# ic990864p.cif Data (IC990864P) _publ_contact_author ; Dr Jean-Pierre Costes Laboratoire de Chimie de Coordination du CNRS 205 Route de Narbonne 31077 Toulouse Cedex 4 France ; _publ_contact_author_phone '(33) 0561333152' _publ_contact_author_fax '(33) 0561553003' _publ_contact_author_email costes@lcc-toulouse.fr _publ_requested_journal 'Inorg. Chem.' _publ_requested_coeditor_name ? _publ_referenced_number IC990864P _publ_section_title ; Is ferromagnetism an intrinsic property of the Cu^II^/Gd^III^ couple? Structures and magnetic properties of two novel dinuclear complexes with a \m-phenolato-\m-oximato (Cu,Gd) core. ; loop_ _publ_author_name _publ_author_address 'Costes, Jean-Pierre' ; Laboratoire de Chimie de Coordination du CNRS 205 Route de Narbonne 31077 Toulouse Cedex 4 France ; 'Dahan, Fran\,coise' ; Laboratoire de Chimie de Coordination du CNRS 205 Route de Narbonne 31077 Toulouse Cedex 4 France ; 'Dupuis, Arnaud' ; Laboratoire de Chimie de Coordination du CNRS 205 Route de Narbonne 31077 Toulouse Cedex 4 France ; 'Laurent, Jean-Pierre' ; Laboratoire de Chimie de Coordination du CNRS 205 Route de Narbonne 31077 Toulouse Cedex 4 France ; data_(1) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H23 Cu Gd N6 O12' _chemical_formula_weight 724.20 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' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Gd' 'Gd' -0.5640 3.9040 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' 'x-1/2, y, -z-1/2' _cell_length_a 12.6295(7) _cell_length_b 20.7874(9) _cell_length_c 18.3301(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4812.3(5) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 13.247 _cell_measurement_theta_max 19.951 _exptl_crystal_description 'Parallelepiped' _exptl_crystal_colour 'Red' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.999 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2848 _exptl_absorpt_coefficient_mu 3.576 _exptl_absorpt_correction_type 'Gaussian' _exptl_absorpt_correction_T_min 0.3288 _exptl_absorpt_correction_T_max 0.6160 _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 'Enraf-Nonius CAD4' _diffrn_measurement_method \w/2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% -0.5 _diffrn_reflns_number 5796 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0311 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 27.97 _reflns_number_total 5796 _reflns_number_gt 3801 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4-EXPRESS' _computing_cell_refinement 'CAD4-EXPRESS' _computing_data_reduction 'MolEN (Fair, 1990)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ZORTEP (Zsolnai, 1990)' _computing_publication_material ? _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 w=1/[\s^2^(Fo^2^)+(0.0185P)^2^+6.0821P] 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 5796 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0573 _refine_ls_R_factor_gt 0.0264 _refine_ls_wR_factor_ref 0.0678 _refine_ls_wR_factor_gt 0.0535 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd Gd 0.303003(15) 0.296153(9) 0.487402(11) 0.02772(6) Uani 1 d . . . Cu Cu 0.48472(4) 0.34973(2) 0.62967(3) 0.02948(11) Uani 1 d . . . O1 O 0.3762(2) 0.38006(12) 0.56116(14) 0.0290(6) Uani 1 d . . . C1 C 0.3501(3) 0.44238(18) 0.5563(2) 0.0257(8) Uani 1 d . . . C2 C 0.2486(3) 0.45826(19) 0.5305(2) 0.0300(8) Uani 1 d . . . C3 C 