# Electronic Supplementary Material for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Catalina Ruiz-Perez' _publ_contact_author_email CARUIZ@ULL.ES _publ_section_title ; Dinuclear and Two- and Three-Dimensional Gadolinium(III) Complexes with Mono- and Dicarboxylate Ligands: Synthesis, Structure 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' 'Joan Cano' 'Fernando S Delgado' 'Oscar Fabelo' ; M.Julve ; 'F Lloret' 'Jorge Pasan' # Attachment 'compound_1-3.cif' data_compound1 _database_code_depnum_ccdc_archive 'CCDC 721062' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H15 Gd O9' _chemical_formula_weight 388.43 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/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 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 9.0103(6) _cell_length_b 14.9957(11) _cell_length_c 9.0466(8) _cell_angle_alpha 90.00 _cell_angle_beta 96.139(7) _cell_angle_gamma 90.00 _cell_volume 1215.33(16) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _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 2.123 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 748 _exptl_absorpt_coefficient_mu 5.487 _exptl_absorpt_correction_type sphere _exptl_absorpt_correction_T_min 0.4066 _exptl_absorpt_correction_T_max 0.6680 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 8925 _diffrn_reflns_av_R_equivalents 0.0279 _diffrn_reflns_av_sigmaI/netI 0.0328 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 5.04 _diffrn_reflns_theta_max 27.50 _reflns_number_total 2770 _reflns_number_gt 2362 _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 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _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^)+(0.0143P)^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 2770 _refine_ls_number_parameters 205 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0289 _refine_ls_R_factor_gt 0.0193 _refine_ls_wR_factor_ref 0.0377 _refine_ls_wR_factor_gt 0.0358 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _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 0.582380(14) 0.129643(8) 0.007699(13) 0.00753(5) Uani 1 1 d . . . C1 C 0.4009(3) 0.05717(18) 0.2258(3) 0.0116(6) Uani 1 1 d . . . C2 C 0.3150(5) 0.0191(2) 0.3435(4) 0.0279(9) Uani 1 1 d . . . C3 C 0.8100(3) 0.11870(19) 0.2463(3) 0.0145(6) Uani 1 1 d . . . C4 C 0.9185(4) 0.1129(3) 0.3838(4) 0.0295(8) Uani 1 1 d . . . C5 C 0.3421(3) 0.16795(18) -0.2140(3) 0.0114(6) Uani 1 1 d . . . C6 C 0.2137(4) 0.1824(3) -0.3292(4) 0.0205(7) Uani 1 1 d . . . O1 O 0.4195(2) 0.01183(12) 0.1113(2) 0.0115(4) Uani 1 1 d . . . O2 O 0.4559(2) 0.13408(12) 0.23934(19) 0.0125(4) Uani 1 1 d . . . O3 O 0.7654(2) 0.04909(12) 0.1766(2) 0.0149(4) Uani 1 1 d . . . O4 O 0.7621(2) 