data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Dr M Mazzanti' _publ_contact_author_address ; Departement de Recherche Fondamentale sur la Matiere Condensee Laboratoire de Reconnaissance Ionique CEA - Grenoble 17 rue des Martyrs Grenoble F-38054 FRANCE ; _publ_contact_author_email MAZZANTI@DRFMC.CENG.CEA.FR _publ_section_title ; The effect of pyridinecarboxylate chelating groups on the stability and electronic relaxation of gadolinium complexes ; loop_ _publ_author_name 'M. Mazzanti' 'Alain Borel' 'Nicholas P. Chatterton' 'Christelle Gateau' 'Lothar Helm' 'Andre E. Merbach' ; J.Pecaut ; data_struc_for_1 _database_code_depnum_ccdc_archive 'CCDC 253404' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H32 Cl2 N4 O12' _chemical_formula_weight 591.40 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.159(2) _cell_length_b 8.014(3) _cell_length_c 24.123(8) _cell_angle_alpha 84.739(6) _cell_angle_beta 87.999(6) _cell_angle_gamma 75.022(6) _cell_volume 1331.3(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.475 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 620 _exptl_absorpt_coefficient_mu 0.312 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5850 _diffrn_reflns_av_R_equivalents 0.0131 _diffrn_reflns_av_sigmaI/netI 0.0267 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 23.21 _reflns_number_total 3727 _reflns_number_gt 3010 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0481P)^2^+0.8156P] 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 3727 _refine_ls_number_parameters 471 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0565 _refine_ls_R_factor_gt 0.0436 _refine_ls_wR_factor_ref 0.1092 _refine_ls_wR_factor_gt 0.1043 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _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 Cl1 Cl 0.63533(13) 0.26102(11) 0.85398(4) 0.0621(3) Uani 1 1 d . . . Cl2 Cl 1.11591(13) 0.77549(11) 0.67502(3) 0.0587(3) Uani 1 1 d . . . O1 O 0.8264(4) 0.3127(3) 1.05913(10) 0.0727(7) Uani 1 1 d . . . O2 O 0.7714(4) 0.2415(3) 0.97694(13) 0.0704(8) Uani 1 1 d . . . H2O H 0.740(5) 0.281(5) 0.9450(16) 0.068(13) Uiso 1 1 d . . . O3 O 1.0799(3) 0.3578(3) 0.84614(10) 0.0575(6) Uani 1 1 d . . . O4 O 1.2855(3) 0.5220(3) 0.82220(10) 0.0592(6) Uani 1 1 d . . . H4O H 1.380(6) 0.419(5) 0.8347(16) 0.082(13) Uiso 1 1 d . . . O5 O 0.7324(3) 0.7820(3) 0.50876(8) 0.0522(6) Uani 1 1 d . . . O6 O 0.6888(3) 0.6834(3) 0.42819(8) 0.0449(5) Uani 1 1 d . . . H6O H 0.671(5) 0.783(5) 0.4166(15) 0.070(13) Uiso 1 1 d . . . O7 O 0.6498(4) 0.1155(3) 0.72188(12) 0.0708(7) Uani 1 1 d . . . O8 O 0.3373(3) 0.2566(3) 0.72078(10) 0.0563(6) Uani 1 1 d . . . H8O H 0.324(7) 0.159(7) 0.738(2) 0.122(19) Uiso 1 1 d . . . N1 N 0.7633(3) 0.6185(3) 0.81732(9) 0.0358(6) Uani 1 1 d . . . H1N H 0.775(4) 0.524(4) 0.8357(12) 0.035(8) Uiso 1 1 d . . . N2 N 0.7468(3) 0.4301(3) 0.67793(9) 0.0327(5) Uani 1 1 d . . . H2N H 0.735(4) 0.528(4) 0.6602(12) 0.039(8) Uiso 1 1 d . . . N3 N 0.7047(3) 0.5673(3) 0.93242(9) 0.0403(6) Uani 1 1 d . . . N4 N 0.8043(3) 0.4623(3) 0.56086(9) 0.0326(5) Uani 1 1 d . . . C1 C 0.6176(5) 0.7507(4) 0.84820(13) 0.0434(8) Uani 1 1 d . . . H1A H 0.615(4) 0.856(4) 0.8327(12) 0.044(9) Uiso 1 1 d . . . H1B H 0.493(4) 0.722(4) 0.8427(11) 0.041(8) Uiso 1 1 d . . . C2 C 0.6675(4) 0.7298(4) 0.90913(11) 0.0386(7) Uani 1 1 d . . . C3 C 0.6704(5) 0.8676(4) 0.93909(13) 0.0502(8) Uani 1 1 d . . . H3 H 0.644(5) 0.979(4) 0.9209(13) 0.061(10) Uiso 1 1 d . . . C4 C 0.7109(6) 0.8380(4) 0.99493(14) 0.0567(9) Uani 1 1 d . . . H4 H 0.712(5) 0.931(5) 1.0161(14) 0.067(10) Uiso 1 1 d . . . C5 C 0.7460(5) 0.6721(4) 1.01969(14) 0.0525(9) Uani 1 1 d . . . H5 H 0.774(5) 0.650(5) 1.0538(16) 0.071(12) Uiso 1 1 d . . . C6 C 0.7431(4) 0.5403(4) 0.98699(12) 0.0429(7) Uani 1 1 d . . . C7 C 0.7835(5) 0.3557(4) 1.01066(15) 0.0528(8) Uani 1 1 d . . . C8 C 0.9588(5) 0.6546(4) 0.81509(14) 0.0437(8) Uani 1 1 d . . . H8A H 0.976(4) 0.712(4) 0.7789(13) 0.045(8) Uiso 1 1 d . . . H8B H 0.960(4) 0.735(4) 0.8399(13) 0.050(9) Uiso 1 1 d . . . C9 C 1.1141(4) 0.4927(4) 0.82944(11) 0.0431(7) Uani 1 1 d . . . C11 C 0.8920(5) 0.2947(4) 0.64786(12) 0.0390(7) Uani 1 1 d . . . H11A H 0.900(4) 0.184(4) 0.6686(12) 0.046(8) Uiso 1 1 d . . . H11B H 1.008(5) 0.324(4) 0.6507(12) 0.044(9) Uiso 1 1 d . . . C12 C 0.8393(4) 0.3035(3) 0.58763(11) 0.0333(6) Uani 1 1 d . . . C13 C 0.8292(5) 0.1606(4) 0.56113(13) 0.0440(8) Uani 1 1 d . . . H13 H 0.849(4) 0.060(4) 0.5813(12) 0.048(9) Uiso 1 1 d . . . C14 C 0.7854(5) 0.1799(4) 0.50569(13) 0.0457(8) Uani 1 1 d . . . H14 H 0.775(5) 0.088(4) 0.4887(13) 0.062(10) Uiso 1 1 d . . . C15 C 0.7535(4) 0.3424(4) 0.47764(13) 0.0394(7) Uani 1 1 d . . . H15 H 0.726(4) 0.358(4) 0.4435(12) 0.036(8) Uiso 1 1 d . . . C16 C 0.7616(4) 0.4806(3) 0.50664(11) 0.0312(6) Uani 1 1 d . . . C17 C 0.7261(4) 0.6644(4) 0.48144(11) 0.0341(6) Uani 1 1 d . . . C18 C 0.5454(4) 0.4069(4) 0.67858(13) 0.0362(7) Uani 1 1 d . . . H18A H 0.457(4) 0.509(3) 0.6919(10) 0.029(7) Uiso 1 1 d . . . H18B H 0.510(4) 0.408(3) 0.6423(12) 0.034(7) Uiso 1 1 d . . . C19 C 0.5208(5) 0.2420(4) 0.71019(12) 0.0421(7) Uani 1 1 d . . . C21 C 0.6910(5) 0.6024(4) 0.76072(12) 0.0387(7) Uani 1 1 d . . . H21A H 0.687(4) 0.711(4) 0.7411(11) 0.034(7) Uiso 1 1 d . . . H21B H 0.563(4) 0.591(3) 0.7686(11) 0.037(8) Uiso 1 1 d . . . C22 C 0.8189(5) 0.4480(4) 0.73423(12) 0.0366(7) Uani 1 1 d . . . H22A H 0.940(4) 0.459(3) 0.7273(11) 0.031(7) Uiso 1 1 d . . . H22B H 0.829(4) 0.346(4) 0.7582(11) 0.037(8) Uiso 1 1 d . . . O11 O 0.3719(6) 1.0049(4) 0.61595(13) 0.0738(9) Uani 1 1 d . . . H1O1 H 0.303(6) 0.955(6) 0.6295(18) 0.077(15) Uiso 1 1 d . . . H2O1 H 0.480(6) 0.955(6) 0.6193(18) 0.080(16) Uiso 1 1 d . . . O12 O 1.1126(11) -0.0160(6) 0.8682(2) 0.144(3) Uani 1 1 d . . . H1O2 H 1.048(10) 0.056(8) 0.867(3) 0.14(3) Uiso 1 1 d . . . H2O2 