0.2161(4) 0.5212(2) 0.5264(3) 0.0426(11) Uani 1 d . . . H3 H 0.1484 0.5307 0.5097 0.047 Uiso 1 calc R . . C4 C 0.2834(4) 0.5705(2) 0.5469(3) 0.0462(12) Uani 1 d . . . H4 H 0.2609 0.6130 0.5443 0.051 Uiso 1 calc R . . C5 C 0.3826(4) 0.5564(2) 0.5708(3) 0.0418(11) Uani 1 d . . . H5 H 0.4281 0.5898 0.5836 0.046 Uiso 1 calc R . . C6 C 0.4179(3) 0.49254(18) 0.5766(2) 0.0300(8) Uani 1 d . . . C7 C 0.5240(3) 0.48193(19) 0.6037(2) 0.0331(9) Uani 1 d . . . H7 H 0.5679 0.5178 0.6063 0.036 Uiso 1 calc R . . O2 O 0.1887(2) 0.40469(13) 0.51260(17) 0.0393(7) Uani 1 d . . . C8 C 0.0814(4) 0.4178(2) 0.4905(3) 0.0547(13) Uani 1 d . . . H8A H 0.0461 0.3781 0.4795 0.060 Uiso 1 calc R . . H8B H 0.0819 0.4447 0.4479 0.060 Uiso 1 calc R . . H8C H 0.0448 0.4394 0.5293 0.060 Uiso 1 calc R . . N1 N 0.5635(3) 0.42898(16) 0.62437(18) 0.0306(7) Uani 1 d . . . C9 C 0.6731(3) 0.4292(2) 0.6519(2) 0.0360(10) Uani 1 d . . . H9A H 0.7032 0.4717 0.6453 0.040 Uiso 1 calc R . . H9B H 0.7151 0.3991 0.6237 0.040 Uiso 1 calc R . . C10 C 0.6788(3) 0.4108(2) 0.7330(2) 0.0380(10) Uani 1 d . . . C11 C 0.6664(4) 0.3376(2) 0.7431(3) 0.0465(12) Uani 1 d . . . H11A H 0.7277 0.3164 0.7222 0.051 Uiso 1 calc R . . H11B H 0.6657 0.3281 0.7950 0.051 Uiso 1 calc R . . C12 C 0.5992(4) 0.4480(2) 0.7776(3) 0.0502(12) Uani 1 d . . . H12A H 0.6047 0.4354 0.8279 0.055 Uiso 1 calc R . . H12B H 0.5291 0.4390 0.7602 0.055 Uiso 1 calc R . . H12C H 0.6133 0.4932 0.7733 0.055 Uiso 1 calc R . . C13 C 0.7908(4) 0.4267(2) 0.7581(3) 0.0527(13) Uani 1 d . . . H13A H 0.7985 0.4155 0.8087 0.058 Uiso 1 calc R . . H13B H 0.8035 0.4720 0.7520 0.058 Uiso 1 calc R . . H13C H 0.8409 0.4028 0.7296 0.058 Uiso 1 calc R . . N2 N 0.5702(3) 0.31055(16) 0.70981(19) 0.0351(8) Uani 1 d . . . C14 C 0.5391(3) 0.2536(2) 0.7268(2) 0.0386(10) Uani 1 d . . . C15 C 0.4460(4) 0.2285(2) 0.6876(2) 0.0379(10) Uani 1 d . . . C16 C 0.5903(4) 0.2116(2) 0.7831(2) 0.0505(12) Uani 1 d . . . H16A H 0.6491 0.2339 0.8045 0.056 Uiso 1 calc R . . H16B H 0.6148 0.1727 0.7605 0.056 Uiso 1 calc R . . H16C H 0.5396 0.2012 0.8204 0.056 Uiso 1 calc R . . C17 C 0.4035(5) 0.1634(2) 0.6978(3) 0.0654(16) Uani 1 d . . . H17A H 0.3436 0.1573 0.6664 0.072 Uiso 1 calc R . . H17B H 0.3821 0.1579 0.7477 0.072 Uiso 1 calc R . . H17C H 0.4572 0.1323 0.6861 0.072 Uiso 1 calc R . . N3 N 0.4077(3) 0.26906(16) 0.64078(18) 0.0335(8) Uani 1 d . . . O3 O 0.3223(2) 0.25349(15) 0.60164(17) 0.0435(8) Uani 1 d . . . O4 O 0.1198(3) 0.27505(16) 0.54100(19) 0.0494(8) Uani 1 d . . . O5 O 0.1553(3) 0.21201(16) 0.4537(2) 0.0599(10) Uani 1 d . . . N4 N 0.0925(3) 0.22881(16) 0.5023(2) 0.0356(8) Uani 1 d . . . O6 O 0.0082(2) 0.20009(15) 0.5117(2) 0.0579(10) Uani 1 d . . . O7 O 0.1911(3) 0.33096(15) 0.38239(18) 0.0481(8) Uani 1 d . . . O8 O 0.3422(3) 0.37879(15) 0.39561(18) 0.0463(8) Uani 1 d . . . N5 N 0.2544(4) 0.37508(17) 0.3622(2) 0.0459(10) Uani 1 d . . . O9 O 0.2314(4) 0.41224(18) 0.3133(2) 0.0773(13) Uani 1 d . . . O10 O 0.3774(3) 0.18679(15) 0.4748(2) 0.0528(9) Uani 1 d . . . O11 O 0.3637(3) 0.24027(19) 0.3755(2) 0.0578(9) Uani 1 d . . . N6 N 0.3928(3) 0.1895(2) 0.4068(3) 0.0540(11) Uani 1 d . . . O12 O 0.4333(4) 0.1451(2) 0.3739(3) 0.0914(15) Uani 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 Gd 0.02780(9) 0.02773(9) 0.02764(9) -0.00051(8) -0.00238(9) -0.00489(8) Cu 0.0306(2) 0.0293(2) 0.0285(3) 0.0017(2) -0.0064(2) 0.0002(2) O1 