0.19459(12) 0.2035(2) 0.0136(4) Uani 1 1 d . . . O5 O 0.3207(2) 0.16447(13) -0.0779(2) 0.0143(4) Uani 1 1 d . . . O6 O 0.4731(2) 0.15682(12) -0.25044(19) 0.0122(4) Uani 1 1 d . . . O1W O 0.5705(2) 0.28813(13) -0.0037(3) 0.0122(4) Uani 1 1 d . . . O2W O 0.7896(3) 0.15466(16) -0.1277(3) 0.0145(5) Uani 1 1 d . . . O3W O 0.0577(3) 0.0876(2) -0.0248(3) 0.0315(7) Uani 1 1 d . . . H2A H 0.220(6) 0.018(4) 0.305(6) 0.11(2) Uiso 1 1 d . . . H2B H 0.344(4) -0.039(3) 0.363(4) 0.041(11) Uiso 1 1 d . . . H2C H 0.307(4) 0.059(3) 0.415(4) 0.046(11) Uiso 1 1 d . . . H4A H 0.947(5) 0.056(3) 0.407(5) 0.070(15) Uiso 1 1 d . . . H4B H 0.873(5) 0.144(3) 0.470(5) 0.058(13) Uiso 1 1 d . . . H4C H 0.997(5) 0.154(3) 0.381(4) 0.061(14) Uiso 1 1 d . . . H6A H 0.145(4) 0.223(2) -0.293(4) 0.030(9) Uiso 1 1 d . . . H6B H 0.170(5) 0.133(3) -0.346(5) 0.053(14) Uiso 1 1 d . . . H6C H 0.246(4) 0.207(2) -0.420(4) 0.033(10) Uiso 1 1 d . . . H1WA H 0.524(4) 0.312(2) -0.081(4) 0.028(10) Uiso 1 1 d . . . H1WB H 0.539(4) 0.307(3) 0.059(4) 0.042(13) Uiso 1 1 d . . . H2WA H 0.864(6) 0.137(3) -0.095(6) 0.071(18) Uiso 1 1 d . . . H2WB H 0.792(4) 0.195(3) -0.174(4) 0.040(13) Uiso 1 1 d . . . H3WA H 0.063(5) 0.044(3) -0.054(5) 0.060(18) Uiso 1 1 d . . . H3WB H 0.116(4) 0.117(2) -0.038(4) 0.026(11) Uiso 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 0.00858(7) 0.00738(7) 0.00634(7) 0.00001(6) -0.00048(5) -0.00019(6) C1 0.0118(14) 0.0128(15) 0.0099(14) -0.0003(11) -0.0003(11) 0.0017(11) C2 0.046(3) 0.0170(19) 0.025(2) -0.0060(15) 0.0237(18) -0.0068(17) C3 0.0115(14) 0.0180(17) 0.0136(14) 0.0035(12) -0.0001(11) -0.0006(12) C4 0.033(2) 0.027(2) 0.0250(19) 0.0048(16) -0.0168(15) -0.0018(17) C5 0.0135(14) 0.0080(14) 0.0122(15) -0.0002(11) -0.0006(12) -0.0025(11) C6 0.0143(16) 0.032(2) 0.0144(17) 0.0015(15) -0.0043(13) 0.0013(15) O1 0.0141(11) 0.0095(10) 0.0110(10) -0.0010(8) 0.0021(8) 0.0002(8) O2 0.0176(10) 0.0106(10) 0.0092(9) -0.0019(8) 0.0007(8) -0.0022(8) O3 0.0149(10) 0.0106(10) 0.0181(11) 0.0011(8) -0.0029(9) 0.0031(8) O4 0.0146(10) 0.0118(10) 0.0131(10) -0.0004(8) -0.0042(8) -0.0003(8) O5 0.0137(10) 0.0197(11) 0.0094(10) 0.0010(8) 0.0002(8) -0.0014(8) O6 0.0127(10) 0.0133(10) 0.0106(10) 0.0005(8) 0.0008(8) 0.0012(8) O1W 0.0167(11) 0.0133(11) 0.0064(11) 0.0004(9) -0.0002(9) 0.0026(9) O2W 0.0117(12) 0.0149(12) 0.0166(12) 0.0050(9) 0.0012(9) 0.0017(9) O3W 0.0126(13) 0.0250(16) 0.0575(19) 0.0186(15) 0.0065(12) -0.0016(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 O2W 2.370(2) . ? Gd1 O1 2.3784(17) 3_655 ? Gd1 O1W 2.381(2) . ? Gd1 O3 2.4442(19) . ? Gd1 O5 2.4583(19) . ? Gd1 O4 2.4684(19) . ? Gd1 O6 2.4693(18) . ? Gd1 O2 2.4912(17) . ? Gd1 O1 2.5390(17) . ? Gd1 C3 2.819(3) . ? Gd1 C5 2.848(3) . ? Gd1 C1 2.905(3) . ? C1 