# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Catalina Ruiz-Perez' _publ_contact_author_email CARUIZ@ULL.ES _publ_section_title ; Intramolecular ferro- and antiferromagnetic interactions in oxo-carboxylate bridged digadolinium(iii) complexes: synthesis, crystal structures and magnetic properties ; _publ_contact_author_address ; Laboratorio de Rayos X y Materiales Moleculares Dpto. F\'isica Fundamental II. Facultad de F\'isica Universidad de La Laguna E-38204. La Laguna. Tenerife Spain ; loop_ _publ_author_name 'Catalina Ruiz-Perez' 'Laura Canadillas-Delgado' 'Fernando S Delgado' 'Oscar Fabelo' ; M.Julve ; 'F Lloret' 'Jorge Pasan' # Attachment 'Compound1-2.cif' data_compound1 _database_code_depnum_ccdc_archive 'CCDC 741329' #TrackingRef 'Compound1-2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H62 Gd2 O16' _chemical_formula_weight 993.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/a' _symmetry_space_group_name_Hall '-P 2yab' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 8.9894(7) _cell_length_b 14.1340(6) _cell_length_c 17.5045(19) _cell_angle_alpha 90.00 _cell_angle_beta 100.164(8) _cell_angle_gamma 90.00 _cell_volume 2189.2(3) _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 prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.507 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 996 _exptl_absorpt_coefficient_mu 3.061 _exptl_absorpt_correction_type sphere _exptl_absorpt_correction_T_min 0.5796 _exptl_absorpt_correction_T_max 0.7918 _exptl_absorpt_process_details ? _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 'horizonally mounted graphite crystal' _diffrn_radiation_probe x-ray _diffrn_source 'Enraf Nonius FR590' _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11558 _diffrn_reflns_av_R_equivalents 0.0395 _diffrn_reflns_av_sigmaI/netI 0.0540 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 6.41 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4824 _reflns_number_gt 3480 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_cell_refinement ? _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0077P)^2^+7.5488P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4824 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0696 _refine_ls_R_factor_gt 0.0402 _refine_ls_wR_factor_ref 0.0870 _refine_ls_wR_factor_gt 0.0747 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _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 Gd1 Gd 0.48221(3) 1.110386(15) 0.422008(17) 0.03714(10) Uani 1 1 d . . . C1 C 0.7036(6) 1.1100(4) 0.5650(4) 0.0496(14) Uani 1 1 d . . . C2 C 0.7970(11) 1.1161(6) 0.6445(6) 0.102(3) Uani 1 1 d . . . H2A H 0.8875 1.1525 0.6420 0.122 Uiso 1 1 calc R . . H2B H 0.8282 1.0529 0.6621 0.122 Uiso 1 1 calc R . . C3 C 0.7115(17) 1.1625(12) 0.7042(7) 0.157(5) Uani 1 1 d . . . H3A H 0.6880 1.2274 0.6886 0.188 Uiso 1 1 calc R . . H3B H 0.6167 1.1294 0.7031 0.188 Uiso 1 1 calc R . . C4 C 0.798(3) 1.1621(19) 0.7860(13) 