Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Srinivasan Natarajan' _publ_contact_author_address ; Solid State and Structural Chemistry Unit Indian Institute of Science C.V. Raman Avenue Bangalore 560 012 INDIA ; _publ_contact_author_email SNATARAJAN@SSCU.IISC.ERNET.IN _publ_section_title ; Synthesis, Structure and Optical Properties of Rare-Earth Benzene Carboxylates ; loop_ _publ_author_name 'Srinivasan Natarajan' 'Partha Mahata' 'K V Ramya' data_Compound(I) _database_code_depnum_ccdc_archive 'CCDC 641732' #======================================================== _chemical_name_systematic ; ? ; _chemical_name_common 'Lanthanum carboxylate' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H22 La2 O18' _chemical_formula_weight 972.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.3780(19) _cell_length_b 14.177(3) _cell_length_c 21.525(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.710(3) _cell_angle_gamma 90.00 _cell_volume 3151.3(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7432 _cell_measurement_theta_min 1.72 _cell_measurement_theta_max 28.00 _exptl_crystal_description 'Block type' _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.049 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1888 _exptl_absorpt_coefficient_mu 2.763 _exptl_absorpt_correction_type 'multi -scan' _exptl_absorpt_correction_T_min 0.6361 _exptl_absorpt_correction_T_max 0.7697 _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _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 'Bruker SMART CCD area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26976 _diffrn_reflns_av_R_equivalents 0.0395 _diffrn_reflns_av_sigmaI/netI 0.0427 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 28.00 _reflns_number_total 7432 _reflns_number_gt 6266 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement 'SAINT (Bruker, 2000)' _computing_data_reduction SAINT _computing_structure_solution 'SIR92 (Altomare et al., 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1999) and CAMERON (Watkin et al., 1993)' _computing_publication_material 'PLATON (Spek, 2003)' _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^)+(0.0229P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7432 _refine_ls_number_parameters 485 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0430 _refine_ls_R_factor_gt 0.0309 _refine_ls_wR_factor_ref 0.0591 _refine_ls_wR_factor_gt 0.0559 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group La1 La 0.142414(17) 0.304683(12) 0.261304(8) 0.01381(5) Uani 1 1 d . . . La2 La 0.065228(18) 0.567115(12) 0.310657(8) 0.01420(5) Uani 1 1 d . . . O1 O -0.0053(2) 0.27593(15) 0.35365(10) 0.0222(5) Uani 1 1 d . . . O2 O -0.0444(2) 0.40814(15) 0.30231(10) 0.0184(5) Uani 1 1 d . . . O3 O 0.2216(2) 0.41837(15) 0.34889(10) 0.0214(5) Uani 1 1 d . . . O4 O 0.1226(2) 0.46489(15) 0.21613(10) 0.0193(5) Uani 1 1 d . . . O5 O 0.0694(2) -0.24271(15) 0.30421(10) 0.0205(5) Uani 1 1 d . . . O6 O 0.2110(2) 0.25559(17) 0.66334(11) 0.0295(6) Uani 1 1 d . . . O7 O 0.3756(3) 0.3569(2) 0.25184(15) 0.0385(7) Uani 1 1 d D . . O8 O 0.1048(2) 0.11419(15) 0.27346(10) 0.0201(5) Uani 1 1 d . . . O9 O 0.2816(2) 0.18320(15) 0.31617(12) 0.0298(6) Uani 1 1 d . . . O10 O 0.1245(3) 0.50129(17) 0.41694(11) 0.0320(6) Uani 1 1 d . . . O11 O 0.2062(2) 0.60720(16) 0.22060(11) 0.0269(6) Uani 1 1 d . . . O12 O 0.2351(2) -0.31620(15) 0.35510(11) 0.0237(5) Uani 1 1 d . . . O13 O 0.1049(2) 0.38532(17) 0.63121(11) 0.0313(6) Uani 1 1 d . . . C1 C 0.1766(3) 0.5347(2) 0.19034(15) 0.0173(7) Uani 1 1 d . . . C2 C 0.1947(3) 0.5266(2) 0.12298(15) 0.0183(7) Uani 1 1 d . . . C3 C 0.1349(3) 0.4541(2) 0.08752(16) 0.0216(7) Uani 1 1 d . . . H3 H 0.0872 0.4089 0.1066 0.026 Uiso 1 1 calc R . . C4 C 0.1458(3) 0.4485(2) 0.02402(16) 0.0224(8) Uani 1 1 d . . . C5 C 0.2195(4) 0.5148(3) -0.00367(17) 0.0304(9) Uani 1 1 d . . . H5 H 0.2283 0.5107 -0.0462 0.036 Uiso 1 1 calc R . . C6 C 0.2801(4) 0.5867(3) 0.03085(17) 0.0325(9) Uani 1 1 d . . . H6 H 0.3301 0.6305 0.0119 0.039 Uiso 1 1 calc R . . C7 C 0.2661(3) 0.5935(2) 0.09413(16) 0.0247(8) Uani 1 1 d . . . H7 H 0.3047 0.6431 0.1173 0.030 Uiso 1 1 calc R . . C8 C 0.0738(3) 0.3712(2) -0.01105(17) 0.0264(8) Uani 1 1 d . . . O21 O 0.0066(3) 0.31530(18) 0.01259(12) 0.0373(7) Uani 1 1 d . . . O22 O 0.0899(3) 0.37082(18) -0.07179(11) 0.0370(7) Uani 1 1 d . . . H22 H 0.0485 0.3272 -0.0890 0.056 Uiso 1 1 calc R . . C11 C -0.0727(3) 0.3488(2) 0.34379(15) 0.0176(7) Uani 1 1 d . . . C12 C -0.1854(3) 0.3710(2) 0.37926(16) 0.0207(7) Uani 1 1 d . . . C13 C -0.2822(3) 0.4308(2) 0.35323(16) 0.0239(8) Uani 1 1 d . . . H13 H -0.2794 0.4535 0.3128 0.029 Uiso 1 1 calc R . . C14 C -0.3829(3) 0.4569(2) 0.38752(16) 0.0233(8) Uani 1 1 d . . . C15 C -0.3867(4) 0.4225(2) 0.44778(17) 0.0289(8) Uani 1 1 d . . . H15 H -0.4536 0.4404 0.4710 0.035 Uiso 1 1 calc R . . C16 C -0.2913(4) 0.3616(3) 0.47336(18) 0.0323(9) Uani 1 1 d . . . H16 H -0.2946 0.3381 0.5135 0.039 Uiso 1 1 calc R . . C17 C -0.1910(3) 0.3359(2) 0.43902(17) 0.0275(8) Uani 1 1 d . . . H17 H -0.1270 0.2949 0.4561 0.033 Uiso 1 1 calc R . . C18 C -0.4821(4) 0.5237(3) 0.35891(19) 0.0308(9) Uani 1 1 d . . . O31 O -0.5481(2) 0.56754(17) 0.39981(12) 0.0375(7) Uani 1 1 d . . . H31 H -0.6011 0.6032 0.3813 0.056 Uiso 1 1 calc R . . O32 O -0.5027(3) 0.5355(2) 0.30320(14) 0.0520(8) Uani 1 1 d . . . C21 C 0.1940(3) 0.4334(2) 0.40499(15) 0.0174(7) Uani 1 1 d . . . C22 C 0.2444(3) 0.3689(2) 0.45641(14) 0.0162(7) Uani 1 1 d . . . C23 C 0.3356(3) 0.2990(2) 0.44672(16) 0.0219(7) Uani 1 1 d . . . H23 H 0.3677 0.2933 0.4081 0.026 Uiso 1 1 calc R . . C24 C 0.3775(3) 0.2387(2) 0.49483(16) 0.0264(8) Uani 1 1 d . . . H24 H 0.4388 0.1926 0.4888 0.032 Uiso 1 1 calc R . . C25 C 0.3289(3) 0.2466(2) 0.55182(16) 0.0230(8) Uani 1 1 d . . . H25 H 0.3574 0.2054 0.5839 0.028 Uiso 1 1 calc R . . C26 C 0.2387(3) 0.3147(2) 0.56202(15) 0.0183(7) Uani 1 1 d . . . C27 C 0.1975(3) 0.3767(2) 0.51437(15) 0.0178(7) Uani 1 1 d . . . H27 H 0.1382 0.4238 0.5213 0.021 Uiso 1 1 calc R . . C28 C 0.1809(3) 0.3189(2) 0.62310(16) 0.0218(7) Uani 1 1 d . . . C31 C 0.2153(3) 0.1101(2) 0.30496(15) 0.0189(7) Uani 1 1 d . . . C32 C 0.2701(3) 0.0179(2) 0.32789(15) 