H 1.113(7) -0.056(6) 0.8898(19) 0.073(16) Uiso 1 1 d . . . O13 O 0.7281(4) 0.7633(3) 0.62808(13) 0.0495(6) Uani 1 1 d . . . H1O3 H 0.826(6) 0.776(5) 0.6414(16) 0.067(14) Uiso 1 1 d . . . H2O3 H 0.747(5) 0.741(4) 0.6016(15) 0.044(13) Uiso 1 1 d . . . O14 O 0.2555(5) -0.0213(4) 0.76347(15) 0.0900(11) Uani 1 1 d . . . H1O4 H 0.202(9) -0.078(8) 0.735(2) 0.16(2) Uiso 1 1 d . . . H2O4 H 0.229(5) -0.025(5) 0.7929(15) 0.054(12) 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 Cl1 0.0651(6) 0.0623(5) 0.0603(5) 0.0104(4) -0.0048(4) -0.0237(4) Cl2 0.0579(5) 0.0651(6) 0.0544(5) -0.0016(4) 0.0015(4) -0.0196(4) O1 0.093(2) 0.0658(16) 0.0495(15) 0.0191(12) -0.0061(14) -0.0101(14) O2 0.101(2) 0.0457(14) 0.0657(18) 0.0141(14) -0.0242(16) -0.0241(14) O3 0.0499(14) 0.0547(14) 0.0688(15) 0.0110(12) -0.0087(11) -0.0197(11) O4 0.0428(14) 0.0748(17) 0.0632(15) 0.0032(13) -0.0009(12) -0.0242(13) O5 0.0832(17) 0.0348(11) 0.0420(12) 0.0003(10) -0.0117(11) -0.0211(11) O6 0.0594(14) 0.0393(13) 0.0349(12) 0.0053(10) -0.0076(10) -0.0125(11) O7 0.0523(15) 0.0534(15) 0.103(2) 0.0203(14) -0.0023(14) -0.0157(13) O8 0.0450(15) 0.0607(15) 0.0660(15) 0.0023(12) 0.0064(11) -0.0221(12) N1 0.0440(15) 0.0350(14) 0.0287(13) 0.0044(11) -0.0016(11) -0.0129(12) N2 0.0351(14) 0.0337(13) 0.0283(12) 0.0065(11) -0.0033(10) -0.0101(11) N3 0.0464(15) 0.0370(14) 0.0366(14) 0.0006(11) -0.0007(11) -0.0100(11) N4 0.0333(13) 0.0326(13) 0.0318(13) -0.0018(10) -0.0002(10) -0.0088(10) C1 0.050(2) 0.0354(18) 0.0415(18) 0.0021(14) -0.0015(15) -0.0071(15) C2 0.0421(17) 0.0354(16) 0.0364(16) 0.0006(13) 0.0020(13) -0.0080(13) C3 0.068(2) 0.0381(19) 0.043(2) -0.0018(15) -0.0006(16) -0.0122(16) C4 0.083(3) 0.045(2) 0.042(2) -0.0127(16) -0.0005(18) -0.0134(18) C5 0.060(2) 0.060(2) 0.0332(19) -0.0034(17) -0.0014(16) -0.0068(17) C6 0.0407(18) 0.0456(18) 0.0393(18) 0.0038(14) 0.0015(14) -0.0085(14) C7 0.054(2) 0.051(2) 0.051(2) 0.0074(18) -0.0014(17) -0.0133(16) C8 0.048(2) 0.0500(19) 0.0400(19) -0.0026(16) 0.0001(15) -0.0252(16) C9 0.043(2) 0.063(2) 0.0291(16) -0.0030(14) -0.0039(13) -0.0242(17) C11 0.0354(19) 0.0413(18) 0.0355(17) 0.0017(14) 0.0012(14) -0.0033(14) C12 0.0318(15) 0.0343(16) 0.0316(15) 0.0021(12) 0.0040(12) -0.0068(12) C13 0.054(2) 0.0304(17) 0.0455(19) 0.0046(15) 0.0034(15) -0.0106(14) C14 0.059(2) 0.0325(17) 0.048(2) -0.0086(15) 0.0000(16) -0.0146(15) C15 0.0442(19) 0.0438(18) 0.0314(17) -0.0051(14) -0.0019(14) -0.0123(14) C16 0.0271(15) 0.0360(15) 0.0300(15) 0.0001(12) -0.0001(12) -0.0085(12) C17 0.0310(16) 0.0397(16) 0.0309(16) 0.0018(13) -0.0025(12) -0.0089(13) C18 0.0329(17) 0.0422(18) 0.0335(17) -0.0032(14) -0.0041(14) -0.0090(14) C19 0.042(2) 0.0476(19) 0.0400(17) -0.0063(14) -0.0009(14) -0.0171(16) C21 0.041(2) 0.0446(19) 0.0301(16) 0.0015(14) -0.0011(14) -0.0126(15) C22 0.0369(19) 0.0441(18) 0.0310(16) 0.0025(13) -0.0039(13) -0.0160(14) O11 0.069(2) 0.0558(17) 0.087(2) 0.0269(15) 0.0030(18) -0.0106(17) O12 0.277(7) 0.051(2) 0.082(3) 0.014(2) 0.046(3) -0.014(3) O13 0.0696(19) 0.0447(13) 0.0377(15) -0.0046(11) -0.0011(14) -0.0203(12) O14 0.128(3) 0.112(3) 0.056(2) 0.0048(18) 0.0021(19) -0.081(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 O1 C7 1.215(4) . ? O2 C7 1.299(4) . ? O3 C9 1.201(4) . ? O4 C9 1.311(4) . ? O5 C17 1.210(3) . ? O6 C17 1.308(3) . ? O7 C19 1.201(4) . ? O8 C19 1.306(4) . ? N1 C8 1.499(4) . ? N1 C21 1.505(4) . ? N1 C1 1.511(4) . ? N2 C18 1.501(4) . ? N2 C22 1.501(4) . ? N2 C11 1.514(4) . ? N3 C2 1.334(4) . ? N3 C6 1.341(4) . ? N4 C12 1.340(3) . ? N4 C16 1.340(3) . ? C1 C2 1.509(4) . ? C2 C3 1.379(4) . ? C3 C4 1.374(5) . ? C4 C5 1.371(5) . ? C5 C6 1.380(5) . ? C6 C7 1.495(4) . ? C8 C9 1.496(5) . ? C11 C12 1.505(4) . ? C12 C13 1.381(4) . ? C13 C14 1.370(4) . ? C14 C15 1.379(4) . ? C15 C16 1.378(4) . ? C16 C17 1.502(4) . ? C18 C19 1.512(4) . ? C21 C22 1.515(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 C8 N1 C21 112.8(2) . . ? C8 N1 C1 111.7(2) . . ? C21 N1 C1 111.3(2) . . ? C18 N2 C22 114.1(2) . . ? C18 N2 C11 113.5(2) . . ? C22 N2 C11 111.1(2) . . ? C2 N3 C6 117.9(2) . . ? C12 N4 C16 118.5(2) . . ? C2 C1 N1 109.9(2) . . ? N3 C2 C3 122.2(3) . . ? N3 C2 C1 114.8(3) . . ? C3 C2 C1 123.0(3) . . ? C4 C3 C2 119.3(3) . . ? C5 C4 C3 119.2(3) . . ? C4 C5 C6 118.3(3) . . ? N3 C6 C5 123.1(3) . . ? N3 C6 C7 115.4(3) . . ? C5 C6 C7 121.5(3) . . ? O1 C7 O2 121.0(3) . . ? O1 C7 C6 122.1(3) . . ? O2 C7 C6 117.0(3) . . ? C9 C8 N1 111.1(2) . . ? O3 C9 O4 126.6(3) . . ? O3 C9 C8 122.7(3) . . ? O4 C9 C8 110.6(3) . . ? C12 C11 N2 110.7(2) . . ? N4 C12 C13 121.8(3) . . ? N4 C12 C11 114.7(2) . . ? C13 C12 C11 123.5(3) . . ? C14 C13 C12 119.5(3) . . ? C13 C14 C15 118.9(3) . . ? C16 C15 C14 118.9(3) . . ? N4 C16 C15 122.4(3) . . ? N4 C16 C17 113.3(2) . . ? C15 C16 C17 124.3(2) . . ? O5 C17 O6 124.1(3) . . ? O5 C17 C16 121.9(2) . . ? O6 C17 C16 113.9(3) . . ? N2 C18 C19 115.0(2) . . ? O7 C19 O8 125.6(3) . . ? O7 C19 C18 125.0(3) . . ? O8 C19 C18 109.4(3) . . ? N1 C21 C22 111.2(2) . . ? N2 C22 C21 111.5(2) . . ? 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 O2 H2O Cl1 0.82(4) 2.38(4) 3.132(3) 153(3) . O4 H4O Cl1 0.95(4) 1.98(4) 2.892(3) 160(3) 1_655 O6 H6O O11 0.80(4) 1.76(4) 2.558(3) 174(4) 2_676 O8 H8O O14 0.88(5) 1.70(5) 2.565(4) 167(5) . N1 H1N Cl1 0.83(3) 2.56(3) 3.266(3) 145(2) . N2 H2N O13 0.84(3) 1.96(3) 2.799(3) 172(3) . O11 H1O1 Cl2 0.76(4) 2.38(4) 3.138(4) 174(4) 1_455 O11 H2O1 O13 0.78(4) 2.03(5) 2.781(4) 163(4) . O12 H1O2 O3 0.64(6) 2.50(6) 2.944(5) 130(8) . O12 H2O2 O1 0.58(4) 2.25(5) 2.769(5) 150(6) 2_757 O13 H1O3 Cl2 0.82(4) 2.25(4) 3.063(3) 172(4) . O13 H2O3 O5 0.68(3) 2.23(4) 2.868(4) 156(4) . O14 H1O4 Cl2 0.99(6) 2.15(6) 3.135(4) 173(5) 1_445 O14 H2O4 O12 0.73(4) 1.97(4) 2.693(6) 170(4) 1_455 C1 H1B O4 0.99(3) 2.54(3) 3.460(4) 154(2) 1_455 C8 H8A Cl2 0.97(3) 2.72(3) 3.649(4) 161(2) . C14 H14 O5 0.90(3) 2.55(3) 3.301(4) 142(3) 1_545 C18 H18A Cl2 0.97(3) 2.81(3) 3.669(3) 147.9(19) 1_455 C18 H18B O6 0.92(3) 2.52(3) 3.352(4) 150(2) 2_666 _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 23.21 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.303 _refine_diff_density_min -0.302 _refine_diff_density_rms 0.042 #===END data_struc_2 #[Gd(bpeda)(H2O)2]3[Gd(H2O)6]2Cl3,(2). 