . . ? C22 C23 C24 Eu2 38.6(10) . . . 4_666 ? C18 C23 C24 Eu2 -138.5(6) . . . 4_666 ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 23.28 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.983 _refine_diff_density_min -1.095 _refine_diff_density_rms 0.149 #===END data_complex3 _database_code_CSD 184847 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H14 O13 Tb2' _chemical_formula_weight 828.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 '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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.024(5) _cell_length_b 26.656(16) _cell_length_c 11.743(7) _cell_angle_alpha 90.00 _cell_angle_beta 107.018(9) _cell_angle_gamma 90.00 _cell_volume 2402(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.290 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1568 _exptl_absorpt_coefficient_mu 5.914 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.2314 _exptl_absorpt_correction_T_max 0.5893 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9019 _diffrn_reflns_av_R_equivalents 0.0961 _diffrn_reflns_av_sigmaI/netI 0.0881 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 25.02 _reflns_number_total 4038 _reflns_number_gt 3475 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+170.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4038 _refine_ls_number_parameters 355 _refine_ls_number_restraints 62 _refine_ls_R_factor_all 0.1026 _refine_ls_R_factor_gt 0.0865 _refine_ls_wR_factor_ref 0.1740 _refine_ls_wR_factor_gt 0.1660 _refine_ls_goodness_of_fit_ref 1.135 _refine_ls_restrained_S_all 1.128 _refine_ls_shift/su_max 0.587 _refine_ls_shift/su_mean 0.014 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 0.41566(11) 0.22599(3) 0.84040(7) 0.0127(2) Uani 1 1 d . . . Tb2 Tb 0.09761(11) 0.19513(3) 1.01304(7) 0.0145(2) Uani 1 1 d . . . O1 O 0.4313(15) 0.1772(5) 1.0288(11) 0.019(3) Uani 1 1 d . . . O2 O 0.2579(18) 0.1173(5) 1.0505(12) 0.027(3) Uani 1 1 d . . . O3 O 0.5843(15) 0.1563(4) 0.8535(11) 0.018(3) Uani 1 1 d . . . O4 O 0.8722(16) 0.1420(5) 0.9273(11) 0.019(3) Uani 1 1 d U . . O5 O 0.308(2) 0.2013(5) 0.6409(11) 0.036(4) Uani 1 1 d . . . O6 O 0.2411(17) 0.2334(4) 0.4592(11) 0.020(3) Uani 1 1 d . . . O7 O 0.2649(16) 0.2026(5) 0.2332(10) 0.018(3) Uani 1 1 d U . . O8 O 0.0142(17) 0.1603(5) 0.1833(11) 0.025(3) Uani 1 1 d . . . O9 O 0.6107(18) 0.2726(5) 0.9839(12) 0.029(3) Uani 1 1 d . . . O10 O 0.8892(18) 0.2508(5) 1.0168(12) 0.029(3) Uani 1 1 d . . . O11 O 0.920(2) 0.2789(5) 1.2659(12) 0.031(3) Uani 1 1 d . . . O12 O 1.1630(15) 0.3249(5) 1.3266(10) 0.017(3) Uani 1 1 d U . . O13 O 0.6053(18) 0.2642(6) 0.7417(12) 