O2 1.256(3) . ? C1 O1 1.265(3) . ? C1 C2 1.495(4) . ? C2 H2A 0.89(6) . ? C2 H2B 0.92(4) . ? C2 H2C 0.89(4) . ? C3 O3 1.263(3) . ? C3 O4 1.263(3) . ? C3 C4 1.500(4) . ? C4 H4A 0.90(5) . ? C4 H4B 1.03(4) . ? C4 H4C 0.95(5) . ? C5 O5 1.267(3) . ? C5 O6 1.270(3) . ? C5 C6 1.487(4) . ? C6 H6A 0.95(4) . ? C6 H6B 0.84(4) . ? C6 H6C 0.97(3) . ? O1 Gd1 2.3784(17) 3_655 ? O1W H1WA 0.85(4) . ? O1W H1WB 0.72(4) . ? O2W H2WA 0.75(5) . ? O2W H2WB 0.73(4) . ? O3W H3WA 0.71(5) . ? O3W H3WB 0.71(4) . ? 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 O1 82.83(7) . 3_655 ? O2W Gd1 O1W 81.60(8) . . ? O1 Gd1 O1W 150.78(7) 3_655 . ? O2W Gd1 O3 83.40(8) . . ? O1 Gd1 O3 79.27(6) 3_655 . ? O1W Gd1 O3 123.00(7) . . ? O2W Gd1 O5 125.86(8) . . ? O1 Gd1 O5 94.97(6) 3_655 . ? O1W Gd1 O5 74.76(7) . . ? O3 Gd1 O5 149.58(6) . . ? O2W Gd1 O4 79.39(7) . . ? O1 Gd1 O4 130.48(6) 3_655 . ? O1W Gd1 O4 70.14(7) . . ? O3 Gd1 O4 53.10(6) . . ? O5 Gd1 O4 132.51(6) . . ? O2W Gd1 O6 75.02(8) . . ? O1 Gd1 O6 74.71(6) 3_655 . ? O1W Gd1 O6 77.45(7) . . ? O3 Gd1 O6 147.87(6) . . ? O5 Gd1 O6 52.77(6) . . ? O4 Gd1 O6 141.08(6) . . ? O2W Gd1 O2 152.53(7) . . ? O1 Gd1 O2 115.01(6) 3_655 . ? O1W Gd1 O2 89.27(7) . . ? O3 Gd1 O2 80.00(6) . . ? O5 Gd1 O2 75.49(6) . . ? O4 Gd1 O2 73.14(6) . . ? O6 Gd1 O2 128.25(6) . . ? O2W Gd1 O1 145.01(7) . . ? O1 Gd1 O1 64.53(7) 3_655 . ? O1W Gd1 O1 133.27(6) . . ? O3 Gd1 O1 78.66(6) . . ? O5 Gd1 O1 72.02(6) . . ? O4 Gd1 O1 111.73(6) . . ? O6 Gd1 O1 106.04(6) . . ? O2 Gd1 O1 51.21(6) . . ? O2W Gd1 C3 81.72(8) . . ? O1 Gd1 C3 105.32(7) 3_655 . ? O1W Gd1 C3 96.72(8) . . ? O3 Gd1 C3 26.56(7) . . ? O5 Gd1 C3 148.05(7) . . ? O4 Gd1 C3 26.60(7) . . ? O6 Gd1 C3 156.59(7) . . ? O2 Gd1 C3 73.64(7) . . ? O1 Gd1 C3 94.51(7) . . ? O2W Gd1 C5 100.70(8) . . ? O1 Gd1 C5 83.85(7) 3_655 . ? O1W Gd1 C5 74.98(8) . . ? O3 Gd1 C5 162.02(7) . . ? O5 Gd1 C5 26.35(6) . . ? O4 Gd1 C5 144.74(7) . . ? O6 Gd1 C5 26.43(6) . . ? O2 Gd1 C5 101.84(7) . . ? O1 Gd1 C5 88.54(7) . . ? C3 Gd1 C5 170.77(8) . . ? O2W Gd1 C1 160.42(9) . . ? O1 Gd1 C1 89.79(7) 3_655 . ? O1W Gd1 C1 112.14(7) . . ? O3 Gd1 C1 77.40(7) . . ? O5 Gd1 C1 72.70(7) . . ? O4 Gd1 C1 91.96(7) . . ? O6 Gd1 C1 120.50(7) . . ? O2 Gd1 C1 25.47(6) . . ? O1 Gd1 C1 25.76(7) . . ? C3 Gd1 C1 82.80(8) . . ? C5 Gd1 C1 96.47(8) . . ? O2 C1 O1 119.2(2) . . ? O2 C1 C2 120.6(3) . . ? O1 C1 C2 120.2(3) . . ? O2 C1 Gd1 58.53(13) . . ? O1 C1 Gd1 60.75(13) . . ? C2 C1 Gd1 176.9(3) . . ? C1 C2 H2A 106(4) . . ? C1 C2 H2B 110(2) . . ? H2A C2 H2B 108(4) . . ? C1 C2 H2C 111(2) . . ? H2A C2 H2C 98(4) . . ? H2B C2 H2C 122(3) . . ? O3 C3 O4 120.7(3) . . ? O3 C3 C4 120.7(3) . . ? O4 C3 C4 118.5(3) . . ? O3 C3 Gd1 59.93(14) . . ? O4 C3 Gd1 61.03(14) . . ? C4 C3 Gd1 174.0(2) . . ? C3 C4 H4A 