data_global _journal_name_full 'Dalton Trans.' #TrackingRef '- compound1.cif' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Josef Hamacek' _publ_contact_author_address ; Department of Inorganic, Analytical and Applied Chemistry University of Geneva 30, quai E. Ansermet CH - 1211 Geneva 4 Switzerland ; _publ_contact_author_email Josef.Hamacek@unige.ch _publ_contact_author_phone '41 22 379 6413' loop_ _publ_author_name _publ_author_address S.Zebret ; Department of Inorganic, Analytical and Applied Chemistry University of Geneva 30, quai E. Ansermet CH - 1211 Geneva 4 Switzerland ; E.Torres ;Dipartimento di Chimica IFM and Molecular Imaging Center University of Torino Via P. Giuria 7 10125, Torino, Italy ; E.Terreno ;Dipartimento di Chimica IFM and Molecular Imaging Center University of Torino Via P. Giuria 7 10125, Torino, Italy ; L.Guenee ; Department of Inorganic, Analytical and Applied Chemistry University of Geneva 30, quai E. Ansermet CH - 1211 Geneva 4 Switzerland ; C.Senatore ;Dipartimento di Chimica IFM and Molecular Imaging Center Department of Condensed Matter Physics University of Geneva Rue de l'Ecole-de-Medecine 20 1211 Geneva 4 Switzerland ; J.Hamacek ; Department of Inorganic, Analytical and Applied Chemistry University of Geneva 30, quai E. Ansermet CH - 1211 Geneva 4 Switzerland ; _publ_section_title ; Structure, Stability and Relaxivity of Trinuclear Triangular Complexes ; data_1 _database_code_depnum_ccdc_archive 'CCDC 799378' #TrackingRef '- compound1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H30 Gd3 N9 O24,3.5(C2H6OS),12(H2O)' _chemical_formula_sum 'C49 H48 Gd3 N9 O39.5 S3.5' _chemical_formula_weight 1978.9 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M 'P a -3' _symmetry_space_group_name_Hall '-P 2AC 2AB 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' 'z, x, y' 'y, z, x' '-z+1/2, -x, y+1/2' '-y, z+1/2, -x+1/2' 'z+1/2, -x+1/2, -y' '-y+1/2, -z, x+1/2' '-z, x+1/2, -y+1/2' 'y+1/2, -z+1/2, -x' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' '-z, -x, -y' '-y, -z, -x' 'z-1/2, x, -y-1/2' 'y, -z-1/2, x-1/2' '-z-1/2, x-1/2, y' 'y-1/2, z, -x-1/2' 'z, -x-1/2, y-1/2' '-y-1/2, z-1/2, x' _cell_length_a 24.4761(11) _cell_length_b 24.4761(11) _cell_length_c 24.4761(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 14663.1(11) _cell_formula_units_Z 8 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 7995 _cell_measurement_theta_min 2.1 _cell_measurement_theta_max 25.95 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.29 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.79 