0.0172(7) Uani 1 1 d . . . C33 C 0.3973(3) 0.0153(2) 0.35438(18) 0.0299(9) Uani 1 1 d . . . H33 H 0.4458 0.0706 0.3579 0.036 Uiso 1 1 calc R . . C34 C 0.4527(4) -0.0689(2) 0.3757(2) 0.0416(11) Uani 1 1 d . . . H34 H 0.5378 -0.0702 0.3938 0.050 Uiso 1 1 calc R . . C35 C 0.3811(3) -0.1509(2) 0.36992(19) 0.0339(10) Uani 1 1 d . . . H35 H 0.4185 -0.2074 0.3843 0.041 Uiso 1 1 calc R . . C36 C 0.2544(3) -0.1502(2) 0.34308(15) 0.0183(7) Uani 1 1 d . . . C37 C 0.1983(3) -0.0648(2) 0.32274(14) 0.0173(7) Uani 1 1 d . . . H37 H 0.1124 -0.0633 0.3057 0.021 Uiso 1 1 calc R . . C38 C 0.1815(3) -0.2411(2) 0.33364(14) 0.0167(7) Uani 1 1 d . . . O100 O 0.5545(4) 0.2171(3) 0.2636(2) 0.0746(12) Uani 1 1 d D . . H51 H 0.429(4) 0.312(3) 0.251(3) 0.11(2) Uiso 1 1 d D . . H52 H 0.409(4) 0.4090(17) 0.264(2) 0.068(16) Uiso 1 1 d D . . H102 H 0.6319(18) 0.198(3) 0.269(2) 0.076(19) Uiso 1 1 d D . . H101 H 0.526(5) 0.171(3) 0.242(2) 0.10(2) 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 0.01788(10) 0.01023(9) 0.01329(10) -0.00097(7) 0.00146(7) 0.00027(7) La2 0.01896(10) 0.01015(9) 0.01340(10) 0.00052(7) 0.00118(7) 0.00102(7) O1 0.0256(13) 0.0181(12) 0.0241(13) 0.0048(10) 0.0084(10) 0.0049(10) O2 0.0193(12) 0.0179(12) 0.0182(12) 0.0021(9) 0.0031(10) -0.0011(9) O3 0.0267(13) 0.0262(13) 0.0112(12) 0.0000(10) 0.0020(10) -0.0028(10) O4 0.0260(13) 0.0146(11) 0.0181(12) 0.0014(9) 0.0059(10) -0.0014(10) O5 0.0191(12) 0.0170(12) 0.0242(13) 0.0006(10) -0.0041(10) -0.0016(9) O6 0.0357(15) 0.0311(14) 0.0228(14) 0.0118(11) 0.0094(12) 0.0079(12) O7 0.0258(15) 0.0349(17) 0.056(2) -0.0174(15) 0.0099(14) -0.0068(14) O8 0.0230(13) 0.0157(12) 0.0204(13) 0.0023(10) -0.0040(10) 0.0014(10) O9 0.0320(14) 0.0132(12) 0.0412(16) 0.0048(11) -0.0122(12) -0.0035(10) O10 0.0490(17) 0.0279(14) 0.0191(13) 0.0044(11) 0.0026(12) 0.0175(12) O11 0.0371(15) 0.0240(13) 0.0211(13) -0.0080(11) 0.0103(11) -0.0130(11) O12 0.0241(13) 0.0127(11) 0.0323(14) 0.0022(10) -0.0075(11) 0.0003(10) O13 0.0427(16) 0.0293(14) 0.0246(14) 0.0075(11) 0.0166(12) 0.0137(12) C1 0.0175(16) 0.0184(16) 0.0157(17) 0.0047(14) 0.0014(14) 0.0005(13) C2 0.0198(17) 0.0188(17) 0.0168(17) 0.0023(13) 0.0042(14) 0.0014(13) C3 0.0244(18) 0.0180(17) 0.0227(19) 0.0008(14) 0.0035(15) 0.0013(14) C4 0.0243(18) 0.0217(18) 0.0213(18) -0.0012(15) 0.0024(15) 0.0024(14) C5 0.038(2) 0.035(2) 0.0177(19) -0.0012(16) 0.0049(17) -0.0019(18) C6 0.042(2) 0.035(2) 0.022(2) 0.0035(17) 0.0083(18) -0.0121(18) C7 0.031(2) 0.0210(18) 0.0229(19) 0.0006(15) 0.0044(16) -0.0059(15) C8 0.029(2) 0.0217(19) 0.027(2) -0.0026(16) -0.0037(17) 0.0036(16) O21 0.0462(17) 0.0332(15) 0.0318(16) -0.0065(12) 0.0006(13) -0.0102(13) O22 0.0494(18) 0.0362(16) 0.0250(15) -0.0123(12) 0.0013(13) -0.0051(13) C11 0.0201(17) 0.0160(16) 0.0163(17) 0.0004(13) -0.0006(14) -0.0042(13) C12 0.0205(17) 0.0194(17) 0.0229(19) 0.0005(14) 0.0050(15) -0.0037(14) C13 0.0258(19) 0.0232(18) 0.0229(19) 0.0011(15) 0.0040(15) 0.0000(15) C14 0.0189(17) 0.0223(18) 0.029(2) -0.0030(15) 0.0018(15) 0.0009(14) C15 0.027(2) 0.030(2) 0.032(2) -0.0029(17) 0.0126(17) 0.0007(16) C16 0.040(2) 0.034(2) 0.025(2) 0.0044(17) 0.0123(18) 0.0048(18) C17 0.030(2) 0.0231(19) 0.030(2) 0.0057(16) 0.0060(17) 0.0045(15) C18 0.027(2) 0.028(2) 0.037(2) -0.0020(18) 0.0013(18) -0.0007(16) O31 0.0292(15) 0.0411(17) 0.0422(17) -0.0051(13) 0.0039(13) 0.0163(13) O32 0.059(2) 0.058(2) 0.0383(19) 0.0058(15) 0.0037(16) 0.0241(17) C21 0.0188(16) 0.0179(17) 0.0147(17) 0.0009(14) -0.0018(13) -0.0024(13) C22 0.0179(16) 0.0151(16) 0.0157(17) 0.0013(13) 0.0010(13) 0.0004(13) C23 0.0238(18) 0.0250(18) 0.0173(18) -0.0029(14) 0.0046(14) -0.0008(14) C24 0.0207(19) 0.0272(19) 0.031(2) 0.0009(16) 0.0024(16) 0.0100(15) C25 0.0216(18) 0.0204(18) 0.026(2) 0.0057(15) -0.0004(15) 0.0060(14) C26 0.0191(17) 0.0169(16) 0.0187(17) 0.0013(14) 0.0008(14) 0.0017(13) C27 0.0201(17) 0.0154(16) 0.0184(17) 0.0004(13) 0.0053(14) 0.0036(13) C28 0.0219(18) 0.0230(18) 0.0205(18) 0.0046(15) 0.0030(14) 0.0001(14) C31 0.0221(18) 0.0188(17) 0.0157(17) 0.0004(14) 0.0008(14) 0.0013(14) C32 0.0187(17) 0.0157(16) 0.0171(17) -0.0008(13) 0.0014(14) 0.0026(13) C33 0.0210(19) 0.0193(18) 0.048(3) 0.0017(17) -0.0041(17) -0.0051(15) C34 0.022(2) 0.024(2) 0.074(3) 0.005(2) -0.018(2) -0.0005(16) C35 0.029(2) 0.0141(18) 0.056(3) 0.0058(17) -0.0125(19) 0.0016(15) C36 0.0181(17) 0.0129(16) 0.0236(19) 0.0013(13) -0.0001(14) 0.0007(13) C37 0.0184(16) 0.0176(16) 0.0150(17) -0.0013(13) -0.0024(13) 0.0007(13) C38 0.0225(17) 0.0141(16) 0.0139(16) -0.0010(13) 0.0032(14) 0.0006(13) O100 0.045(2) 0.049(2) 0.128(4) -0.009(2) 0.002(2) 0.0149(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag La1 O6 2.446(2) 4_565 ? La1 O4 2.471(2) . ? La1 O9 2.472(2) . ? La1 O3 2.553(2) . ? La1 O7 2.558(3) . ? La1 O5 2.580(2) 2 ? La1 O2 2.651(2) . ? La1 O1 2.659(2) . ? La1 O8 2.745(2) . ? La1 C31 2.987(3) . ? La1 C11 3.052(3) . ? La1 La2 3.9727(7) . ? La2 O13 2.361(2) 3_566 ? La2 O8 2.490(2) 2 ? La2 O10 2.491(2) . ? La2 O2 2.523(2) . ? La2 O12 2.535(2) 1_565 ? La2 O11 2.605(2) . ? La2 O4 2.615(2) . ? La2 O5 2.700(2) 1_565 ? La2 O3 2.737(2) . ? La2 C1 2.975(3) . ? La2 C21 2.994(3) . ? La2 C38 2.996(3) 1_565 ? O1 C11 1.254(4) . ? O2 C11 1.282(4) . ? O3 C21 1.286(4) . ? O4 C1 1.290(4) . ? O5 C38 1.268(4) . ? O5 La1 2.580(2) 2_545 ? O5 La2 2.700(2) 1_545 ? O6 C28 1.265(4) . ? O6 La1 2.446(2) 4_566 ? O7 H51 0.849(10) . ? O7 H52 0.846(10) . ? O8 C31 1.274(4) . ? O8 La2 2.490(2) 2_545 ? O9 C31 1.255(4) . ? O10 C21 1.245(4) . ? O11 C1 1.239(4) . ? O12 C38 1.267(4) . ? O12 La2 2.535(2) 1_545 ? O13 C28 1.252(4) . ? O13 La2 2.361(2) 3_566 ? C1 C2 1.485(4) . ? C2 C7 1.388(4) . ? C2 C3 1.389(4) . ? C3 C4 1.385(4) . ? C3 H3 0.9300 . ? C4 C5 1.384(5) . ? C4 C8 1.489(5) . ? C5 C6 1.376(5) . ? C5 H5 0.9300 . ? C6 C7 1.388(5) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 O21 1.201(4) . ? C8 O22 1.335(4) . ? O22 H22 0.8200 . ? C11 C12 1.493(5) . ? C12 C17 1.386(5) . ? C12 C13 1.389(4) . ? C13 C14 1.389(5) . ? C13 H13 0.9300 . ? C14 C15 1.390(5) . ? C14 C18 1.487(5) . ? C15 C16 1.386(5) . ? C15 H15 0.9300 . ? C16 C17 1.384(5) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 O32 1.209(4) . ? C18 O31 1.323(4) . ? O31 