113(3) . . ? C3 C4 H4B 109(2) . . ? H4A C4 H4B 111(3) . . ? C3 C4 H4C 111(3) . . ? H4A C4 H4C 116(4) . . ? H4B C4 H4C 95(3) . . ? O5 C5 O6 119.3(3) . . ? O5 C5 C6 119.9(3) . . ? O6 C5 C6 120.8(2) . . ? O5 C5 Gd1 59.40(14) . . ? O6 C5 Gd1 59.91(14) . . ? C6 C5 Gd1 176.6(2) . . ? C5 C6 H6A 110(2) . . ? C5 C6 H6B 108(3) . . ? H6A C6 H6B 108(4) . . ? C5 C6 H6C 111(2) . . ? H6A C6 H6C 108(3) . . ? H6B C6 H6C 111(3) . . ? C1 O1 Gd1 148.75(17) . 3_655 ? C1 O1 Gd1 93.50(15) . . ? Gd1 O1 Gd1 115.47(7) 3_655 . ? C1 O2 Gd1 95.99(15) . . ? C3 O3 Gd1 93.51(16) . . ? C3 O4 Gd1 92.37(16) . . ? C5 O5 Gd1 94.25(16) . . ? C5 O6 Gd1 93.66(15) . . ? Gd1 O1W H1WA 118(2) . . ? Gd1 O1W H1WB 112(3) . . ? H1WA O1W H1WB 107(4) . . ? Gd1 O2W H2WA 118(4) . . ? Gd1 O2W H2WB 120(3) . . ? H2WA O2W H2WB 116(4) . . ? H3WA O3W H3WB 116(4) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.573 _refine_diff_density_min -0.496 _refine_diff_density_rms 0.119 data_compound2 _database_code_depnum_ccdc_archive 'CCDC 721063' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H9 Gd O8' _chemical_formula_weight 366.38 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 triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.4598(3) _cell_length_b 8.5490(6) _cell_length_c 8.8472(6) _cell_angle_alpha 118.662(5) _cell_angle_beta 113.552(5) _cell_angle_gamma 90.379(4) _cell_volume 498.80(5) _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 sheet _exptl_crystal_colour colourless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.439 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 346 _exptl_absorpt_coefficient_mu 6.670 _exptl_absorpt_correction_type sphere _exptl_absorpt_correction_T_min 0.4150 _exptl_absorpt_correction_T_max 0.6904 _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 4476 _diffrn_reflns_av_R_equivalents 0.0150 _diffrn_reflns_av_sigmaI/netI 0.0352 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 4.64 _diffrn_reflns_theta_max 27.49 _reflns_number_total 2907 _reflns_number_gt 1751 _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 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _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^)+(0.1012P)^2^+4.4846P] 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 geom _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2907 _refine_ls_number_parameters 136 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0526 _refine_ls_R_factor_gt 0.0476 _refine_ls_wR_factor_ref 0.1484 _refine_ls_wR_factor_gt 0.1450 _refine_ls_goodness_of_fit_ref 1.143 _refine_ls_restrained_S_all 1.143 _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 0.11164(6) 0.25979(6) 0.14687(6) 0.0138(2) Uani 1 1 d . . . C1 C -0.1671(17) 0.1392(17) 0.2063(17) 0.027(3) Uani 