0.247(11) Uani 1 1 d . . . H4A H 0.8471 1.1010 0.7946 0.296 Uiso 1 1 calc R . . H4B H 0.8774 1.2090 0.7887 0.296 Uiso 1 1 calc R . . C5 C 0.733(4) 1.177(3) 0.8406(18) 0.340(19) Uani 1 1 d . . . H5A H 0.8047 1.1741 0.8882 0.510 Uiso 1 1 calc R . . H5B H 0.6568 1.1292 0.8413 0.510 Uiso 1 1 calc R . . H5C H 0.6867 1.2380 0.8352 0.510 Uiso 1 1 calc R . . C6 C 0.7129(6) 1.0371(4) 0.3466(4) 0.0563(16) Uani 1 1 d . . . C7 C 0.8193(11) 0.9986(6) 0.2990(8) 0.105(4) Uani 1 1 d . . . H7A H 0.8981 1.0453 0.2985 0.126 Uiso 1 1 calc R . . H7B H 0.8670 0.9433 0.3257 0.126 Uiso 1 1 calc R . . C8 C 0.771(3) 0.975(4) 0.230(3) 0.38(3) Uani 1 1 d . . . H8A1 H 0.8546 0.9850 0.2030 0.461 Uiso 1 1 calc R . . H8A2 H 0.7556 0.9074 0.2314 0.461 Uiso 1 1 calc R . . C9 C 0.663(4) 1.005(3) 0.1877(16) 0.33(2) Uani 1 1 d . . . H9A1 H 0.6629 1.0723 0.1981 0.392 Uiso 1 1 calc R . . H9A2 H 0.5772 0.9791 0.2072 0.392 Uiso 1 1 calc R . . C10 C 0.621(5) 0.996(3) 0.0981(18) 0.42(2) Uani 1 1 d . . . H10A H 0.5306 1.0312 0.0800 0.626 Uiso 1 1 calc R . . H10B H 0.6054 0.9308 0.0841 0.626 Uiso 1 1 calc R . . H10C H 0.7021 1.0210 0.0748 0.626 Uiso 1 1 calc R . . C11 C 0.2547(7) 1.1357(4) 0.2912(4) 0.0529(15) Uani 1 1 d . . . C12 C 0.1435(8) 1.1683(7) 0.2231(5) 0.086(2) Uani 1 1 d . . . H12A H 0.0540 1.1290 0.2193 0.103 Uiso 1 1 calc R . . H12B H 0.1141 1.2324 0.2332 0.103 Uiso 1 1 calc R . . C13 C 0.1918(13) 1.1673(12) 0.1478(6) 0.147(5) Uani 1 1 d . . . H13A H 0.2282 1.1042 0.1395 0.176 Uiso 1 1 calc R . . H13B H 0.2772 1.2099 0.1507 0.176 Uiso 1 1 calc R . . C14 C 0.080(2) 1.1933(19) 0.0788(9) 0.239(10) Uani 1 1 d . . . H14A H -0.0058 1.1511 0.0757 0.286 Uiso 1 1 calc R . . H14B H 0.0445 1.2569 0.0863 0.286 Uiso 1 1 calc R . . C15 C 0.131(4) 1.191(4) 0.0062(13) 0.43(3) Uani 1 1 d . . . H15A H 0.0503 1.2086 -0.0346 0.643 Uiso 1 1 calc R . . H15B H 0.1640 1.1276 -0.0031 0.643 Uiso 1 1 calc R . . H15C H 0.2143 1.2337 0.0075 0.643 Uiso 1 1 calc R . . O1 O 0.6278(4) 1.0347(2) 0.5445(2) 0.0431(9) Uani 1 1 d . . . O2 O 0.6904(5) 1.1785(3) 0.5200(3) 0.0615(12) Uani 1 1 d . . . O3 O 0.6236(4) 0.9831(2) 0.3729(3) 0.0550(11) Uani 1 1 d . . . O4 O 0.7092(4) 1.1249(3) 0.3594(3) 0.0589(12) Uani 1 1 d . . . O5 O 0.3834(5) 1.1073(3) 0.2834(3) 0.0690(13) Uani 1 1 d . . . O6 O 0.2202(4) 1.1397(3) 0.3577(3) 0.0499(10) Uani 1 1 d . . . O1W O 0.4748(4) 1.2752(2) 0.3957(3) 0.0560(12) Uani 1 1 d . . . O2W O 0.3571(5) 1.1617(3) 0.5251(3) 0.0552(11) 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 Gd1 0.02566(13) 0.02098(12) 0.06637(19) 0.00266(13) 0.01245(11) 0.00098(10) C1 0.029(3) 0.034(3) 0.081(4) -0.004(3) -0.003(3) -0.003(2) C2 0.095(6) 0.055(5) 0.133(8) 0.008(5) -0.043(6) -0.017(4) C3 0.163(12) 0.212(14) 0.088(8) -0.024(9) 0.000(8) 0.006(11) C4 0.28(3) 0.32(3) 0.127(15) -0.085(17) 0.004(16) -0.09(2) C5 0.34(4) 0.49(5) 0.18(2) -0.12(3) 0.02(2) -0.05(3) C6 0.032(3) 0.049(4) 0.092(5) -0.007(3) 0.022(3) 0.004(3) C7 0.096(7) 0.063(5) 