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7752 _exptl_absorpt_coefficient_mu 2.89 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.4529 _exptl_absorpt_correction_T_max 0.5387 _exptl_absorpt_process_details 'XRED; Stoe & Cie, 1999' _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe Ipds' _diffrn_measurement_method \f _diffrn_detector_area_resol_mean 6 _diffrn_standards_decay_% 0 _diffrn_reflns_number 112918 _diffrn_reflns_av_R_equivalents 0.0554 _diffrn_reflns_av_sigmaI/netI 0.0208 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 26.03 _reflns_number_total 4816 _reflns_number_gt 3841 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'EXPOSE (Stoe & Cie, 1999)' _computing_cell_refinement 'CELL (Stoe & Cie, 1999)' _computing_data_reduction 'XRED (Stoe & Cie, 1999)' _computing_structure_solution SIR97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'diamond ' _computing_publication_material Shelxl_ACTA _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. hydrogen treatment: Hydrogen atoms of water molecules O1w O2w O4w O7 and O8 were observed and refined with restrains on bond lengths and bond angles. Hydrogen atoms of the disordered water molecule and of the two disordered DMSO solvant molecules were not observed nor calculated. All other hydrogen atoms were calculated and refined with restrains on bond lengths and bond angles. disorder : The water molecule O3W/O3Wb is disordered over two sites and occupancy parameters refined to 0.6 and 0.4 resp. One DMSO molecule is disordered over two sites with population parameters refined to 0.6 and 0.4 respectively. The other DMSO molecule is located around a -3 symmetry axes and refined with fixed population parameter of 1/6. ; _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^)+(0.0966P)^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 4816 _refine_ls_number_parameters 340 _refine_ls_number_restraints 28 _refine_ls_R_factor_all 0.0540 _refine_ls_R_factor_gt 0.0444 _refine_ls_wR_factor_ref 0.1314 _refine_ls_wR_factor_gt 0.1261 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.111 _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 0.160192(10) 0.365478(10) 0.203140(11) 0.02369(13) Uani 1 1 d . . . C1 C 0.1974(2) 0.4816(2) 0.2583(2) 0.0302(12) Uani 1 1 d . . . C2 C 0.2525(2) 0.4521(2) 0.2571(2) 0.0302(12) Uani 1 1 d . . . C3 C 0.2981(3) 0.4700(3) 0.2848(3) 0.0436(16) Uani 1 1 d . . . H3 H 0.2973 0.5038 0.3038 0.052 Uiso 1 1 calc R . . C4 C 0.3448(3) 0.4388(3) 0.2848(3) 0.0480(17) Uani 