0.5MeCN.18.5 H2O _database_code_depnum_ccdc_archive 'CCDC 253405' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; [Gd(bpeda)(H2O)2]3[Gd(H2O)6]2Cl3,(2). 0.5MeCN.18.5 H2O ; _chemical_formula_sum 'C66 H127 Cl3 Gd5 N12.50 O60.50' _chemical_formula_weight 2956.40 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 15.9134(10) _cell_length_b 19.2805(13) _cell_length_c 17.3626(11) _cell_angle_alpha 90.00 _cell_angle_beta 98.2810(10) _cell_angle_gamma 90.00 _cell_volume 5271.6(6) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.5 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.863 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2931 _exptl_absorpt_coefficient_mu 3.285 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33844 _diffrn_reflns_av_R_equivalents 0.0378 _diffrn_reflns_av_sigmaI/netI 0.1048 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 28.92 _reflns_number_total 22551 _reflns_number_gt 14685 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1367P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.053(16) _refine_ls_number_reflns 22551 _refine_ls_number_parameters 1069 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1165 _refine_ls_R_factor_gt 0.0788 _refine_ls_wR_factor_ref 0.2220 _refine_ls_wR_factor_gt 0.2056 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.076 _refine_ls_shift/su_mean 0.003 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 0.50321(8) 0.84707(16) 0.79007(5) 0.0563(3) Uani 1 1 d . . . O1 O 0.5934(9) 0.7453(7) 0.8352(7) 0.052(3) Uani 1 1 d . . . O2 O 0.7140(11) 0.6891(8) 0.8682(11) 0.083(6) Uani 1 1 d . . . O3 O 0.4364(18) 0.9023(10) 0.6685(10) 0.169(15) Uani 1 1 d . . . O4 O 0.465(3) 0.9491(16) 0.5531(12) 0.26(2) Uani 1 1 d . . . O11 O 0.4377(10) 0.7470(6) 0.7233(7) 0.053(4) Uani 1 1 d . . . O12 O 0.3305(9) 0.6744(7) 0.6906(8) 0.062(4) Uani 1 1 d . . . O13 O 0.5557(8) 0.8885(6) 0.9238(7) 0.047(3) Uani 1 1 d . . . O14 O 0.5175(8) 0.9122(9) 1.0391(8) 0.062(4) Uani 1 1 d . . . O21 O 0.5702(19) 0.8109(10) 0.6729(10) 0.146(11) Uani 1 1 d . . . O22 O 0.4402(8) 0.7765(7) 0.8922(7) 0.048(3) Uani 1 1 d . . . N1 N 0.5578(15) 0.9709(11) 0.7512(9) 0.089(8) Uani 1 1 d . . . N2 N 0.4237(15) 0.9562(9) 0.8451(10) 0.081(7) Uani 1 1 d . . . N3 N 0.6682(18) 0.8638(11) 0.8135(11) 0.096(9) Uani 1 1 d . . . N4 N 0.3383(11) 0.8434(7) 0.7699(7) 0.055(5) Uani 1 1 d . . . C1 C 0.6531(18) 0.9856(11) 0.7927(12) 0.086(9) Uani 1 1 d . . . H1A H 0.6792 1.0202 0.7614 0.103 Uiso 1 1 calc R . . H1B H 0.6503 1.0066 0.8443 0.103 Uiso 1 1 calc R . . C2 C 0.7067(18) 0.9275(12) 0.8033(11) 0.070(7) Uani 1 1 d . . . C3 C 0.7923(15) 0.9320(14) 0.8057(13) 0.071(6) Uiso 1 1 d . . . H3A H 0.8163 0.9739 0.7900 0.085 Uiso 1 1 calc R . . C4 C 0.852(2) 0.8699(19) 0.834(2) 0.116(11) Uiso 1 1 d . . . H4A H 0.9122 0.8712 0.8490 0.139 Uiso 1 1 calc R . . C5 C 0.7978(18) 0.8106(14) 0.8313(16) 0.095(10) Uani 1 1 d . . . H5A H 0.8251 0.7671 0.8279 0.114 Uiso 1 1 calc R . . C6 C 0.718(2) 0.8075(13) 0.8330(13) 0.081(9) Uani 1 1 d . . . C7 C 0.6687(16) 0.7410(10) 0.8455(13) 0.057(6) Uani 1 1 d . . . C8 C 0.5502(17) 0.9717(16) 0.6737(15) 0.091(8) Uiso 1 1 d . . . H8A H 0.5971 0.9445 0.6570 0.109 Uiso 1 1 calc R . . H8B H 0.5554 1.0201 0.6558 0.109 Uiso 1 1 calc R . . C9 C 0.461(2) 0.9402(19) 0.633(2) 0.107(9) Uiso 1 1 d . . . C11 C 0.335(2) 0.9644(13) 0.8065(13) 0.113(12) Uani 1 1 d . . . H11A H 0.3341 0.9923 0.7585 0.136 Uiso 1 1 calc R . . H11B H 0.3016 0.9895 0.8416 0.136 Uiso 1 1 calc R . . C12 C 0.2937(16) 0.8936(8) 0.7857(9) 0.060(7) Uani 1 1 d . . . C13 C 0.2014(14) 0.8904(9) 0.7810(9) 0.049(5) Uani 1 1 d . . . H13A H 0.1678 0.9286 0.7929 0.059 Uiso 1 1 calc R . . C14 C 0.1689(13) 0.8289(10) 0.7586(10) 0.050(5) Uani 1 1 d . . . H14A H 0.1103 0.8204 0.7596 0.059 Uiso 1 1 calc R . . C15 C 0.2186(19) 0.7770(11) 0.7338(12) 0.076(8) Uani 1 1 d . . . H15A H 0.1925 0.7363 0.7105 0.091 Uiso 1 1 calc R . . C16 C 0.3015(13) 0.7834(10) 0.7419(12) 0.049(5) Uani 1 1 d . . . C17 C 0.3620(16) 0.7306(10) 0.7178(10) 0.055(5) Uani 1 1 d . . . C18 C 0.4199(13) 0.9388(10) 0.9298(10) 0.059(6) Uani 1 1 d . . . H18A H 0.4060 0.9813 0.9574 0.070 Uiso 1 1 calc R . . H18B H 0.3740 0.9047 0.9328 0.070 Uiso 1 1 calc R . . C19 C 0.5018(12) 0.9099(11) 0.9692(10) 0.048(5) Uani 1 1 d . . . C21 C 0.504(2) 1.031(2) 0.763(2) 0.111(10) Uiso 1 1 d . . . H21A H 0.5372 1.0748 0.7654 0.133 Uiso 1 1 calc R . . H21B H 0.4551 1.0346 0.7216 0.133 Uiso 1 1 calc R . . C22 C 0.474(2) 1.0153(13) 0.8456(16) 0.126(15) Uani 1 1 d . . . H22A H 0.5244 1.0097 0.8855 0.151 Uiso 1 1 calc R . . H22B H 0.4412 1.0556 0.8607 0.151 Uiso 1 1 calc R . . Gd2 Gd 0.79819(5) 0.44309(15) 0.59015(4) 0.03037(18) Uani 1 1 d . . . O101 O 0.8083(7) 0.4840(6) 0.7211(6) 0.038(3) Uani 1 1 d . . . O102 O 0.7812(8) 0.4674(7) 0.8401(6) 0.049(3) Uani 1 1 d . . . O103 O 0.6942(8) 0.3923(6) 0.4843(7) 0.048(3) Uani 1 1 d . . . O104 O 0.6102(11) 0.3034(8) 0.4530(15) 0.142(11) Uani 1 1 d . . . O111 O 0.6796(9) 0.5268(6) 0.5872(6) 0.046(3) Uani 1 1 d . . . O112 O 0.6283(9) 0.6296(8) 0.5590(8) 0.062(4) Uani 1 1 d . . . O113 O 0.9552(7) 0.4349(6) 0.6343(6) 0.033(2) Uani 1 1 d . . . O114 O 1.0748(7) 0.4872(6) 0.6222(7) 0.046(3) Uani 1 1 d . . . O121 O 0.6723(8) 0.3911(6) 0.6417(7) 0.053(3) Uani 1 1 d . . . O122 O 0.8638(7) 0.5604(6) 0.6113(5) 0.040(3) Uani 1 1 d . . . N101 N 0.8244(8) 0.3133(6) 0.5481(6) 0.028(3) Uani 1 1 d . . . N102 N 0.9043(9) 0.4320(6) 