A novel 3D Ln(III)-Cu(I) supramolecular architecture based on 2D MOFs with (6,3) topology data_complex 1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H22.50 Cu La1.50 N6 O20' _chemical_formula_weight 914.83 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' 'La' 'La' -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M P-31c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-y, -x, -z+1/2' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'y, x, z-1/2' 'x-y, -y, z-1/2' '-x, -x+y, z-1/2' _cell_length_a 12.814(4) _cell_length_b 12.814(4) _cell_length_c 9.338(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1327.9(8) _cell_formula_units_Z 2 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 1861 _cell_measurement_theta_min 2.85 _cell_measurement_theta_max 26.14 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 2.289 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 894 _exptl_absorpt_coefficient_mu 3.293 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.502453 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(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 7257 _diffrn_reflns_av_R_equivalents 0.0628 _diffrn_reflns_av_sigmaI/netI 0.0325 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_theta_min 3.67 _diffrn_reflns_theta_max 26.36 _reflns_number_total 909 _reflns_number_gt 751 _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^)+(0.0000P)^2^+13.4881P] 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 SHELXL _refine_ls_extinction_coef 0.0033(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 909 _refine_ls_number_parameters 95 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0606 _refine_ls_R_factor_gt 0.0462 _refine_ls_wR_factor_ref 0.1087 _refine_ls_wR_factor_gt 0.1028 _refine_ls_goodness_of_fit_ref 1.221 _refine_ls_restrained_S_all 1.221 _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 La1 La 0.6667 0.3333 0.2500 0.0251(3) Uani 1 6 d S . . Cu1 Cu 0.3333 -0.3333 0.2500 0.0332(6) Uani 1 6 d S . . O1 O 0.7239(5) 0.2208(5) 0.0706(6) 0.0449(14) Uani 1 1 d . . . O2 O 0.7148(6) 0.0574(6) -0.0214(6) 0.0509(16) Uani 1 1 d . . . N1 N 0.5475(4) 0.0950(8) 0.2500 0.0241(18) Uani 1 2 d S . . N2 N 0.4223(4) -0.1553(8) 0.2500 0.0298(19) Uani 1 2 d S . . C1 C 0.6820(7) 0.1102(7) 0.0611(7) 0.0323(17) Uani 1 1 d . . . C2 C 0.5771(6) 0.0324(6) 0.1626(7) 0.0266(15) Uani 1 1 d . . . C3 C 0.5153(7) -0.0914(7) 0.1610(7) 0.0307(16) Uani 1 1 d . . . H3 H 0.5384 -0.1318 0.0971 0.037 Uiso 1 1 calc R . . La2 La 1.0000 0.0000 0.2500 0.0418(8) Uani 0.36 6 d SP . . O3 O 0.7552(13) -0.1224(6) 0.2500 0.089(5) Uani 0.80 2 d SP A 1 O4 O 0.9088(6) -0.1469(6) -0.0402(9) 0.0316(16) Uani 0.43 1 d P . 