0.029(3) Uani 1 1 d D . . C1 C 0.407(2) 0.1305(6) 1.0436(14) 0.009(3) Uani 1 1 d U . . C2 C 0.544(2) 0.0916(6) 1.0587(15) 0.017(4) Uani 1 1 d U . . C3 C 0.533(3) 0.0491(7) 1.1294(18) 0.026(4) Uani 1 1 d . . . H3A H 0.4401 0.0472 1.1614 0.031 Uiso 1 1 calc R . . C4 C 0.654(3) 0.0100(8) 1.154(2) 0.038(5) Uani 1 1 d . . . H4A H 0.6433 -0.0168 1.2015 0.045 Uiso 1 1 calc R . . C5 C 0.793(3) 0.0127(8) 1.102(2) 0.039(6) Uani 1 1 d . . . H5A H 0.8729 -0.0134 1.1154 0.047 Uiso 1 1 calc R . . C6 C 0.812(3) 0.0524(7) 1.034(2) 0.036(5) Uani 1 1 d . . . H6A H 0.9075 0.0536 1.0046 0.043 Uiso 1 1 calc R . . C7 C 0.686(3) 0.0926(6) 1.0082(17) 0.024(4) Uani 1 1 d . . . C8 C 0.715(2) 0.1338(7) 0.9251(16) 0.021(4) Uani 1 1 d U . . C9 C 0.287(2) 0.1955(6) 0.5316(15) 0.015(3) Uani 1 1 d U . . C10 C 0.299(2) 0.1441(7) 0.4794(16) 0.019(4) Uani 1 1 d . . . C11 C 0.374(3) 0.1065(6) 0.5662(17) 0.032(5) Uani 1 1 d . . . H11A H 0.4194 0.1145 0.6465 0.038 Uiso 1 1 calc R . . C12 C 0.377(4) 0.0565(10) 0.525(2) 0.056(8) Uani 1 1 d . . . H12A H 0.4332 0.0315 0.5778 0.067 Uiso 1 1 calc R . . C13 C 0.296(3) 0.0449(8) 0.407(2) 0.041(6) Uani 1 1 d . . . H13A H 0.2867 0.0115 0.3827 0.049 Uiso 1 1 calc R . . C14 C 0.229(3) 0.0821(8) 0.3227(17) 0.027(4) Uani 1 1 d . . . H14A H 0.1768 0.0737 0.2433 0.033 Uiso 1 1 calc R . . C15 C 0.240(3) 0.1323(7) 0.3591(17) 0.025(4) Uani 1 1 d . . . C16 C 0.161(3) 0.1693(7) 0.2556(16) 0.027(4) Uani 1 1 d . . . C17 C 0.776(2) 0.2850(6) 1.0175(13) 0.010(3) Uani 1 1 d U . . C18 C 0.826(2) 0.3369(7) 1.0418(16) 0.020(4) Uani 1 1 d U . . C19 C 0.764(3) 0.3732(7) 0.9516(19) 0.046(7) Uani 1 1 d . . . H19A H 0.6766 0.3644 0.8828 0.055 Uiso 1 1 calc R . . C20 C 0.830(3) 0.4220(9) 0.964(2) 0.036(5) Uiso 1 1 d . . . H20A H 0.7965 0.4448 0.9014 0.043 Uiso 1 1 calc R . . C21 C 0.950(3) 0.4357(8) 1.075(2) 0.039(6) Uani 1 1 d . . . H21A H 0.9905 0.4686 1.0868 0.047 Uiso 1 1 calc R . . C22 C 1.007(2) 0.4017(7) 1.1640(17) 0.024(4) Uani 1 1 d U . . H22A H 1.0846 0.4116 1.2361 0.029 Uiso 1 1 calc R . . C23 C 0.950(3) 0.3519(7) 1.1478(16) 0.022(4) Uani 1 1 d . . . C24 C 1.010(2) 0.3152(7) 1.2485(15) 0.019(4) Uani 1 1 d . . . H1 H 0.720(7) 0.253(6) 0.756(15) 0.00(4) Uiso 1 1 d D . . H2 H 0.526(15) 0.270(6) 0.667(7) 0.00(4) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tb1 0.0149(4) 0.0102(4) 0.0106(4) 0.0003(3) 0.0002(3) 0.0011(3) Tb2 0.0157(4) 0.0120(4) 0.0146(4) 0.0002(3) 0.0023(3) -0.0008(3) O1 0.016(7) 0.020(6) 0.017(6) -0.004(5) -0.003(5) -0.004(5) O2 0.034(8) 0.026(7) 0.022(7) 0.005(6) 0.008(6) 0.004(6) O3 0.013(6) 0.013(6) 0.026(7) 0.000(5) 0.005(5) 0.003(5) O4 0.018(4) 0.019(4) 0.020(4) -0.001(4) 