1 1 d . . . C2 C -0.293(4) 0.074(3) 0.249(4) 0.090(9) Uani 1 1 d . . . H2A H -0.3076 -0.0556 0.1968 0.135 Uiso 1 1 calc R . . H2B H -0.4057 0.0981 0.1916 0.135 Uiso 1 1 calc R . . H2C H -0.2494 0.1373 0.3869 0.135 Uiso 1 1 calc R . . C3 C 0.3729(16) 0.4162(16) 0.0951(16) 0.024(2) Uani 1 1 d . . . C4 C 0.5120(19) 0.501(2) 0.078(2) 0.037(3) Uani 1 1 d . . . H4 H 0.6236 0.5608 0.1852 0.044 Uiso 1 1 calc R . . C5 C -0.2863(14) 0.0545(15) -0.2663(14) 0.019(2) Uani 1 1 d . . . C6 C -0.4315(15) 0.0718(15) -0.4237(16) 0.021(2) Uani 1 1 d . . . H6 H -0.4257 0.1849 -0.4146 0.025 Uiso 1 1 calc R . . O1 O -0.0885(10) 0.0300(11) 0.1201(11) 0.0198(16) Uani 1 1 d . . . O2 O -0.1246(12) 0.3052(12) 0.2593(13) 0.0294(19) Uani 1 1 d . . . O3 O 0.4121(12) 0.4174(14) 0.2494(13) 0.033(2) Uani 1 1 d . . . O4 O 0.2176(11) 0.3425(12) -0.0387(12) 0.0266(18) Uani 1 1 d . . . O5 O -0.1648(10) 0.1989(12) -0.1356(11) 0.0205(16) Uani 1 1 d . . . O6 O -0.2999(11) -0.0981(10) -0.2773(12) 0.0236(17) Uani 1 1 d . . . O1W O 0.2384(12) 0.4353(13) 0.4920(11) 0.030(2) Uani 1 1 d . . . O2W O 0.0700(12) 0.5649(12) 0.2269(13) 0.0303(19) 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 0.0133(3) 0.0131(3) 0.0142(3) 0.0072(2) 0.0056(2) 0.0020(2) C1 0.029(6) 0.024(6) 0.025(6) 0.008(5) 0.016(5) 0.006(5) C2 0.13(2) 0.037(9) 0.16(2) 0.034(12) 0.13(2) 0.020(11) C3 0.023(5) 0.023(5) 0.020(5) 0.009(4) 0.008(4) -0.001(5) C4 0.022(6) 0.054(9) 0.042(7) 0.034(7) 0.010(6) 0.001(6) C5 0.013(5) 0.023(5) 0.011(4) 0.008(4) -0.003(4) 0.002(4) C6 0.020(5) 0.021(5) 0.023(5) 0.013(4) 0.008(4) 0.008(4) O1 0.021(4) 0.022(4) 0.022(4) 0.011(3) 0.014(3) 0.005(3) O2 0.033(5) 0.022(4) 0.039(5) 0.013(4) 0.026(4) 0.006(4) O3 0.022(4) 0.052(6) 0.030(4) 0.026(4) 0.010(4) -0.002(4) O4 0.018(4) 0.032(4) 0.025(4) 0.016(4) 0.006(3) -0.003(3) O5 0.014(3) 0.032(4) 0.019(3) 0.014(3) 0.009(3) 0.000(3) O6 0.021(4) 0.015(4) 0.029(4) 0.015(3) 0.003(3) -0.002(3) O1W 0.029(4) 0.038(5) 0.016(4) 0.008(4) 0.011(3) 0.012(4) O2W 0.033(5) 0.023(4) 0.038(5) 0.019(4) 0.016(4) 0.009(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 O1W 2.386(8) . ? Gd1 O1 2.401(7) 2 ? Gd1 O2W 2.422(8) . ? Gd1 O6 2.423(8) 2 ? Gd1 O1 2.443(8) . ? Gd1 O3 2.457(9) . ? Gd1 O5 2.460(7) . ? Gd1 O4 2.506(9) . ? Gd1 O2 2.522(8) . ? Gd1 C3 2.870(13) . ? Gd1 C1 2.894(14) . ? Gd1 Gd1 3.8659(10) 2 ? C1 O2 1.258(16) . ? C1 O1 1.274(14) . ? C1 C2 1.45(2) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 O4 1.247(14) . ? C3 O3 1.264(16) . ? C3 C4 1.48(2) . ? C4 C4 1.30(3) 2_665 ? C4 H4 0.9300 . ? C5 O5 1.257(13) . ? C5 O6 1.262(13) . ? C5 C6 1.517(14) . ? C6 C6 1.35(2) 2_454 ? C6 H6 0.9300 . ? O1 Gd1 2.401(7) 2 ? O6 Gd1 2.423(8) 2 ? 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 142.4(3) . 