1 La3 La 0.9088(6) -0.1469(6) -0.0402(9) 0.0316(16) Uani 0.02 1 d P . 1 O5 O 0.862(4) -0.218(5) 0.194(6) 0.12(2) Uani 0.20 1 d P . 2 O6 O 0.910(3) -0.163(3) 0.080(3) 0.087(9) Uani 0.30 1 d P . 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 La1 0.0291(4) 0.0291(4) 0.0171(5) 0.000 0.000 0.0145(2) Cu1 0.0342(8) 0.0342(8) 0.0314(11) 0.000 0.000 0.0171(4) O1 0.047(3) 0.039(3) 0.043(3) -0.001(3) 0.017(3) 0.018(3) O2 0.055(4) 0.062(4) 0.045(3) -0.001(3) 0.020(3) 0.035(3) N1 0.025(3) 0.033(5) 0.016(4) 0.000 -0.001(3) 0.017(2) N2 0.031(3) 0.029(5) 0.029(4) 0.000 -0.004(3) 0.015(2) C1 0.031(4) 0.047(5) 0.024(3) -0.002(3) 0.004(3) 0.023(4) C2 0.025(4) 0.035(4) 0.025(3) 0.001(3) 0.000(3) 0.019(3) C3 0.037(4) 0.032(4) 0.030(4) -0.002(3) 0.002(3) 0.022(4) La2 0.0219(10) 0.0219(10) 0.082(2) 0.000 0.000 0.0110(5) O3 0.057(9) 0.108(10) 0.084(10) -0.020(8) 0.000 0.029(4) O4 0.021(4) 0.021(3) 0.055(5) 0.001(3) -0.003(3) 0.012(3) La3 0.021(4) 0.021(3) 0.055(5) 0.001(3) -0.003(3) 0.012(3) O5 0.08(3) 0.17(5) 0.16(5) 0.12(4) 0.06(3) 0.10(3) O6 0.12(2) 0.084(19) 0.057(16) 0.019(14) 0.051(16) 0.053(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag La1 O1 2.545(6) . ? La1 O1 2.545(6) 4_665 ? La1 O1 2.545(6) 3_665 ? La1 O1 2.545(6) 2_655 ? La1 O1 2.545(6) 6 ? La1 O1 2.545(6) 5_655 ? La1 N1 2.645(8) 2_655 ? La1 N1 2.645(8) . ? La1 N1 2.645(8) 3_665 ? Cu1 N2 1.975(9) 2_545 ? Cu1 N2 1.975(9) . ? Cu1 N2 1.975(9) 3_655 ? O1 C1 1.243(10) . ? O2 C1 1.230(9) . ? O2 La3 2.756(9) 3_765 ? O2 La3 2.854(10) 8_665 ? N1 C2 1.326(8) . ? N1 C2 1.326(8) 5_655 ? N2 C3 1.344(8) 5_655 ? N2 C3 1.344(8) . ? C1 C2 1.536(10) . ? C2 C3 1.374(10) . ? C3 H3 0.9300 . ? La2 O6 2.41(3) 4_665 ? La2 O6 2.41(3) . ? La2 O6 2.41(3) 5_755 ? La2 O6 2.41(3) 2_645 ? La2 O6 2.41(3) 6_545 ? La2 O6 2.41(3) 3_765 ? La2 O5 2.50(6) . ? La2 O5 2.50(6) 4_665 ? La2 O5 2.50(6) 2_645 ? La2 O5 2.50(6) 5_755 ? La2 O5 2.50(6) 3_765 ? La2 O5 2.50(6) 6_545 ? O3 La3 2.252(10) 10_646 ? O3 La3 2.252(10) 8_665 ? O4 La3 1.809(9) 8_665 ? O4 O4 1.809(9) 8_665 ? O4 La3 1.809(9) 9_545 ? O4 O4 1.809(9) 9_545 ? O4 La2 2.559(8) 7_755 ? O4 La3 2.850(12) 2_645 ? O4 La3 2.850(12) 3_765 ? O5 O6 1.25(5) . ? O5 O5 1.29(9) 5_755 ? 