0.006(3) -0.005(4) O5 0.065(11) 0.026(8) 0.011(6) -0.004(6) 0.000(6) 0.004(7) O6 0.026(7) 0.014(6) 0.024(7) 0.003(5) 0.011(5) 0.002(5) O7 0.024(5) 0.017(4) 0.013(4) -0.003(3) 0.003(3) -0.004(4) O8 0.022(7) 0.035(8) 0.011(6) -0.003(5) -0.008(5) -0.011(6) O9 0.033(8) 0.027(7) 0.023(7) -0.013(6) 0.002(6) -0.018(6) O10 0.027(8) 0.027(7) 0.032(8) -0.008(6) 0.006(6) -0.006(6) O11 0.053(10) 0.013(7) 0.024(7) 0.007(5) 0.008(6) -0.010(6) O12 0.013(4) 0.021(4) 0.017(4) 0.001(4) 0.003(3) -0.003(4) O13 0.022(8) 0.042(9) 0.019(7) 0.001(6) -0.001(5) -0.001(7) C1 0.007(5) 0.007(5) 0.011(5) 0.002(4) -0.001(4) 0.000(4) C2 0.019(5) 0.012(5) 0.018(5) -0.001(4) 0.004(4) -0.002(4) C3 0.023(11) 0.022(10) 0.036(11) 0.001(8) 0.014(8) 0.006(8) C4 0.064(16) 0.019(10) 0.034(12) 0.014(9) 0.020(11) 0.007(10) C5 0.044(14) 0.016(10) 0.049(14) 0.012(9) 0.000(11) 0.017(9) C6 0.029(12) 0.020(11) 0.050(14) 0.005(9) -0.002(10) 0.017(9) C7 0.028(11) 0.007(8) 0.026(10) 0.001(7) -0.008(8) 0.002(8) C8 0.021(6) 0.019(5) 0.023(5) -0.006(4) 0.004(4) 0.001(4) C9 0.015(5) 0.015(5) 0.013(5) -0.004(4) 0.003(4) -0.002(4) C10 0.018(10) 0.013(9) 0.023(9) -0.002(7) 0.003(7) -0.003(7) C11 0.067(16) 0.003(8) 0.017(9) -0.004(7) -0.002(9) 0.007(9) C12 0.08(2) 0.042(15) 0.050(16) 0.023(12) 0.029(14) 0.035(14) C13 0.057(16) 0.015(10) 0.055(15) -0.012(10) 0.023(12) -0.010(10) C14 0.036(12) 0.032(11) 0.021(10) -0.003(8) 0.018(8) 0.003(9) C15 0.039(12) 0.012(9) 0.020(10) 0.003(7) 0.005(8) -0.006(8) C16 0.044(13) 0.022(10) 0.012(9) 0.005(7) 0.003(8) -0.001(9) C17 0.010(5) 0.009(5) 0.007(5) -0.006(4) -0.001(4) 0.001(4) C18 0.020(6) 0.019(6) 0.023(5) 0.002(4) 0.009(4) 0.001(4) C19 0.061(16) 0.017(10) 0.030(12) -0.005(9) -0.032(11) 0.025(10) C21 0.049(15) 0.023(11) 0.039(13) 0.002(9) 0.001(11) 0.005(10) C22 0.024(6) 0.020(6) 0.025(6) -0.001(4) 0.001(4) -0.004(4) C23 0.031(11) 0.020(9) 0.018(9) -0.012(7) 0.014(8) -0.007(8) C24 0.020(10) 0.018(9) 0.014(8) 0.004(7) -0.004(7) 0.006(7) _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 O3 2.277(11) . ? Tb1 O9 2.300(12) . ? Tb1 O5 2.342(13) . ? Tb1 O7 2.405(12) 4_566 ? Tb1 O13 2.394(15) . ? Tb1 O12 2.405(12) 4_465 ? Tb1 O6 2.495(12) 4_566 ? Tb1 O1 2.538(13) . ? Tb1 Tb2 3.785(2) . ? Tb2 O10 2.246(14) 1_455 ? Tb2 O4 2.286(12) 1_455 ? Tb2 O6 2.405(12) 4_566 ? Tb2 O2 2.412(13) . ? Tb2 O12 2.455(12) 4_465 ? Tb2 O8 2.468(13) 1_556 ? Tb2 O7 2.548(11) 1_556 ? Tb2 O1 2.672(12) . ? Tb2 C16 2.828(18) 1_556 ? Tb2 O11 2.917(14) 4_465 ? Tb2 C1 2.955(16) . ? Tb2 C24 2.990(18) 4_465 ? O1 C1 1.28(2) . ? O2 C1 1.27(2) . ? O3 C8 1.29(2) . ? O4 C8 1.27(2) . ? O4 Tb2 2.286(12) 1_655 ? O5 C9 1.25(2) . ? O6 C9 1.30(2) . ? O6 