0.0313(14) 0.0270(13) 0.0286(15) -0.0028(11) -0.0063(12) 0.0031(11) C1 0.031(2) 0.0284(19) 0.0176(19) 0.0015(15) 0.0043(15) 0.0037(16) C2 0.032(2) 0.028(2) 0.029(2) 0.0006(17) -0.0002(18) -0.0003(16) C3 0.037(2) 0.037(2) 0.053(3) 0.010(2) 0.004(2) 0.0099(19) C4 0.059(3) 0.025(2) 0.055(3) 0.007(2) 0.000(2) 0.010(2) C5 0.048(3) 0.031(2) 0.047(3) 0.003(2) 0.003(2) -0.004(2) C6 0.037(2) 0.0269(19) 0.026(2) 0.0051(16) -0.0008(17) -0.0011(17) C7 0.039(2) 0.034(2) 0.027(2) -0.0013(17) -0.0015(18) -0.0098(18) O2 0.0265(14) 0.0363(15) 0.0553(19) -0.0021(14) -0.0115(15) 0.0018(12) C8 0.030(2) 0.058(3) 0.076(4) -0.001(3) -0.012(3) 0.002(2) N1 0.0297(17) 0.0358(18) 0.0263(17) 0.0011(14) -0.0035(14) -0.0057(14) C9 0.026(2) 0.047(3) 0.035(2) 0.0015(19) -0.0055(17) -0.0068(18) C10 0.030(2) 0.055(3) 0.029(2) -0.0031(19) -0.0081(17) -0.0053(19) C11 0.041(3) 0.058(3) 0.041(3) 0.005(2) -0.016(2) 0.003(2) C12 0.048(3) 0.068(3) 0.035(3) -0.011(2) 0.006(2) -0.010(3) C13 0.043(3) 0.074(3) 0.041(3) -0.001(3) -0.016(2) -0.010(3) N2 0.0379(19) 0.041(2) 0.0264(18) 0.0014(15) -0.0100(15) 0.0028(15) C14 0.046(2) 0.040(2) 0.030(2) 0.0027(18) 0.0028(19) 0.012(2) C15 0.045(3) 0.042(2) 0.026(2) 0.0082(19) 0.0056(19) -0.001(2) C16 0.065(3) 0.053(3) 0.034(2) 0.007(2) -0.007(2) 0.014(3) C17 0.081(4) 0.055(3) 0.060(4) 0.027(3) -0.012(3) -0.015(3) N3 0.0379(19) 0.0341(18) 0.0284(19) 0.0036(15) -0.0025(16) -0.0020(15) O3 0.0435(18) 0.0499(18) 0.0371(18) 0.0071(14) -0.0105(14) -0.0182(15) O4 0.0472(19) 0.052(2) 0.049(2) -0.0118(16) 0.0012(16) -0.0156(16) O5 0.074(3) 0.047(2) 0.059(2) -0.0071(18) 0.019(2) -0.0027(19) N4 0.0322(17) 0.0299(16) 0.045(2) 0.0053(15) -0.0066(17) 0.0023(15) O6 0.0267(15) 0.0423(18) 0.105(3) 0.009(2) -0.0121(17) -0.0113(14) O7 0.0510(19) 0.0463(18) 0.0469(19) 0.0024(15) -0.0159(17) -0.0085(16) O8 0.0514(19) 0.0419(18) 0.046(2) 0.0032(15) -0.0021(16) -0.0142(15) N5 0.069(3) 0.035(2) 0.034(2) 0.0012(17) -0.005(2) -0.006(2) O9 0.123(4) 0.055(2) 0.054(2) 0.0181(19) -0.019(2) 0.002(2) O10 0.050(2) 0.0422(19) 0.066(3) 0.0009(17) 0.0100(18) 0.0013(15) O11 0.061(2) 0.065(2) 0.047(2) -0.0074(19) 0.0069(18) 0.003(2) N6 0.045(2) 0.051(3) 0.065(3) -0.023(2) 0.003(2) -0.001(2) O12 0.089(3) 0.088(3) 0.097(4) -0.055(3) -0.008(3) 0.031(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 Gd O3 2.287(3) . ? Gd O1 2.393(3) . ? Gd O8 2.455(3) . ? Gd O10 2.471(3) . ? Gd O11 2.479(3) . ? Gd O7 2.496(3) . ? Gd O4 2.551(3) . ? Gd O6 2.593(3) 2_556 ? Gd O5 2.631(4) . ? Gd O2 2.718(3) . ? Cu N1 1.927(3) . ? Cu N3 1.949(3) . ? Cu O1 1.963(3) . ? Cu N2 1.997(3) . ? O1 C1 1.340(4) . ? C1 C6 1.399(5) . ? C1 C2 1.405(5) . ? C2 C3 1.372(5) . ? C2 O2 1.386(5) . ? C3 C4 1.384(6) . ? C4 C5 1.359(6) . ? C5 C6 1.405(5) . ? C6 C7 1.447(6) . ? C7 N1 1.266(5) . ? O2 C8 1.440(5) . ? N1 C9 1.472(5) . ? C9 C10 1.537(6) . ? C10 C12 1.509(6) . ? C10 C13 1.524(6) . ? C10 C11 1.540(6) . ? C11 N2 1.472(5) . ? N2 C14 1.285(5) . ? C14 C15 1.472(6) . ? C14 C16 1.500(6) . ? C15 N3 1.296(5) . ? C15 C17 1.469(6) . ? N3 O3 1.336(4) . ? O4 N4 1.244(4) . ? O5 N4 1.243(5) . ? N4 O6 1.232(4) . ? O6 Gd 2.593(3) 2_456 ? O7 N5 1.272(5) . ? O8 N5 1.269(5) . ? N5 O9 1.218(5) . ? O10 N6 1.262(5) . ? O11 N6 1.256(5) . ? N6 O12 1.216(5) . ? 