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 La1 O1 84.5(3) . 4_665 ? O1 La1 O1 81.4(2) . 3_665 ? O1 La1 O1 151.1(3) 4_665 3_665 ? O1 La1 O1 81.4(2) . 2_655 ? O1 La1 O1 121.2(3) 4_665 2_655 ? O1 La1 O1 81.4(2) 3_665 2_655 ? O1 La1 O1 151.1(3) . 6 ? O1 La1 O1 81.4(2) 4_665 6 ? O1 La1 O1 121.2(3) 3_665 6 ? O1 La1 O1 84.5(3) 2_655 6 ? O1 La1 O1 121.2(3) . 5_655 ? O1 La1 O1 81.4(2) 4_665 5_655 ? O1 La1 O1 84.5(3) 3_665 5_655 ? O1 La1 O1 151.1(3) 2_655 5_655 ? O1 La1 O1 81.4(2) 6 5_655 ? O1 La1 N1 75.55(13) . 2_655 ? O1 La1 N1 60.62(13) 4_665 2_655 ? O1 La1 N1 137.73(14) 3_665 2_655 ? O1 La1 N1 60.62(13) 2_655 2_655 ? O1 La1 N1 75.55(13) 6 2_655 ? O1 La1 N1 137.73(14) 5_655 2_655 ? O1 La1 N1 60.62(13) . . ? O1 La1 N1 75.55(13) 4_665 . ? O1 La1 N1 75.55(13) 3_665 . ? O1 La1 N1 137.73(14) 2_655 . ? O1 La1 N1 137.73(14) 6 . ? O1 La1 N1 60.62(13) 5_655 . ? N1 La1 N1 120.0 2_655 . ? O1 La1 N1 137.73(14) . 3_665 ? O1 La1 N1 137.73(14) 4_665 3_665 ? O1 La1 N1 60.62(13) 3_665 3_665 ? O1 La1 N1 75.55(13) 2_655 3_665 ? O1 La1 N1 60.62(13) 6 3_665 ? O1 La1 N1 75.55(13) 5_655 3_665 ? N1 La1 N1 120.0 2_655 3_665 ? N1 La1 N1 120.0 . 3_665 ? N2 Cu1 N2 120.0 2_545 . ? N2 Cu1 N2 120.0 2_545 3_655 ? N2 Cu1 N2 120.0 . 3_655 ? C1 O1 La1 127.6(5) . . ? C1 O2 La3 125.8(6) . 3_765 ? C1 O2 La3 128.5(5) . 8_665 ? La3 O2 La3 37.6(3) 3_765 8_665 ? C2 N1 C2 116.8(9) . 5_655 ? C2 N1 La1 121.6(4) . . ? C2 N1 La1 121.6(4) 5_655 . ? C3 N2 C3 116.3(9) 5_655 . ? C3 N2 Cu1 121.9(4) 5_655 . ? C3 N2 Cu1 121.9(4) . . ? O2 C1 O1 127.0(7) . . ? O2 C1 C2 117.2(7) . . ? O1 C1 C2 115.8(6) . . ? N1 C2 C3 122.1(7) . . ? N1 C2 C1 114.2(6) . . ? C3 C2 C1 123.7(6) . . ? N2 C3 C2 121.4(7) . . ? N2 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? O6 La2 O6 140.9(16) 4_665 . ? O6 La2 O6 81.3(9) 4_665 5_755 ? O6 La2 O6 82.7(12) . 5_755 ? O6 La2 O6 82.7(12) 4_665 2_645 ? O6 La2 O6 81.3(9) . 2_645 ? O6 La2 O6 130.8(14) 5_755 2_645 ? O6 La2 O6 81.3(9) 4_665 6_545 ? O6 La2 O6 130.8(14) . 6_545 ? O6 La2 O6 81.3(9) 5_755 6_545 ? O6 La2 O6 140.9(16) 2_645 6_545 ? O6 La2 O6 130.8(14) 4_665 3_765 ? O6 La2 O6 81.3(9) . 