1 1 d . . . H4 H 0.3764 0.4503 0.3042 0.058 Uiso 1 1 calc R . . C5 C 0.3446(2) 0.3889(3) 0.2550(3) 0.0380(14) Uani 1 1 d . . . H5 H 0.3761 0.3661 0.2540 0.046 Uiso 1 1 calc R . . C6 C 0.2977(2) 0.3745(2) 0.2278(2) 0.0268(11) Uani 1 1 d . . . C7 C 0.2942(2) 0.3209(2) 0.1971(2) 0.0253(11) Uani 1 1 d . . . C8 C 0.2387(2) 0.2659(2) 0.1410(2) 0.0236(10) Uani 1 1 d . . . C9 C 0.1856(2) 0.2631(2) 0.1104(2) 0.0255(11) Uani 1 1 d . . . C10 C 0.1751(3) 0.2225(3) 0.0727(2) 0.0383(14) Uani 1 1 d . . . H10 H 0.2005 0.1937 0.0669 0.046 Uiso 1 1 calc R . . C11 C 0.1258(3) 0.2250(4) 0.0432(3) 0.0516(19) Uani 1 1 d . . . H11 H 0.1175 0.1982 0.0163 0.062 Uiso 1 1 calc R . . C12 C 0.0894(3) 0.2672(3) 0.0541(3) 0.0444(16) Uani 1 1 d . . . H12 H 0.0560 0.2698 0.0345 0.053 Uiso 1 1 calc R . . C13 C 0.1023(2) 0.3052(3) 0.0936(2) 0.0342(13) Uani 1 1 d . . . C14 C 0.0648(2) 0.3521(3) 0.1114(3) 0.0422(16) Uani 1 1 d . . . N1 N 0.25190(18) 0.40525(18) 0.22880(18) 0.0249(9) Uani 1 1 d . . . N2 N 0.24409(17) 0.31022(18) 0.17501(18) 0.0238(9) Uani 1 1 d . . . N3 N 0.14935(19) 0.3030(2) 0.12123(18) 0.0275(10) Uani 1 1 d . . . O1 O 0.15795(16) 0.45717(15) 0.23618(18) 0.0345(9) Uani 1 1 d . . . O2 O 0.19526(17) 0.52769(16) 0.28134(18) 0.0352(9) Uani 1 1 d . . . O3 O 0.07984(18) 0.3784(2) 0.1519(2) 0.0448(11) Uani 1 1 d . . . O4 O 0.02163(19) 0.3608(3) 0.0849(2) 0.0606(15) Uani 1 1 d . . . O5 O 0.33644(15) 0.29306(16) 0.19497(17) 0.0291(8) Uani 1 1 d . . . O6 O 0.27289(15) 0.22832(15) 0.13259(14) 0.0256(8) Uani 1 1 d . . . O7 O 0.08647(17) 0.37247(18) 0.2699(2) 0.0402(10) Uani 1 1 d D . . H7A H 0.068(2) 0.3441(16) 0.282(3) 0.048 Uiso 1 1 d D . . H7B H 0.069(2) 0.4046(14) 0.270(3) 0.048 Uiso 1 1 d D . . O8 O 0.1880(2) 0.4199(2) 0.12429(19) 0.0459(11) Uani 1 1 d D . . H8A H 0.172(2) 0.442(3) 0.099(2) 0.055 Uiso 1 1 d D . . H8B H 0.2237(12) 0.417(3) 0.114(3) 0.055 Uiso 1 1 d D . . O1W O 0.2830(2) 0.4128(2) 0.0643(3) 0.0614(14) Uiso 1 1 d D . . H1W H 0.291(3) 0.393(3) 0.0338(19) 0.074 Uiso 1 1 d D . . H2W H 0.305(3) 0.404(3) 0.092(2) 0.074 Uiso 1 1 d D . . O2W O 0.0266(3) 0.4645(3) 0.2679(3) 0.0686(15) Uiso 1 1 d D . . H3W H 0.015(3) 0.458(4) 0.2347(14) 0.082 Uiso 1 1 d D . . H4W H 0.015(4) 0.465(4) 0.3012(14) 0.082 Uiso 1 1 d D . . O3W O 0.4623(5) 0.3421(5) 0.4984(5) 0.072(2) Uiso 0.577(10) 1 d P . . O3WB O 0.4304(7) 0.3201(7) 0.4783(6) 0.072(2) Uiso 0.423(10) 1 d P . . O4W O 0.1412(3) 0.4053(3) 0.0217(3) 0.0780(18) Uiso 1 1 d D . . H7W H 0.1773(13) 0.413(4) 0.026(4) 0.094 Uiso 1 1 d D . . H8W H 0.127(3) 0.431(3) -0.002(3) 0.094 Uiso 1 