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 Gd O1 73.99(10) . . ? O3 Gd O8 151.34(11) . . ? O1 Gd O8 78.43(10) . . ? O3 Gd O10 71.85(12) . . ? O1 Gd O10 125.23(11) . . ? O8 Gd O10 120.20(11) . . ? O3 Gd O11 122.88(13) . . ? O1 Gd O11 133.61(11) . . ? O8 Gd O11 72.45(12) . . ? O10 Gd O11 51.22(12) . . ? O3 Gd O7 151.52(11) . . ? O1 Gd O7 116.32(9) . . ? O8 Gd O7 51.87(11) . . ? O10 Gd O7 114.20(12) . . ? O11 Gd O7 70.91(12) . . ? O3 Gd O4 71.17(11) . . ? O1 Gd O4 104.95(10) . . ? O8 Gd O4 124.54(11) . . ? O10 Gd O4 102.86(11) . . ? O11 Gd O4 121.24(11) . . ? O7 Gd O4 80.40(11) . . ? O3 Gd O6 84.24(11) . 2_556 ? O1 Gd O6 65.70(10) . 2_556 ? O8 Gd O6 77.40(11) . 2_556 ? O10 Gd O6 69.41(11) . 2_556 ? O11 Gd O6 73.14(12) . 2_556 ? O7 Gd O6 124.21(12) . 2_556 ? O4 Gd O6 155.38(12) . 2_556 ? O3 Gd O5 91.89(11) . . ? O1 Gd O5 153.04(10) . . ? O8 Gd O5 116.55(12) . . ? O10 Gd O5 68.64(11) . . ? O11 Gd O5 73.34(11) . . ? O7 Gd O5 67.03(11) . . ? O4 Gd O5 48.19(10) . . ? O6 Gd O5 136.90(11) 2_556 . ? O3 Gd O2 102.88(11) . . ? O1 Gd O2 60.26(8) . . ? O8 Gd O2 69.06(10) . . ? O10 Gd O2 169.00(10) . . ? O11 Gd O2 133.94(11) . . ? O7 Gd O2 65.76(10) . . ? O4 Gd O2 66.15(10) . . ? O6 Gd O2 120.32(9) 2_556 . ? O5 Gd O2 102.42(10) . . ? N1 Cu N3 176.72(14) . . ? N1 Cu O1 93.09(12) . . ? N3 Cu O1 89.70(13) . . ? N1 Cu N2 96.11(14) . . ? N3 Cu N2 80.90(14) . . ? O1 Cu N2 168.30(13) . . ? C1 O1 Cu 121.7(2) . . ? C1 O1 Gd 124.9(2) . . ? Cu O1 Gd 113.40(11) . . ? O1 C1 C6 123.5(3) . . ? O1 C1 C2 118.3(3) . . ? C6 C1 C2 118.2(3) . . ? C3 C2 O2 126.1(4) . . ? C3 C2 C1 121.0(4) . . ? O2 C2 C1 112.9(3) . . ? C2 C3 C4 120.4(4) . . ? C5 C4 C3 119.7(4) . . ? C4 C5 C6 121.3(4) . . ? C1 C6 C5 119.4(4) . . ? C1 C6 C7 123.0(4) . . ? C5 C6 C7 117.6(4) . . ? N1 C7 C6 126.9(4) . . ? C2 O2 C8 115.3(3) . . ? C2 O2 Gd 114.7(2) . . ? C8 O2 Gd 127.5(3) . . ? C7 N1 C9 118.0(4) . . ? C7 N1 Cu 123.7(3) . . ? C9 N1 Cu 118.1(3) . . ? N1 C9 C10 112.0(3) . . ? C12 C10 C13 110.0(4) . . ? C12 C10 C9 111.5(4) . . ? C13 C10 C9 106.4(4) . . ? C12 C10 C11 111.9(4) . . ? C13 C10 C11 105.8(4) . . ? C9 C10 C11 111.0(4) . . ? N2 C11 C10 114.2(4) . . ? C14 N2 C11 120.3(4) . . ? C14 N2 Cu 112.8(3) . . ? C11 N2 Cu 126.6(3) . . ? N2 C14 C15 116.9(4) . . ? N2 C14 C16 124.8(4) . . ? C15 C14 C16 118.3(4) . . ? N3 C15 C17 123.2(4) . . ? N3 C15 C14 113.0(4) . . ? C17 C15 C14 123.8(4) . . ? C15 N3 O3 120.0(4) . . ? C15 N3 Cu 116.2(3) . . ? O3 N3 Cu 123.7(3) . . ? N3 O3 Gd 118.9(2) . . ? N4 O4 Gd 99.5(3) . . ? N4 O5 Gd 95.6(3) . . ? O6 N4 O5 121.0(4) . . ? O6 N4 O4 122.3(4) . . ? O5 N4 O4 116.7(4) . . ? N4 O6 Gd 148.2(3) . 2_456 ? N5 O7 Gd 94.4(2) . . ? N5 O8 Gd 96.5(2) . . ? O9 N5 O8 121.7(4) . . ? O9 N5 O7 121.4(4) . . ? O8 N5 O7 116.9(4) . . ? N6 O10 Gd 96.3(3) . . ? N6 O11 Gd 96.1(3) . . ? O12 N6 O11 122.3(5) . . ? O12 N6 O10 121.4(5) . . ? O11 N6 O10 116.4(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Gd O1 Cu N3 -34.23(14) . . . . ? O1 Cu N3 O3 5.9(3) . . . . ? Cu N3 O3 Gd 27.6(4) . . . . ? N3 O3 Gd O1 -38.5(2) . . . . ? O3 Gd O1 Cu 40.08(12) . . . . ? _diffrn_measured_fraction_theta_max 0.909 _diffrn_reflns_theta_full 27.97 _diffrn_measured_fraction_theta_full 0.909 _refine_diff_density_max 0.593 _refine_diff_density_min -0.610 _refine_diff_density_rms 0.129 data_(2) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H25 Cu Gd N6 O14' _chemical_formula_weight 746.21 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' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Gd' 