H31 0.8200 . ? C21 C22 1.490(4) . ? C22 C27 1.388(4) . ? C22 C23 1.400(4) . ? C23 C24 1.380(4) . ? C23 H23 0.9300 . ? C24 C25 1.377(5) . ? C24 H24 0.9300 . ? C25 C26 1.377(4) . ? C25 H25 0.9300 . ? C26 C27 1.386(4) . ? C26 C28 1.500(5) . ? C27 H27 0.9300 . ? C31 C32 1.489(4) . ? C32 C33 1.385(4) . ? C32 C37 1.388(4) . ? C33 C34 1.384(5) . ? C33 H33 0.9300 . ? C34 C35 1.378(5) . ? C34 H34 0.9300 . ? C35 C36 1.382(4) . ? C35 H35 0.9300 . ? C36 C37 1.395(4) . ? C36 C38 1.499(4) . ? C37 H37 0.9300 . ? C38 La2 2.996(3) 1_545 ? O100 H102 0.843(10) . ? O100 H101 0.844(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 La1 O4 90.11(8) 4_565 . ? O6 La1 O9 87.82(9) 4_565 . ? O4 La1 O9 148.25(7) . . ? O6 La1 O3 139.22(8) 4_565 . ? O4 La1 O3 73.65(7) . . ? O9 La1 O3 87.55(7) . . ? O6 La1 O7 70.94(9) 4_565 . ? O4 La1 O7 75.24(9) . . ? O9 La1 O7 74.15(9) . . ? O3 La1 O7 68.82(8) . . ? O6 La1 O5 75.12(8) 4_565 2 ? O4 La1 O5 89.49(7) . 2 ? O9 La1 O5 120.37(7) . 2 ? O3 La1 O5 139.65(7) . 2 ? O7 La1 O5 142.49(9) . 2 ? O6 La1 O2 139.96(7) 4_565 . ? O4 La1 O2 65.64(7) . . ? O9 La1 O2 129.68(8) . . ? O3 La1 O2 66.24(7) . . ? O7 La1 O2 126.54(8) . . ? O5 La1 O2 73.41(7) 2 . ? O6 La1 O1 146.07(7) 4_565 . ? O4 La1 O1 113.78(7) . . ? O9 La1 O1 83.63(8) . . ? O3 La1 O1 73.25(7) . . ? O7 La1 O1 136.38(9) . . ? O5 La1 O1 81.11(7) 2 . ? O2 La1 O1 48.78(6) . . ? O6 La1 O8 78.16(7) 4_565 . ? O4 La1 O8 159.18(7) . . ? O9 La1 O8 49.52(7) . . ? O3 La1 O8 126.09(7) . . ? O7 La1 O8 115.91(8) . . ? O5 La1 O8 70.99(6) 2 . ? O2 La1 O8 113.38(7) . . ? O1 La1 O8 71.33(7) . . ? O6 La1 C31 82.09(9) 4_565 . ? O4 La1 C31 168.86(8) . . ? O9 La1 C31 24.30(8) . . ? O3 La1 C31 107.34(8) . . ? O7 La1 C31 94.62(10) . . ? O5 La1 C31 96.12(8) 2 . ? O2 La1 C31 125.22(8) . . ? O1 La1 C31 76.70(8) . . ? O8 La1 C31 25.22(7) . . ? O6 La1 C11 149.96(8) 4_565 . ? O4 La1 C11 90.19(8) . . ? O9 La1 C11 106.95(9) . . ? O3 La1 C11 68.97(8) . . ? O7 La1 C11 137.68(9) . . ? O5 La1 C11 74.85(8) 2 . ? O2 La1 C11 24.71(7) . . ? O1 La1 C11 24.13(7) . . ? O8 La1 C11 91.55(7) . . ? C31 La1 C11 100.56(9) . . ? O6 La1 La2 129.90(6) 4_565 . ? O4 La1 La2 39.94(5) . . ? O9 La1 La2 130.44(6) . . ? O3 La1 La2 43.11(5) . . ? O7 La1 La2 88.16(7) . . ? O5 La1 La2 101.92(5) 2 . ? O2 La1 La2 38.68(5) . . ? O1 La1 La2 78.30(5) . . ? O8 La1 La2 149.49(5) . . ? C31 La1 La2 146.33(6) . . ? C11 La1 La2 58.25(6) . . ? O13 La2 O8 78.22(8) 3_566 2 ? O13 La2 O10 75.51(8) 3_566 . ? O8 La2 O10 149.40(8) 2 . ? O13 La2 O2 86.40(8) 3_566 . ? O8 La2 O2 84.60(7) 2 . ? O10 La2 O2 78.41(8) . . ? O13 La2 O12 98.18(8) 3_566 1_565 ? O8 La2 O12 121.03(7) 2 1_565 ? O10 La2 O12 78.39(8) . 1_565 ? O2 La2 O12 154.38(7) . 1_565 ? O13 La2 O11 146.81(8) 3_566 . ? O8 La2 O11 79.06(8) 2 . ? O10 La2 O11 131.26(8) . . ? O2 La2 O11 115.12(7) . . ? O12 La2 O11 73.59(7) 1_565 . ? O13 La2 O4 144.16(8) 3_566 . ? O8 La2 O4 77.43(7) 2 . ? O10 La2 O4 116.91(7) . . ? O2 La2 O4 65.50(7) . . ? O12 La2 O4 116.87(7) 1_565 . ? O11 La2 O4 49.73(7) . . ? O13 La2 O5 76.05(8) 3_566 1_565 ? O8 La2 O5 73.07(7) 2 1_565 ? O10 La2 O5 114.68(7) . 1_565 ? O2 La2 O5 153.86(7) . 1_565 ? O12 La2 O5 49.73(6) 1_565 1_565 ? O11 La2 O5 74.38(7) . 1_565 ? O4 La2 O5 120.49(7) . 1_565 ? O13 La2 O3 120.84(7) 3_566 . ? O8 La2 O3 141.36(7) 2 . ? O10 La2 O3 49.47(7) . . ? O2 La2 O3 65.34(7) . . ? O12 La2 O3 91.15(7) 1_565 . ? O11 La2 O3 91.82(7) . . ? O4 La2 O3 68.47(6) . . ? O5 La2 O3 140.59(6) 1_565 . ? O13 La2 C1 151.77(8) 3_566 . ? O8 La2 C1 73.55(8) 2 . ? O10 La2 C1 131.30(8) . . ? O2 La2 C1 90.67(8) . . ? O12 La2 C1 96.51(8) 1_565 . ? O11 La2 C1 24.52(7) . . ? O4 La2 C1 25.67(7) . . ? O5 La2 C1 95.72(8) 1_565 . ? O3 La2 C1 82.70(7) . . ? O13 La2 C21 97.37(9) 3_566 . ? O8 La2 C21 154.03(8) 2 . ? O10 La2 C21 24.07(8) . . ? O2 La2 C21 69.53(8) . . ? O12 La2 C21 84.87(8) 1_565 . ? O11 La2 C21 113.39(8) . . ? O4 La2 C21 93.21(8) . . ? O5 La2 C21 131.21(7) 1_565 . ? O3 La2 C21 25.42(7) . . ? C1 La2 C21 107.87(9) . . ? O13 La2 C38 87.91(9) 3_566 1_565 ? O8 La2 C38 96.98(8) 2 1_565 ? O10 La2 C38 97.45(8) . 1_565 ? O2 La2 C38 173.66(8) . 1_565 ? O12 La2 C38 24.72(7) 1_565 1_565 ? O11 La2 C38 71.22(8) . 1_565 ? O4 La2 C38 120.83(8) . 1_565 ? O5 La2 C38 25.05(7) 1_565 1_565 ? O3 La2 C38 115.63(8) . 1_565 ? C1 La2 C38 95.67(9) . 1_565 ? C21 La2 C38 108.51(8) . 1_565 ? C11 O1 La1 95.76(19) . . ? C11 O2 La2 132.02(19) . . ? C11 O2 La1 95.43(18) . . ? La2 O2 La1 100.27(7) . . ? C21 O3 La1 135.43(19) . . ? C21 O3 La2 88.54(18) . . ? La1 O3 La2 97.28(7) . . ? C1 O4 La1 148.4(2) . . ? C1 O4 La2 92.96(18) . . ? La1 O4 La2 102.69(8) . . ? C38 O5 La1 163.3(2) . 2_545 ? C38 O5 La2 90.61(18) . 1_545 ? La1 O5 La2 105.72(7) 2_545 1_545 ? C28 O6 La1 139.9(2) . 4_566 ? La1 O7 H51 114(4) . . ? La1 O7 H52 127(3) . . ? H51 O7 H52 114(5) . . ? C31 O8 La2 155.5(2) . 2_545 ? C31 O8 La1 88.10(18) . . ? La2 O8 La1 106.95(7) 2_545 . ? C31 O9 La1 101.54(19) . . ? C21 O10 La2 101.3(2) . . ? C1 O11 La2 94.70(19) . . ? C38 O12 La2 98.46(18) . 1_545 ? C28 O13 La2 143.5(2) . 3_566 ? O11 C1 O4 120.4(3) . . ? O11 C1 C2 121.9(3) . . ? O4 C1 C2 117.6(3) . . ? O11 C1 La2 60.78(17) . . ? O4 C1 La2 61.37(16) . . ? C2 C1 La2 163.7(2) . . ? C7 C2 C3 119.3(3) . . ? C7 C2 C1 120.6(3) . . ? C3 C2 C1 120.1(3) . . ? C4 C3 C2 120.6(3) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C5 C4 C3 119.3(3) . . ? C5 C4 C8 123.6(3) . . ? C3 C4 C8 117.2(3) . . ? C6 C5 C4 120.9(3) . . ? C6 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? C5 C6 C7 119.6(3) . . ? C5 C6 H6 120.2 . . ? C7 C6 H6 120.2 . . ? C6 C7 C2 120.3(3) . . ? C6 C7 H7 119.8 . . ? C2 C7 H7 119.8 . . ? O21 C8 O22 123.2(3) . . ? O21 C8 C4 123.6(3) . . ? O22 C8 C4 113.2(3) . . ? C8 O22 H22 109.5 . . ? O1 C11 O2 119.7(3) . . ? O1 C11 C12 122.6(3) . . ? O2 C11 C12 117.6(3) . . ? O1 C11 La1 60.11(17) . . ? O2 C11 La1 59.86(16) . . ? C12 C11 La1 175.2(2) . . ? C17 C12 C13 119.9(3) . . ? C17 C12 C11 120.4(3) . . ? C13 C12 C11 119.6(3) . . ? C14 C13 C12 120.0(3) . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C13 C14 C15 119.7(3) . . ? C13 C14 C18 118.5(3) . . ? C15 C14 C18 121.8(3) . . ? C16 C15 C14 120.2(3) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C17 C16 C15 119.9(4) . . ? C17 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? C16 C17 C12 120.2(3) . . ? C16 C17 H17 119.9 . . ? C12 C17 H17 119.9 . . ? O32 C18 O31 122.9(4) . . ? O32 C18 C14 123.1(4) . . ? O31 C18 C14 114.0(3) . . ? C18 O31 H31 109.5 . . ? O10 C21 O3 120.6(3) . . ? O10 C21 C22 119.3(3) . . ? O3 C21 C22 120.1(3) . . ? O10 C21 La2 54.67(16) . . ? O3 C21 La2 66.04(16) . . ? C22 C21 La2 173.0(2) . . ? C27 C22 C23 119.6(3) . . ? C27 C22 C21 119.4(3) . . ? C23 C22 C21 121.1(3) . . ? C24 C23 C22 119.6(3) . . ? C24 C23 H23 120.2 . . ? C22 C23 H23 120.2 . . ? C25 C24 C23 120.1(3) . . ? C25 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? C24 C25 C26 121.0(3) . . ? C24 C25 H25 119.5 . . ? C26 C25 H25 119.5 . . ? C25 C26 C27 119.4(3) . . ? C25 C26 C28 120.3(3) . . ? C27 C26 C28 120.2(3) . . ? C26 C27 C22 120.3(3) . . ? C26 C27 H27 119.9 . . ? C22 C27 H27 119.9 . . ? O13 C28 O6 123.7(3) . . ? O13 C28 C26 117.7(3) . . ? O6 C28 C26 118.6(3) . . ? O9 C31 O8 120.8(3) . . ? O9 C31 C32 118.4(3) . . ? O8 C31 C32 120.7(3) . . ? O9 C31 La1 54.16(16) . . ? O8 C31 La1 66.68(16) . . ? C32 C31 La1 172.2(2) . . ? C33 C32 C37 119.5(3) . . ? C33 C32 C31 118.5(3) . . ? C37 C32 C31 122.0(3) . . ? C34 C33 C32 120.5(3) . . ? C34 C33 H33 119.8 . . ? C32 C33 H33 119.8 . . ? C35 C34 C33 119.7(3) . . ? C35 C34 H34 120.1 . . ? C33 C34 H34 120.1 . . ? C34 C35 C36 120.9(3) . . ? C34 C35 H35 119.6 . . ? C36 C35 H35 119.6 . . ? C35 C36 C37 119.2(3) . . ? C35 C36 C38 119.8(3) . . ? C37 C36 C38 121.0(3) . . ? C32 C37 C36 120.3(3) . . ? C32 C37 H37 119.9 . . ? C36 C37 H37 119.9 . . ? O12 C38 O5 121.0(3) . . ? O12 C38 C36 118.4(3) . . ? O5 C38 C36 120.6(3) . . ? O12 C38 La2 56.81(15) . 1_545 ? O5 C38 La2 64.34(16) . 1_545 ? C36 C38 La2 173.2(2) . 1_545 ? H102 O100 H101 96(5) . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.774 _refine_diff_density_min -0.479 _refine_diff_density_rms 0.118 #===================================================== data_Compound(II) _database_code_depnum_ccdc_archive 'CCDC 641733' #===================================================== _chemical_name_systematic ; ? ; _chemical_name_common 'Yttrium Carboxylate' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H16 O15 Y2' _chemical_formula_weight 722.19 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.587(2) _cell_length_b 14.227(3) _cell_length_c 17.130(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.998(4) _cell_angle_gamma 90.00 _cell_volume 2554.8(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6007 _cell_measurement_theta_min 1.87 _cell_measurement_theta_max 28.01 _exptl_crystal_description 'Block like' _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.878 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1432 _exptl_absorpt_coefficient_mu 4.599 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6083 _exptl_absorpt_correction_T_max 0.6563 _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _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 'Bruker SMART CCD area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22039 _diffrn_reflns_av_R_equivalents 0.0930 _diffrn_reflns_av_sigmaI/netI 0.1056 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 28.01 _reflns_number_total 6007 _reflns_number_gt 3808 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement 'SAINT (Bruker, 2000)' _computing_data_reduction SAINT _computing_structure_solution 'SIR92 (Altomare et al., 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1999) and CWMERON (Watkin et al., 1993)' _computing_publication_material 'PLATON (Spek, 2003)' _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^)+(0.0415P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6007 _refine_ls_number_parameters 386 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1083 _refine_ls_R_factor_gt 0.0529 _refine_ls_wR_factor_ref 0.1054 _refine_ls_wR_factor_gt 0.0896 _refine_ls_goodness_of_fit_ref 0.993 _refine_ls_restrained_S_all 0.993 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Y1 Y 0.07841(4) 0.28120(3) 0.15552(3) 0.01644(12) Uani 1 1 d . . . Y2 Y -0.17786(4) 0.51275(3) 0.16549(3) 0.01883(13) Uani 1 1 d . . . O1 O -0.9381(3) 0.6971(3) -0.0436(2) 0.0317(9) Uani 1 1 d . . . O2 O -0.0356(3) 0.6314(2) 0.3757(2) 0.0273(8) Uani 1 1 d . . . O3 O 0.2891(3) 0.2222(3) 0.1729(3) 0.0355(10) Uani 1 1 d D . . O4 O 0.0996(3) 0.2186(2) 0.28366(18) 0.0218(8) Uani 1 1 d . . . O5 O -0.1817(3) -0.0958(2) 0.2814(2) 0.0310(9) Uani 1 1 d . . . O6 O -0.1129(3) 0.3361(2) 0.19648(18) 0.0206(8) Uani 1 1 d . . . O7 O 0.1838(4) 0.3524(3) 0.0629(2) 0.0454(12) Uani 1 1 d D . . O8 O -0.8375(3) 0.5601(2) -0.04935(19) 0.0266(8) Uani 1 1 d . . . O9 O -0.0392(3) 0.0166(3) 0.3172(2) 0.0323(9) Uani 1 1 d . . . O10 O -0.1346(3) 0.5194(2) 0.29901(19) 0.0269(8) Uani 1 1 d . . . O11 O -0.3133(3) 0.3806(2) 0.1781(2) 0.0283(9) Uani 1 1 d . . . O12 O -0.3876(3) 0.5457(2) 0.0843(2) 0.0296(9) Uani 1 1 d . . . O13 O -0.3501(3) 0.6073(2) 0.20215(19) 0.0283(9) Uani 1 1 d . . . O14 O 0.1545(3) 0.1539(2) 0.40028(19) 0.0249(8) Uani 1 1 d . . . C1 C 0.1277(4) 0.2248(4) 0.3572(3) 0.0208(11) Uani 1 1 d . . . C2 C 0.1304(4) 0.3205(3) 0.3943(3) 0.0205(11) Uani 1 1 d . . . C3 C 0.2216(5) 0.3463(4) 0.4565(3) 0.0317(14) Uani 1 1 d . . . H3 H 0.2800 0.3020 0.4793 0.038 Uiso 1 1 calc R . . C4 C 0.2266(5) 0.4368(4) 0.4848(3) 0.0375(15) Uani 1 1 d . . . H4 H 0.2895 0.4539 0.5258 0.045 Uiso 1 1 calc R . . C5 C 0.1384(5) 0.5023(4) 0.4524(3) 0.0320(14) Uani 1 1 d . . . H5 H 0.1426 0.5639 0.4709 0.038 Uiso 1 1 calc R . . C6 C 0.0434(4) 0.4760(4) 0.3922(3) 0.0209(11) Uani 1 1 d . . . C7 C 0.0402(4) 0.3861(3) 0.3644(3) 0.0185(11) Uani 1 1 d . . . H7 H -0.0241 0.3685 0.3245 0.022 Uiso 1 1 calc R . . C8 C -0.0500(4) 0.5471(3) 0.3532(3) 0.0195(11) Uani 1 1 d . . . C11 C -0.4192(4) 0.6001(4) 0.1360(3) 0.0239(12) Uani 1 1 d . . . C12 C -0.5390(4) 0.6576(4) 0.1180(3) 0.0260(13) Uani 1 1 d . . . C13 C -0.5514(5) 0.7441(4) 0.1523(3) 0.0319(14) Uani 1 1 d . . . H13 H -0.4865 0.7667 0.1898 0.038 Uiso 1 1 calc R . . C14 C -0.6600(5) 0.7974(4) 0.1312(3) 0.0368(15) Uani 1 1 d . . . H14 H -0.6672 0.8563 0.1536 0.044 Uiso 1 1 calc R . . C15 C -0.7577(5) 0.7631(4) 0.0768(3) 