1 d D . . S2S S 0.0411(7) 0.5271(8) -0.0114(5) 0.053(4) Uani 0.17 1 d P A -1 O2S O 0.0355(14) 0.5500(12) 0.0436(12) 0.053(8) Uani 0.17 1 d P A -1 C3S C 0.078(2) 0.465(2) -0.004(2) 0.054(11) Uiso 0.17 1 d P A -1 C4S C -0.015(3) 0.488(3) -0.037(2) 0.065(14) Uiso 0.17 1 d P A -1 S1A S 0.1365(3) 0.4158(3) 0.4478(3) 0.1177(17) Uiso 0.577(6) 1 d PD B 1 O1A O 0.1455(8) 0.4473(8) 0.3883(7) 0.121(5) Uiso 0.577(6) 1 d PD B 1 C1A C 0.0721(6) 0.3892(7) 0.4440(7) 0.077(4) Uiso 0.577(6) 1 d PD B 1 C2A C 0.1113(13) 0.4740(10) 0.4877(12) 0.152(9) Uiso 0.577(6) 1 d PD B 1 S1B S 0.1006(4) 0.4369(4) 0.4449(4) 0.1177(17) Uiso 0.423(6) 1 d PD B 2 O1B O 0.1253(11) 0.4536(11) 0.3870(8) 0.121(5) Uiso 0.423(6) 1 d PD B 2 C1B C 0.1180(10) 0.3648(7) 0.4387(10) 0.077(4) Uiso 0.423(6) 1 d PD B 2 C2B C 0.1500(15) 0.4497(17) 0.4961(12) 0.152(9) Uiso 0.423(6) 1 d PD B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.02069(17) 0.02112(17) 0.02926(18) 0.00333(10) 0.00042(10) 0.00188(9) C1 0.037(3) 0.021(3) 0.034(3) 0.002(2) 0.005(2) 0.000(2) C2 0.034(3) 0.024(3) 0.033(3) 0.004(2) 0.000(2) -0.001(2) C3 0.044(4) 0.031(3) 0.056(4) -0.011(3) -0.003(3) -0.004(3) C4 0.038(4) 0.044(4) 0.062(4) -0.023(3) -0.017(3) -0.002(3) C5 0.027(3) 0.034(3) 0.053(4) -0.009(3) -0.011(3) 0.004(2) C6 0.026(3) 0.025(3) 0.030(3) -0.004(2) -0.002(2) -0.001(2) C7 0.027(3) 0.025(3) 0.024(3) 0.002(2) -0.002(2) 0.002(2) C8 0.021(3) 0.028(3) 0.021(2) 0.005(2) 0.0014(19) -0.002(2) C9 0.022(3) 0.036(3) 0.018(2) 0.000(2) 0.000(2) -0.006(2) C10 0.036(3) 0.048(4) 0.031(3) -0.010(3) -0.002(3) -0.004(3) C11 0.047(4) 0.072(5) 0.035(4) -0.014(3) -0.013(3) -0.012(4) C12 0.027(3) 0.070(5) 0.036(3) -0.003(3) -0.008(3) -0.008(3) C13 0.020(3) 0.049(4) 0.034(3) 0.008(3) -0.006(2) -0.006(2) C14 0.021(3) 0.052(4) 0.053(4) 0.022(3) 0.000(3) 0.001(3) N1 0.026(2) 0.023(2) 0.026(2) 0.0019(18) -0.0016(18) 0.0001(17) N2 0.019(2) 0.026(2) 0.027(2) -0.0012(18) -0.0034(17) -0.0014(17) N3 0.023(2) 0.037(3) 0.022(2) 0.0078(19) -0.0003(18) -0.0028(19) O1 0.033(2) 0.0218(19) 0.048(3) -0.0012(17) 0.0000(19) 0.0041(16) O2 0.039(2) 0.024(2) 0.042(2) -0.0030(18) 0.0024(18) -0.0005(17) O3 0.032(2) 0.046(3) 0.057(3) 0.002(2) -0.011(2) 0.012(2) O4 0.024(2) 0.087(4) 0.070(4) 0.034(3) -0.015(2) 0.006(2) O5 0.0203(19) 0.028(2) 0.039(2) -0.0031(16) -0.0055(16) 0.0056(15) O6 0.0256(19) 0.0248(19) 0.0263(19) -0.0021(15) -0.0004(15) 0.0034(15) O7 0.030(2) 0.033(2) 0.058(3) 0.002(2) 0.013(2) 0.0015(17) O8 0.053(3) 0.044(3) 0.040(3) 0.019(2) -0.009(2) -0.008(2) S2S 0.068(12) 0.046(7) 0.046(7) -0.011(7) -0.007(6) -0.015(8) O2S 