3_765 ? O6 La2 O6 140.9(16) 5_755 3_765 ? O6 La2 O6 81.3(9) 2_645 3_765 ? O6 La2 O6 82.7(12) 6_545 3_765 ? O6 La2 O5 129.3(11) 4_665 . ? O6 La2 O5 29.5(12) . . ? O6 La2 O5 54.5(12) 5_755 . ? O6 La2 O5 106.6(13) 2_645 . ? O6 La2 O5 111.1(13) 6_545 . ? O6 La2 O5 99.8(11) 3_765 . ? O6 La2 O5 29.5(12) 4_665 4_665 ? O6 La2 O5 129.3(11) . 4_665 ? O6 La2 O5 106.6(13) 5_755 4_665 ? O6 La2 O5 54.5(12) 2_645 4_665 ? O6 La2 O5 99.8(11) 6_545 4_665 ? O6 La2 O5 111.1(13) 3_765 4_665 ? O5 La2 O5 138.6(15) . 4_665 ? O6 La2 O5 54.5(12) 4_665 2_645 ? O6 La2 O5 99.8(11) . 2_645 ? O6 La2 O5 111.1(13) 5_755 2_645 ? O6 La2 O5 29.5(12) 2_645 2_645 ? O6 La2 O5 129.3(11) 6_545 2_645 ? O6 La2 O5 106.6(13) 3_765 2_645 ? O5 La2 O5 115.7(7) . 2_645 ? O5 La2 O5 29.9(18) 4_665 2_645 ? O6 La2 O5 99.8(11) 4_665 5_755 ? O6 La2 O5 54.5(12) . 5_755 ? O6 La2 O5 29.5(12) 5_755 5_755 ? O6 La2 O5 111.1(13) 2_645 5_755 ? O6 La2 O5 106.6(13) 6_545 5_755 ? O6 La2 O5 129.3(11) 3_765 5_755 ? O5 La2 O5 29.9(18) . 5_755 ? O5 La2 O5 115.7(7) 4_665 5_755 ? O5 La2 O5 104.4(16) 2_645 5_755 ? O6 La2 O5 111.1(13) 4_665 3_765 ? O6 La2 O5 106.6(13) . 3_765 ? O6 La2 O5 129.3(11) 5_755 3_765 ? O6 La2 O5 99.8(11) 2_645 3_765 ? O6 La2 O5 54.5(12) 6_545 3_765 ? O6 La2 O5 29.5(12) 3_765 3_765 ? O5 La2 O5 115.7(7) . 3_765 ? O5 La2 O5 104.4(16) 4_665 3_765 ? O5 La2 O5 115.7(7) 2_645 3_765 ? O5 La2 O5 138.6(15) 5_755 3_765 ? O6 La2 O5 106.6(13) 4_665 6_545 ? O6 La2 O5 111.1(13) . 6_545 ? O6 La2 O5 99.8(11) 5_755 6_545 ? O6 La2 O5 129.3(11) 2_645 6_545 ? O6 La2 O5 29.5(12) 6_545 6_545 ? O6 La2 O5 54.5(12) 3_765 6_545 ? O5 La2 O5 104.4(16) . 6_545 ? O5 La2 O5 115.7(7) 4_665 6_545 ? O5 La2 O5 138.6(15) 2_645 6_545 ? O5 La2 O5 115.7(7) 5_755 6_545 ? O5 La2 O5 29.9(18) 3_765 6_545 ? La3 O3 La3 122.3(7) 10_646 8_665 ? La3 O3 La2 61.2(4) 10_646 . ? La3 O3 La2 61.2(4) 8_665 . ? La3 O4 O4 0.0(6) 8_665 8_665 ? La3 O4 La3 104.0(6) 8_665 9_545 ? O4 O4 La3 104.0(6) 8_665 9_545 ? La3 O4 O4 104.0(6) 8_665 9_545 ? O4 O4 O4 104.0(6) 8_665 9_545 ? La3 O4 O4 0.0(6) 9_545 9_545 ? La3 O4 La2 91.4(4) 8_665 7_755 ? O4 O4 La2 91.4(4) 8_665 7_755 ? La3 O4 La2 91.4(4) 9_545 7_755 ? O4 O4 La2 91.4(4) 9_545 7_755 ? La3 O4 La3 90.000(1) 8_665 2_645 ? O4 O4 La3 90.000(1) 8_665 2_645 ? La3 O4 La3 38.0(3) 9_545 2_645 ? O4 O4 La3 38.0(3) 9_545 2_645 ? La2 O4 La3 56.15(13) 7_755 2_645 ? La3 O4 La3 38.0(3) 8_665 3_765 ? O4 O4 La3 38.0(3) 8_665 3_765 ? La3 O4 La3 90.0 9_545 3_765 ? O4 O4 La3 90.0 9_545 3_765 ? La2 O4 La3 56.15(13) 7_755 3_765 ? La3 O4 La3 60.0 2_645 3_765 ? O6 O5 O5 125(4) . 