0.183(11) -0.034(6) 0.096(8) -0.003(4) C8 0.17(2) 0.65(8) 0.36(5) -0.31(6) 0.13(3) 0.03(3) C9 0.32(4) 0.52(5) 0.17(2) -0.04(2) 0.12(3) 0.20(4) C10 0.61(6) 0.44(5) 0.23(3) -0.13(3) 0.17(4) -0.04(4) C11 0.038(3) 0.051(4) 0.069(4) 0.004(3) 0.007(3) 0.000(3) C12 0.056(4) 0.123(7) 0.077(6) 0.019(5) 0.006(4) 0.010(5) C13 0.110(8) 0.239(15) 0.085(7) 0.024(8) 0.000(6) 0.038(9) C14 0.166(14) 0.45(3) 0.094(10) 0.059(14) 0.000(10) 0.072(17) C15 0.32(3) 0.84(9) 0.120(16) 0.04(3) 0.033(19) 0.08(4) O1 0.0284(17) 0.0238(17) 0.076(3) 0.0024(18) 0.0071(18) -0.0021(14) O2 0.056(3) 0.031(2) 0.093(3) 0.010(2) -0.001(2) -0.0188(18) O3 0.049(2) 0.0303(19) 0.090(3) 0.002(2) 0.024(2) 0.0041(17) O4 0.036(2) 0.038(2) 0.108(4) -0.008(2) 0.029(2) -0.0032(17) O5 0.046(2) 0.087(3) 0.075(3) 0.001(3) 0.016(2) 0.019(2) O6 0.0311(19) 0.044(2) 0.076(3) 0.006(2) 0.0141(19) 0.0024(16) O1W 0.037(2) 0.0268(18) 0.107(4) 0.014(2) 0.021(2) 0.0017(16) O2W 0.066(3) 0.0321(19) 0.073(3) 0.006(2) 0.028(2) 0.0186(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 Gd1 O1W 2.374(3) . ? Gd1 O1 2.394(3) 3_676 ? Gd1 O2W 2.401(4) . ? Gd1 O5 2.433(5) . ? Gd1 O3 2.444(4) . ? Gd1 O6 2.459(4) . ? Gd1 O4 2.490(4) . ? Gd1 O2 2.498(4) . ? Gd1 O1 2.543(4) . ? Gd1 C11 2.811(6) . ? Gd1 C6 2.843(6) . ? Gd1 C1 2.910(6) . ? C1 O2 1.239(7) . ? C1 O1 1.280(6) . ? C1 C2 1.496(11) . ? C2 C3 1.547(16) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.50(2) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.22(3) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 O3 1.253(7) . ? C6 O4 1.262(7) . ? C6 C7 1.478(10) . ? C7 C8 1.25(4) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.18(4) . ? C8 H8A1 0.9700 . ? C8 H8A2 0.9700 . ? C9 C10 1.55(4) . ? C9 H9A1 0.9700 . ? C9 H9A2 0.9700 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 O5 1.255(7) . ? C11 O6 1.258(7) . ? C11 C12 1.487(10) . ? C12 C13 1.459(12) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.475(16) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.43(2) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? O1 Gd1 2.394(3) 3_676 ? 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 O1W Gd1 O1 152.83(12) . 3_676 ? O1W Gd1 O2W 81.28(14) . . ? O1 Gd1 O2W 78.84(13) 3_676 . ? O1W Gd1 O5 80.29(16) . . ? O1 Gd1 O5 97.74(15) 3_676 . ? O2W Gd1 O5 128.19(14) . . ? O1W Gd1 O3 130.74(14) . . ? O1 Gd1 O3 73.65(13) 3_676 . ? O2W Gd1 O3 145.93(14) . . ? O5 Gd1 O3 75.93(15) . . ? O1W Gd1 O6 75.76(13) . . ? O1 Gd1 O6 81.53(12) 3_676 . ? O2W Gd1 O6 75.85(15) . . ? O5 Gd1 O6 52.77(14) . . ? O3 Gd1 O6 118.56(14) . . ? O1W Gd1 O4 80.25(13) . . ? O1 Gd1 O4 125.77(12) 3_676 . ? O2W Gd1 O4 146.63(15) . . ? O5 Gd1 O4 75.26(15) . . ? O3 Gd1 O4 52.30(12) . . ? O6 Gd1 O4 125.28(15) . . ? O1W Gd1 O2 75.35(14) . . ? O1 Gd1 O2 116.99(13) 3_676 . ? O2W Gd1 O2 76.16(15) . . ? O5 Gd1 O2 142.14(15) . . ? O3 Gd1 O2 98.75(15) . . ? O6 Gd1 O2 142.22(14) . . ? O4 Gd1 O2 72.40(15) . . ? O1W Gd1 O1 124.69(13) . . ? O1 