0.08(2) 0.039(15) 0.039(15) -0.012(12) 0.010(15) -0.019(16) _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 O3 2.354(4) . ? Gd1 O1 2.386(4) . ? Gd1 O7 2.440(4) . ? Gd1 O8 2.442(4) . ? Gd1 O6 2.444(4) 5 ? Gd1 O5 2.465(4) 5 ? Gd1 N1 2.526(4) . ? Gd1 N3 2.536(5) . ? Gd1 N2 2.553(4) . ? C1 O1 1.259(7) . ? C1 O2 1.262(7) . ? C1 C2 1.530(8) . ? C2 N1 1.339(7) . ? C2 C3 1.377(9) . ? C3 C4 1.376(10) . ? C3 H3 0.9500 . ? C4 C5 1.422(9) . ? C4 H4 0.9500 . ? C5 C6 1.374(8) . ? C5 H5 0.9500 . ? C6 N1 1.349(7) . ? C6 C7 1.517(7) . ? C7 O5 1.239(7) . ? C7 N2 1.365(7) . ? C8 O6 1.260(6) . ? C8 N2 1.374(7) . ? C8 C9 1.502(7) . ? C9 N3 1.344(7) . ? C9 C10 1.381(8) . ? C10 C11 1.409(9) . ? C10 H10 0.9500 . ? C11 C12 1.390(11) . ? C11 H11 0.9500 . ? C12 C13 1.379(9) . ? C12 H12 0.9500 . ? C13 N3 1.337(7) . ? C13 C14 1.531(10) . ? C14 O3 1.238(9) . ? C14 O4 1.259(8) . ? O5 Gd1 2.464(4) 6 ? O6 Gd1 2.444(4) 6 ? O7 H7A 0.88(2) . ? O7 H7B 0.89(2) . ? O8 H8A 0.900(15) . ? O8 H8B 0.91(2) . ? O1W H1W 0.91(2) . ? O1W H2W 0.89(2) . ? O2W H3W 0.87(2) . ? O2W H4W 0.86(2) . ? O3W O3WB 1.068(16) . ? O4W H7W 0.91(2) . ? O4W H8W 0.92(2) . ? S2S O2S 1.47(3) . ? S2S C3S 1.77(6) . ? S2S C4S 1.79(6) . ? S1A O1A 1.664(14) . ? S1A C1A 1.706(14) . ? S1A C2A 1.832(17) . ? S1B O1B 1.592(16) . ? S1B C2B 1.771(18) . ? S1B C1B 1.822(16) . ? 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 Gd1 O1 92.00(16) . . ? O3 Gd1 O7 74.32(17) . . ? O1 Gd1 O7 71.95(14) . . ? O3 Gd1 O8 74.83(17) . . ? O1 Gd1 O8 76.19(16) . . ? O7 Gd1 O8 134.20(17) . . ? O3 Gd1 O6 91.62(15) . 5 ? O1 Gd1 O6 141.30(14) . 5 ? O7 Gd1 O6 72.05(13) . 5 ? O8 Gd1 O6 141.46(15) . 5 ? O3 Gd1 O5 143.45(16) . 5 ? O1 Gd1 O5 88.66(14) . 5 ? O7 Gd1 O5 71.19(15) . 5 ? O8 Gd1 O5 140.08(15) . 5 ? O6 Gd1 O5 66.60(12) 5 5 ? O3 Gd1 N1 145.39(16) . . ? O1 Gd1 N1 64.77(14) . . ? O7 Gd1 N1 117.62(16) . . ? O8 Gd1 N1 74.85(16) . . ? O6 Gd1 N1 122.70(13) 5 . ? O5 Gd1 N1 65.30(13) 5 . ? O3 Gd1 N3 64.68(16) . . ? O1 Gd1 N3 146.41(14) . . ? O7 Gd1 N3 119.62(15) . . ? O8 Gd1 N3 74.54(16) . . ? O6 Gd1 N3 67.10(13) 5 . ? O5 Gd1 N3 124.62(14) 5 . ? N1 Gd1 N3 121.47(15) . . ? O3 Gd1 N2 126.82(16) . . ? O1 Gd1 N2 127.45(14) . . ? O7 Gd1 N2 144.33(15) . . ? O8 Gd1 N2 81.46(16) . . ? O6 Gd1 N2 78.41(13) 5 . ? O5 Gd1 N2 79.07(14) 5 . ? N1 Gd1 N2 63.67(14) . . ? N3 Gd1 N2 63.34(15) . . ? O1 C1 O2 125.8(5) . . ? O1 C1 C2 116.3(5) . . ? O2 C1 C2 117.9(5) . . ? N1 C2 C3 122.4(5) . . ? N1 C2 C1 113.9(5) . . ? C3 C2 C1 123.6(5) . . ? C4 C3 C2 119.7(6) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C3 