Tb2 2.405(12) 4_565 ? O6 Tb1 2.495(12) 4_565 ? O7 C16 1.29(2) . ? O7 Tb1 2.405(12) 4_565 ? O7 Tb2 2.548(11) 1_554 ? O8 C16 1.26(2) . ? O8 Tb2 2.468(13) 1_554 ? O9 C17 1.31(2) . ? O10 C17 1.29(2) . ? O10 Tb2 2.246(14) 1_655 ? O11 C24 1.26(2) . ? O11 Tb2 2.917(14) 4_666 ? O12 C24 1.33(2) . ? O12 Tb1 2.405(12) 4_666 ? O12 Tb2 2.455(12) 4_666 ? C1 C2 1.48(2) . ? C2 C3 1.42(3) . ? C2 C7 1.43(3) . ? C3 C4 1.39(3) . ? C4 C5 1.42(3) . ? C5 C6 1.36(3) . ? C6 C7 1.44(3) . ? C7 C8 1.53(3) . ? C9 C10 1.51(2) . ? C10 C15 1.39(3) . ? C10 C11 1.43(3) . ? C11 C12 1.42(3) . ? C12 C13 1.39(4) . ? C13 C14 1.39(3) . ? C14 C15 1.40(3) . ? C15 C16 1.55(2) . ? C16 Tb2 2.828(18) 1_554 ? C17 C18 1.45(2) . ? C18 C23 1.40(3) . ? C18 C19 1.41(3) . ? C19 C20 1.40(3) . ? C20 C21 1.43(3) . ? C21 C22 1.36(3) . ? C22 C23 1.40(3) . ? C23 C24 1.50(3) . ? C24 Tb2 2.990(18) 4_666 ? 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 O3 Tb1 O9 97.3(5) . . ? O3 Tb1 O5 82.9(5) . . ? O9 Tb1 O5 149.1(6) . . ? O3 Tb1 O7 151.6(4) . 4_566 ? O9 Tb1 O7 94.9(5) . 4_566 ? O5 Tb1 O7 73.5(5) . 4_566 ? O3 Tb1 O13 86.0(5) . . ? O9 Tb1 O13 74.4(5) . . ? O5 Tb1 O13 74.8(5) . . ? O7 Tb1 O13 72.7(5) 4_566 . ? O3 Tb1 O12 91.0(4) . 4_465 ? O9 Tb1 O12 137.2(5) . 4_465 ? O5 Tb1 O12 73.5(5) . 4_465 ? O7 Tb1 O12 97.3(4) 4_566 4_465 ? O13 Tb1 O12 148.3(4) . 4_465 ? O3 Tb1 O6 137.4(4) . 4_566 ? O9 Tb1 O6 74.3(5) . 4_566 ? O5 Tb1 O6 125.3(5) . 4_566 ? O7 Tb1 O6 70.7(4) 4_566 4_566 ? O13 Tb1 O6 128.8(4) . 4_566 ? O12 Tb1 O6 71.5(4) 4_465 4_566 ? O3 Tb1 O1 69.3(4) . . ? O9 Tb1 O1 77.8(4) . . ? O5 Tb1 O1 129.6(5) . . ? O7 Tb1 O1 138.7(4) 4_566 . ? O13 Tb1 O1 139.8(4) . . ? O12 Tb1 O1 66.1(4) 4_465 . ? O6 Tb1 O1 68.2(4) 4_566 . ? O3 Tb1 Tb2 105.5(3) . . ? O9 Tb1 Tb2 98.4(4) . . ? O5 Tb1 Tb2 111.4(4) . . ? O7 Tb1 Tb2 97.9(3) 4_566 . ? O13 Tb1 Tb2 167.3(4) . . ? O12 Tb1 Tb2 39.3(3) 4_465 . ? O6 Tb1 Tb2 38.6(3) 4_566 . ? O1 Tb1 Tb2 44.8(3) . . ? O10 Tb2 O4 85.5(5) 1_455 1_455 ? O10 Tb2 O6 84.1(5) 1_455 4_566 ? O4 Tb2 O6 138.9(4) 1_455 4_566 ? O10 Tb2 O2 157.7(5) 1_455 . ? O4 Tb2 O2 81.9(5) 1_455 . ? O6 Tb2 O2 117.3(5) 4_566 . ? O10 Tb2 O12 121.1(5) 1_455 4_465 ? O4 Tb2 O12 79.7(4) 1_455 4_465 ? O6 Tb2 O12 72.2(4) 4_566 4_465 ? O2 Tb2 O12 74.6(4) . 4_465 ? O10 Tb2 O8 81.5(5) 1_455 1_556 ? O4 Tb2 O8 75.9(4) 1_455 1_556 ? O6 Tb2 O8 140.8(4) 4_566 1_556 ? O2 Tb2 O8 77.6(5) . 1_556 ? O12 Tb2 O8 145.1(4) 4_465 1_556 ? O10 Tb2 O7 95.9(4) 1_455 1_556 ? O4 Tb2 O7 127.5(4) 1_455 1_556 ? O6 Tb2 O7 93.1(4) 4_566 1_556 ? O2 Tb2 O7 77.7(4) . 