0.0307(13) Uani 1 1 d . . . H15 H -0.8309 0.7990 0.0631 0.037 Uiso 1 1 calc R . . C16 C -0.7475(5) 0.6753(4) 0.0424(3) 0.0251(12) Uani 1 1 d . . . C18 C -0.8495(4) 0.6400(4) -0.0215(3) 0.0235(12) Uani 1 1 d . . . C17 C -0.6383(4) 0.6232(4) 0.0631(3) 0.0228(12) Uani 1 1 d . . . H17 H -0.6305 0.5645 0.0403 0.027 Uiso 1 1 calc R . . C21 C -0.2317(4) 0.3154(3) 0.1874(3) 0.0185(11) Uani 1 1 d . . . C22 C -0.2725(4) 0.2161(3) 0.1893(3) 0.0218(11) Uani 1 1 d . . . C23 C -0.3868(5) 0.1858(4) 0.1468(3) 0.0358(15) Uani 1 1 d . . . H23 H -0.4383 0.2282 0.1156 0.043 Uiso 1 1 calc R . . C24 C -0.4243(5) 0.0934(4) 0.1506(4) 0.0488(19) Uani 1 1 d . . . H24 H -0.5010 0.0738 0.1222 0.059 Uiso 1 1 calc R . . C25 C -0.3483(5) 0.0294(4) 0.1966(3) 0.0364(15) Uani 1 1 d . . . H25 H -0.3743 -0.0327 0.1993 0.044 Uiso 1 1 calc R . . C26 C -0.2335(4) 0.0583(4) 0.2384(3) 0.0224(12) Uani 1 1 d . . . C27 C -0.1961(4) 0.1512(3) 0.2347(3) 0.0215(11) Uani 1 1 d . . . H27 H -0.1190 0.1705 0.2629 0.026 Uiso 1 1 calc R . . C28 C -0.1456(5) -0.0113(4) 0.2823(3) 0.0233(12) Uani 1 1 d . . . O100 O 0.4381(4) 0.3746(3) 0.0749(3) 0.0668(15) Uani 1 1 d . . . H51 H 0.348(3) 0.256(3) 0.159(3) 0.031(16) Uiso 1 1 d D . . H52 H 0.308(6) 0.187(4) 0.213(2) 0.08(3) Uiso 1 1 d D . . H61 H 0.262(2) 0.366(5) 0.066(5) 0.11(3) Uiso 1 1 d D . . H62 H 0.161(5) 0.353(4) 0.0133(8) 0.029(16) 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 Y1 0.0158(2) 0.0132(3) 0.0189(3) -0.0001(2) -0.00262(18) 0.00041(19) Y2 0.0178(2) 0.0136(3) 0.0233(3) 0.0018(2) -0.00326(19) -0.0003(2) O1 0.0242(19) 0.040(2) 0.027(2) -0.0026(18) -0.0082(16) 0.0114(17) O2 0.038(2) 0.017(2) 0.026(2) -0.0010(16) 0.0004(16) 0.0056(16) O3 0.020(2) 0.035(3) 0.052(3) 0.013(2) 0.0071(19) 0.0015(19) O4 0.0252(18) 0.024(2) 0.0153(18) -0.0039(16) -0.0018(14) 0.0001(15) O5 0.037(2) 0.017(2) 0.039(2) 0.0093(17) 0.0063(18) 0.0061(17) O6 0.0171(17) 0.020(2) 0.0235(19) 0.0033(16) 0.0001(14) -0.0020(14) O7 0.044(3) 0.070(3) 0.020(2) 0.011(2) -0.001(2) -0.022(2) O8 0.031(2) 0.026(2) 0.021(2) -0.0030(17) -0.0037(16) 0.0011(16) O9 0.0193(18) 0.033(2) 0.043(2) 0.0109(19) -0.0003(17) 0.0082(16) O10 0.0297(19) 0.021(2) 0.026(2) -0.0021(16) -0.0081(16) 0.0049(16) O11 0.0174(18) 0.018(2) 0.048(2) 0.0082(17) -0.0004(17) 0.0030(15) O12 0.0252(19) 0.022(2) 0.038(2) -0.0098(18) -0.0103(17) 0.0067(16) O13 0.0219(18) 0.033(2) 0.027(2) -0.0038(17) -0.0085(16) 0.0041(16) O14 0.035(2) 0.016(2) 0.0204(19) 0.0005(16) -0.0045(16) 0.0072(16) C1 0.016(2) 0.023(3) 0.022(3) 0.002(2) -0.002(2) 0.001(2) C2 0.026(3) 0.017(3) 0.017(3) 0.001(2) -0.001(2) 0.003(2) C3 0.036(3) 0.023(3) 0.032(3) 0.000(3) -0.010(3) 0.005(2) C4 0.038(3) 0.029(3) 0.038(4) -0.008(3) -0.021(3) 0.000(3) C5 0.040(3) 0.021(3) 0.032(3) -0.007(3) -0.006(3) 0.003(2) C6 0.024(3) 0.020(3) 0.020(3) 0.001(2) 0.005(2) 0.000(2) C7 0.020(2) 0.016(3) 0.017(3) 0.002(2) -0.002(2) 0.001(2) C8 0.025(3) 0.013(3) 0.021(3) 0.001(2) 0.006(2) 0.004(2) C11 0.016(2) 0.018(3) 0.035(3) 0.001(2) -0.005(2) -0.002(2) C12 0.019(3) 0.026(3) 0.031(3) 0.007(3) -0.004(2) 0.004(2) C13 0.034(3) 0.028(3) 0.029(3) -0.012(3) -0.013(2) 0.005(2) C14 0.042(3) 0.028(4) 0.038(4) -0.012(3) -0.003(3) 0.008(3) C15 0.026(3) 0.029(3) 0.034(3) -0.001(3) -0.006(2) 0.012(2) C16 0.021(3) 0.030(3) 0.022(3) 0.002(2) -0.002(2) 0.004(2) C18 0.020(3) 0.035(4) 0.015(3) 0.002(2) -0.002(2) 0.002(2) C17 0.021(3) 0.021(3) 0.024(3) 0.002(2) -0.005(2) 0.007(2) C21 0.019(2) 0.014(3) 0.022(3) 0.000(2) 0.002(2) -0.001(2) C22 0.018(2) 0.017(3) 0.029(3) 0.006(2) -0.003(2) 0.005(2) C23 0.024(3) 0.023(3) 0.055(4) 0.006(3) -0.012(3) 0.006(2) C24 0.025(3) 0.024(3) 0.088(5) 0.009(3) -0.023(3) -0.007(3) C25 0.028(3) 0.018(3) 0.059(4) 0.008(3) -0.008(3) -0.004(2) C26 0.017(2) 0.020(3) 0.030(3) 0.004(2) 0.002(2) 0.004(2) C27 0.019(3) 0.019(3) 0.026(3) 0.000(2) -0.001(2) 0.002(2) C28 0.021(3) 0.023(3) 0.027(3) 0.011(2) 0.011(2) 0.009(2) O100 0.034(2) 0.048(3) 0.114(4) 0.014(3) -0.003(3) -0.003(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Y1 O2 2.228(3) 2_545 ? Y1 O5 2.258(3) 2 ? Y1 O1 2.277(3) 3_465 ? Y1 O7 2.297(4) . ? Y1 O4 2.350(3) . ? Y1 O3 2.363(4) . ? Y1 O6 2.366(3) . ? Y2 O8 2.269(3) 3_465 ? Y2 O10 2.271(3) . ? Y2 O9 2.276(3) 2 ? Y2 O14 2.332(3) 2 ? Y2 O11 2.392(3) . ? Y2 O13 2.418(3) . ? Y2 O12 2.495(3) . ? Y2 O6 2.640(3) . ? Y2 C11 2.822(5) . ? Y2 C21 2.900(5) . ? O1 C18 1.259(6) . ? O1 Y1 2.277(3) 3_465 ? O2 C8 1.262(5) . ? O2 Y1 2.228(3) 2 ? O3 H51 0.848(10) . ? O3 H52 0.851(10) . ? O4 C1 1.256(5) . ? O5 C28 1.261(6) . ? O5 Y1 2.258(3) 2_545 ? O6 C21 1.280(5) . ? O7 H61 0.849(10) . ? O7 H62 0.850(10) . ? O8 C18 1.246(6) . ? O8 Y2 2.269(3) 3_465 ? O9 C28 1.264(6) . ? O9 Y2 2.276(3) 2_545 ? O10 C8 1.259(5) . ? O11 C21 1.263(5) . ? O12 C11 1.256(6) . ? O13 C11 1.265(5) . ? O14 C1 1.260(5) . ? O14 Y2 2.332(3) 2_545 ? C1 C2 1.502(7) . ? C2 C7 1.382(6) . ? C2 C3 1.383(6) . ? C3 C4 1.374(7) . ? C3 H3 0.9300 . ? C4 C5 1.380(7) . ? C4 H4 0.9300 . ? C5 C6 1.389(6) . ? C5 H5 0.9300 . ? C6 C7 1.363(6) . ? C6 C8 1.505(6) . ? C7 H7 0.9300 . ? C11 C12 1.505(6) . ? C12 C13 1.377(7) . ? C12 C17 1.398(6) . ? C13 C14 1.383(7) . ? C13 H13 0.9300 . ? C14 C15 1.381(7) . ? C14 H14 0.9300 . ? C15 C16 1.392(7) . ? C15 H15 0.9300 . ? C16 C17 1.378(6) . ? C16 C18 1.513(6) . ? C17 H17 0.9300 . ? C21 C22 1.479(7) . ? C22 C23 1.391(6) . ? C22 C27 1.392(6) . ? C23 C24 1.378(7) . ? C23 H23 0.9300 . ? C24 C25 1.384(7) . ? C24 H24 0.9300 . ? C25 C26 1.385(6) . ? C25 H25 0.9300 . ? C26 C27 1.383(7) . ? C26 C28 1.489(6) . ? C27 H27 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Y1 O5 157.66(13) 2_545 2 ? O2 Y1 O1 80.83(13) 2_545 3_465 ? O5 Y1 O1 120.90(13) 2 3_465 ? O2 Y1 O7 111.00(15) 2_545 . ? O5 Y1 O7 74.88(15) 2 . ? O1 Y1 O7 71.41(14) 3_465 . ? O2 Y1 O4 81.46(12) 2_545 . ? O5 Y1 O4 82.52(12) 2 . ? O1 Y1 O4 143.52(12) 3_465 . ? O7 Y1 O4 145.03(13) . . ? O2 Y1 O3 81.21(14) 2_545 . ? O5 Y1 O3 80.18(14) 2 . ? O1 Y1 O3 130.37(14) 3_465 . ? O7 Y1 O3 72.74(16) . . ? O4 Y1 O3 77.42(13) . . ? O2 Y1 O6 103.45(12) 2_545 . ? O5 Y1 O6 88.85(12) 2 . ? O1 Y1 O6 73.75(11) 3_465 . ? O7 Y1 O6 125.24(15) . . ? O4 Y1 O6 79.76(11) . . ? O3 Y1 O6 155.75(13) . . ? O8 Y2 O10 150.81(12) 3_465 . ? O8 Y2 O9 86.04(12) 3_465 2 ? O10 Y2 O9 78.99(12) . 