0.4799(7) 0.032(3) Uani 1 1 d . . . N103 N 0.8409(8) 0.3540(7) 0.7007(7) 0.033(3) Uani 1 1 d . . . N104 N 0.7703(9) 0.5246(7) 0.4688(6) 0.032(3) Uani 1 1 d . . . C101 C 0.8826(12) 0.2703(8) 0.6111(10) 0.042(4) Uani 1 1 d . . . H10A H 0.8713 0.2202 0.6027 0.050 Uiso 1 1 calc R . . H10B H 0.9430 0.2791 0.6065 0.050 Uiso 1 1 calc R . . C102 C 0.8660(10) 0.2898(8) 0.6877(9) 0.034(4) Uani 1 1 d . . . C103 C 0.8831(12) 0.2418(9) 0.7555(10) 0.044(4) Uani 1 1 d . . . H10C H 0.9027 0.1961 0.7480 0.053 Uiso 1 1 calc R . . C104 C 0.8712(10) 0.2618(8) 0.8250(9) 0.036(4) Uani 1 1 d . . . H10D H 0.8811 0.2301 0.8672 0.043 Uiso 1 1 calc R . . C105 C 0.8441(10) 0.3292(9) 0.8384(9) 0.038(4) Uani 1 1 d . . . H10E H 0.8355 0.3438 0.8889 0.046 Uiso 1 1 calc R . . C106 C 0.8300(10) 0.3750(9) 0.7741(8) 0.035(4) Uani 1 1 d . . . C107 C 0.8036(10) 0.4480(8) 0.7797(8) 0.033(3) Uani 1 1 d . . . C108 C 0.7372(9) 0.2799(8) 0.5335(9) 0.032(4) Uani 1 1 d . . . H10F H 0.7401 0.2367 0.5033 0.039 Uiso 1 1 calc R . . H10G H 0.7187 0.2679 0.5839 0.039 Uiso 1 1 calc R . . C109 C 0.6763(14) 0.3270(10) 0.4909(11) 0.062(6) Uani 1 1 d . . . C111 C 0.8623(10) 0.4563(8) 0.4025(8) 0.033(4) Uani 1 1 d . . . H11C H 0.8292 0.4175 0.3761 0.040 Uiso 1 1 calc R . . H11D H 0.9067 0.4691 0.3706 0.040 Uiso 1 1 calc R . . C112 C 0.8045(11) 0.5170(8) 0.4061(8) 0.033(4) Uani 1 1 d . . . C113 C 0.7927(14) 0.5638(9) 0.3454(9) 0.052(5) Uani 1 1 d . . . H11E H 0.8222 0.5587 0.3019 0.063 Uiso 1 1 calc R . . C114 C 0.7365(13) 0.6190(9) 0.3494(10) 0.051(5) Uani 1 1 d . . . H11F H 0.7267 0.6520 0.3085 0.062 Uiso 1 1 calc R . . C115 C 0.6939(9) 0.6246(8) 0.4164(7) 0.026(3) Uani 1 1 d . . . H11G H 0.6536 0.6604 0.4197 0.032 Uiso 1 1 calc R . . C116 C 0.7109(10) 0.5806(10) 0.4717(8) 0.039(4) Uani 1 1 d . . . C117 C 0.6725(9) 0.5793(8) 0.5461(8) 0.030(3) Uani 1 1 d . . . C118 C 0.9789(10) 0.4750(10) 0.5087(9) 0.040(4) Uani 1 1 d . . . H11H H 1.0274 0.4614 0.4821 0.048 Uiso 1 1 calc R . . H11I H 0.9659 0.5244 0.4971 0.048 Uiso 1 1 calc R . . C119 C 1.0011(9) 0.4656(9) 0.5916(9) 0.034(4) Uani 1 1 d . . . C121 C 0.8645(12) 0.3103(9) 0.4741(9) 0.046(5) Uani 1 1 d . . . H12A H 0.8867 0.2629 0.4684 0.055 Uiso 1 1 calc R . . H12B H 0.8199 0.3189 0.4292 0.055 Uiso 1 1 calc R . . C122 C 0.9347(11) 0.3607(10) 0.4711(9) 0.044(4) Uani 1 1 d . . . H12C H 0.9566 0.3562 0.4207 0.053 Uiso 1 1 calc R . . H12D H 0.9819 0.3504 0.5132 0.053 Uiso 1 1 calc R . . Gd3 Gd 0.21842(4) 0.47684(15) 0.85288(4) 0.02627(16) Uani 1 1 d . . . O201 O 0.2668(7) 0.5044(5) 0.7291(5) 0.030(2) Uani 1 1 d . . . O202 O 0.3266(8) 0.4653(6) 0.6315(7) 0.047(3) Uani 1 1 d . . . O203 O 0.2617(7) 0.4138(6) 0.9729(7) 0.040(3) Uani 1 1 d . . . O204 O 0.3229(7) 0.3149(6) 1.0063(6) 0.039(3) Uani 1 1 d . . . O211 O 0.3524(7) 0.5337(6) 0.8859(6) 0.035(3) Uani 1 1 d . . . O212 O 0.4478(6) 0.5963(5) 0.9624(6) 0.034(2) Uani 1 1 d . . . O213 O 0.0855(7) 0.4990(5) 0.7694(6) 0.032(2) Uani 1 1 d . . . O214 O -0.0057(8) 0.5846(7) 0.7409(6) 0.052(3) Uani 1 1 d . . . O221 O 0.3431(7) 0.3981(6) 0.8442(7) 0.042(3) Uani 1 1 d . . . O222 O 0.2018(7) 0.6028(6) 0.8160(6) 0.037(3) Uani 1 1 d . . . N201 N 0.1367(8) 0.3581(6) 0.8810(7) 0.031(3) Uani 1 1 d . . . N202 N 0.0803(8) 0.4998(6) 0.9214(7) 0.029(3) Uani 1 1 d . . . N203 N 0.1884(7) 0.3822(7) 0.7415(7) 0.029(3) Uani 1 1 d . . . N204 N 0.2370(9) 0.5545(7) 0.9771(7) 0.036(3) Uani 1 1 d . . . C201 C 0.0882(10) 0.3226(8) 0.8076(11) 0.041(4) Uani 1 1 d . . . H20A H 0.0781 0.2731 0.8184 0.049 Uiso 1 1 calc R . . H20B H 0.0326 0.3454 0.7923 0.049 Uiso 1 1 calc R . . C202 C 0.1406(9) 0.3288(8) 0.7448(9) 0.030(3) Uani 1 1 d . . . C203 C 0.1387(10) 0.2773(10) 0.6877(10) 0.042(4) Uani 1 1 d . . . H20C H 0.1110 0.2344 0.6935 0.050 Uiso 1 1 calc R . . C204 C 0.1779(12) 0.2897(10) 0.6219(11) 0.052(5) Uani 1 1 d . . . H20D H 0.1717 0.2573 0.5802 0.062 Uiso 1 1 calc R . . C205 C 0.2237(10) 0.3466(8) 0.6178(10) 0.037(4) Uani 1 1 d . . . H20E H 0.2507 0.3561 0.5736 0.044 Uiso 1 1 calc R . . C206 C 0.2309(10) 0.3932(8) 0.6823(8) 0.030(3) Uani 1 1 d . . . C207 C 0.2785(10) 0.4599(7) 0.6812(8) 0.030(3) Uani 1 1 d . . . C208 C 0.2016(10) 0.3077(8) 0.9156(9) 0.036(4) Uani 1 1 d . . . H20F H 0.2287 0.2849 0.8744 0.043 Uiso 1 1 calc R . . H20G H 0.1754 0.2716 0.9450 0.043 Uiso 1 1 calc R . . C209 C 0.2682(9) 0.3496(8) 0.9709(9) 0.028(3) Uani 1 1 d . . . C211 C 0.0933(9) 0.5200(8) 1.0006(10) 0.037(4) Uani 1 1 d . . . H21C H 0.0967 0.4780 1.0336 0.044 Uiso 1 1 calc R . . H21D H 0.0439 0.5476 1.0115 0.044 Uiso 1 1 calc R . . C212 C 0.1748(9) 0.5633(7) 1.0227(9) 0.030(3) Uani 1 1 d . . . C213 C 0.1859(10) 0.6039(8) 1.0877(9) 0.036(4) Uani 1 1 d . . . H21E H 0.1417 0.6083 1.1188 0.044 Uiso 1 1 calc R . . C214 C 0.2616(11) 0.6386(10) 1.1078(10) 0.042(4) Uiso 1 1 d . . . H21F H 0.2702 0.6688 1.1515 0.050 Uiso 1 1 calc R . . C215 C 0.3277(11) 0.6273(8) 1.0597(10) 0.039(4) Uani 1 1 d . . . H21G H 0.3814 0.6493 1.0717 0.047 Uiso 1 1 calc R . . C216 C 0.3113(9) 0.5849(7) 0.9978(8) 0.026(3) Uani 1 1 d . . . C217 C 0.3771(8) 0.5716(8) 0.9433(8) 0.026(3) Uani 1 1 d . . . C218 C 0.0350(11) 0.5559(9) 0.8769(10) 0.042(4) Uani 1 1 d . . . H21H H 0.0613 0.6010 0.8938 0.051 Uiso 1 1 calc R . . H21I H -0.0249 0.5568 0.8863 0.051 Uiso 1 1 calc R . . C219 C 0.0387(10) 0.5448(10) 0.7886(9) 0.038(4) Uani 1 1 d . . . C221 C 0.0719(12) 0.3732(8) 0.9338(10) 0.043(4) Uani 1 1 d . . . H22C H 0.0317 0.3338 0.9314 0.052 Uiso 1 1 calc R . . H22D H 0.1012 0.3767 0.9880 0.052 Uiso 1 1 calc R . . C222 C 0.0236(9) 0.4375(8) 0.9139(9) 0.032(3) Uani 1 1 d . . . H22E H -0.0199 0.4428 0.9489 0.038 Uiso 1 1 calc R . . H22F H -0.0061 0.4343 0.8599 0.038 Uiso 1 1 calc R . . Gd4 Gd 0.37878(6) 0.57932(15) 0.61960(5) 0.0393(2) Uani 1 1 d . . . O301 O 0.4057(9) 0.6650(7) 0.5246(9) 0.066(4) Uani 1 1 d . . . O302 O 0.4340(7) 0.5452(6) 