1_556 ? O12 Tb2 O7 137.3(4) 4_465 1_556 ? O8 Tb2 O7 52.7(4) 1_556 1_556 ? O10 Tb2 O1 148.6(4) 1_455 . ? O4 Tb2 O1 124.6(4) 1_455 . ? O6 Tb2 O1 67.3(4) 4_566 . ? O2 Tb2 O1 50.5(4) . . ? O12 Tb2 O1 63.4(4) 4_465 . ? O8 Tb2 O1 112.3(4) 1_556 . ? O7 Tb2 O1 74.0(4) 1_556 . ? O10 Tb2 C16 93.3(6) 1_455 1_556 ? O4 Tb2 C16 100.3(5) 1_455 1_556 ? O6 Tb2 C16 119.9(5) 4_566 1_556 ? O2 Tb2 C16 71.2(5) . 1_556 ? O12 Tb2 C16 145.3(5) 4_465 1_556 ? O8 Tb2 C16 26.4(5) 1_556 1_556 ? O7 Tb2 C16 27.2(5) 1_556 1_556 ? O1 Tb2 C16 90.2(5) . 1_556 ? O10 Tb2 O11 73.3(4) 1_455 4_465 ? O4 Tb2 O11 67.4(4) 1_455 4_465 ? O6 Tb2 O11 71.5(4) 4_566 4_465 ? O2 Tb2 O11 117.7(4) . 4_465 ? O12 Tb2 O11 48.3(4) 4_465 4_465 ? O8 Tb2 O11 136.5(4) 1_556 4_465 ? O7 Tb2 O11 161.7(4) 1_556 4_465 ? O1 Tb2 O11 107.4(4) . 4_465 ? C16 Tb2 O11 162.1(5) 1_556 4_465 ? O10 Tb2 C1 170.5(5) 1_455 . ? O4 Tb2 C1 102.7(4) 1_455 . ? O6 Tb2 C1 92.6(4) 4_566 . ? O2 Tb2 C1 24.8(5) . . ? O12 Tb2 C1 65.8(4) 4_465 . ? O8 Tb2 C1 95.7(4) 1_556 . ? O7 Tb2 C1 75.4(4) 1_556 . ? O1 Tb2 C1 25.7(4) . . ? C16 Tb2 C1 80.7(5) 1_556 . ? O11 Tb2 C1 114.1(4) 4_465 . ? O10 Tb2 C24 97.5(5) 1_455 4_465 ? O4 Tb2 C24 64.5(5) 1_455 4_465 ? O6 Tb2 C24 77.6(4) 4_566 4_465 ? O2 Tb2 C24 93.5(5) . 4_465 ? O12 Tb2 C24 25.9(4) 4_465 4_465 ? O8 Tb2 C24 140.3(4) 1_556 4_465 ? O7 Tb2 C24 162.8(5) 1_556 4_465 ? O1 Tb2 C24 89.0(4) . 4_465 ? C16 Tb2 C24 160.4(5) 1_556 4_465 ? O11 Tb2 C24 24.6(4) 4_465 4_465 ? C1 Tb2 C24 90.4(5) . 4_465 ? C1 O1 Tb1 130.3(10) . . ? C1 O1 Tb2 89.6(9) . . ? Tb1 O1 Tb2 93.1(4) . . ? C1 O2 Tb2 102.3(10) . . ? C8 O3 Tb1 141.3(11) . . ? C8 O4 Tb2 140.1(11) . 1_655 ? C9 O5 Tb1 163.2(14) . . ? C9 O6 Tb2 120.6(10) . 4_565 ? C9 O6 Tb1 127.1(11) . 4_565 ? Tb2 O6 Tb1 101.1(4) 4_565 4_565 ? C16 O7 Tb1 133.7(11) . 4_565 ? C16 O7 Tb2 88.5(10) . 1_554 ? Tb1 O7 Tb2 128.9(5) 4_565 1_554 ? C16 O8 Tb2 92.9(11) . 1_554 ? C17 O9 Tb1 140.3(11) . . ? C17 O10 Tb2 176.5(12) . 1_655 ? C24 O11 Tb2 81.0(10) . 4_666 ? C24 O12 Tb1 122.0(11) . 4_666 ? C24 O12 Tb2 100.2(10) . 4_666 ? Tb1 O12 Tb2 102.3(4) 4_666 4_666 ? O2 C1 O1 117.5(15) . . ? O2 C1 C2 118.6(14) . . ? O1 C1 C2 123.8(15) . . ? O2 C1 Tb2 52.9(8) . . ? O1 C1 Tb2 64.7(8) . . ? C2 C1 Tb2 171.4(11) . . ? C3 C2 C7 116.6(16) . . ? C3 C2 C1 117.1(16) . . ? C7 C2 C1 126.3(15) . . ? C4 C3 C2 123.9(19) . . ? C3 C4 C5 117.5(18) . . ? C6 C5 C4 122(2) . . ? C5 C6 C7 120(2) . . ? C2 C7 C6 119.5(18) . . ? C2 C7 C8 124.5(16) . . ? C6 C7 C8 116.0(19) . . ? O4 C8 O3 123.3(18) . . ? O4 C8 C7 116.5(16) . . ? O3 C8 C7 120.0(16) . . ? O5 C9 O6 119.9(16) . . ? O5 C9 C10 121.4(16) . . ? O6 C9 C10 118.4(14) . . ? C15 C10 C11 120.9(16) . . ? C15 C10 C9 125.0(16) . . ? C11 C10 C9 114.1(15) . . ? C12 C11 C10 117.5(18) . . ? C13 C12 C11 120(2) . . ? C12 C13 C14 121(2) . . ? C13 C14 C15 119.3(19) . . ? C10 C15 C14 119.9(17) . . ? C10 C15 C16 126.5(17) . . ? C14 C15 C16 113.2(17) . . ? O8 C16 O7 121.6(16) . . ? O8 C16 C15 119.6(17) . . ? O7 C16 C15 117.3(17) . . ? O8 C16 Tb2 60.6(9) . 