2 ? O8 Y2 O14 86.82(12) 3_465 2 ? O10 Y2 O14 115.48(12) . 2 ? O9 Y2 O14 82.51(13) 2 2 ? O8 Y2 O11 80.64(12) 3_465 . ? O10 Y2 O11 88.93(12) . . ? O9 Y2 O11 127.86(12) 2 . ? O14 Y2 O11 145.63(11) 2 . ? O8 Y2 O13 129.09(11) 3_465 . ? O10 Y2 O13 76.64(11) . . ? O9 Y2 O13 137.46(12) 2 . ? O14 Y2 O13 77.34(12) 2 . ? O11 Y2 O13 86.03(12) . . ? O8 Y2 O12 76.33(12) 3_465 . ? O10 Y2 O12 126.36(12) . . ? O9 Y2 O12 150.70(13) 2 . ? O14 Y2 O12 73.42(11) 2 . ? O11 Y2 O12 72.56(11) . . ? O13 Y2 O12 52.82(11) . . ? O8 Y2 O6 72.12(11) 3_465 . ? O10 Y2 O6 80.04(11) . . ? O9 Y2 O6 76.50(11) 2 . ? O14 Y2 O6 151.00(11) 2 . ? O11 Y2 O6 51.41(10) . . ? O13 Y2 O6 131.47(11) . . ? O12 Y2 O6 118.53(10) . . ? O8 Y2 C11 102.56(14) 3_465 . ? O10 Y2 C11 102.29(14) . . ? O9 Y2 C11 152.25(14) 2 . ? O14 Y2 C11 71.85(13) 2 . ? O11 Y2 C11 79.82(13) . . ? O13 Y2 C11 26.52(12) . . ? O12 Y2 C11 26.41(12) . . ? O6 Y2 C11 131.22(12) . . ? O8 Y2 C21 73.18(13) 3_465 . ? O10 Y2 C21 85.74(13) . . ? O9 Y2 C21 102.66(13) 2 . ? O14 Y2 C21 158.77(12) 2 . ? O11 Y2 C21 25.35(11) . . ? O13 Y2 C21 109.65(13) . . ? O12 Y2 C21 94.51(12) . . ? O6 Y2 C21 26.17(11) . . ? C11 Y2 C21 105.08(14) . . ? C18 O1 Y1 135.4(3) . 3_465 ? C8 O2 Y1 145.4(3) . 2 ? Y1 O3 H51 118(4) . . ? Y1 O3 H52 115(5) . . ? H51 O3 H52 118(6) . . ? C1 O4 Y1 152.6(3) . . ? C28 O5 Y1 127.4(3) . 2_545 ? C21 O6 Y1 139.1(3) . . ? C21 O6 Y2 88.3(3) . . ? Y1 O6 Y2 117.65(12) . . ? Y1 O7 H61 128(5) . . ? Y1 O7 H62 127(4) . . ? H61 O7 H62 102(6) . . ? C18 O8 Y2 140.9(3) . 3_465 ? C28 O9 Y2 150.7(3) . 2_545 ? C8 O10 Y2 141.1(3) . . ? C21 O11 Y2 100.4(3) . . ? C11 O12 Y2 91.5(3) . . ? C11 O13 Y2 94.9(3) . . ? C1 O14 Y2 115.9(3) . 2_545 ? O4 C1 O14 122.3(5) . . ? O4 C1 C2 118.5(4) . . ? O14 C1 C2 119.2(4) . . ? C7 C2 C3 118.6(5) . . ? C7 C2 C1 118.9(4) . . ? C3 C2 C1 122.5(4) . . ? C4 C3 C2 120.6(5) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C3 C4 C5 120.0(5) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C4 C5 C6 119.8(5) . . ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? C7 C6 C5 119.5(5) . . ? C7 C6 C8 119.6(4) . . ? C5 C6 C8 120.8(5) . . ? C6 C7 C2 121.5(4) . . ? C6 C7 H7 119.3 . . ? C2 C7 H7 119.3 . . ? O10 C8 O2 124.5(4) . . ? O10 C8 C6 118.2(4) . . ? O2 C8 C6 117.3(4) . . ? O12 C11 O13 120.3(4) . . ? O12 C11 C12 119.4(4) . . ? O13 C11 C12 120.3(5) . . ? O12 C11 Y2 62.1(2) . . ? O13 C11 Y2 58.6(2) . . ? C12 C11 Y2 172.8(4) . . ? C13 C12 C17 119.6(4) . . ? C13 C12 C11 121.7(4) . . ? C17 C12 C11 118.7(5) . . ? C12 C13 C14 120.2(5) . . ? C12 C13 H13 119.9 . . ? C14 C13 H13 119.9 . . ? C15 C14 C13 120.1(5) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C14 C15 C16 120.5(5) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? C17 C16 C15 119.1(5) . . ? C17 C16 C18 119.7(5) . . ? C15 C16 C18 121.0(4) . . ? O8 C18 O1 125.8(4) . . ? O8 C18 C16 118.7(4) . . ? O1 C18 C16 115.5(5) . . ? C16 C17 C12 120.6(5) . . ? C16 C17 H17 119.7 . . ? C12 C17 H17 119.7 . . ? O11 C21 O6 119.3(4) . . ? O11 C21 C22 120.5(4) . . ? O6 C21 C22 120.1(4) . . ? O11 C21 Y2 54.2(2) . . ? O6 C21 Y2 65.5(2) . . ? C22 C21 Y2 172.3(3) . . ? C23 C22 C27 118.9(5) . . ? C23 C22 C21 121.4(4) . . ? C27 C22 C21 119.8(4) . . ? C24 C23 C22 120.4(5) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? C23 C24 C25 120.4(5) . . ? C23 C24 H24 119.8 . . ? C25 C24 H24 119.8 . . ? C24 C25 C26 119.9(5) . . ? C24 C25 H25 120.1 . . ? C26 C25 H25 120.1 . . ? C27 C26 C25 119.7(5) . . ? C27 C26 C28 119.7(4) . . ? C25 C26 C28 120.4(5) . . ? C26 C27 C22 120.7(4) . . ? C26 C27 H27 119.6 . . ? C22 C27 H27 119.6 . . ? O5 C28 O9 123.6(5) . . ? O5 C28 C26 117.5(4) . . ? O9 C28 C26 118.9(5) . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 28.01 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 1.145 _refine_diff_density_min -0.549 _refine_diff_density_rms 0.129 #======================================================== data_Compound(IIa) _database_code_depnum_ccdc_archive 'CCDC 641734' #======================================================== _chemical_name_systematic ; ? ; _chemical_name_common 'Gadolinium carboxylate' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H16 Gd2 O15' _chemical_formula_weight 858.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.6293(18) _cell_length_b 14.219(2) _cell_length_c 17.175(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.915(3) _cell_angle_gamma 90.00 _cell_volume 2571.2(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6055 _cell_measurement_theta_min 1.87 _cell_measurement_theta_max 28.03 _exptl_crystal_description 'Block like' _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.219 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1632 _exptl_absorpt_coefficient_mu 5.192 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5746 _exptl_absorpt_correction_T_max 0.6248 _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _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 'Bruker SMART CCD area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22072 _diffrn_reflns_av_R_equivalents 0.0357 _diffrn_reflns_av_sigmaI/netI 0.0376 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 28.03 _reflns_number_total 6055 _reflns_number_gt 5270 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement 'SAINT (Bruker, 2000)' _computing_data_reduction SAINT _computing_structure_solution 'SIR92 (Altomare et al., 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1999) and CAMERON (Watkin et al., 1993)' _computing_publication_material 'PLATON (Spek, 2003)' _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^)+(0.0189P)^2^+2.1060P] 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 6055 _refine_ls_number_parameters 386 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0387 _refine_ls_R_factor_gt 0.0297 _refine_ls_wR_factor_ref 0.0563 _refine_ls_wR_factor_gt 0.0537 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd1 Gd 0.075244(18) 0.277979(13) 0.156500(11) 0.01651(5) Uani 1 1 d . . . Gd2 Gd -0.177145(18) 0.508581(13) 0.167838(11) 0.01839(6) Uani 1 1 d . . . O1 O -0.9335(3) 0.7039(2) -0.04224(16) 0.0307(7) Uani 1 1 d . . . O2 O -0.0334(3) 0.62561(19) 