5_755 ? O6 O5 La2 71(3) . . ? O5 O5 La2 75.1(9) 5_755 . ? O5 O6 La2 79(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.36 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.591 _refine_diff_density_min -0.524 _refine_diff_density_rms 0.121 #===END data_complex 2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H22.50 Cu Eu1.50 N6 O20' _chemical_formula_weight 934.40 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' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Eu' 'Eu' -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M P-31c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-y, -x, -z+1/2' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'y, x, z-1/2' 'x-y, -y, z-1/2' '-x, -x+y, z-1/2' _cell_length_a 12.659(8) _cell_length_b 12.659(8) _cell_length_c 9.492(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1317.3(14) _cell_formula_units_Z 2 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 2500 _cell_measurement_theta_min 2.84 _cell_measurement_theta_max 26.44 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 2.356 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 912 _exptl_absorpt_coefficient_mu 4.444 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.482030 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(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 7144 _diffrn_reflns_av_R_equivalents 0.0479 _diffrn_reflns_av_sigmaI/netI 0.0240 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 26.41 _reflns_number_total 904 _reflns_number_gt 751 _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^)+(0.0393P)^2^+3.8580P] 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 904 _refine_ls_number_parameters 91 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0385 _refine_ls_R_factor_gt 0.0284 _refine_ls_wR_factor_ref 0.0841 _refine_ls_wR_factor_gt 0.0779 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _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 Eu1 Eu 0.6667 0.3333 0.2500 0.02151(19) Uani 1 6 d S . . Cu1 Cu 0.3333 -0.3333 0.2500 0.0292(3) Uani 1 6 d S . . O1 O 0.7290(3) 0.2309(3) 0.0767(3) 0.0353(8) Uani 1 1 d . . . O2 O 0.7202(3) 0.0671(3) -0.0221(4) 0.0440(9) Uani 1 1 d . . . N1 N 0.5508(2) 0.1015(4) 0.2500 0.0219(10) Uani 1 2 d S . . N2 N 0.4245(2) -0.1510(5) 0.2500 0.0253(11) Uani 1 2 d S . . C1 C 0.6865(4) 0.1190(4) 0.0644(5) 