'Gd' -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, -z-1/2' _cell_length_a 12.7246(16) _cell_length_b 13.5691(17) _cell_length_c 14.5310(19) _cell_angle_alpha 90.00 _cell_angle_beta 94.629(16) _cell_angle_gamma 90.00 _cell_volume 2500.8(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12.0 _cell_measurement_theta_max 19.6 _exptl_crystal_description 'Plate' _exptl_crystal_colour 'Dark-red' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.982 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1472 _exptl_absorpt_coefficient_mu 3.559 _exptl_absorpt_correction_type 'Psi-scans' _exptl_absorpt_correction_T_min 0.5929 _exptl_absorpt_correction_T_max 0.9996 _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 'Enraf-Nonius CAD4' _diffrn_measurement_method \w-2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% -0.8 _diffrn_reflns_number 5641 _diffrn_reflns_av_R_equivalents 0.0151 _diffrn_reflns_av_sigmaI/netI 0.0250 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 27.00 _reflns_number_total 5436 _reflns_number_gt 4480 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4-EXPRESS' _computing_cell_refinement 'CAD4-EXPRESS' _computing_data_reduction 'MolEN (Fair, 1990)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ZORTEP (Zsolnai, 1996)' _computing_publication_material ? _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 w=1/[\s^2^(Fo^2^)+(0.0444P)^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 5436 _refine_ls_number_parameters 359 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0364 _refine_ls_R_factor_gt 0.0279 _refine_ls_wR_factor_ref 0.0608 _refine_ls_wR_factor_gt 0.0578 _refine_ls_goodness_of_fit_ref 1.157 _refine_ls_restrained_S_all 1.157 _refine_ls_shift/su_max 0.004 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd Gd 0.532842(12) 0.141771(11) 0.333468(11) 0.02816(7) Uani 1 d . . . Cu Cu 0.27019(3) 0.20116(3) 0.39531(3) 0.03352(11) Uani 1 d . . . O1 O 0.40220(18) 0.25861(16) 0.36629(16) 0.0314(5) Uani 1 d . . . C1 C 0.4192(3) 0.3562(2) 0.3727(2) 0.0278(7) Uani 1 d . . . C2 C 0.5247(3) 0.3876(3) 0.3740(2) 0.0298(7) Uani 1 d . . . C3 C 0.5526(3) 0.4863(3) 0.3775(3) 0.0420(9) Uani 1 d . . . H3 H 0.6230 0.5048 0.3776 0.046 Uiso 1 calc R . . C4 C 0.4739(3) 0.5578(3) 0.3808(3) 0.0446(9) Uani 1 d . . . H4 H 0.4916 0.6243 0.3843 0.049 Uiso 1 calc R . . C5 C 0.3702(3) 0.5292(3) 0.3789(3) 0.0384(8) Uani 1 d . . . H5 H 0.3178 0.5769 0.3791 0.042 Uiso 1 calc R . . C6 C 0.3417(3) 0.4283(2) 0.3766(2) 0.0352(8) Uani 1 d . . . C7 C 0.2299(3) 0.4088(3) 0.3762(2) 0.0339(7) Uani 1 d . . . H7 H 0.1844 0.4625 0.3712 0.037 Uiso 1 calc R . . O2 O 0.59760(19) 0.31172(18) 0.37061(18) 0.0366(6) Uani 1 d . . . C8 C 0.7083(3) 0.3396(3) 0.3825(4) 0.0656(15) Uani 1 d . . . H8A H 0.7514 0.2819 0.3787 0.072 Uiso 1 calc R . . H8B H 0.7229 0.3700 0.4418 0.072 Uiso 1 calc R . . H8C H 0.7237 0.3852 0.3350 0.072 Uiso 1 calc R . . N1 N 0.1885(2) 0.3218(2) 0.3824(2) 0.0348(6) Uani 1 d . . . C9 C 0.0707(3) 0.3083(3) 0.3774(3) 0.0443(9) Uani 1 d . . . C10 C 0.0508(3) 0.2100(2) 0.4260(3) 0.0415(9) Uani 1 d . . . H10A H 0.0518 0.2199 0.4921 0.046 Uiso 1 calc R . . H10B H -0.0176 0.1837 0.4041 0.046 Uiso 1 calc R . . C11 C 0.0329(4) 0.3026(4) 0.2755(3) 0.0620(13) Uani 1 d . . . H11A H 0.0675 0.2488 0.2474 0.068 Uiso 1 calc R . . H11B H 0.0494 0.3631 0.2456 0.068 Uiso 1 calc R . . H11C H -0.0419 0.2923 