0.37630(17) 0.0299(7) Uani 1 1 d . . . O3 O 0.2897(3) 0.2166(2) 0.1691(2) 0.0357(8) Uani 1 1 d D . . O4 O 0.0962(3) 0.20923(19) 0.28632(15) 0.0221(6) Uani 1 1 d . . . O5 O -0.1913(3) -0.1036(2) 0.27425(17) 0.0330(7) Uani 1 1 d . . . O6 O -0.1187(2) 0.33068(18) 0.19846(15) 0.0212(6) Uani 1 1 d . . . O7 O 0.1789(3) 0.3585(3) 0.06454(19) 0.0402(9) Uani 1 1 d D . . O8 O -0.8370(3) 0.5659(2) -0.04902(16) 0.0275(7) Uani 1 1 d . . . O9 O -0.0453(3) 0.0045(2) 0.31149(18) 0.0347(8) Uani 1 1 d . . . O10 O -0.1378(3) 0.5139(2) 0.30399(16) 0.0277(7) Uani 1 1 d . . . O11 O -0.3182(3) 0.37503(19) 0.17815(18) 0.0299(7) Uani 1 1 d . . . O12 O -0.3896(3) 0.5442(2) 0.08574(17) 0.0313(7) Uani 1 1 d . . . O13 O -0.3498(3) 0.6071(2) 0.20254(17) 0.0306(7) Uani 1 1 d . . . O14 O 0.1505(3) 0.14755(19) 0.40422(16) 0.0277(7) Uani 1 1 d . . . C1 C 0.1241(4) 0.2180(3) 0.3599(2) 0.0207(8) Uani 1 1 d . . . C2 C 0.1281(4) 0.3135(3) 0.3956(2) 0.0212(9) Uani 1 1 d . . . C3 C 0.2217(4) 0.3391(3) 0.4568(2) 0.0305(10) Uani 1 1 d . . . H3 H 0.2809 0.2951 0.4787 0.037 Uiso 1 1 calc R . . C4 C 0.2264(5) 0.4306(3) 0.4850(3) 0.0379(12) Uani 1 1 d . . . H4 H 0.2894 0.4479 0.5255 0.046 Uiso 1 1 calc R . . C5 C 0.1384(4) 0.4960(3) 0.4534(3) 0.0305(11) Uani 1 1 d . . . H5 H 0.1430 0.5575 0.4721 0.037 Uiso 1 1 calc R . . C6 C 0.0427(4) 0.4706(3) 0.3938(2) 0.0204(8) Uani 1 1 d . . . C7 C 0.0379(4) 0.3795(3) 0.3657(2) 0.0208(9) Uani 1 1 d . . . H7 H -0.0267 0.3622 0.3262 0.025 Uiso 1 1 calc R . . C8 C -0.0505(4) 0.5416(3) 0.3557(2) 0.0218(9) Uani 1 1 d . . . C11 C -0.4203(4) 0.5995(3) 0.1371(2) 0.0250(9) Uani 1 1 d . . . C12 C -0.5376(4) 0.6577(3) 0.1190(2) 0.0252(9) Uani 1 1 d . . . C13 C -0.5471(4) 0.7449(3) 0.1532(3) 0.0318(11) Uani 1 1 d . . . H13 H -0.4816 0.7662 0.1905 0.038 Uiso 1 1 calc R . . C14 C -0.6535(4) 0.8010(3) 0.1324(3) 0.0347(11) Uani 1 1 d . . . H14 H -0.6590 0.8601 0.1549 0.042 Uiso 1 1 calc R . . C15 C -0.7520(4) 0.7675(3) 0.0773(2) 0.0310(10) Uani 1 1 d . . . H15 H -0.8235 0.8047 0.0631 0.037 Uiso 1 1 calc R . . C16 C -0.7446(4) 0.6792(3) 0.0434(2) 0.0216(9) Uani 1 1 d . . . C18 C -0.8461(4) 0.6460(3) -0.0202(2) 0.0223(9) Uani 1 1 d . . . C17 C -0.6363(4) 0.6250(3) 0.0638(2) 0.0236(9) Uani 1 1 d . . . H17 H -0.6296 0.5665 0.0405 0.028 Uiso 1 1 calc R . . C21 C -0.2370(4) 0.3106(3) 0.1884(2) 0.0214(9) Uani 1 1 d . . . C22 C -0.2777(4) 0.2103(3) 0.1891(2) 0.0221(9) Uani 1 1 d . . . C23 C -0.3918(4) 0.1821(3) 0.1465(3) 0.0358(12) Uani 1 1 d . . . H23 H -0.4429 0.2256 0.1166 0.043 Uiso 1 1 calc R . . C24 C -0.4296(5) 0.0891(3) 0.1486(3) 0.0501(16) Uani 1 1 d . . . H24 H -0.5064 0.0703 0.1203 0.060 Uiso 1 1 calc R . . C25 C -0.3538(4) 0.0245(3) 0.1924(3) 0.0378(12) Uani 1 1 d . . . H25 H -0.3799 -0.0378 0.1938 0.045 Uiso 1 1 calc R . . C26 C -0.2392(4) 0.0514(3) 0.2343(2) 0.0233(9) Uani 1 1 d . . . C27 C -0.2010(4) 0.1446(3) 0.2327(2) 0.0211(9) Uani 1 1 d . . . H27 H -0.1239 0.1631 0.2608 0.025 Uiso 1 1 calc R . . C28 C -0.1523(4) -0.0205(3) 0.2769(2) 0.0247(9) Uani 1 1 d . . . O100 O 0.4341(3) 0.3741(3) 0.0730(3) 0.0604(11) Uani 1 1 d . . . H51 H 0.346(4) 0.253(4) 0.157(4) 0.09(2) Uiso 1 1 d D . . H52 H 0.321(7) 0.186(5) 0.209(3) 0.12(3) Uiso 1 1 d D . . H61 H 0.2568(17) 0.373(4) 0.075(3) 0.060(19) Uiso 1 1 d D . . H62 H 0.158(5) 0.364(4) 0.0152(8) 0.058(17) 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 Gd1 0.01570(10) 0.01482(10) 0.01774(10) 0.00094(7) -0.00221(7) 0.00033(7) Gd2 0.01767(10) 0.01445(10) 0.02150(10) 0.00158(7) -0.00286(8) 0.00026(7) O1 0.0260(17) 0.0375(18) 0.0251(16) -0.0012(13) -0.0094(13) 0.0129(14) O2 0.0397(19) 0.0146(15) 0.0334(17) -0.0022(12) -0.0023(14) 0.0064(13) O3 0.0227(18) 0.036(2) 0.048(2) 0.0121(17) 0.0045(15) 0.0051(15) O4 0.0233(15) 0.0239(15) 0.0181(14) -0.0008(11) -0.0009(11) 0.0008(12) O5 0.0423(19) 0.0211(16) 0.0349(18) 0.0085(13) 0.0033(15) 0.0074(14) O6 0.0180(15) 0.0198(15) 0.0252(15) 0.0024(11) 0.0012(12) -0.0013(11) O7 0.039(2) 0.060(2) 0.0201(17) 0.0094(16) 0.0014(16) -0.0187(19) O8 0.0299(17) 0.0271(17) 0.0229(15) -0.0038(13) -0.0051(13) 0.0027(13) O9 0.0222(17) 0.041(2) 0.0393(18) 0.0107(15) -0.0003(14) 0.0086(14) O10 0.0298(17) 0.0276(17) 0.0240(15) -0.0032(12) -0.0019(13) 0.0074(13) O11 0.0210(16) 0.0175(15) 0.050(2) 0.0068(14) 0.0003(14) 0.0026(12) O12 0.0233(16) 0.0284(17) 0.0382(18) -0.0091(14) -0.0103(13) 0.0079(13) O13 0.0231(16) 0.0378(18) 0.0279(16) -0.0052(13) -0.0071(13) 0.0063(14) O14 0.0456(19) 0.0145(14) 0.0212(15) 0.0002(11) -0.0025(13) 0.0081(13) C1 0.021(2) 0.018(2) 0.022(2) -0.0014(16) 0.0014(16) 0.0030(16) C2 0.026(2) 0.017(2) 0.019(2) 0.0000(16) -0.0006(17) 0.0041(17) C3 0.033(3) 0.022(2) 0.033(2) -0.0008(18) -0.008(2) 0.0088(19) C4 0.039(3) 0.029(3) 0.037(3) -0.008(2) -0.022(2) 0.003(2) C5 0.039(3) 0.018(2) 0.031(2) -0.0061(18) -0.007(2) 0.0048(19) C6 0.027(2) 0.017(2) 0.0174(19) 0.0010(15) 0.0027(16) 0.0022(17) C7 0.026(2) 0.018(2) 0.0170(19) -0.0009(15) -0.0003(16) 0.0018(17) C8 0.025(2) 0.024(2) 0.018(2) 0.0034(16) 0.0047(16) 0.0034(17) C11 0.018(2) 0.020(2) 0.034(2) -0.0015(18) -0.0059(18) -0.0011(17) C12 0.023(2) 0.025(2) 0.026(2) -0.0008(17) -0.0026(17) 0.0039(18) C13 0.030(2) 0.031(3) 0.030(2) -0.0077(19) -0.0128(19) 0.003(2) C14 0.039(3) 0.028(2) 0.034(3) -0.013(2) -0.005(2) 0.007(2) C15 0.029(2) 0.032(3) 0.030(2) -0.0018(19) -0.0051(19) 0.015(2) C16 0.021(2) 0.025(2) 0.0177(19) -0.0014(16) -0.0015(16) 0.0050(17) C18 0.019(2) 0.032(2) 0.016(2) 0.0016(17) 0.0006(16) 0.0018(18) C17 0.022(2) 0.019(2) 0.028(2) -0.0028(17) -0.0020(17) 0.0052(17) C21 0.021(2) 0.021(2) 0.022(2) -0.0001(16) 0.0015(16) -0.0017(17) C22 0.018(2) 0.017(2) 0.031(2) 0.0026(17) -0.0013(17) 0.0038(16) C23 0.023(2) 0.021(2) 0.058(3) 0.006(2) -0.011(2) 0.0081(19) C24 0.033(3) 0.026(3) 0.080(4) 0.002(3) -0.031(3) -0.004(2) C25 0.024(2) 0.021(2) 0.064(3) 0.004(2) -0.012(2) -0.0062(19) C26 0.023(2) 0.018(2) 0.030(2) 0.0050(17) 0.0050(17) 0.0025(17) C27 0.0122(19) 0.022(2) 0.029(2) 0.0033(17) 0.0015(16) -0.0004(16) C28 0.027(2) 0.027(2) 0.023(2) 0.0060(17) 0.0098(18) 0.0083(18) O100 0.034(2) 0.047(2) 0.097(3) 0.005(2) -0.003(2) -0.0024(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 Gd1 O2 2.267(3) 2_545 ? Gd1 O5 2.316(3) 