0.0285(10) Uani 1 1 d . . . C2 C 0.5807(4) 0.0384(4) 0.1621(4) 0.0238(9) Uani 1 1 d . . . C3 C 0.5181(4) -0.0868(4) 0.1612(4) 0.0258(9) Uani 1 1 d . . . H3 H 0.5408 -0.1281 0.0981 0.039(15) Uiso 1 1 calc R . . Eu2 Eu 1.0000 0.0000 0.2500 0.0223(3) Uani 0.40 6 d SP . . O3 O 0.7592(7) -0.1204(3) 0.2500 0.067(2) Uani 0.80 2 d SP A 1 O4 O 0.9287(10) 0.0851(10) 0.0707(11) 0.080(3) Uani 0.50 1 d P B 1 O41 O 0.924(3) 0.146(3) 0.193(4) 0.047(9) Uiso 0.10 1 d P B 1 O5 O 1.0647(5) -0.0890(5) 0.0490(7) 0.0349(13) Uani 0.33 1 d P . 2 Eu3 Eu 1.0647(5) -0.0890(5) 0.0490(7) 0.0349(13) Uani 0.02 1 d P . 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Eu1 0.0230(2) 0.0230(2) 0.0186(3) 0.000 0.000 0.01148(11) Cu1 0.0260(4) 0.0260(4) 0.0354(7) 0.000 0.000 0.0130(2) O1 0.0356(18) 0.0304(18) 0.0334(18) 0.0008(14) 0.0140(15) 0.0117(15) O2 0.049(2) 0.044(2) 0.041(2) -0.0021(16) 0.0177(17) 0.0248(19) N1 0.0244(18) 0.023(2) 0.018(2) 0.000 0.0007(16) 0.0114(12) N2 0.0251(19) 0.026(3) 0.025(3) 0.000 -0.0022(18) 0.0128(13) C1 0.030(2) 0.036(3) 0.021(2) -0.0001(18) 0.0038(18) 0.018(2) C2 0.026(2) 0.028(2) 0.021(2) -0.0008(18) 0.0008(17) 0.0160(19) C3 0.029(2) 0.027(2) 0.024(2) -0.0003(17) 0.0031(18) 0.0157(19) Eu2 0.0208(4) 0.0208(4) 0.0253(7) 0.000 0.000 0.0104(2) O3 0.055(5) 0.084(5) 0.053(5) -0.013(4) 0.000 0.027(2) O4 0.078(7) 0.083(7) 0.074(7) 0.014(6) -0.020(5) 0.037(6) O5 0.034(3) 0.031(3) 0.044(4) 0.007(3) 0.011(3) 0.020(3) Eu3 0.034(3) 0.031(3) 0.044(4) 0.007(3) 0.011(3) 0.020(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 Eu1 O1 2.457(3) 4_665 ? Eu1 O1 2.457(3) . ? Eu1 O1 2.457(3) 6 ? Eu1 O1 2.457(3) 5_655 ? Eu1 O1 2.457(3) 3_665 ? Eu1 O1 2.457(3) 2_655 ? Eu1 N1 2.542(5) . ? Eu1 N1 2.542(5) 2_655 ? Eu1 N1 2.542(5) 3_665 ? Cu1 N2 1.999(5) . ? Cu1 N2 1.999(5) 2_545 ? Cu1 N2 1.999(5) 3_655 ? O1 C1 1.244(6) . ? O2 C1 1.251(5) . ? O2 Eu3 2.610(7) 7_755 ? O2 Eu3 2.908(7) 3_765 ? N1 C2 1.335(5) . ? N1 C2 1.335(5) 5_655 ? N2 C3 1.346(5) 5_655 ? N2 C3 1.346(5) . ? C1 C2 1.526(6) . ? C2 C3 1.373(6) . ? C3 H3 0.9300 . ? Eu2 O4 2.418(9) 5_755 ? Eu2 O4 2.418(9) 2_645 ? Eu2 O4 2.418(9) 4_665 ? Eu2 O4 2.418(9) . ? Eu2 O4 2.418(9) 6_545 ? Eu2 O4 2.418(9) 3_765 ? Eu2 O41 2.52(4) 5_755 ? Eu2 O41 2.52(4) 2_645 ? Eu2 O41 2.52(4) 6_545 ? Eu2 O41 2.52(4) 3_765 ? Eu2 O41 2.52(4) 4_665 ? Eu2 O41 2.52(4) . ? O4 O41 1.40(4) . ? O41 O41 1.41(7) 4_665 ? O5 Eu3 1.930(9) 8_665 ? O5 Eu3 1.930(9) 9_545 ? O5 Eu3 2.929(10) 2_645 ? O5 Eu3 2.929(10) 3_765 ? 