1_554 ? O7 C16 Tb2 64.3(9) . 1_554 ? C15 C16 Tb2 149.1(14) . 1_554 ? O10 C17 O9 118.4(14) . . ? O10 C17 C18 121.2(15) . . ? O9 C17 C18 120.1(15) . . ? C23 C18 C19 118.3(18) . . ? C23 C18 C17 122.1(16) . . ? C19 C18 C17 119.3(17) . . ? C20 C19 C18 121.3(19) . . ? C19 C20 C21 118(2) . . ? C22 C21 C20 121(2) . . ? C21 C22 C23 120.4(19) . . ? C22 C23 C18 120.6(18) . . ? C22 C23 C24 119.6(16) . . ? C18 C23 C24 119.6(16) . . ? O11 C24 O12 119.7(15) . . ? O11 C24 C23 124.3(16) . . ? O12 C24 C23 115.9(16) . . ? O11 C24 Tb2 74.5(10) . 4_666 ? O12 C24 Tb2 53.9(8) . 4_666 ? C23 C24 Tb2 143.4(12) . 4_666 ? 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 -49.7(13) . . . . ? O9 Tb1 O1 C1 -152.5(14) . . . . ? O5 Tb1 O1 C1 11.4(16) . . . . ? O7 Tb1 O1 C1 124.0(13) 4_566 . . . ? O13 Tb1 O1 C1 -105.4(14) . . . . ? O12 Tb1 O1 C1 51.1(13) 4_465 . . . ? O6 Tb1 O1 C1 129.8(14) 4_566 . . . ? Tb2 Tb1 O1 C1 92.1(14) . . . . ? O3 Tb1 O1 Tb2 -141.8(5) . . . . ? O9 Tb1 O1 Tb2 115.4(5) . . . . ? O5 Tb1 O1 Tb2 -80.7(7) . . . . ? O7 Tb1 O1 Tb2 31.9(7) 4_566 . . . ? O13 Tb1 O1 Tb2 162.5(6) . . . . ? O12 Tb1 O1 Tb2 -41.0(4) 4_465 . . . ? O6 Tb1 O1 Tb2 37.7(4) 4_566 . . . ? O10 Tb2 O1 C1 164.2(10) 1_455 . . . ? O4 Tb2 O1 C1 -35.3(11) 1_455 . . . ? O6 Tb2 O1 C1 -170.0(10) 4_566 . . . ? O2 Tb2 O1 C1 2.4(9) . . . . ? O12 Tb2 O1 C1 -89.2(9) 4_465 . . . ? O8 Tb2 O1 C1 52.6(10) 1_556 . . . ? O7 Tb2 O1 C1 89.5(9) 1_556 . . . ? C16 Tb2 O1 C1 67.4(10) 1_556 . . . ? O11 Tb2 O1 C1 -109.5(9) 4_465 . . . ? C24 Tb2 O1 C1 -93.0(9) 4_465 . . . ? O10 Tb2 O1 Tb1 -65.5(9) 1_455 . . . ? O4 Tb2 O1 Tb1 95.0(5) 1_455 . . . ? O6 Tb2 O1 Tb1 -39.6(4) 4_566 . . . ? O2 Tb2 O1 Tb1 132.7(6) . . . . ? O12 Tb2 O1 Tb1 41.1(4) 4_465 . . . ? O8 Tb2 O1 Tb1 -177.1(4) 1_556 . . . ? O7 Tb2 O1 Tb1 -140.1(4) 1_556 . . . ? C16 Tb2 O1 Tb1 -162.2(5) 1_556 . . . ? O11 Tb2 O1 Tb1 20.8(4) 4_465 . . . ? C1 Tb2 O1 Tb1 130.3(10) . . . . ? C24 Tb2 O1 Tb1 37.3(4) 4_465 . . . ? O10 Tb2 O2 C1 -157.0(12) 1_455 . . . ? O4 Tb2 O2 C1 147.0(11) 1_455 . . . ? O6 Tb2 O2 C1 5.5(12) 4_566 . . . ? O12 Tb2 O2 C1 65.5(10) 4_465 . . . ? O8 Tb2 O2 C1 -135.8(11) 1_556 . . . ? O7 Tb2 O2 C1 -81.7(10) 1_556 . . . ? O1 Tb2 O2 C1 -2.5(9) . . . . ? C16 Tb2 O2 C1 -109.1(11) 1_556 . . . ? O11 Tb2 O2 C1 87.8(11) 4_465 . . . ? C24 Tb2 O2 C1 83.4(11) 4_465 . . . ? O9 Tb1 O3 C8 21(2) . . . . ? O5 Tb1 O3 C8 170(2) . . . . ? O7 Tb1 O3 C8 136.1(19) 4_566 . . . ? O13 Tb1 O3 C8 