Gd1 O1 66.84(13) 3_676 . ? O2W Gd1 O1 74.51(13) . . ? O5 Gd1 O1 151.24(13) . . ? O3 Gd1 O1 76.40(13) . . ? O6 Gd1 O1 139.97(13) . . ? O4 Gd1 O1 93.79(13) . . ? O2 Gd1 O1 51.02(12) . . ? O1W Gd1 C11 74.06(16) . . ? O1 Gd1 C11 92.05(15) 3_676 . ? O2W Gd1 C11 101.76(18) . . ? O5 Gd1 C11 26.45(16) . . ? O3 Gd1 C11 98.97(17) . . ? O6 Gd1 C11 26.55(15) . . ? O4 Gd1 C11 99.55(18) . . ? O2 Gd1 C11 149.29(16) . . ? O1 Gd1 C11 158.88(15) . . ? O1W Gd1 C6 105.38(16) . . ? O1 Gd1 C6 99.69(15) 3_676 . ? O2W Gd1 C6 159.40(18) . . ? O5 Gd1 C6 72.42(17) . . ? O3 Gd1 C6 26.04(15) . . ? O6 Gd1 C6 124.52(17) . . ? O4 Gd1 C6 26.33(14) . . ? O2 Gd1 C6 86.56(17) . . ? O1 Gd1 C6 85.96(16) . . ? C11 Gd1 C6 98.8(2) . . ? O1W Gd1 C1 99.22(15) . . ? O1 Gd1 C1 92.15(15) 3_676 . ? O2W Gd1 C1 72.19(16) . . ? O5 Gd1 C1 158.72(16) . . ? O3 Gd1 C1 88.97(16) . . ? O6 Gd1 C1 148.03(16) . . ? O4 Gd1 C1 83.65(17) . . ? O2 Gd1 C1 25.04(13) . . ? O1 Gd1 C1 26.06(13) . . ? C11 Gd1 C1 171.80(17) . . ? C6 Gd1 C1 87.40(18) . . ? O2 C1 O1 119.0(5) . . ? O2 C1 C2 121.4(5) . . ? O1 C1 C2 119.4(6) . . ? O2 C1 Gd1 58.6(3) . . ? O1 C1 Gd1 60.7(3) . . ? C2 C1 Gd1 170.6(6) . . ? C1 C2 C3 112.9(8) . . ? C1 C2 H2A 109.0 . . ? C3 C2 H2A 109.0 . . ? C1 C2 H2B 109.0 . . ? C3 C2 H2B 109.0 . . ? H2A C2 H2B 107.8 . . ? C4 C3 C2 114.0(15) . . ? C4 C3 H3A 108.8 . . ? C2 C3 H3A 108.8 . . ? C4 C3 H3B 108.8 . . ? C2 C3 H3B 108.8 . . ? H3A C3 H3B 107.6 . . ? C5 C4 C3 120(3) . . ? C5 C4 H4A 107.2 . . ? C3 C4 H4A 107.2 . . ? C5 C4 H4B 107.2 . . ? C3 C4 H4B 107.2 . . ? H4A C4 H4B 106.8 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? O3 C6 O4 119.7(5) . . ? O3 C6 C7 120.2(6) . . ? O4 C6 C7 120.1(6) . . ? O3 C6 Gd1 58.9(3) . . ? O4 C6 Gd1 61.0(3) . . ? C7 C6 Gd1 173.3(7) . . ? C8 C7 C6 119.2(14) . . ? C8 C7 H7A 107.5 . . ? C6 C7 H7A 107.5 . . ? C8 C7 H7B 107.5 . . ? C6 C7 H7B 107.5 . . ? H7A C7 H7B 107.0 . . ? C9 C8 C7 128(3) . . ? C9 C8 H8A1 105.2 . . ? C7 C8 H8A1 105.2 . . ? C9 C8 H8A2 105.2 . . ? C7 C8 H8A2 105.2 . . ? H8A1 C8 H8A2 106.0 . . ? C8 C9 C10 129(3) . . ? C8 C9 H9A1 105.0 . . ? C10 C9 H9A1 105.0 . . ? C8 C9 H9A2 105.0 . . ? C10 C9 H9A2 105.0 . . ? H9A1 C9 H9A2 105.9 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O5 C11 O6 119.8(6) . . ? O5 C11 C12 120.9(7) . . ? O6 C11 C12 119.2(6) . . ? O5 C11 Gd1 59.7(3) . . ? O6 C11 Gd1 60.9(3) . . ? C12 C11 Gd1 169.1(5) . . ? C13 C12 C11 117.2(7) . . ? C13 C12 H12A 108.0 . . ? C11 C12 H12A 108.0 . . ? C13 C12 H12B 108.0 . . ? C11 C12 H12B 108.0 . . ? H12A C12 H12B 107.2 . . ? C12 C13 C14 118.0(11) . . ? C12 C13 H13A 107.8 . . ? C14 C13 H13A 107.8 . . ? C12 C13 H13B 107.8 . . ? C14 C13 H13B 107.8 . . ? H13A C13 H13B 107.1 . . ? C15 C14 C13 116.2(17) . . ? C15 C14 H14A 108.2 . . ? C13 C14 H14A 108.2 . . ? C15 C14 H14B 108.2 . . ? C13 C14 H14B 108.2 . . ? H14A C14 H14B 107.4 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C1 O1 Gd1 150.0(4) . 