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 Eu1 O1 85.31(17) 4_665 . ? O1 Eu1 O1 80.06(13) 4_665 6 ? O1 Eu1 O1 147.70(16) . 6 ? O1 Eu1 O1 80.06(13) 4_665 5_655 ? O1 Eu1 O1 125.57(15) . 5_655 ? O1 Eu1 O1 80.06(13) 6 5_655 ? O1 Eu1 O1 147.70(16) 4_665 3_665 ? O1 Eu1 O1 80.06(13) . 3_665 ? O1 Eu1 O1 125.57(15) 6 3_665 ? O1 Eu1 O1 85.31(17) 5_655 3_665 ? O1 Eu1 O1 125.57(15) 4_665 2_655 ? O1 Eu1 O1 80.06(13) . 2_655 ? O1 Eu1 O1 85.31(17) 6 2_655 ? O1 Eu1 O1 147.70(16) 5_655 2_655 ? O1 Eu1 O1 80.06(13) 3_665 2_655 ? O1 Eu1 N1 73.85(8) 4_665 . ? O1 Eu1 N1 62.79(7) . . ? O1 Eu1 N1 137.34(9) 6 . ? O1 Eu1 N1 62.79(7) 5_655 . ? O1 Eu1 N1 73.85(8) 3_665 . ? O1 Eu1 N1 137.34(9) 2_655 . ? O1 Eu1 N1 62.79(7) 4_665 2_655 ? O1 Eu1 N1 73.85(8) . 2_655 ? O1 Eu1 N1 73.85(8) 6 2_655 ? O1 Eu1 N1 137.34(9) 5_655 2_655 ? O1 Eu1 N1 137.34(9) 3_665 2_655 ? O1 Eu1 N1 62.79(7) 2_655 2_655 ? N1 Eu1 N1 120.0 . 2_655 ? O1 Eu1 N1 137.34(9) 4_665 3_665 ? O1 Eu1 N1 137.34(9) . 3_665 ? O1 Eu1 N1 62.79(7) 6 3_665 ? O1 Eu1 N1 73.85(8) 5_655 3_665 ? O1 Eu1 N1 62.79(7) 3_665 3_665 ? O1 Eu1 N1 73.85(8) 2_655 3_665 ? N1 Eu1 N1 120.0 . 3_665 ? N1 Eu1 N1 120.0 2_655 3_665 ? N2 Cu1 N2 120.0 . 2_545 ? N2 Cu1 N2 120.0 . 3_655 ? N2 Cu1 N2 120.0 2_545 3_655 ? C1 O1 Eu1 126.4(3) . . ? C1 O2 Eu3 128.3(4) . 7_755 ? C1 O2 Eu3 125.3(3) . 3_765 ? Eu3 O2 Eu3 40.5(2) 7_755 3_765 ? C2 N1 C2 117.5(5) . 5_655 ? C2 N1 Eu1 121.2(3) . . ? C2 N1 Eu1 121.2(3) 5_655 . ? C3 N2 C3 117.0(5) 5_655 . ? C3 N2 Cu1 121.5(3) 5_655 . ? C3 N2 Cu1 121.5(3) . . ? O1 C1 O2 126.3(4) . . ? O1 C1 C2 116.1(4) . . ? O2 C1 C2 117.6(4) . . ? N1 C2 C3 121.5(4) . . ? N1 C2 C1 113.4(4) . . ? C3 C2 C1 125.1(4) . . ? N2 C3 C2 121.2(4) . . ? N2 C3 H3 119.4 . . ? C2 C3 H3 119.4 . . ? O4 Eu2 O4 142.3(5) 5_755 2_645 ? O4 Eu2 O4 75.9(4) 5_755 4_665 ? O4 Eu2 O4 134.6(5) 2_645 4_665 ? O4 Eu2 O4 134.6(5) 5_755 . ? O4 Eu2 O4 75.9(4) 2_645 . ? O4 Eu2 O4 89.7(6) 4_665 . ? O4 Eu2 O4 75.9(4) 5_755 6_545 ? O4 Eu2 O4 89.7(6) 2_645 6_545 ? O4 Eu2 O4 75.9(4) 4_665 6_545 ? O4 Eu2 O4 142.3(5) . 6_545 ? O4 Eu2 O4 89.7(6) 5_755 3_765 ? O4 Eu2 O4 75.9(4) 2_645 3_765 ? O4 Eu2 O4 142.3(5) 4_665 3_765 ? O4 Eu2 O4 75.9(4) . 3_765 ? O4 Eu2 O4 134.6(5) 6_545 3_765 ? O4 Eu2 O41 32.9(9) 5_755 5_755 ? O4 Eu2 O41 128.9(8) 2_645 5_755 ? O4 Eu2 O41 96.5(9) 4_665 5_755 ? O4 Eu2 O41 110.6(9) . 