2 ? O1W Gd1 O2W 75.2(3) . . ? O1 Gd1 O2W 141.4(3) 2 . ? O1W Gd1 O6 70.7(3) . 2 ? O1 Gd1 O6 71.9(3) 2 2 ? O2W Gd1 O6 142.3(3) . 2 ? O1W Gd1 O1 92.4(3) . . ? O1 Gd1 O1 74.1(3) 2 . ? O2W Gd1 O1 123.4(3) . . ? O6 Gd1 O1 74.2(3) 2 . ? O1W Gd1 O3 76.5(3) . . ? O1 Gd1 O3 98.4(3) 2 . ? O2W Gd1 O3 80.0(3) . . ? O6 Gd1 O3 76.9(3) 2 . ? O1 Gd1 O3 151.1(3) . . ? O1W Gd1 O5 138.7(3) . . ? O1 Gd1 O5 73.8(3) 2 . ? O2W Gd1 O5 76.9(3) . . ? O6 Gd1 O5 140.6(3) 2 . ? O1 Gd1 O5 78.4(3) . . ? O3 Gd1 O5 127.2(3) . . ? O1W Gd1 O4 122.9(3) . . ? O1 Gd1 O4 75.2(3) 2 . ? O2W Gd1 O4 73.9(3) . . ? O6 Gd1 O4 112.2(3) 2 . ? O1 Gd1 O4 144.6(3) . . ? O3 Gd1 O4 51.7(3) . . ? O5 Gd1 O4 76.4(3) . . ? O1W Gd1 O2 68.3(3) . . ? O1 Gd1 O2 121.2(3) 2 . ? O2W Gd1 O2 73.0(3) . . ? O6 Gd1 O2 107.7(3) 2 . ? O1 Gd1 O2 51.6(3) . . ? O3 Gd1 O2 139.9(3) . . ? O5 Gd1 O2 74.7(3) . . ? O4 Gd1 O2 140.0(3) . . ? O1W Gd1 C3 100.0(3) . . ? O1 Gd1 C3 86.7(3) 2 . ? O2W Gd1 C3 75.2(3) . . ? O6 Gd1 C3 95.1(3) 2 . ? O1 Gd1 C3 160.1(3) . . ? O3 Gd1 C3 26.0(3) . . ? O5 Gd1 C3 101.6(3) . . ? O4 Gd1 C3 25.7(3) . . ? O2 Gd1 C3 148.0(3) . . ? O1W Gd1 C1 78.8(3) . . ? O1 Gd1 C1 98.2(3) 2 . ? O2W Gd1 C1 98.3(3) . . ? O6 Gd1 C1 90.5(3) 2 . ? O1 Gd1 C1 25.9(3) . . ? O3 Gd1 C1 154.8(3) . . ? O5 Gd1 C1 75.8(3) . . ? O4 Gd1 C1 152.2(3) . . ? O2 Gd1 C1 25.7(3) . . ? C3 Gd1 C1 173.5(3) . . ? O1W Gd1 Gd1 121.2(2) . 2 ? O1 Gd1 Gd1 37.44(19) 2 2 ? O2W Gd1 Gd1 146.5(2) . 2 ? O6 Gd1 Gd1 68.57(18) 2 2 ? O1 Gd1 Gd1 36.69(17) . 2 ? O3 Gd1 Gd1 130.1(2) . 2 ? O5 Gd1 Gd1 72.5(2) . 2 ? O4 Gd1 Gd1 110.9(2) . 2 ? O2 Gd1 Gd1 85.9(2) . 2 ? C3 Gd1 Gd1 124.0(2) . 2 ? C1 Gd1 Gd1 61.3(2) . 2 ? O2 C1 O1 117.2(12) . . ? O2 C1 C2 122.1(12) . . ? O1 C1 C2 120.6(13) . . ? O2 C1 Gd1 60.4(7) . . ? O1 C1 Gd1 56.9(6) . . ? C2 C1 Gd1 174.2(15) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? O4 C3 O3 119.0(13) . . ? O4 C3 C4 121.8(12) . . ? O3 C3 C4 119.2(11) . . ? O4 C3 Gd1 60.6(7) . . ? O3 C3 Gd1 58.4(7) . . ? C4 C3 Gd1 177.4(9) . . ? C4 C4 C3 123.9(17) 2_665 . ? C4 C4 H4 118.0 2_665 . ? C3 C4 H4 118.0 . . ? O5 C5 O6 127.1(9) . . ? O5 C5 C6 114.8(10) . . ? O6 C5 C6 118.1(9) . . ? C6 C6 C5 121.9(13) 2_454 . ? C6 C6 H6 119.0 2_454 . ? C5 C6 H6 119.0 . . ? C1 O1 Gd1 148.1(8) . 2 ? C1 O1 Gd1 97.2(8) . . ? Gd1 O1 Gd1 105.9(3) 2 . ? C1 O2 Gd1 93.9(7) . . ? C3 O3 Gd1 95.6(8) . . ? C3 O4 Gd1 93.7(8) . . ? C5 O5 Gd1 131.2(7) . . ? C5 O6 Gd1 138.6(7) . 