3_676 ? C1 O1 Gd1 93.2(3) . . ? Gd1 O1 Gd1 113.16(13) 3_676 . ? C1 O2 Gd1 96.4(3) . . ? C6 O3 Gd1 95.0(3) . . ? C6 O4 Gd1 92.7(3) . . ? C11 O5 Gd1 93.9(4) . . ? C11 O6 Gd1 92.5(3) . . ? _diffrn_measured_fraction_theta_max 0.959 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 0.935 _refine_diff_density_min -0.642 _refine_diff_density_rms 0.123 data_compound2 _database_code_depnum_ccdc_archive 'CCDC 741330' #TrackingRef 'Compound1-2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H38 Gd2 O16 S6' _chemical_formula_weight 1233.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/a' _symmetry_space_group_name_Hall '-P 2yab' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 8.9500(3) _cell_length_b 14.1933(4) _cell_length_c 17.8465(7) _cell_angle_alpha 90.00 _cell_angle_beta 100.7540(10) _cell_angle_gamma 90.00 _cell_volume 2227.23(13) _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 prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.02 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.839 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1212 _exptl_absorpt_coefficient_mu 3.300 _exptl_absorpt_correction_type sphere _exptl_absorpt_correction_T_min 0.9369 _exptl_absorpt_correction_T_max 0.9369 _exptl_absorpt_process_details ? _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 'horizonally mounted graphite crystal' _diffrn_radiation_probe x-ray _diffrn_source 'Enraf Nonius FR590' _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5551 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0806 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 28.60 _reflns_number_total 5551 _reflns_number_gt 4222 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_reduction 'HKL2000 (Otwinowski & Minor, 1997)' _computing_cell_refinement ? _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0935P)^2^+6.5999P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5551 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0929 _refine_ls_R_factor_gt 0.0621 _refine_ls_wR_factor_ref 0.1877 _refine_ls_wR_factor_gt 0.1560 _refine_ls_goodness_of_fit_ref 1.136 _refine_ls_restrained_S_all 1.136 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd1 Gd 0.50835(4) 0.38530(3) 0.07164(2) 0.01978(15) Uani 1 1 d . . . C1 C 0.6810(10) 0.3929(5) -0.0510(5) 0.0253(18) Uani 1 1 d . . . C2 C 0.7951(11) 0.4007(6) -0.1040(6) 0.034(2) Uani 1 1 d . . . H2A H 0.8179 0.4666 -0.1109 0.040 Uiso 1 1 calc R . . H2B H 0.8889 0.3695 -0.0809 0.040 Uiso 1 1 calc R . . C3 C 0.7356(11) 0.3571(6) -0.1800(5) 0.032(2) Uani 1 1 d . . . C4 C 0.7967(16) 0.2785(7) -0.2071(6) 0.054(3) Uani 1 1 d . . . H4 H 0.8795 0.2454 -0.1804 0.064 Uiso 1 1 calc R . . C5 C 0.5784(9) 0.3325(6) -0.3070(4) 0.0205(16) Uani 1 1 d . . . H5 H 0.5014 0.3423 -0.3491 0.025 Uiso 1 1 calc R . . C6 C 0.6158(14) 0.3926(8) -0.2326(7) 0.048(3) Uani 1 1 d . . . H6 H 0.5627 0.4468 -0.2244 0.058 Uiso 1 1 calc R . . C7 C 0.3732(11) 0.3545(6) 0.2007(5) 0.031(2) Uani 1 1 d . . . C8 C 0.2996(13) 