2 ? Gd1 O1 2.318(3) 3_465 ? Gd1 O7 2.345(3) . ? Gd1 O6 2.396(3) . ? Gd1 O4 2.417(3) . ? Gd1 O3 2.423(3) . ? Gd2 O10 2.319(3) . ? Gd2 O8 2.322(3) 3_465 ? Gd2 O9 2.342(3) 2 ? Gd2 O14 2.369(3) 2 ? Gd2 O11 2.441(3) . ? Gd2 O13 2.447(3) . ? Gd2 O12 2.543(3) . ? Gd2 O6 2.640(3) . ? Gd2 C11 2.873(4) . ? Gd2 C21 2.918(4) . ? O1 C18 1.260(5) . ? O1 Gd1 2.318(3) 3_465 ? O2 C8 1.253(5) . ? O2 Gd1 2.267(3) 2 ? O3 H51 0.846(10) . ? O3 H52 0.847(10) . ? O4 C1 1.264(4) . ? O5 C28 1.252(5) . ? O5 Gd1 2.316(3) 2_545 ? O6 C21 1.277(5) . ? O7 H61 0.847(10) . ? O7 H62 0.849(10) . ? O8 C18 1.251(5) . ? O8 Gd2 2.322(3) 3_465 ? O9 C28 1.260(5) . ? O9 Gd2 2.342(3) 2_545 ? O10 C8 1.256(5) . ? O11 C21 1.254(5) . ? O12 C11 1.258(5) . ? O13 C11 1.267(5) . ? O14 C1 1.266(4) . ? O14 Gd2 2.369(3) 2_545 ? C1 C2 1.488(5) . ? C2 C7 1.390(5) . ? C2 C3 1.393(5) . ? C3 C4 1.386(6) . ? C3 H3 0.9300 . ? C4 C5 1.377(6) . ? C4 H4 0.9300 . ? C5 C6 1.389(5) . ? C5 H5 0.9300 . ? C6 C7 1.380(5) . ? C6 C8 1.500(5) . ? C7 H7 0.9300 . ? C11 C12 1.493(5) . ? C12 C13 1.381(6) . ? C12 C17 1.393(5) . ? C13 C14 1.391(6) . ? C13 H13 0.9300 . ? C14 C15 1.394(6) . ? C14 H14 0.9300 . ? C15 C16 1.392(6) . ? C15 H15 0.9300 . ? C16 C17 1.390(5) . ? C16 C18 1.502(5) . ? C17 H17 0.9300 . ? C21 C22 1.491(5) . ? C22 C23 1.387(6) . ? C22 C27 1.389(5) . ? C23 C24 1.383(6) . ? C23 H23 0.9300 . ? C24 C25 1.376(6) . ? C24 H24 0.9300 . ? C25 C26 1.380(6) . ? C25 H25 0.9300 . ? C26 C27 1.388(5) . ? C26 C28 1.499(5) . ? C27 H27 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Gd1 O5 153.44(11) 2_545 2 ? O2 Gd1 O1 79.24(10) 2_545 3_465 ? O5 Gd1 O1 126.30(11) 2 3_465 ? O2 Gd1 O7 113.18(12) 2_545 . ? O5 Gd1 O7 74.02(11) 2 . ? O1 Gd1 O7 71.72(11) 3_465 . ? O2 Gd1 O6 103.06(10) 2_545 . ? O5 Gd1 O6 92.16(10) 2 . ? O1 Gd1 O6 74.58(10) 3_465 . ? O7 Gd1 O6 123.60(12) . . ? O2 Gd1 O4 80.37(10) 2_545 . ? O5 Gd1 O4 81.10(10) 2 . ? O1 Gd1 O4 142.44(10) 3_465 . ? O7 Gd1 O4 145.77(11) . . ? O6 Gd1 O4 79.79(9) . . ? O2 Gd1 O3 80.10(11) 2_545 . ? O5 Gd1 O3 77.76(12) 2 . ? O1 Gd1 O3 127.56(11) 3_465 . ? O7 Gd1 O3 73.30(13) . . ? O6 Gd1 O3 157.48(11) . . ? O4 Gd1 O3 78.79(11) . . ? O10 Gd2 O8 151.20(10) . 3_465 ? O10 Gd2 O9 79.04(11) . 2 ? O8 Gd2 O9 86.31(10) 3_465 2 ? O10 Gd2 O14 118.79(10) . 2 ? O8 Gd2 O14 83.93(10) 3_465 2 ? O9 Gd2 O14 84.81(11) 2 2 ? O10 Gd2 O11 88.82(10) . . ? O8 Gd2 O11 79.86(10) 3_465 . ? O9 Gd2 O11 125.93(10) 2 . ? O14 Gd2 O11 143.65(9) 2 . ? O10 Gd2 O13 76.87(9) . . ? O8 Gd2 O13 128.08(9) 3_465 . ? O9 Gd2 O13 138.80(10) 2 . ? O14 Gd2 O13 78.30(11) 2 . ? O11 Gd2 O13 86.50(10) . . ? O10 Gd2 O12 125.14(10) . . ? O8 Gd2 O12 76.34(10) 3_465 . ? O9 Gd2 O12 152.82(11) 2 . ? O14 Gd2 O12 72.83(10) 2 . ? O11 Gd2 O12 71.82(9) . . ? O13 Gd2 O12 51.86(9) . . ? O10 Gd2 O6 79.96(9) . . ? O8 Gd2 O6 72.32(9) 3_465 . ? O9 Gd2 O6 75.00(9) 2 . ? O14 Gd2 O6 149.48(10) 2 . ? O11 Gd2 O6 50.96(8) . . ? O13 Gd2 O6 131.58(9) . . ? O12 Gd2 O6 117.90(9) . . ? O10 Gd2 C11 101.72(11) . . ? O8 Gd2 C11 102.09(11) 3_465 . ? O9 Gd2 C11 154.51(11) 2 . ? O14 Gd2 C11 72.41(11) 2 . ? O11 Gd2 C11 79.48(10) . . ? O13 Gd2 C11 25.99(10) . . ? O12 Gd2 C11 25.96(10) . . ? O6 Gd2 C11 130.44(10) . . ? O10 Gd2 C21 85.50(10) . . ? O8 Gd2 C21 73.03(11) 3_465 . ? O9 Gd2 C21 100.95(11) 2 . ? O14 Gd2 C21 155.71(10) 2 . ? O11 Gd2 C21 25.10(10) . . ? O13 Gd2 C21 109.84(11) . . ? O12 Gd2 C21 93.88(10) . . ? O6 Gd2 C21 25.96(9) . . ? C11 Gd2 C21 104.52(11) . . ? C18 O1 Gd1 133.9(3) . 3_465 ? C8 O2 Gd1 145.6(3) . 2 ? Gd1 O3 H51 117(5) . . ? Gd1 O3 H52 121(5) . . ? H51 O3 H52 108(6) . . ? C1 O4 Gd1 149.5(3) . . ? C28 O5 Gd1 121.2(3) . 2_545 ? C21 O6 Gd1 139.6(3) . . ? C21 O6 Gd2 89.2(2) . . ? Gd1 O6 Gd2 115.35(10) . . ? Gd1 O7 H61 121(4) . . ? Gd1 O7 H62 130(4) . . ? H61 O7 H62 107(5) . . ? C18 O8 Gd2 141.3(3) . 3_465 ? C28 O9 Gd2 154.9(3) . 2_545 ? C8 O10 Gd2 137.4(3) . . ? C21 O11 Gd2 99.2(2) . . ? C11 O12 Gd2 91.8(2) . . ? C11 O13 Gd2 96.2(3) . . ? C1 O14 Gd2 112.2(2) . 2_545 ? O4 C1 O14 121.7(3) . . ? O4 C1 C2 119.5(3) . . ? O14 C1 C2 118.9(3) . . ? C7 C2 C3 119.1(4) . . ? C7 C2 C1 119.0(3) . . ? C3 C2 C1 121.8(4) . . ? C4 C3 C2 119.8(4) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C5 C4 C3 120.5(4) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? C4 C5 C6 120.2(4) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C7 C6 C5 119.4(4) . . ? C7 C6 C8 119.2(3) . . ? C5 C6 C8 121.3(4) . . ? C6 C7 C2 121.0(4) . . ? C6 C7 H7 119.5 . . ? C2 C7 H7 119.5 . . ? O2 C8 O10 124.3(4) . . ? O2 C8 C6 117.2(4) . . ? O10 C8 C6 118.5(4) . . ? O12 C11 O13 119.7(4) . . ? O12 C11 C12 119.3(4) . . ? O13 C11 C12 120.9(4) . . ? O12 C11 Gd2 62.2(2) . . ? O13 C11 Gd2 57.8(2) . . ? C12 C11 Gd2 172.7(3) . . ? C13 C12 C17 119.8(4) . . ? C13 C12 C11 121.1(4) . . ? C17 C12 C11 119.1(4) . . ? C12 C13 C14 120.7(4) . . ? C12 C13 H13 119.6 . . ? C14 C13 H13 119.6 . . ? C13 C14 C15 119.1(4) . . ? C13 C14 H14 120.5 . . ? C15 C14 H14 120.5 . . ? C16 C15 C14 120.8(4) . . ? C16 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? C17 C16 C15 119.2(4) . . ? C17 C16 C18 119.8(4) . . ? C15 C16 C18 120.8(4) . . ? O8 C18 O1 124.8(4) . . ? O8 C18 C16 119.1(3) . . ? O1 C18 C16 116.1(4) . . ? C16 C17 C12 120.4(4) . . ? C16 C17 H17 119.8 . . ? C12 C17 H17 119.8 . . ? O11 C21 O6 120.1(4) . . ? O11 C21 C22 120.3(4) . . ? O6 C21 C22 119.6(3) . . ? O11 C21 Gd2 55.7(2) . . ? O6 C21 Gd2 64.8(2) . . ? C22 C21 Gd2 172.8(3) . . ? C23 C22 C27 119.7(4) . . ? C23 C22 C21 120.4(3) . . ? C27 C22 C21 119.9(3) . . ? C24 C23 C22 119.9(4) . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? C25 C24 C23 120.1(4) . . ? C25 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? C24 C25 C26 120.5(4) . . ? C24 C25 H25 119.7 . . ? C26 C25 H25 119.7 . . ? C25 C26 C27 119.6(4) . . ? C25 C26 C28 120.3(4) . . ? C27 C26 C28 119.9(4) . . ? C26 C27 C22 120.1(4) . . ? C26 C27 H27 119.9 . . ? C22 C27 H27 119.9 . . ? O5 C28 O9 123.8(4) . . ? O5 C28 C26 116.6(4) . . ? O9 C28 C26 119.6(4) . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 28.03 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 1.072 _refine_diff_density_min -0.629 _refine_diff_density_rms 0.132 #============================================