2 ? _diffrn_measured_fraction_theta_max 0.933 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 1.461 _refine_diff_density_min -O.957 _refine_diff_density_rms 0.387 data_compound3 _database_code_depnum_ccdc_archive 'CCDC 721064' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C5 H10 Gd O10' _chemical_formula_weight 387.38 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 orthorhombic _symmetry_space_group_name_H-M 'F d d d' _symmetry_space_group_name_Hall '-F 2uv 2vw' _symmetry_Int_Tables_number 70 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/4, -y+1/4, z' 'x, -y+1/4, -z+1/4' '-x+1/4, y, -z+1/4' 'x, y+1/2, z+1/2' '-x+1/4, -y+3/4, z+1/2' 'x, -y+3/4, -z+3/4' '-x+1/4, y+1/2, -z+3/4' 'x+1/2, y, z+1/2' '-x+3/4, -y+1/4, z+1/2' 'x+1/2, -y+1/4, -z+3/4' '-x+3/4, y, -z+3/4' 'x+1/2, y+1/2, z' '-x+3/4, -y+3/4, z' 'x+1/2, -y+3/4, -z+1/4' '-x+3/4, y+1/2, -z+1/4' '-x, -y, -z' 'x-1/4, y-1/4, -z' '-x, y-1/4, z-1/4' 'x-1/4, -y, z-1/4' '-x, -y+1/2, -z+1/2' 'x-1/4, y+1/4, -z+1/2' '-x, y+1/4, z+1/4' 'x-1/4, -y+1/2, z+1/4' '-x+1/2, -y, -z+1/2' 'x+1/4, y-1/4, -z+1/2' '-x+1/2, y-1/4, z+1/4' 'x+1/4, -y, z+1/4' '-x+1/2, -y+1/2, -z' 'x+1/4, y+1/4, -z' '-x+1/2, y+1/4, z-1/4' 'x+1/4, -y+1/2, z-1/4' _cell_length_a 9.6673(3) _cell_length_b 15.4344(3) _cell_length_c 27.2399(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4064.44(16) _cell_formula_units_Z 16 _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 0.18 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.532 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2944 _exptl_absorpt_coefficient_mu 6.570 _exptl_absorpt_correction_type sphere _exptl_absorpt_correction_T_min 0.3843 _exptl_absorpt_correction_T_max 0.5595 _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 6738 _diffrn_reflns_av_R_equivalents 0.0328 _diffrn_reflns_av_sigmaI/netI 0.0255 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 6.51 _diffrn_reflns_theta_max 27.49 _reflns_number_total 1154 _reflns_number_gt 944 _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 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _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^)+(0.0011P)^2^+13.8866P] 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 1154 _refine_ls_number_parameters 86 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0363 _refine_ls_R_factor_gt 0.0238 _refine_ls_wR_factor_ref 0.0375 _refine_ls_wR_factor_gt 0.0354 _refine_ls_goodness_of_fit_ref 1.143 _refine_ls_restrained_S_all 1.143 _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 1.1250 0.1250 0.509381(8) 0.02052(8) Uani 1 2 d S . . C1 C 0.8151(4) 0.0902(2) 0.52909(13) 0.0207(8) Uani 1 1 d . . . C2 C 0.6622(4) 0.0906(3) 0.53217(16) 0.0341(10) Uani 1 1 d . . . C3 C 1.1250 0.0751(3) 0.6250 0.0173(9) Uani 1 2 d S . . O1 O 0.8700(3) 0.01984(15) 0.51640(8) 0.0293(6) Uani 1 1 d . . . O2 O 0.8871(3) 0.15571(14) 0.53787(9) 0.0301(6) Uani 1 1 d . . . O3 O 1.1147(3) 0.03891(14) 0.58415(8) 0.0224(5) Uani 1 1 d . . . O1W O 1.2753(3) 0.1238(3) 0.43637(11) 0.0319(7) Uani 1 1 d . . . O2W O 1.1970(5) 0.0478(3) 0.34744(18) 0.1000(16) Uani 