0.3257(8) 0.2665(6) 0.050(3) Uani 1 1 d . . . H8A H 0.2170 0.3692 0.2691 0.059 Uiso 1 1 calc R . . H8B H 0.2551 0.2638 0.2556 0.059 Uiso 1 1 calc R . . C9 C 0.3998(12) 0.3226(7) 0.3427(5) 0.039(2) Uani 1 1 d . . . C10 C 0.4955(17) 0.2484(12) 0.3720(9) 0.085(5) Uani 1 1 d . . . H10 H 0.5047 0.1937 0.3445 0.102 Uiso 1 1 calc R . . C11 C 0.5843(13) 0.2647(8) 0.4533(6) 0.050(3) Uani 1 1 d . . . H11 H 0.6542 0.2246 0.4825 0.060 Uiso 1 1 calc R . . C12 C 0.410(2) 0.3906(9) 0.3928(9) 0.078(5) Uani 1 1 d . . . H12 H 0.3571 0.4472 0.3841 0.094 Uiso 1 1 calc R . . C13 C 0.7859(10) 0.4622(6) 0.1542(5) 0.0264(18) Uani 1 1 d . . . C14 C 0.9302(11) 0.5003(7) 0.2008(6) 0.039(2) Uani 1 1 d . . . H14A H 0.9541 0.5602 0.1797 0.047 Uiso 1 1 calc R . . H14B H 1.0129 0.4571 0.1981 0.047 Uiso 1 1 calc R . . C15 C 0.9171(11) 0.5140(6) 0.2831(5) 0.036(2) Uani 1 1 d . . . C16 C 0.8009(13) 0.4890(8) 0.3166(6) 0.046(3) Uani 1 1 d . . . H16 H 0.7149 0.4575 0.2914 0.055 Uiso 1 1 calc R . . C17 C 1.0046(16) 0.5689(10) 0.4076(7) 0.066(4) Uani 1 1 d . . . H17 H 1.0685 0.5979 0.4481 0.080 Uiso 1 1 calc R . . C18 C 1.0349(13) 0.5567(8) 0.3348(6) 0.049(3) Uani 1 1 d . . . H18 H 1.1260 0.5753 0.3214 0.059 Uiso 1 1 calc R . . O1 O 0.6155(7) 0.4666(4) -0.0341(3) 0.0244(12) Uani 1 1 d . . . O2 O 0.6544(8) 0.3160(4) -0.0233(4) 0.0357(16) Uani 1 1 d . . . O3 O 0.5104(8) 0.3701(5) 0.2091(4) 0.0409(17) Uani 1 1 d . . . O4 O 0.2883(7) 0.3600(4) 0.1338(3) 0.0296(13) Uani 1 1 d . . . O5 O 0.7790(7) 0.3757(4) 0.1330(4) 0.0335(15) Uani 1 1 d . . . O6 O 0.6708(7) 0.5141(4) 0.1353(3) 0.0305(14) Uani 1 1 d . . . O1W O 0.5133(7) 0.2175(4) 0.0892(4) 0.0345(15) Uani 1 1 d . . . O2W O 0.3108(8) 0.3441(4) -0.0327(3) 0.0373(15) Uani 1 1 d . . . S1 S 0.7040(7) 0.2495(3) -0.2941(3) 0.1049(16) Uani 1 1 d . . . S2 S 0.5305(9) 0.3642(5) 0.4761(3) 0.146(3) Uani 1 1 d . . . S3 S 0.8269(5) 0.5208(3) 0.41027(18) 0.0769(11) 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 Gd1 0.0201(2) 0.0167(2) 0.0235(2) 0.00200(15) 0.00650(16) -0.00014(15) C1 0.021(4) 0.026(4) 0.028(4) -0.004(3) 0.003(3) 0.001(3) C2 0.031(5) 0.029(5) 0.047(6) 0.002(4) 0.023(4) 0.003(4) C3 0.037(5) 0.027(4) 0.036(5) -0.001(4) 0.019(4) 0.001(4) C4 0.092(10) 0.029(5) 0.048(6) -0.004(5) 0.034(6) 0.004(6) C5 0.018(4) 0.030(4) 0.016(4) -0.003(3) 0.008(3) -0.011(3) C6 0.043(7) 0.052(7) 0.054(7) 0.002(5) 0.021(6) 0.005(5) C7 0.031(5) 0.032(5) 0.034(5) -0.008(4) 0.016(4) -0.010(4) C8 0.045(7) 0.068(8) 0.040(6) -0.001(5) 0.020(5) -0.010(5) C9 0.042(6) 0.049(6) 0.028(5) 0.002(4) 0.016(4) -0.013(5) C10 0.070(10) 0.096(11) 0.099(12) -0.006(9) 0.045(9) 0.015(9) C11 0.049(7) 0.061(7) 0.040(6) 0.024(5) 0.006(5) 0.015(6) C12 0.112(14) 0.063(9) 0.056(9) -0.001(7) 0.008(9) 0.000(8) C13 0.029(5) 0.030(5) 0.022(4) 0.002(3) 0.009(4) -0.007(4) C14 0.025(5) 0.040(5) 0.052(6) -0.009(5) 0.009(4) -0.011(4) C15 0.036(5) 0.031(5) 0.035(5) 0.000(4) -0.008(4) 0.000(4) C16 0.041(6) 0.059(7) 0.035(6) 0.003(5) 