0.2692 0.068 Uiso 1 calc R . . C12 C 0.0162(3) 0.3902(3) 0.4249(3) 0.0540(11) Uani 1 d . . . H12A H 0.0423 0.3927 0.4887 0.059 Uiso 1 calc R . . H12B H -0.0584 0.3781 0.4205 0.059 Uiso 1 calc R . . H12C H 0.0299 0.4518 0.3958 0.059 Uiso 1 calc R . . N2 N 0.1350(2) 0.1410(2) 0.4046(2) 0.0369(7) Uani 1 d . . . C13 C 0.1283(3) 0.0486(3) 0.3875(2) 0.0317(7) Uani 1 d . . . C14 C 0.2323(3) 0.0012(2) 0.3752(2) 0.0314(7) Uani 1 d . . . C15 C 0.0299(3) -0.0107(3) 0.3803(3) 0.0490(10) Uani 1 d . . . H15A H -0.0290 0.0309 0.3907 0.054 Uiso 1 calc R . . H15B H 0.0352 -0.0622 0.4258 0.054 Uiso 1 calc R . . H15C H 0.0197 -0.0393 0.3198 0.054 Uiso 1 calc R . . C16 C 0.2396(3) -0.1080(3) 0.3625(3) 0.0405(9) Uani 1 d . . . H16A H 0.3113 -0.1259 0.3549 0.045 Uiso 1 calc R . . H16B H 0.1957 -0.1273 0.3087 0.045 Uiso 1 calc R . . H16C H 0.2163 -0.1408 0.4158 0.045 Uiso 1 calc R . . N3 N 0.3106(2) 0.0603(2) 0.3801(2) 0.0314(6) Uani 1 d . . . O3 O 0.40849(19) 0.02471(17) 0.37611(18) 0.0374(6) Uani 1 d . . . O4 O 0.3352(2) 0.2219(2) 0.5531(2) 0.0485(7) Uani 1 d . . . H41 H 0.303(3) 0.166(2) 0.574(3) 0.051(13) Uiso 1 d . . . H42 H 0.305(4) 0.280(3) 0.577(3) 0.061(14) Uiso 1 d . . . O5 O 0.5365(2) 0.1506(2) 0.50411(19) 0.0415(6) Uani 1 d . . . H51 H 0.478(3) 0.189(3) 0.520(4) 0.065(15) Uiso 1 d . . . H52 H 0.544(3) 0.094(2) 0.540(3) 0.069(15) Uiso 1 d . . . O6 O 0.6158(2) -0.0179(2) 0.3836(2) 0.0470(7) Uani 1 d . . . O7 O 0.7226(2) 0.1050(2) 0.3933(2) 0.0503(7) Uani 1 d . . . N4 N 0.7092(3) 0.0131(3) 0.3933(2) 0.0463(8) Uani 1 d . . . O8 O 0.7849(2) -0.0445(3) 0.4023(3) 0.0726(11) Uani 1 d . . . O9 O 0.4839(2) 0.2408(2) 0.18374(19) 0.0457(7) Uani 1 d . . . O10 O 0.3941(2) 0.1106(2) 0.20865(19) 0.0434(6) Uani 1 d . . . N5 N 0.4116(3) 0.1807(3) 0.1544(2) 0.0442(8) Uani 1 d . . . O11 O 0.3623(3) 0.1908(3) 0.0802(2) 0.0674(10) Uani 1 d . . . O12 O 0.6833(3) 0.2018(2) 0.2212(2) 0.0636(9) Uani 1 d . . . O13 O 0.6151(2) 0.0589(2) 0.2051(2) 0.0498(7) Uani 1 d . . . N6 N 0.6797(3) 0.1214(3) 0.1808(2) 0.0433(8) Uani 1 d . . . O14 O 0.7206(2) 0.1089(3) 0.1069(2) 0.0576(8) Uani 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 Gd 0.03284(10) 0.02393(9) 0.02681(10) 0.00069(6) -0.00320(6) -0.00169(6) Cu 0.0355(2) 0.0230(2) 0.0416(3) 0.00186(17) 0.00040(18) -0.00129(16) O1 0.0381(12) 0.0223(11) 0.0336(13) -0.0008(10) 0.0015(10) 0.0001(9) C1 0.0369(17) 0.0215(14) 0.0242(16) 0.0003(12) -0.0031(13) -0.0035(12) C2 0.0348(17) 0.0334(17) 0.0208(16) 0.0021(13) 0.0001(13) -0.0046(14) C3 0.049(2) 0.0309(18) 0.044(2) -0.0009(16) -0.0080(17) -0.0153(16) C4 0.055(2) 0.0255(18) 0.053(3) -0.0060(16) 0.0007(19) -0.0056(16) C5 0.047(2) 0.0239(17) 0.044(2) 0.0030(15) 0.0057(17) 0.0013(15) C6 0.051(2) 0.0227(15) 0.0304(18) 0.0019(13) -0.0074(15) -0.0046(14) C7 0.0413(18) 0.0300(17) 0.0303(18) 0.0035(14) 0.0017(14) 0.0062(15) O2 0.0346(12) 0.0319(13) 0.0421(15) -0.0021(11) -0.0032(11) -0.0060(10) C8 0.045(2) 0.047(2) 0.101(4) -0.018(3) -0.016(3) -0.010(2) N1 0.0489(17) 0.0288(14) 0.0268(15) -0.0013(12) 0.0034(13) 0.0019(13) C9 0.051(2) 0.038(2) 0.042(2) 0.0099(17) -0.0093(18) -0.0062(17) C10 0.0318(17) 0.0326(18) 0.061(3) 0.0073(17) 0.0086(17) 0.0009(15) C11 0.057(3) 0.089(4) 0.038(2) 0.008(2) -0.008(2) 0.004(3) C12 0.054(2) 0.041(2) 0.068(3) 0.010(2) 0.011(2) 0.0101(19) N2 0.0304(14) 0.0319(16) 0.0478(19) 0.0029(13) -0.0013(13) 0.0005(11) C13 0.0317(16) 