0.7542(6) 0.041(3) Uani 1 1 d . . . O303 O 0.4946(7) 0.5077(7) 0.5951(7) 0.051(3) Uani 1 1 d . . . O304 O 0.5192(9) 0.6392(7) 0.6677(7) 0.061(4) Uani 1 1 d . . . O305 O 0.3447(12) 0.5318(10) 0.4870(9) 0.091(6) Uani 1 1 d . . . O306 O 0.2306(9) 0.6004(7) 0.5698(7) 0.053(3) Uani 1 1 d . . . Gd5 Gd 0.70698(8) 0.56754(16) 0.88269(7) 0.0686(3) Uani 1 1 d . . . O311 O 0.8184(12) 0.6119(11) 0.8036(11) 0.110(7) Uani 1 1 d . . . O312 O 0.8435(12) 0.5853(12) 0.9659(12) 0.118(8) Uani 1 1 d . . . O313 O 0.6495(11) 0.5537(9) 0.7498(7) 0.079(5) Uani 1 1 d . . . O314 O 0.5565(8) 0.6122(6) 0.8572(6) 0.041(3) Uani 1 1 d . . . O315 O 0.6113(8) 0.4699(7) 0.8844(6) 0.050(3) Uani 1 1 d . . . O316 O 0.6669(10) 0.6121(9) 1.0016(8) 0.072(4) Uani 1 1 d . . . Cl1 Cl 0.0618(3) 0.1737(3) 0.4887(3) 0.0578(13) Uani 1 1 d . . . Cl2 Cl 0.7046(7) 0.1256(4) 0.6634(5) 0.117(3) Uani 1 1 d . . . Cl3 Cl 0.3736(3) 0.2416(3) 0.8081(3) 0.0504(11) Uani 1 1 d . . . O401 O 0.5655 0.1708 0.6204 0.050 Uiso 1 1 d . . . O402 O 0.6988 0.3153 0.0021 0.050 Uiso 0.50 1 d P . . O403 O 0.0355 0.2206 0.2234 0.050 Uiso 1 1 d . . . O404 O 0.6478 0.2622 0.7183 0.050 Uiso 1 1 d . . . O405 O 0.2984 0.3987 0.4329 0.050 Uiso 1 1 d . . . O406 O 0.5279 0.4135 0.7341 0.050 Uiso 1 1 d . . . O407 O 0.1235 0.2742 0.3582 0.050 Uiso 1 1 d . . . O408 O 0.4531 0.2778 0.6524 0.050 Uiso 1 1 d . . . O409 O 0.5287 0.8653 0.4527 0.050 Uiso 1 1 d . . . O410 O 0.5770 0.2860 0.8472 0.050 Uiso 1 1 d . . . O411 O 0.9001 0.1517 0.3628 0.050 Uiso 1 1 d . . . O412 O 0.8515 0.0611 0.5800 0.050 Uiso 1 1 d . . . O413 O 0.0723 0.1336 0.8219 0.050 Uiso 1 1 d . . . O414 O 0.9989 0.1185 0.6415 0.050 Uiso 1 1 d . . . O415 O 0.1067 0.4170 0.3700 0.050 Uiso 1 1 d . . . O416 O 0.2754 0.2251 0.3263 0.050 Uiso 1 1 d . . . O417 O 0.2526 0.1238 0.8553 0.050 Uiso 1 1 d . . . O418 O 0.4603 0.2100 0.9856 0.050 Uiso 1 1 d . . . O419 O 0.9981 0.0081 0.7604 0.050 Uiso 1 1 d . . . N421 N 0.0033 0.2191 1.0376 0.050 Uiso 0.50 1 d P . . C421 C 0.0287 0.1940 0.9813 0.050 Uiso 0.50 1 d P . . C422 C 0.0499 0.1675 0.9525 0.050 Uiso 0.50 1 d P . . 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 0.1158(9) 0.0232(4) 0.0257(4) -0.0007(3) -0.0035(5) -0.0232(5) O1 0.073(10) 0.038(7) 0.057(8) -0.009(6) 0.046(7) -0.013(7) O2 0.113(13) 0.028(8) 0.125(14) -0.031(8) 0.077(11) -0.016(8) O3 0.32(3) 0.082(13) 0.064(10) 0.056(10) -0.106(16) -0.152(19) O4 0.50(6) 0.19(3) 0.073(13) 0.039(15) -0.04(2) -0.28(4) O11 0.093(11) 0.026(6) 0.041(7) -0.013(5) 0.016(7) -0.035(7) O12 0.087(10) 0.032(7) 0.076(9) -0.017(7) 0.036(8) -0.001(7) O13 0.059(8) 0.031(7) 0.049(7) 0.012(5) 0.004(6) 0.009(6) O14 0.037(7) 0.090(11) 0.059(9) -0.023(8) 0.008(6) 0.012(7) O21 0.31(3) 0.076(13) 0.066(11) -0.020(9) 0.072(15) -0.130(18) O22 0.055(8) 0.044(8) 0.046(7) 0.013(6) 0.010(6) -0.001(6) N1 0.150(19) 0.073(14) 0.032(8) 0.025(9) -0.026(10) -0.058(14) N2 0.132(17) 0.044(12) 0.053(10) 0.009(8) -0.037(11) 0.007(10) N3 0.19(2) 0.060(14) 0.058(11) -0.031(9) 0.085(14) -0.074(15) N4 0.117(14) 0.014(7) 0.022(6) 0.003(5) -0.031(7) 0.000(8) C1 0.16(2) 0.038(13) 0.046(11) -0.006(9) -0.021(13) -0.055(15) C2 0.13(2) 0.048(14) 0.036(10) -0.010(9) 0.031(12) -0.024(13) C5 0.10(2) 0.081(18) 0.12(2) -0.050(16) 0.095(19) -0.032(15) C6 0.15(3) 0.049(14) 0.055(13) -0.032(11) 0.075(15) -0.043(15) C7 0.086(17) 0.027(10) 0.073(14) -0.014(9) 0.059(12) -0.006(10) C11 0.20(3) 0.074(19) 0.046(12) 0.007(11) -0.047(16) 0.067(19) C12 0.13(2) 0.013(8) 0.027(8) 0.009(6) -0.039(10) 0.009(9) C13 0.095(16) 0.022(9) 0.022(8) 0.007(6) -0.021(9) 0.003(9) C14 0.063(13) 0.043(11) 0.044(10) 0.012(8) 0.015(9) -0.005(9) C15 0.15(3) 0.036(12) 0.043(11) 0.008(9) 0.024(14) 0.030(14) C16 0.045(12) 0.031(10) 0.068(13) 0.000(8) -0.004(9) -0.014(8) C17 0.102(17) 0.029(10) 0.034(9) -0.006(7) 0.015(10) -0.025(10) C18 0.089(14) 0.033(10) 0.042(9) -0.019(8) -0.031(9) 0.034(10) C19 0.044(11) 0.063(13) 0.031(9) -0.017(8) -0.016(8) 0.019(9) C22 0.19(3) 0.045(15) 0.11(2) 0.016(13) -0.11(2) -0.056(17) Gd2 0.0511(5) 0.0169(3) 0.0229(3) -0.0019(3) 0.0046(3) -0.0031(3) O101 0.069(7) 0.015(5) 0.035(6) -0.006(4) 0.021(5) -0.003(5) O102 0.078(9) 0.041(7) 0.034(6) 0.004(5) 0.024(6) 0.016(6) O103 0.073(9) 0.022(6) 0.043(7) -0.009(5) -0.013(6) 0.001(5) O104 0.089(12) 0.019(8) 0.28(3) -0.054(12) -0.109(15) 0.012(7) O111 0.091(10) 0.013(5) 0.039(6) 0.010(4) 0.022(6) 0.011(5) O112 0.069(9) 0.072(10) 0.054(8) 0.017(7) 0.043(7) 0.011(8) O113 0.039(6) 0.030(6) 0.027(5) -0.008(4) -0.005(4) -0.001(5) O114 0.044(7) 0.026(6) 0.068(8) 0.001(6) 0.013(6) -0.011(5) O121 0.065(8) 0.028(7) 0.060(8) -0.001(6) -0.011(6) -0.016(6) O122 0.056(7) 0.040(7) 0.020(5) 0.004(4) -0.007(5) -0.009(5) N101 0.034(7) 0.023(6) 0.024(6) -0.003(5) -0.006(5) -0.009(5) N102 0.064(9) 0.007(6) 0.028(6) -0.009(4) 0.016(6) 0.002(5) N103 0.027(7) 0.037(8) 0.034(7) -0.015(6) 0.005(5) -0.013(6) N104 0.055(9) 0.026(7) 0.015(6) -0.002(5) 0.001(6) 0.003(6) C101 0.060(11) 0.011(7) 0.058(11) 0.011(7) 0.023(9) -0.006(7) C102 0.039(9) 0.032(9) 0.027(8) 0.001(6) -0.012(7) -0.009(7) C103 0.068(12) 0.017(8) 0.049(10) -0.003(7) 0.016(9) -0.022(8) C104 0.041(9) 0.030(9) 0.037(9) 0.013(7) 0.004(7) -0.009(7) C105 0.035(9) 0.051(11) 0.031(8) 0.004(7) 0.013(7) 0.005(7) C106 0.039(9) 0.049(10) 0.012(6) -0.001(6) -0.010(6) 0.000(7) C107 0.051(10) 0.026(8) 0.018(6) -0.010(6) -0.005(6) 0.005(7) C108 0.029(8) 0.032(9) 0.034(8) -0.024(7) 0.001(6) -0.003(6) C109 0.080(15) 0.037(11) 0.056(11) -0.019(9) -0.041(11) -0.007(9) C111 0.049(10) 0.026(9) 0.023(7) 0.001(5) 0.000(7) -0.004(6) C112 0.051(10) 0.026(8) 0.020(7) 0.006(6) -0.005(7) -0.015(7) C113 0.113(16) 0.020(9) 0.025(8) -0.009(6) 0.015(9) 0.006(9) C114 0.089(15) 0.028(9) 0.035(9) 0.008(7) 0.001(9) 0.015(9) C115 0.033(8) 0.033(8) 0.012(6) -0.005(5) 0.000(6) -0.013(6) C116 0.044(10) 0.048(10) 0.027(8) -0.006(7) 