0.003(5) -0.009(5) C17 0.082(10) 0.068(9) 0.036(6) 0.004(6) -0.022(6) -0.024(7) C18 0.042(6) 0.052(7) 0.048(6) 0.003(5) -0.008(5) -0.011(5) O1 0.027(3) 0.017(3) 0.031(3) 0.001(2) 0.011(3) 0.003(2) O2 0.051(4) 0.025(3) 0.037(4) 0.003(3) 0.022(3) 0.004(3) O3 0.027(4) 0.069(5) 0.028(3) 0.001(3) 0.008(3) -0.012(3) O4 0.025(3) 0.030(3) 0.033(3) 0.005(3) 0.003(3) 0.000(3) O5 0.027(3) 0.024(3) 0.051(4) -0.004(3) 0.010(3) 0.002(2) O6 0.031(3) 0.024(3) 0.035(3) 0.005(3) 0.002(3) 0.002(3) O1W 0.032(4) 0.020(3) 0.053(4) 0.011(3) 0.014(3) 0.002(2) O2W 0.049(4) 0.026(3) 0.034(3) 0.005(3) -0.003(3) -0.010(3) S1 0.139(4) 0.087(3) 0.100(3) -0.035(3) 0.052(3) -0.030(3) S2 0.161(6) 0.207(7) 0.061(3) -0.004(4) -0.005(3) -0.038(5) S3 0.086(3) 0.109(3) 0.0334(16) 0.0044(17) 0.0064(16) -0.018(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 O2W 2.389(6) . ? Gd1 O1W 2.401(6) . ? Gd1 O1 2.412(5) 3_665 ? Gd1 O3 2.460(6) . ? Gd1 O4 2.461(6) . ? Gd1 O5 2.469(7) . ? Gd1 O6 2.476(6) . ? Gd1 O2 2.524(6) . ? Gd1 O1 2.547(5) . ? Gd1 C7 2.828(8) . ? Gd1 C13 2.857(9) . ? Gd1 C1 2.907(9) . ? C1 O2 1.239(10) . ? C1 O1 1.262(9) . ? C1 C2 1.520(12) . ? C2 C3 1.495(13) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.371(13) . ? C3 C6 1.381(15) . ? C4 S1 1.670(13) . ? C4 H4 0.9300 . ? C5 C6 1.561(14) . ? C5 S1 1.615(10) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 O3 1.230(11) . ? C7 O4 1.292(11) . ? C7 C8 1.506(13) . ? C8 C9 1.484(15) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C12 1.307(17) . ? C9 C10 1.395(18) . ? C10 C11 1.54(2) . ? C10 H10 0.9300 . ? C11 S2 1.569(13) . ? C11 H11 0.9300 . ? C12 S2 1.707(18) . ? C12 H12 0.9300 . ? C13 O6 1.260(10) . ? C13 O5 1.283(10) . ? C13 C14 1.501(12) . ? C14 C15 1.507(14) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.341(14) . ? C15 C18 1.403(13) . ? C16 S3 1.704(11) . ? C16 H16 0.9300 . ? C17 C18 1.386(17) . ? C17 S3 1.740(14) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? O1 Gd1 2.412(5) 3_665 ? 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 O2W Gd1 O1W 81.5(2) . . ? O2W Gd1 O1 76.2(2) . 3_665 ? O1W Gd1 O1 153.7(2) . 3_665 ? O2W Gd1 O3 128.5(2) . . ? O1W Gd1 O3 77.7(2) . . ? O1 Gd1 O3 105.7(2) 3_665 . ? O2W Gd1 O4 77.2(2) . . ? O1W Gd1 O4 78.1(2) . . ? O1 Gd1 O4 83.53(19) 3_665 . ? O3 Gd1 O4 52.8(2) . . ? O2W Gd1 O5 148.7(2) . . ? O1W Gd1 O5 83.9(2) . . ? O1 Gd1 O5 122.23(19) 3_665 . ? O3 Gd1 O5 74.3(2) . . ? O4 Gd1 O5 126.4(2) . . ? O2W Gd1 O6 145.51(19) . . ? O1W Gd1 O6 132.6(2) . . ? O1 Gd1 O6 71.59(19) 3_665 . ? O3 Gd1 O6 73.3(2) . . ? O4 Gd1 O6 110.6(2) . . ? O5 Gd1 O6 52.68(19) . . ? O2W Gd1 O2 77.4(2) . . ? O1W Gd1 O2 72.7(2) . . ? O1 Gd1 O2 114.95(18) 3_665 . ? O3 Gd1 O2 136.6(2) . . ? O4 Gd1 O2 143.5(2) . . ? O5 Gd1 O2 71.8(2) . . ? O6 Gd1 O2 105.2(2) . . ? O2W Gd1 O1 81.9(2) . . ? O1W Gd1 O1 123.06(19) . . ? O1 Gd1 O1 67.5(2) 3_665 . ? O3 Gd1 O1 147.7(2) . . ? O4 Gd1 O1 147.55(19) . . ? O5 Gd1 O1 83.1(2) . . ? O6 Gd1 O1 