94.9(19) . . . . ? O12 Tb1 O3 C8 -116.7(19) 4_465 . . . ? O6 Tb1 O3 C8 -53(2) 4_566 . . . ? O1 Tb1 O3 C8 -52.7(19) . . . . ? Tb2 Tb1 O3 C8 -79.6(19) . . . . ? O3 Tb1 O5 C9 -87(5) . . . . ? O9 Tb1 O5 C9 6(5) . . . . ? O7 Tb1 O5 C9 77(4) 4_566 . . . ? O13 Tb1 O5 C9 1(4) . . . . ? O12 Tb1 O5 C9 -180(100) 4_465 . . . ? O6 Tb1 O5 C9 128(4) 4_566 . . . ? O1 Tb1 O5 C9 -142(4) . . . . ? Tb2 Tb1 O5 C9 169(4) . . . . ? O3 Tb1 O9 C17 45.9(18) . . . . ? O5 Tb1 O9 C17 -43(2) . . . . ? O7 Tb1 O9 C17 -108.5(18) 4_566 . . . ? O13 Tb1 O9 C17 -37.9(17) . . . . ? O12 Tb1 O9 C17 145.3(16) 4_465 . . . ? O6 Tb1 O9 C17 -176.8(19) 4_566 . . . ? O1 Tb1 O9 C17 112.7(18) . . . . ? Tb2 Tb1 O9 C17 152.8(17) . . . . ? Tb2 O2 C1 O1 4.5(16) . . . . ? Tb2 O2 C1 C2 -178.3(12) . . . . ? Tb1 O1 C1 O2 -97.7(17) . . . . ? Tb2 O1 C1 O2 -3.9(14) . . . . ? Tb1 O1 C1 C2 85.2(18) . . . . ? Tb2 O1 C1 C2 179.0(14) . . . . ? Tb1 O1 C1 Tb2 -93.8(10) . . . . ? O10 Tb2 C1 O2 116(3) 1_455 . . . ? O4 Tb2 C1 O2 -33.6(11) 1_455 . . . ? O6 Tb2 C1 O2 -175.1(10) 4_566 . . . ? O12 Tb2 C1 O2 -105.9(11) 4_465 . . . ? O8 Tb2 C1 O2 43.2(10) 1_556 . . . ? O7 Tb2 C1 O2 92.3(10) 1_556 . . . ? O1 Tb2 C1 O2 175.6(16) . . . . ? C16 Tb2 C1 O2 65.0(11) 1_556 . . . ? O11 Tb2 C1 O2 -104.3(10) 4_465 . . . ? C24 Tb2 C1 O2 -97.5(11) 4_465 . . . ? O10 Tb2 C1 O1 -60(3) 1_455 . . . ? O4 Tb2 C1 O1 150.8(9) 1_455 . . . ? O6 Tb2 C1 O1 9.2(9) 4_566 . . . ? O2 Tb2 C1 O1 -175.6(16) . . . . ? O12 Tb2 C1 O1 78.4(9) 4_465 . . . ? O8 Tb2 C1 O1 -132.4(9) 1_556 . . . ? O7 Tb2 C1 O1 -83.3(9) 1_556 . . . ? C16 Tb2 C1 O1 -110.6(10) 1_556 . . . ? O11 Tb2 C1 O1 80.1(9) 4_465 . . . ? C24 Tb2 C1 O1 86.9(9) 4_465 . . . ? O10 Tb2 C1 C2 126(7) 1_455 . . . ? O4 Tb2 C1 C2 -24(7) 1_455 . . . ? O6 Tb2 C1 C2 -165(7) 4_566 . . . ? O2 Tb2 C1 C2 10(7) . . . . ? O12 Tb2 C1 C2 -96(7) 4_465 . . . ? O8 Tb2 C1 C2 53(7) 1_556 . . . ? O7 Tb2 C1 C2 102(7) 1_556 . . . ? O1 Tb2 C1 C2 -174(8) . . . . ? C16 Tb2 C1 C2 75(7) 1_556 . . . ? O11 Tb2 C1 C2 -94(7) 4_465 . . . ? C24 Tb2 C1 C2 -88(7) 4_465 . . . ? O2 C1 C2 C3 -27(2) . . . . ? O1 C1 C2 C3 149.7(17) . . . . ? Tb2 C1 C2 C3 -36(8) . . . . ? O2 C1 C2 C7 152.2(17) . . . . ? O1 C1 C2 C7 -31(3) . . . . ? Tb2 C1 C2 C7 143(7) . . . . ? C7 C2 C3 C4 2(3) . . . . ? C1 C2 C3 C4 -178.7(19) . . . . ? C2 C3 C4 C5 -1(3) . . . . ? C3 C4 C5 C6 2(4) . . . . ? C4 C5 C6 C7 -3(4) . . . . ? C3 C2 C7 C6 -2(3) . . . . ? C1 C2 C7 C6 178.1(17) . . . . ? C3 C2 C7 C8 177.1(17) . . . . ? C1 C2 C7 C8 -3(3) . . . . ? C5 C6 C7 C2 3(3) . . . . ? C5 C6 C7 C8 -177(2) . . . . ? Tb2 O4 C8 O3 87(2) 1_655 . . . ? Tb2 O4 C8 C7 -97(2) 1_655 . . . ? Tb1 O3 C8 O4 -90(2) . . . . ? Tb1 O3 C8 