C4 C5 118.3(6) . . ? C3 C4 H4 120.8 . . ? C5 C4 H4 120.8 . . ? C6 C5 C4 118.0(6) . . ? C6 C5 H5 121.0 . . ? C4 C5 H5 121.0 . . ? N1 C6 C5 123.0(5) . . ? N1 C6 C7 116.4(5) . . ? C5 C6 C7 120.6(5) . . ? O5 C7 N2 129.0(5) . . ? O5 C7 C6 116.7(5) . . ? N2 C7 C6 114.3(4) . . ? O6 C8 N2 127.7(5) . . ? O6 C8 C9 117.4(5) . . ? N2 C8 C9 114.8(5) . . ? N3 C9 C10 122.1(5) . . ? N3 C9 C8 116.2(5) . . ? C10 C9 C8 121.7(5) . . ? C9 C10 C11 118.1(6) . . ? C9 C10 H10 121.0 . . ? C11 C10 H10 121.0 . . ? C12 C11 C10 118.9(6) . . ? C12 C11 H11 120.6 . . ? C10 C11 H11 120.6 . . ? C13 C12 C11 119.3(6) . . ? C13 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? N3 C13 C12 121.6(6) . . ? N3 C13 C14 113.8(6) . . ? C12 C13 C14 124.6(6) . . ? O3 C14 O4 124.9(7) . . ? O3 C14 C13 116.1(5) . . ? O4 C14 C13 118.9(7) . . ? C2 N1 C6 118.5(5) . . ? C2 N1 Gd1 117.9(4) . . ? C6 N1 Gd1 121.3(3) . . ? C7 N2 C8 118.4(5) . . ? C7 N2 Gd1 121.0(3) . . ? C8 N2 Gd1 120.3(3) . . ? C13 N3 C9 119.9(5) . . ? C13 N3 Gd1 117.7(4) . . ? C9 N3 Gd1 121.6(3) . . ? C1 O1 Gd1 125.1(3) . . ? C14 O3 Gd1 127.2(4) . . ? C7 O5 Gd1 138.2(4) . 6 ? C8 O6 Gd1 139.0(3) . 6 ? Gd1 O7 H7A 124(4) . . ? Gd1 O7 H7B 114(4) . . ? H7A O7 H7B 116(5) . . ? Gd1 O8 H8A 138(4) . . ? Gd1 O8 H8B 116(4) . . ? H8A O8 H8B 106(4) . . ? H1W O1W H2W 111(5) . . ? H3W O2W H4W 141(7) . . ? H7W O4W H8W 107(4) . . ? O2S S2S C3S 106(2) . . ? O2S S2S C4S 117(2) . . ? C3S S2S C4S 89(3) . . ? S2S C3S H8W 156(5) . . ? O1A S1A C1A 104.6(10) . . ? O1A S1A C2A 98.7(12) . . ? C1A S1A C2A 90.9(12) . . ? O1B S1B C2B 109.0(16) . . ? O1B S1B C1B 94.9(12) . . ? C2B S1B C1B 94.0(15) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O7 H7A O2 0.88(2) 1.90(2) 2.788(6) 177(7) 22_556 O7 H7B O2W 0.89(2) 1.80(2) 2.688(8) 173(7) . O8 H8A O4W 0.900(15) 2.23(7) 2.784(9) 119(6) . O8 H8B O1W 0.91(2) 1.89(4) 2.756(8) 157(7) . O1W H1W O2 0.91(2) 2.17(8) 2.792(7) 124(7) 23_565 O1W H1W O1 0.91(2) 2.62(6) 3.345(7) 138(7) 23_565 O1W H2W S1A 0.89(2) 3.11(7) 3.796(9) 135(7) 6 O2W H3W O3WB 0.87(2) 1.76(4) 2.594(17) 161(9) 19_556 O2W H3W O3W 0.87(2) 1.93(3) 2.780(13) 166(9) 19_556 O2W H4W S1A 0.86(2) 2.90(6) 3.606(10) 140(7) 22_556 O4W H7W O8 0.91(2) 2.43(10) 2.784(9) 103(7) . O4W H7W O1 0.91(2) 2.80(10) 3.209(8) 108(8) 23_565 O4W H8W O3W 0.92(2) 2.08(7) 2.800(14) 135(7) 10_564 O4W H8W O2S 0.92(2) 2.16(6) 2.91(3) 139(7) 12_455 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.03 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 3.202 _refine_diff_density_min -1.372 _refine_diff_density_rms 0.149