0.011(7) -0.034(9) C117 0.027(8) 0.030(8) 0.029(7) -0.001(6) -0.007(6) -0.002(7) C118 0.053(10) 0.036(9) 0.037(8) -0.008(7) 0.029(7) -0.015(8) C119 0.026(8) 0.043(10) 0.034(8) 0.006(7) 0.007(6) 0.006(7) C121 0.078(13) 0.024(9) 0.031(8) -0.021(7) -0.009(8) -0.006(8) C122 0.043(10) 0.057(12) 0.034(8) 0.010(8) 0.016(7) 0.024(8) Gd3 0.0339(4) 0.0175(3) 0.0281(3) 0.0008(3) 0.0068(3) -0.0051(3) O201 0.054(7) 0.012(5) 0.024(5) -0.001(4) 0.002(5) -0.003(4) O202 0.062(8) 0.031(7) 0.051(7) -0.006(5) 0.019(6) -0.012(5) O203 0.049(7) 0.016(5) 0.058(7) 0.002(5) 0.018(6) -0.011(5) O204 0.040(7) 0.042(7) 0.038(6) 0.012(5) 0.022(5) 0.000(5) O211 0.049(7) 0.030(6) 0.031(6) -0.008(4) 0.020(5) -0.022(5) O212 0.031(6) 0.021(6) 0.054(7) -0.003(5) 0.020(5) -0.013(4) O213 0.051(7) 0.020(5) 0.027(5) 0.001(4) 0.012(5) -0.001(5) O214 0.068(8) 0.050(8) 0.033(6) 0.004(6) -0.004(6) 0.025(7) O221 0.047(7) 0.037(7) 0.041(6) 0.003(5) 0.007(5) -0.007(5) O222 0.048(7) 0.024(6) 0.036(6) 0.001(4) 0.000(5) -0.007(5) N201 0.033(7) 0.019(6) 0.046(7) 0.000(5) 0.022(6) 0.001(5) N202 0.034(7) 0.023(6) 0.027(6) 0.004(5) -0.003(5) -0.008(5) N203 0.019(6) 0.026(7) 0.042(7) -0.005(5) 0.006(5) 0.002(5) N204 0.058(9) 0.026(7) 0.025(6) 0.006(5) 0.011(6) 0.018(6) C201 0.026(9) 0.022(8) 0.074(12) 0.004(8) 0.004(8) -0.013(6) C202 0.026(8) 0.021(8) 0.040(8) -0.008(6) -0.008(6) -0.008(6) C203 0.030(9) 0.044(10) 0.048(10) -0.008(8) -0.010(8) -0.001(7) C204 0.050(12) 0.049(12) 0.059(12) -0.025(9) 0.013(9) -0.016(9) C205 0.035(9) 0.022(8) 0.062(10) -0.022(7) 0.038(8) -0.013(7) C206 0.044(9) 0.029(8) 0.017(7) 0.005(6) 0.001(6) -0.003(7) C207 0.041(9) 0.028(9) 0.021(7) 0.008(5) 0.007(6) -0.006(6) C208 0.041(9) 0.024(8) 0.042(9) 0.009(7) 0.005(7) -0.007(7) C209 0.024(8) 0.021(7) 0.044(8) 0.006(6) 0.029(7) -0.001(6) C211 0.021(8) 0.028(9) 0.065(11) 0.007(7) 0.020(7) -0.001(6) C212 0.042(9) 0.007(6) 0.045(8) -0.011(6) 0.020(7) -0.009(6) C213 0.043(10) 0.034(9) 0.036(8) -0.003(7) 0.022(7) 0.010(7) C215 0.048(10) 0.023(8) 0.050(10) 0.006(7) 0.019(8) -0.005(7) C216 0.038(8) 0.013(7) 0.026(7) -0.003(5) 0.001(6) -0.003(6) C217 0.018(7) 0.020(7) 0.040(8) -0.001(6) 0.008(6) -0.008(6) C218 0.036(9) 0.046(11) 0.044(9) -0.012(8) 0.006(7) -0.008(8) C219 0.041(10) 0.047(11) 0.023(8) 0.000(7) -0.002(7) -0.006(8) C221 0.080(13) 0.014(7) 0.038(9) -0.001(6) 0.018(9) -0.017(8) C222 0.027(8) 0.027(8) 0.042(8) 0.004(7) 0.011(6) 0.005(6) Gd4 0.0592(6) 0.0219(4) 0.0402(4) -0.0062(3) 0.0185(4) -0.0068(4) O301 0.082(10) 0.026(7) 0.092(11) 0.027(7) 0.023(8) 0.015(6) O302 0.055(7) 0.043(7) 0.028(6) 0.005(5) 0.014(5) 0.000(5) O303 0.032(7) 0.061(9) 0.062(8) -0.017(7) 0.010(6) -0.003(6) O304 0.090(10) 0.049(8) 0.052(8) -0.009(6) 0.040(7) -0.021(7) O305 0.121(15) 0.091(14) 0.061(10) -0.014(9) 0.017(9) 0.034(11) O306 0.068(9) 0.048(8) 0.045(7) 0.001(6) 0.011(6) 0.000(6) Gd5 0.0815(8) 0.0421(6) 0.0892(8) -0.0283(6) 0.0356(6) -0.0023(5) O311 0.100(14) 0.133(18) 0.110(14) -0.034(13) 0.060(11) 0.053(12) O312 0.111(15) 0.133(18) 0.118(15) 0.024(13) 0.048(12) 0.093(14) O313 0.123(13) 0.098(13) 0.025(6) 0.019(7) 0.037(7) 0.050(10) O314 0.063(8) 0.033(6) 0.032(6) -0.005(5) 0.028(5) 0.014(5) O315 0.077(9) 0.041(7) 0.038(6) 0.019(5) 0.023(6) 0.012(6) O316 0.083(11) 0.079(11) 0.053(8) -0.015(8) 0.007(7) 0.022(8) Cl1 0.079(3) 0.046(3) 0.046(3) -0.015(2) 0.001(2) 0.011(2) Cl2 0.194(9) 0.057(4) 0.114(6) 0.002(4) 0.064(6) -0.034(5) Cl3 0.054(3) 0.043(3) 0.058(3) -0.005(2) 0.019(2) -0.005(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 O11 2.410(11) . ? Gd1 O3 2.465(15) . ? Gd1 O13 2.484(12) . ? Gd1 O1 2.490(15) . ? Gd1 O21 2.53(2) . ? Gd1 O22 2.552(11) . ? Gd1 N4 2.598(18) . ? Gd1 N3 2.62(3) . ? Gd1 N1 2.662(18) . ? Gd1 N2 2.70(2) . ? O1 C7 1.19(3) . ? O2 C7 1.26(3) . ? O2 Gd5 2.362(15) . ? O3 C9 1.06(4) . ? O4 C9 1.41(4) . ? O11 C17 1.23(2) . ? O12 C17 1.26(2) . ? O12 Gd4 2.396(12) . ? O13 C19 1.31(2) . ? O14 C19 1.21(2) . ? N1 C8 1.33(3) . ? N1 C1 1.61(3) . ? N1 C21 1.47(4) . ? N2 C22 1.39(3) . ? N2 C11 1.48(3) . ? N2 C18 1.52(3) . ? N3 C6 1.36(4) . ? N3 C2 1.39(3) . ? N4 C12 1.26(3) . ? N4 C16 1.35(2) . ? C1 C2 1.40(4) . ? C2 C3 1.36(3) . ? C3 C4 1.57(4) . ? C4 C5 1.43(4) . ? C5 C6 1.28(4) . ? C6 C7 1.53(3) . ? C8 C9 1.61(4) . ? C11 C12 1.53(3) . ? C12 C13 1.46(3) . ? C13 C14 1.33(3) . ? C14 C15 1.38(3) . ? C15 C16 1.31(3) . ? C16 C17 1.50(3) . ? C18 C19 1.49(2) . ? C21 C22 1.60(4) . ? Gd2 O101 2.390(10) . ? Gd2 O111 2.479(12) . ? Gd2 O103 2.490(11) . ? Gd2 O122 2.495(11) . ? Gd2 O113 2.510(10) . ? Gd2 O121 2.518(13) . ? Gd2 N103 2.592(14) . ? Gd2 N104 2.615(12) . ? Gd2 N101 2.657(12) . ? Gd2 N102 2.737(12) . ? O101 C107 1.242(18) . ? O102 C107 1.215(17) . ? O102 Gd5 2.433(12) . ? O103 C109 1.30(2) . ? O104 C109 1.24(2) . ? O111 C117 1.232(18) . ? O112 C117 1.24(2) . ? O113 C119 1.262(19) . ? O114 C119 1.285(19) . ? N101 C108 1.517(18) . ? N101 C121 1.52(2) . ? N101 C101 1.56(2) . ? N102 C118 1.47(2) . ? N102 C111 1.488(18) . ? N102 C122 1.47(2) . ? N103 C102 1.33(2) . ? N103 C106 1.373(18) . ? N104 C112 1.29(2) . ? N104 C116 1.44(2) . ? C101 C102 1.44(2) . ? C102 C103 1.49(2) . ? C103 C104 1.31(2) . ? C104 C105 1.40(2) . ? C105 C106 1.41(2) . ? C106 C107 1.48(2) . ? C108 C109 1.45(2) . ? C111 C112 1.49(2) . ? C112 C113 1.38(2) . ? C113 C114 1.40(3) . ? C114 C115 1.43(2) . ? C115 C116 1.28(2) . ? C116 C117 1.51(2) . ? C118 C119 1.44(2) . ? C121 C122 1.49(3) . ? Gd3 O211 2.393(10) . ? Gd3 O213 2.424(11) . ? Gd3 O203 2.425(12) . ? Gd3 O201 2.444(10) . ? Gd3 O222 2.515(11) . ? Gd3 O221 2.520(12) . ? Gd3 N204 2.607(13) . ? Gd3 N203 2.652(12) . ? Gd3 N202 2.682(13) . ? Gd3 N201 2.712(12) . ? O201 C207 1.228(17) . ? O202 C207 1.237(18) . ? O202 Gd4 2.370(11) . ? O203 C209 1.243(18) . ? O204 C209 1.196(18) . ? O211 C217 1.251(17) . ? O212 C217 1.223(16) . ? O213 C219 