C7 94(2) . . . . ? C2 C7 C8 O4 151.3(17) . . . . ? C6 C7 C8 O4 -29(2) . . . . ? C2 C7 C8 O3 -32(3) . . . . ? C6 C7 C8 O3 147.1(18) . . . . ? Tb1 O5 C9 O6 -69(5) . . . . ? Tb1 O5 C9 C10 117(4) . . . . ? Tb2 O6 C9 O5 -22(2) 4_565 . . . ? Tb1 O6 C9 O5 114.8(17) 4_565 . . . ? Tb2 O6 C9 C10 152.6(12) 4_565 . . . ? Tb1 O6 C9 C10 -70.6(19) 4_565 . . . ? O5 C9 C10 C15 164(2) . . . . ? O6 C9 C10 C15 -10(3) . . . . ? O5 C9 C10 C11 -14(3) . . . . ? O6 C9 C10 C11 171.4(18) . . . . ? C15 C10 C11 C12 -3(3) . . . . ? C9 C10 C11 C12 175(2) . . . . ? C10 C11 C12 C13 -5(4) . . . . ? C11 C12 C13 C14 8(4) . . . . ? C12 C13 C14 C15 -1(4) . . . . ? C11 C10 C15 C14 10(3) . . . . ? C9 C10 C15 C14 -168.5(18) . . . . ? C11 C10 C15 C16 -178(2) . . . . ? C9 C10 C15 C16 4(3) . . . . ? C13 C14 C15 C10 -7(3) . . . . ? C13 C14 C15 C16 179(2) . . . . ? Tb2 O8 C16 O7 21(2) 1_554 . . . ? Tb2 O8 C16 C15 -144.3(17) 1_554 . . . ? Tb1 O7 C16 O8 127.0(17) 4_565 . . . ? Tb2 O7 C16 O8 -20.6(19) 1_554 . . . ? Tb1 O7 C16 C15 -67(2) 4_565 . . . ? Tb2 O7 C16 C15 145.4(16) 1_554 . . . ? Tb1 O7 C16 Tb2 147.6(15) 4_565 . . 1_554 ? C10 C15 C16 O8 -126(2) . . . . ? C14 C15 C16 O8 47(3) . . . . ? C10 C15 C16 O7 68(3) . . . . ? C14 C15 C16 O7 -119(2) . . . . ? C10 C15 C16 Tb2 153(2) . . . 1_554 ? C14 C15 C16 Tb2 -35(4) . . . 1_554 ? Tb2 O10 C17 O9 149(19) 1_655 . . . ? Tb2 O10 C17 C18 -24(20) 1_655 . . . ? Tb1 O9 C17 O10 -42(3) . . . . ? Tb1 O9 C17 C18 131.6(16) . . . . ? O10 C17 C18 C23 -58(2) . . . . ? O9 C17 C18 C23 129.2(18) . . . . ? O10 C17 C18 C19 115(2) . . . . ? O9 C17 C18 C19 -58(3) . . . . ? C23 C18 C19 C20 4(4) . . . . ? C17 C18 C19 C20 -170(2) . . . . ? C18 C19 C20 C21 -6(4) . . . . ? C19 C20 C21 C22 4(4) . . . . ? C20 C21 C22 C23 1(4) . . . . ? C21 C22 C23 C18 -3(3) . . . . ? C21 C22 C23 C24 -178(2) . . . . ? C19 C18 C23 C22 1(3) . . . . ? C17 C18 C23 C22 174.3(17) . . . . ? C19 C18 C23 C24 176(2) . . . . ? C17 C18 C23 C24 -11(3) . . . . ? Tb2 O11 C24 O12 30.5(15) 4_666 . . . ? Tb2 O11 C24 C23 -145.0(18) 4_666 . . . ? Tb1 O12 C24 O11 74(2) 4_666 . . . ? Tb2 O12 C24 O11 -37.2(18) 4_666 . . . ? Tb1 O12 C24 C23 -109.8(15) 4_666 . . . ? Tb2 O12 C24 C23 138.6(14) 4_666 . . . ? Tb1 O12 C24 Tb2 111.6(10) 4_666 . . 4_666 ? C22 C23 C24 O11 148.3(19) . . . . ? C18 C23 C24 O11 -27(3) . . . . ? C22 C23 C24 O12 -27(3) . . . . ? C18 C23 C24 O12 157.7(17) . . . . ? C22 C23 C24 Tb2 36(3) . . . 4_666 ? C18 C23 C24 Tb2 -138.7(18) . . . 4_666 ? _diffrn_measured_fraction_theta_max 0.950 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.950 _refine_diff_density_max 2.014 _refine_diff_density_min -4.325 _refine_diff_density_rms 0.348 #===END