0.0385(18) 0.0251(17) 0.0043(14) 0.0033(13) -0.0073(14) C14 0.0410(18) 0.0287(17) 0.0240(16) -0.0007(13) -0.0003(14) -0.0024(14) C15 0.0360(19) 0.044(2) 0.066(3) -0.006(2) 0.0020(18) -0.0182(17) C16 0.049(2) 0.0280(17) 0.043(2) -0.0018(15) -0.0074(17) -0.0050(16) N3 0.0407(15) 0.0246(13) 0.0277(15) -0.0013(11) -0.0048(12) 0.0042(12) O3 0.0398(13) 0.0293(12) 0.0425(15) 0.0038(11) 0.0003(11) 0.0001(10) O4 0.0637(18) 0.0469(17) 0.0358(15) 0.0067(13) 0.0099(13) -0.0004(15) O5 0.0475(15) 0.0429(15) 0.0331(14) 0.0030(12) -0.0026(12) 0.0052(12) O6 0.0421(14) 0.0435(15) 0.0552(18) 0.0192(14) 0.0025(13) 0.0020(12) O7 0.0396(14) 0.0547(17) 0.0547(19) 0.0037(15) -0.0079(13) -0.0059(13) N4 0.0481(19) 0.051(2) 0.0391(19) 0.0145(16) 0.0004(15) -0.0043(16) O8 0.0539(18) 0.072(2) 0.091(3) 0.034(2) -0.0007(18) 0.0241(17) O9 0.0536(16) 0.0395(15) 0.0438(16) 0.0034(12) 0.0031(13) -0.0015(12) O10 0.0545(16) 0.0401(14) 0.0343(15) -0.0027(12) -0.0043(12) -0.0059(12) N5 0.056(2) 0.0451(18) 0.0295(17) -0.0059(15) -0.0061(15) 0.0113(16) O11 0.089(2) 0.073(2) 0.0354(17) -0.0069(15) -0.0203(16) 0.0254(19) O12 0.080(2) 0.0536(19) 0.056(2) -0.0099(16) 0.0001(17) -0.0031(17) O13 0.0589(17) 0.0456(16) 0.0454(17) 0.0056(13) 0.0067(14) -0.0035(14) N6 0.0445(18) 0.0484(19) 0.0368(18) 0.0124(15) 0.0015(14) 0.0096(15) O14 0.0598(18) 0.069(2) 0.0480(19) 0.0111(16) 0.0272(15) 0.0188(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 Gd O3 2.360(2) . ? Gd O1 2.373(2) . ? Gd O10 2.464(3) . ? Gd O5 2.479(3) . ? Gd O13 2.481(3) . ? Gd O2 2.493(2) . ? Gd O6 2.493(3) . ? Gd O7 2.549(3) . ? Gd O9 2.590(3) . ? Gd O12 2.738(4) . ? Cu N2 1.919(3) . ? Cu O1 1.929(2) . ? Cu N1 1.941(3) . ? Cu N3 1.996(3) . ? Cu O4 2.391(3) . ? O1 C1 1.344(4) . ? C1 C6 1.394(5) . ? C1 C2 1.407(5) . ? C2 C3 1.385(5) . ? C2 O2 1.390(4) . ? C3 C4 1.398(5) . ? C3 H3 0.9300 . ? C4 C5 1.373(5) . ? C4 H4 0.9300 . ? C5 C6 1.416(5) . ? C5 H5 0.9300 . ? C6 C7 1.446(5) . ? C7 N1 1.298(5) . ? C7 H7 0.9300 . ? O2 C8 1.455(5) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? N1 C9 1.506(5) . ? C9 C12 1.506(6) . ? C9 C11 1.520(6) . ? C9 C10 1.541(5) . ? C10 N2 1.475(5) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? N2 C13 1.280(4) . ? C13 C15 1.485(4) . ? C13 C14 1.496(5) . ? C14 N3 1.276(4) . ? C14 C16 1.497(5) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? N3 O3 1.341(4) . ? O4 H41 0.93(4) . ? O4 H42 0.95(4) . ? O5 H51 0.95(4) . ? O5 H52 0.93(3) . ? O6 N4 1.259(4) . ? O7 N4 1.259(5) . ? N4 O8 1.239(4) . ? O9 N5 1.276(4) . ? O10 N5 1.267(4) . ? N5 O11 1.210(4) . ? O12 N6 1.238(4) . ? O13 N6 1.251(4) . ? N6 O14 1.242(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 O3 Gd O1 84.35(8) . . ? O3 Gd O10 67.77(9) . . ? O1 Gd O10 77.92(9) . . ? O3 Gd O5 74.26(9) . . ? O1 Gd O5 73.96(9) . . ? O10 Gd O5 134.35(9) . . ? O3 Gd O13 103.00(9) . . ? O1 Gd O13 143.01(9) . . ? O10 Gd O13 71.91(9) . . ? O5 Gd O13 143.03(9) . . ? O3 Gd O2 141.50(9) . . ? O1 Gd O2 64.10(8) . . ? O10 Gd O2 121.54(8) . . ? O5 Gd O2 76.09(9) . . ? O13 Gd O2 115.45(9) . . ? O3 Gd O6 67.37(8) . . ? O1 Gd O6 143.97(9) . . ? O10 Gd O6 109.09(9) . . ? O5 Gd O6 77.07(9) . . ? O13 Gd O6 68.39(10) . . ? O2 Gd O6 128.02(9) . . ? O3 Gd O7 114.57(9) . . ? O1 Gd O7 136.20(9) . . ? O10 Gd O7 145.14(10) . . ? O5 Gd O7 74.19(10) . . ? O13 Gd O7 73.87(10) . . ? O2 Gd O7 79.60(9) . . ? O6 Gd O7 50.46(9) . . ? O3 Gd