1.23(2) . ? O214 C219 1.267(19) . ? N201 C208 1.48(2) . ? N201 C221 1.50(2) . ? N201 C201 1.55(2) . ? N202 C211 1.42(2) . ? N202 C218 1.46(2) . ? N202 C222 1.496(19) . ? N203 C202 1.286(19) . ? N203 C206 1.327(19) . ? N204 C216 1.32(2) . ? N204 C212 1.364(19) . ? C201 C202 1.47(2) . ? C202 C203 1.40(2) . ? C203 C204 1.40(3) . ? C204 C205 1.32(2) . ? C205 C206 1.43(2) . ? C206 C207 1.49(2) . ? C208 C209 1.55(2) . ? C211 C212 1.54(2) . ? C212 C213 1.36(2) . ? C213 C214 1.38(2) . ? C214 C215 1.45(2) . ? C215 C216 1.35(2) . ? C216 C217 1.53(2) . ? C218 C219 1.56(2) . ? C221 C222 1.47(2) . ? Gd4 O303 2.390(12) . ? Gd4 O301 2.416(13) . ? Gd4 O306 2.426(13) . ? Gd4 O302 2.465(10) . ? Gd4 O305 2.464(16) . ? Gd4 O304 2.547(14) . ? Gd5 O313 2.371(14) . ? Gd5 O316 2.405(14) . ? Gd5 O315 2.424(13) . ? Gd5 O312 2.45(2) . ? Gd5 O314 2.523(12) . ? Gd5 O311 2.54(2) . ? N421 C421 1.2124 . ? C421 C422 0.8205 . ? 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 O11 Gd1 O3 80.2(5) . . ? O11 Gd1 O13 140.5(4) . . ? O3 Gd1 O13 135.0(6) . . ? O11 Gd1 O1 73.1(5) . . ? O3 Gd1 O1 140.2(8) . . ? O13 Gd1 O1 81.9(4) . . ? O11 Gd1 O21 66.1(5) . . ? O3 Gd1 O21 67.0(10) . . ? O13 Gd1 O21 135.8(7) . . ? O1 Gd1 O21 75.2(7) . . ? O11 Gd1 O22 73.8(4) . . ? O3 Gd1 O22 131.4(7) . . ? O13 Gd1 O22 68.6(4) . . ? O1 Gd1 O22 68.1(4) . . ? O21 Gd1 O22 131.7(5) . . ? O11 Gd1 N4 63.5(5) . . ? O3 Gd1 N4 66.0(7) . . ? O13 Gd1 N4 109.4(4) . . ? O1 Gd1 N4 123.1(4) . . ? O21 Gd1 N4 114.8(7) . . ? O22 Gd1 N4 65.7(4) . . ? O11 Gd1 N3 121.9(6) . . ? O3 Gd1 N3 112.3(8) . . ? O13 Gd1 N3 67.7(5) . . ? O1 Gd1 N3 61.9(6) . . ? O21 Gd1 N3 68.2(7) . . ? O22 Gd1 N3 116.3(5) . . ? N4 Gd1 N3 174.4(6) . . ? O11 Gd1 N1 137.0(4) . . ? O3 Gd1 N1 60.8(5) . . ? O13 Gd1 N1 82.6(4) . . ? O1 Gd1 N1 126.3(6) . . ? O21 Gd1 N1 81.5(6) . . ? O22 Gd1 N1 146.1(5) . . ? N4 Gd1 N1 110.5(6) . . ? N3 Gd1 N1 64.7(7) . . ? O11 Gd1 N2 127.0(6) . . ? O3 Gd1 N2 78.5(8) . . ? O13 Gd1 N2 62.0(4) . . ? O1 Gd1 N2 141.3(4) . . ? O21 Gd1 N2 140.7(7) . . ? O22 Gd1 N2 85.3(5) . . ? N4 Gd1 N2 63.5(5) . . ? N3 Gd1 N2 111.1(6) . . ? N1 Gd1 N2 65.0(8) . . ? C7 O1 Gd1 128.7(12) . . ? C7 O2 Gd5 141.8(15) . . ? C9 O3 Gd1 130(2) . . ? C17 O11 Gd1 126.3(12) . . ? C17 O12 Gd4 135.5(14) . . ? C19 O13 Gd1 120.1(10) . . ? C8 N1 C1 113(2) . . ? C8 N1 C21 100(2) . . ? C1 N1 C21 109(2) . . ? C8 N1 Gd1 106.3(17) . . ? C1 N1 Gd1 111.4(12) . . ? C21 N1 Gd1 116.9(19) . . ? C22 N2 C11 115.0(19) . . ? C22 N2 C18 106.1(18) . . ? C11 N2 C18 107(2) . . ? C22 N2 Gd1 110(2) . . ? C11 N2 Gd1 112.8(13) . . ? C18 N2 Gd1 104.9(10) . . ? C6 N3 C2 119(3) . . ? C6 N3 Gd1 118.5(14) . . ? C2 N3 Gd1 123(2) . . ? C12 N4 C16 120.5(19) . . ? C12 N4 Gd1 122.8(13) . . ? C16 N4 Gd1 116.6(13) . . ? C2 C1 N1 115.7(18) . . ? C3 C2 N3 121(3) . . ? C3 C2 C1 123(2) . . ? N3 C2 C1 117(3) . . ? C2 C3 C4 122(3) . . ? C5 C4 C3 105(3) . . ? C6 C5 C4 130(3) . . ? C5 C6 N3 120(2) . . ? C5 C6 C7 125(3) . . ? N3 C6 C7 114(2) . . ? O1 C7 O2 128.3(19) . . ? O1 C7 C6 116(2) . . ? O2 C7 C6 115(2) . . ? N1 C8 C9 113(2) . . ? O3 C9 O4 137(3) . . ? O3 C9 C8 112(3) . . ? O4 C9 C8 102(3) . . ? N2 C11 C12 111.0(17) . . ? N4 C12 C13 123.5(17) . . ? N4 C12 C11 120(2) . . ? C13 C12 C11 116.3(19) . . ? C14 C13 C12 113.5(18) . . ? C13 C14 C15 121(2) . . ? C16 C15 C14 121(2) . . ? C15 C16 N4 120(2) . . ? C15 C16 C17 125.6(18) . . ? N4 C16 C17 114.6(18) . . ? O11 C17 O12 125(2) . . ? O11 C17 C16 117.6(16) . . ? O12 C17 C16 117(2) . . ? C19 C18 N2 111.9(18) . . ? O14 C19 O13 123.9(15) . . ? O14 C19 C18 119.3(17) . . ? O13 C19 C18 116.5(15) . . ? C22 C21 N1 104(3) . . ? N2 C22 C21 113(2) . . ? O101 Gd2 O111 75.6(4) . . ? O101 Gd2 O103 141.1(4) . . ? O111 Gd2 O103 79.5(4) . . ? O101 Gd2 O122 65.9(3) . . ? O111 Gd2 O122 73.4(4) . . ? O103 Gd2 O122 133.2(4) . . ? O101 Gd2 O113 78.6(4) . . ? O111 Gd2 O113 140.3(4) . . ? O103 Gd2 O113 136.6(4) . . ? O122 Gd2 O113 68.6(4) . . ? O101 Gd2 O121 75.0(4) . . ? O111 Gd2 O121 67.9(4) . . ? O103 Gd2 O121 68.1(4) . . ? O122 Gd2 O121 130.3(4) . . ? O113 Gd2 O121 132.4(4) . . ? O101 Gd2 N103 62.6(4) . . ? O111 Gd2 N103 124.4(4) . . ? O103 Gd2 N103 111.2(4) . . ? O122 Gd2 N103 115.6(3) . . ? O113 Gd2 N103 65.7(4) . . ? O121 Gd2 N103 67.1(4) . . ? O101 Gd2 N104 123.3(4) . . ? O111 Gd2 N104 63.4(4) . . ? O103 Gd2 N104 67.9(4) . . ? O122 Gd2 N104 66.0(3) . . ? O113 Gd2 N104 109.3(4) . . ? O121 Gd2 N104 118.3(4) . . ? N103 Gd2 N104 172.2(4) . . ? O101 Gd2 N101 125.5(4) . . ? O111 Gd2 N101 139.2(4) . . ? O103 Gd2 N101 62.7(4) . . ? O122 Gd2 N101 144.6(4) . . ? O113 Gd2 N101 80.5(3) . . ? O121 Gd2 N101 83.5(4) . . ? N103 Gd2 N101 62.9(4) . . ? N104 Gd2 N101 111.1(4) . . ? O101 Gd2 N102 136.7(4) . . ? O111 Gd2 N102 125.5(4) . . ? O103 Gd2 N102 82.2(4) . . ? O122 Gd2 N102 83.5(4) . . ? O113 Gd2 N102 61.4(4) . . ? O121 Gd2 N102 145.1(4) . . ? N103 Gd2 N102 110.1(4) . . ? N104 Gd2 N102 62.2(4) . . ? N101 Gd2 N102 66.2(3) . . ? C107 O101 Gd2 126.2(9) . . ? C107 O102 Gd5 136.2(11) . . ? C109 O103 Gd2 116.5(10) . . ? C117 O111 Gd2 123.6(11) . . ? C119 O113 Gd2 115.2(9) . . ? C108 N101 C121 109.3(11) . . ? C108 N101 C101 109.1(11) . . ? C121 N101 C101 107.1(12) . . ? C108 N101 Gd2 105.6(8) . . ? C121 N101 Gd2 111.8(9) . . ? C101 N101 Gd2 114.0(8) . . ? C118 N102 C111 111.4(12) . . ? C118 N102 C122 107.4(13) . . ? C111 N102 C122 108.1(11) . . ? C118 N102 Gd2 105.5(8) . . ? C111 N102 Gd2 111.4(9) . . ? C122 N102 Gd2 113.0(9) . . ? C102 N103 C106 120.9(14) . . ? C102 N103 Gd2 123.0(10) . . ? C106 N103 Gd2 116.0(10) . . ? C112 N104 C116 118.2(13) . . ? C112 N104 Gd2 124.5(11) . . ? C116 N104 Gd2 117.2(9) . . ? C102 C101 N101 109.8(13) . . ? N103 C102 C101 119.9(14) . . ? N103 C102 C103 117.9(14) . . ? C101 C102 C103 122.0(15) . . ? C104 C103 C102 120.8(16) . . ? C103 C104 C105 121.0(15) . . ? C104 C105 C106 117.9(14) . . ? N103 C106 