74.67(19) . . ? O2 Gd1 O1 50.62(18) . . ? O2W Gd1 C7 103.3(2) . . ? O1W Gd1 C7 75.0(2) . . ? O1 Gd1 C7 96.7(2) 3_665 . ? O3 Gd1 C7 25.7(2) . . ? O4 Gd1 C7 27.2(2) . . ? O5 Gd1 C7 99.4(3) . . ? O6 Gd1 C7 92.5(2) . . ? O2 Gd1 C7 147.2(2) . . ? O1 Gd1 C7 161.9(2) . . ? O2W Gd1 C13 160.2(2) . . ? O1W Gd1 C13 108.6(2) . . ? O1 Gd1 C13 96.9(2) 3_665 . ? O3 Gd1 C13 71.1(2) . . ? O4 Gd1 C13 121.0(2) . . ? O5 Gd1 C13 26.6(2) . . ? O6 Gd1 C13 26.1(2) . . ? O2 Gd1 C13 89.2(2) . . ? O1 Gd1 C13 78.3(2) . . ? C7 Gd1 C13 95.9(2) . . ? O2W Gd1 C1 80.9(2) . . ? O1W Gd1 C1 97.8(2) . . ? O1 Gd1 C1 92.3(2) 3_665 . ? O3 Gd1 C1 148.0(2) . . ? O4 Gd1 C1 158.0(2) . . ? O5 Gd1 C1 73.8(2) . . ? O6 Gd1 C1 88.2(2) . . ? O2 Gd1 C1 25.13(19) . . ? O1 Gd1 C1 25.70(19) . . ? C7 Gd1 C1 170.8(3) . . ? C13 Gd1 C1 80.8(2) . . ? O2 C1 O1 120.2(8) . . ? O2 C1 C2 120.9(7) . . ? O1 C1 C2 118.9(7) . . ? O2 C1 Gd1 59.9(4) . . ? O1 C1 Gd1 61.0(4) . . ? C2 C1 Gd1 169.9(6) . . ? C3 C2 C1 111.5(8) . . ? C3 C2 H2A 109.3 . . ? C1 C2 H2A 109.3 . . ? C3 C2 H2B 109.3 . . ? C1 C2 H2B 109.3 . . ? H2A C2 H2B 108.0 . . ? C4 C3 C6 111.5(10) . . ? C4 C3 C2 124.0(10) . . ? C6 C3 C2 124.5(9) . . ? C3 C4 S1 111.6(9) . . ? C3 C4 H4 124.2 . . ? S1 C4 H4 124.2 . . ? C6 C5 S1 104.2(7) . . ? C6 C5 H5 127.9 . . ? S1 C5 H5 127.9 . . ? C3 C6 C5 113.3(9) . . ? C3 C6 H6 123.4 . . ? C5 C6 H6 123.4 . . ? O3 C7 O4 120.3(8) . . ? O3 C7 C8 121.7(9) . . ? O4 C7 C8 118.0(8) . . ? O3 C7 Gd1 60.2(5) . . ? O4 C7 Gd1 60.4(4) . . ? C8 C7 Gd1 173.0(7) . . ? C9 C8 C7 116.4(9) . . ? C9 C8 H8A 108.2 . . ? C7 C8 H8A 108.2 . . ? C9 C8 H8B 108.2 . . ? C7 C8 H8B 108.2 . . ? H8A C8 H8B 107.3 . . ? C12 C9 C10 110.0(13) . . ? C12 C9 C8 123.9(12) . . ? C10 C9 C8 126.1(11) . . ? C9 C10 C11 114.4(12) . . ? C9 C10 H10 122.8 . . ? C11 C10 H10 122.8 . . ? C10 C11 S2 104.5(9) . . ? C10 C11 H11 127.8 . . ? S2 C11 H11 127.8 . . ? C9 C12 S2 112.6(12) . . ? C9 C12 H12 123.7 . . ? S2 C12 H12 123.7 . . ? O6 C13 O5 119.3(8) . . ? O6 C13 C14 120.9(8) . . ? O5 C13 C14 119.8(8) . . ? O6 C13 Gd1 59.8(4) . . ? O5 C13 Gd1 59.5(4) . . ? C14 C13 Gd1 177.3(6) . . ? C13 C14 C15 111.8(8) . . ? C13 C14 H14A 109.3 . . ? C15 C14 H14A 109.3 . . ? C13 C14 H14B 109.3 . . ? C15 C14 H14B 109.3 . . ? H14A C14 H14B 107.9 . . ? C16 C15 C18 111.8(10) . . ? C16 C15 C14 127.5(9) . . ? C18 C15 C14 120.7(9) . . ? C15 C16 S3 113.1(8) . . ? C15 C16 H16 123.5 . . ? S3 C16 H16 123.5 . . ? C18 C17 S3 108.4(8) . . ? C18 C17 H17 125.8 . . ? S3 C17 H17 125.8 . . ? C17 C18 C15 114.6(11) . . ? C17 C18 H18 122.7 . . ? C15 C18 H18 122.7 . . ? C1 O1 Gd1 149.9(5) . 3_665 ? C1 O1 Gd1 93.3(5) . . ? Gd1 O1 Gd1 112.5(2) 3_665 . ? C1 O2 Gd1 95.0(5) . . ? C7 O3 Gd1 94.1(6) . . ? C7 O4 Gd1 92.5(5) . . ? C13 O5 Gd1 93.8(5) . . ? C13 O6 Gd1 94.1(5) . . ? C5 S1 C4 99.4(5) . . ? C11 S2 C12 98.5(7) . . ? C16 S3 C17 92.0(6) . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.658 _refine_diff_density_min -1.536 _refine_diff_density_rms 0.369