O9 116.67(9) . . ? O1 Gd O9 72.39(9) . . ? O10 Gd O9 50.30(9) . . ? O5 Gd O9 143.04(9) . . ? O13 Gd O9 71.99(9) . . ? O2 Gd O9 75.82(8) . . ? O6 Gd O9 139.80(9) . . ? O7 Gd O9 123.02(9) . . ? O3 Gd O12 150.77(9) . . ? O1 Gd O12 117.12(9) . . ? O10 Gd O12 96.12(9) . . ? O5 Gd O12 128.62(9) . . ? O13 Gd O12 47.84(9) . . ? O2 Gd O12 67.60(9) . . ? O6 Gd O12 97.64(9) . . ? O7 Gd O12 64.70(10) . . ? O9 Gd O12 58.49(9) . . ? N2 Cu O1 171.40(13) . . ? N2 Cu N1 83.66(13) . . ? O1 Cu N1 96.14(11) . . ? N2 Cu N3 80.84(12) . . ? O1 Cu N3 97.25(11) . . ? N1 Cu N3 159.74(12) . . ? N2 Cu O4 103.03(13) . . ? O1 Cu O4 85.53(10) . . ? N1 Cu O4 97.72(11) . . ? N3 Cu O4 98.42(11) . . ? C1 O1 Cu 121.4(2) . . ? C1 O1 Gd 124.1(2) . . ? Cu O1 Gd 114.23(10) . . ? O1 C1 C6 125.7(3) . . ? O1 C1 C2 116.6(3) . . ? C6 C1 C2 117.6(3) . . ? C3 C2 O2 123.2(3) . . ? C3 C2 C1 122.4(3) . . ? O2 C2 C1 114.4(3) . . ? C2 C3 C4 119.3(3) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C5 C4 C3 119.5(3) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? C4 C5 C6 121.2(3) . . ? C4 C5 H5 119.4 . . ? C6 C5 H5 119.4 . . ? C1 C6 C5 119.9(3) . . ? C1 C6 C7 124.8(3) . . ? C5 C6 C7 115.3(3) . . ? N1 C7 C6 124.8(3) . . ? N1 C7 H7 117.6 . . ? C6 C7 H7 117.6 . . ? C2 O2 C8 116.5(3) . . ? C2 O2 Gd 118.90(19) . . ? C8 O2 Gd 124.5(2) . . ? O2 C8 H8A 109.5 . . ? O2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? O2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 N1 C9 121.0(3) . . ? C7 N1 Cu 123.8(3) . . ? C9 N1 Cu 115.2(2) . . ? C12 C9 N1 112.4(3) . . ? C12 C9 C11 111.3(4) . . ? N1 C9 C11 106.8(3) . . ? C12 C9 C10 109.2(3) . . ? N1 C9 C10 106.4(3) . . ? C11 C9 C10 110.6(3) . . ? N2 C10 C9 107.7(3) . . ? N2 C10 H10A 110.2 . . ? C9 C10 H10A 110.2 . . ? N2 C10 H10B 110.2 . . ? C9 C10 H10B 110.2 . . ? H10A C10 H10B 108.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C13 N2 C10 128.6(3) . . ? C13 N2 Cu 116.7(3) . . ? C10 N2 Cu 114.6(2) . . ? N2 C13 C15 126.0(3) . . ? N2 C13 C14 113.5(3) . . ? C15 C13 C14 120.5(3) . . ? N3 C14 C13 114.7(3) . . ? N3 C14 C16 125.0(3) . . ? C13 C14 C16 120.3(3) . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C14 N3 O3 119.6(3) . . ? C14 N3 Cu 113.6(2) . . ? O3 N3 Cu 126.7(2) . . ? N3 O3 Gd 114.45(18) . . ? Cu O4 H41 95(3) . . ? Cu O4 H42 109(3) . . ? H41 O4 H42 111(4) . . ? Gd O5 H51 108(3) . . ? Gd O5 H52 121(2) . . ? H51 O5 H52 112(4) . . ? N4 O6 Gd 96.6(2) . . ? N4 O7 Gd 94.0(2) . . ? O8 N4 O6 121.3(4) . . ? O8 N4 O7 121.4(4) . . ? O6 N4 O7 117.3(3) . . ? N5 O9 Gd 93.9(2) . . ? N5 O10 Gd 100.2(2) . . ? O11 N5 O10 122.3(4) . . ? O11 N5 O9 122.2(4) . . ? O10 N5 O9 115.5(3) . . ? N6 O12 Gd 91.1(2) . . ? N6 O13 Gd 103.4(2) . . ? O12 N6 O14 121.9(4) . . ? O12 N6 O13 117.6(4) . . ? O14 N6 O13 118.8(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Gd O1 Cu N3 -1.01(13) . . . . ? O1 Cu N3 O3 15.2(3) . . . . ? Cu N3 O3 Gd -21.6(3) . . . . ? N3 O3 Gd O1 14.7(2) . . . . ? O3 Gd O1 Cu -5.64(11) . . . . ? 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 O4 H41 O8 0.93(4) 2.03(4) 2.951(5) 170(4) 3_656 O4 H41 O6 0.93(4) 2.32(3) 2.967(4) 127(3) 3_656 O4 H42 O14 0.95(4) 1.92(4) 2.862(5) 168(4) 2_455 O5 H51 O4 0.95(4) 1.97(4) 2.881(4) 160(4) . O5 H52 O3 0.93(3) 2.08(4) 2.997(4) 169(3) 3_656 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.809 _refine_diff_density_min -1.152 _refine_diff_density_rms 0.096