1 1 d . . . H1WA H 1.302(6) 0.168(4) 0.428(2) 0.08(2) Uiso 1 1 d . . . H1WB H 1.261(6) 0.098(4) 0.416(2) 0.06(2) Uiso 1 1 d . . . H2 H 0.610(6) 0.042(4) 0.527(2) 0.077(18) Uiso 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 0.03006(14) 0.01826(12) 0.01323(11) 0.000 0.000 0.00702(13) C1 0.0179(19) 0.0263(18) 0.0181(17) -0.0003(15) 0.0018(15) 0.0027(15) C2 0.030(3) 0.030(2) 0.043(2) -0.0039(19) 0.0028(19) 0.0003(17) C3 0.014(2) 0.020(2) 0.018(2) 0.000 -0.001(2) 0.000 O1 0.0376(15) 0.0241(13) 0.0262(13) -0.0040(10) 0.0008(15) 0.0063(13) O2 0.0308(16) 0.0233(12) 0.0362(14) -0.0028(11) 0.0000(15) -0.0054(13) O3 0.0341(15) 0.0179(11) 0.0152(11) -0.0013(9) -0.0019(13) 0.0004(12) O1W 0.0450(18) 0.0272(16) 0.0235(15) -0.0042(17) 0.0056(13) -0.0072(16) O2W 0.096(4) 0.108(4) 0.096(3) -0.059(3) -0.005(3) -0.015(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 O1 2.344(2) 17_756 ? Gd1 O1 2.344(2) 30_556 ? Gd1 O3 2.434(2) 2_755 ? Gd1 O3 2.434(2) . ? Gd1 O1W 2.463(3) 2_755 ? Gd1 O1W 2.463(3) . ? Gd1 O2 2.474(3) 2_755 ? Gd1 O2 2.474(3) . ? C1 O2 1.250(4) . ? C1 O1 1.257(4) . ? C1 C2 1.481(5) . ? C2 C2 1.282(8) 2_655 ? C2 H2 0.92(6) . ? C3 O3 1.249(3) . ? C3 O3 1.249(3) 4_756 ? C3 C3 1.540(8) 2_755 ? O1 Gd1 2.344(2) 17_756 ? O1W H1WA 0.76(7) . ? O1W H1WB 0.69(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Gd1 O1 145.13(11) 17_756 30_556 ? O1 Gd1 O3 140.41(8) 17_756 2_755 ? O1 Gd1 O3 74.39(8) 30_556 2_755 ? O1 Gd1 O3 74.39(8) 17_756 . ? O1 Gd1 O3 140.41(8) 30_556 . ? O3 Gd1 O3 66.39(10) 2_755 . ? O1 Gd1 O1W 77.14(12) 17_756 2_755 ? O1 Gd1 O1W 74.85(12) 30_556 2_755 ? O3 Gd1 O1W 134.09(10) 2_755 2_755 ? O3 Gd1 O1W 130.97(11) . 2_755 ? O1 Gd1 O1W 74.85(12) 17_756 . ? O1 Gd1 O1W 77.14(12) 30_556 . ? O3 Gd1 O1W 130.97(12) 2_755 . ? O3 Gd1 O1W 134.09(10) . . ? O1W Gd1 O1W 72.30(15) 2_755 . ? O1 Gd1 O2 83.79(9) 17_756 2_755 ? O1 Gd1 O2 107.23(9) 30_556 2_755 ? O3 Gd1 O2 78.70(9) 2_755 2_755 ? O3 Gd1 O2 70.79(9) . 2_755 ? O1W Gd1 O2 143.45(9) 2_755 2_755 ? O1W Gd1 O2 72.75(10) . 2_755 ? O1 Gd1 O2 107.23(9) 17_756 . ? O1 Gd1 O2 83.79(9) 30_556 . ? O3 Gd1 O2 70.79(9) 2_755 . ? O3 Gd1 O2 78.70(9) . . ? O1W Gd1 O2 72.75(10) 2_755 . ? O1W Gd1 O2 143.45(9) . . ? O2 Gd1 O2 143.43(12) 2_755 . ? O2 C1 O1 121.1(3) . . ? O2 C1 C2 122.8(3) . . ? O1 C1 C2 116.1(3) . . ? C2 C2 C1 124.3(6) 2_655 . ? C2 C2 H2 112(4) 2_655 . ? C1 C2 H2 123(4) . . ? O3 C3 O3 126.9(4) . 4_756 ? O3 C3 C3 116.6(2) . 2_755 ? O3 C3 C3 116.6(2) 4_756 2_755 ? C1 O1 Gd1 156.2(3) . 17_756 ? C1 O2 Gd1 107.6(2) . . ? C3 O3 Gd1 119.9(2) . . ? Gd1 O1W H1WA 116(5) . . ? Gd1 O1W H1WB 121(5) . . ? H1WA O1W H1WB 109(6) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.628 _refine_diff_density_min -0.504 _refine_diff_density_rms 0.111