C105 121.5(15) . . ? N103 C106 C107 114.6(13) . . ? C105 C106 C107 123.9(13) . . ? O102 C107 O101 126.5(15) . . ? O102 C107 C106 118.1(14) . . ? O101 C107 C106 115.4(12) . . ? C109 C108 N101 110.4(15) . . ? O104 C109 O103 119.1(18) . . ? O104 C109 C108 119.6(17) . . ? O103 C109 C108 120.8(16) . . ? N102 C111 C112 114.1(12) . . ? N104 C112 C113 122.7(16) . . ? N104 C112 C111 117.4(13) . . ? C113 C112 C111 119.8(15) . . ? C114 C113 C112 118.6(16) . . ? C113 C114 C115 118.6(15) . . ? C116 C115 C114 119.1(16) . . ? C115 C116 N104 122.5(14) . . ? C115 C116 C117 125.9(17) . . ? N104 C116 C117 111.5(14) . . ? O111 C117 O112 123.2(15) . . ? O111 C117 C116 119.6(15) . . ? O112 C117 C116 116.9(14) . . ? C119 C118 N102 109.7(13) . . ? O113 C119 O114 118.7(13) . . ? O113 C119 C118 124.5(14) . . ? O114 C119 C118 116.7(14) . . ? C122 C121 N101 114.5(12) . . ? C121 C122 N102 110.3(13) . . ? O211 Gd3 O213 137.2(4) . . ? O211 Gd3 O203 83.7(4) . . ? O213 Gd3 O203 135.9(4) . . ? O211 Gd3 O201 74.2(3) . . ? O213 Gd3 O201 78.1(3) . . ? O203 Gd3 O201 141.1(4) . . ? O211 Gd3 O222 71.1(4) . . ? O213 Gd3 O222 68.1(3) . . ? O203 Gd3 O222 135.2(3) . . ? O201 Gd3 O222 66.5(3) . . ? O211 Gd3 O221 67.0(4) . . ? O213 Gd3 O221 134.2(4) . . ? O203 Gd3 O221 67.7(4) . . ? O201 Gd3 O221 74.2(3) . . ? O222 Gd3 O221 128.4(4) . . ? O211 Gd3 N204 63.1(4) . . ? O213 Gd3 N204 112.3(4) . . ? O203 Gd3 N204 66.0(4) . . ? O201 Gd3 N204 126.2(4) . . ? O222 Gd3 N204 69.6(4) . . ? O221 Gd3 N204 113.5(4) . . ? O211 Gd3 N203 123.4(4) . . ? O213 Gd3 N203 68.6(3) . . ? O203 Gd3 N203 106.3(4) . . ? O201 Gd3 N203 63.6(4) . . ? O222 Gd3 N203 118.5(4) . . ? O221 Gd3 N203 66.6(4) . . ? N204 Gd3 N203 170.2(4) . . ? O211 Gd3 N202 125.2(3) . . ? O213 Gd3 N202 62.4(3) . . ? O203 Gd3 N202 81.4(4) . . ? O201 Gd3 N202 137.4(3) . . ? O222 Gd3 N202 83.7(4) . . ? O221 Gd3 N202 145.9(4) . . ? N204 Gd3 N202 62.7(4) . . ? N203 Gd3 N202 111.3(4) . . ? O211 Gd3 N201 141.0(4) . . ? O213 Gd3 N201 81.8(4) . . ? O203 Gd3 N201 60.4(4) . . ? O201 Gd3 N201 124.2(3) . . ? O222 Gd3 N201 145.6(4) . . ? O221 Gd3 N201 84.5(4) . . ? N204 Gd3 N201 109.6(4) . . ? N203 Gd3 N201 60.6(4) . . ? N202 Gd3 N201 67.3(3) . . ? C207 O201 Gd3 122.7(9) . . ? C207 O202 Gd4 113.5(9) . . ? C209 O203 Gd3 119.3(10) . . ? C217 O211 Gd3 128.6(9) . . ? C219 O213 Gd3 118.3(9) . . ? C208 N201 C221 112.3(12) . . ? C208 N201 C201 106.2(12) . . ? C221 N201 C201 106.4(12) . . ? C208 N201 Gd3 107.6(9) . . ? C221 N201 Gd3 109.6(8) . . ? C201 N201 Gd3 114.8(9) . . ? C211 N202 C218 107.6(12) . . ? C211 N202 C222 107.9(11) . . ? C218 N202 C222 107.7(11) . . ? C211 N202 Gd3 117.5(9) . . ? C218 N202 Gd3 105.1(9) . . ? C222 N202 Gd3 110.6(9) . . ? C202 N203 C206 122.2(14) . . ? C202 N203 Gd3 124.4(10) . . ? C206 N203 Gd3 113.4(9) . . ? C216 N204 C212 118.9(13) . . ? C216 N204 Gd3 118.0(9) . . ? C212 N204 Gd3 123.1(10) . . ? C202 C201 N201 107.8(11) . . ? N203 C202 C203 119.3(16) . . ? N203 C202 C201 120.0(13) . . ? C203 C202 C201 120.8(14) . . ? C202 C203 C204 119.4(16) . . ? C205 C204 C203 119.9(16) . . ? C204 C205 C206 117.6(15) . . ? N203 C206 C205 121.0(14) . . ? N203 C206 C207 117.6(13) . . ? C205 C206 C207 121.0(13) . . ? O202 C207 O201 125.6(13) . . ? O202 C207 C206 116.5(13) . . ? O201 C207 C206 117.8(13) . . ? N201 C208 C209 106.5(12) . . ? O204 C209 O203 126.8(16) . . ? O204 C209 C208 114.1(14) . . ? O203 C209 C208 119.0(14) . . ? N202 C211 C212 113.0(12) . . ? N204 C212 C213 122.2(14) . . ? N204 C212 C211 116.2(13) . . ? C213 C212 C211 121.3(14) . . ? C212 C213 C214 119.5(15) . . ? C213 C214 C215 117.4(16) . . ? C216 C215 C214 118.6(16) . . ? N204 C216 C215 123.2(14) . . ? N204 C216 C217 115.0(12) . . ? C215 C216 C217 121.7(13) . . ? O212 C217 O211 127.8(13) . . ? O212 C217 C216 116.8(12) . . ? O211 C217 C216 115.3(11) . . ? N202 C218 C219 109.5(14) . . ? O213 C219 O214 124.0(14) . . ? O213 C219 C218 118.4(14) . . ? O214 C219 C218 117.6(15) . . ? C222 C221 N201 113.7(12) . . ? C221 C222 N202 111.5(12) . . ? O202 Gd4 O303 76.6(4) . . ? O202 Gd4 O12 121.5(4) . . ? O303 Gd4 O12 147.8(5) . . ? O202 Gd4 O301 142.5(5) . . ? O303 Gd4 O301 93.2(5) . . ? O12 Gd4 O301 86.0(5) . . ? O202 Gd4 O306 81.5(4) . . ? O303 Gd4 O306 140.2(4) . . ? O12 Gd4 O306 71.8(5) . . ? O301 Gd4 O306 84.3(5) . . ? O202 Gd4 O302 75.6(4) . . ? O303 Gd4 O302 80.6(4) . . ? O12 Gd4 O302 79.2(5) . . ? O301 Gd4 O302 139.1(5) . . ? O306 Gd4 O302 125.3(4) . . ? O202 Gd4 O305 72.8(6) . . ? O303 Gd4 O305 72.0(5) . . ? O12 Gd4 O305 136.2(6) . . ? O301 Gd4 O305 69.7(6) . . ? O306 Gd4 O305 70.0(5) . . ? O302 Gd4 O305 141.9(5) . . ? O202 Gd4 O304 133.9(5) . . ? O303 Gd4 O304 70.0(4) . . ? O12 Gd4 O304 79.4(5) . . ? O301 Gd4 O304 71.4(5) . . ? O306 Gd4 O304 143.4(5) . . ? O302 Gd4 O304 68.5(4) . . ? O305 Gd4 O304 122.7(5) . . ? O2 Gd5 O313 91.5(6) . . ? O2 Gd5 O316 76.1(6) . . ? O313 Gd5 O316 139.7(5) . . ? O2 Gd5 O315 144.2(5) . . ? O313 Gd5 O315 76.7(5) . . ? O316 Gd5 O315 91.3(5) . . ? O2 Gd5 O102 136.3(5) . . ? O313 Gd5 O102 75.6(4) . . ? O316 Gd5 O102 138.1(5) . . ? O315 Gd5 O102 73.8(4) . . ? O2 Gd5 O312 82.7(7) . . ? O313 Gd5 O312 140.6(6) . . ? O316 Gd5 O312 76.5(5) . . ? O315 Gd5 O312 127.3(6) . . ? O102 Gd5 O312 82.1(5) . . ? O2 Gd5 O314 72.6(5) . . ? O313 Gd5 O314 69.2(4) . . ? O316 Gd5 O314 70.5(4) . . ? O315 Gd5 O314 71.7(4) . . ? O102 Gd5 O314 135.0(4) . . ? O312 Gd5 O314 142.5(5) . . ? O2 Gd5 O311 64.0(5) . . ? O313 Gd5 O311 73.4(6) . . ? O316 Gd5 O311 129.4(6) . . ? O315 Gd5 O311 139.1(5) . . ? O102 Gd5 O311 72.3(5) . . ? O312 Gd5 O311 69.1(7) . . ? O314 Gd5 O311 120.6(5) . . ? C422 C421 N421 162.8 . . ? _diffrn_measured_fraction_theta_max 0.905 _diffrn_reflns_theta_full 28.92 _diffrn_measured_fraction_theta_full 0.905 _refine_diff_density_max 3.841 _refine_diff_density_min -3.567 _refine_diff_density_rms 0.284 #===END