5_755 ? O4 Eu2 O41 105.6(9) 6_545 5_755 ? O4 Eu2 O41 58.5(9) 3_765 5_755 ? O4 Eu2 O41 128.9(8) 5_755 2_645 ? O4 Eu2 O41 32.9(9) 2_645 2_645 ? O4 Eu2 O41 110.6(9) 4_665 2_645 ? O4 Eu2 O41 96.5(9) . 2_645 ? O4 Eu2 O41 58.5(9) 6_545 2_645 ? O4 Eu2 O41 105.6(9) 3_765 2_645 ? O41 Eu2 O41 141.7(16) 5_755 2_645 ? O4 Eu2 O41 96.5(9) 5_755 6_545 ? O4 Eu2 O41 58.5(9) 2_645 6_545 ? O4 Eu2 O41 105.6(9) 4_665 6_545 ? O4 Eu2 O41 128.9(8) . 6_545 ? O4 Eu2 O41 32.9(9) 6_545 6_545 ? O4 Eu2 O41 110.6(9) 3_765 6_545 ? O41 Eu2 O41 115.5(6) 5_755 6_545 ? O41 Eu2 O41 32.3(16) 2_645 6_545 ? O4 Eu2 O41 58.5(9) 5_755 3_765 ? O4 Eu2 O41 96.5(9) 2_645 3_765 ? O4 Eu2 O41 128.9(8) 4_665 3_765 ? O4 Eu2 O41 105.6(9) . 3_765 ? O4 Eu2 O41 110.6(9) 6_545 3_765 ? O4 Eu2 O41 32.9(9) 3_765 3_765 ? O41 Eu2 O41 32.3(16) 5_755 3_765 ? O41 Eu2 O41 115.5(6) 2_645 3_765 ? O41 Eu2 O41 101.6(17) 6_545 3_765 ? O4 Eu2 O41 105.6(9) 5_755 4_665 ? O4 Eu2 O41 110.6(9) 2_645 4_665 ? O4 Eu2 O41 32.9(9) 4_665 4_665 ? O4 Eu2 O41 58.5(9) . 4_665 ? O4 Eu2 O41 96.5(9) 6_545 4_665 ? O4 Eu2 O41 128.9(8) 3_765 4_665 ? O41 Eu2 O41 115.5(6) 5_755 4_665 ? O41 Eu2 O41 101.6(17) 2_645 4_665 ? O41 Eu2 O41 115.5(6) 6_545 4_665 ? O41 Eu2 O41 141.7(16) 3_765 4_665 ? O4 Eu2 O41 110.6(9) 5_755 . ? O4 Eu2 O41 105.6(9) 2_645 . ? O4 Eu2 O41 58.5(9) 4_665 . ? O4 Eu2 O41 32.9(9) . . ? O4 Eu2 O41 128.9(8) 6_545 . ? O4 Eu2 O41 96.5(9) 3_765 . ? O41 Eu2 O41 101.6(17) 5_755 . ? O41 Eu2 O41 115.5(6) 2_645 . ? O41 Eu2 O41 141.7(16) 6_545 . ? O41 Eu2 O41 115.5(6) 3_765 . ? O41 Eu2 O41 32.3(16) 4_665 . ? O41 O4 Eu2 77.8(15) . . ? O4 O41 O41 119(3) . 4_665 ? O4 O41 Eu2 69.3(15) . . ? O41 O41 Eu2 73.8(8) 4_665 . ? Eu3 O5 Eu3 98.7(5) 8_665 9_545 ? Eu3 O5 Eu2 94.0(3) 8_665 . ? Eu3 O5 Eu2 94.0(3) 9_545 . ? Eu3 O5 Eu3 90.0 8_665 2_645 ? Eu3 O5 Eu3 40.6(2) 9_545 2_645 ? Eu2 O5 Eu3 54.94(12) . 2_645 ? Eu3 O5 Eu3 40.6(2) 8_665 3_765 ? Eu3 O5 Eu3 90.0 9_545 3_765 ? Eu2 O5 Eu3 54.94(12) . 3_765 ? Eu3 O5 Eu3 60.0 2_645 3_765 ? 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 O1 Eu1 O1 C1 71.3(4) 4_665 . . . ? O1 Eu1 O1 C1 134.3(4) 6 . . . ? O1 Eu1 O1 C1 -3.0(3) 5_655 . . . ? O1 Eu1 O1 C1 -79.8(4) 3_665 . . . ? O1 Eu1 O1 C1 -161.4(4) 2_655 . . . ? N1 Eu1 O1 C1 -3.0(3) . . . . ? N1 Eu1 O1 C1 134.3(4) 2_655 . . . ? N1 Eu1 O1 C1 -108.7(4) 3_665 . . . ? O1 Eu1 N1 C2 -91.2(2) 4_665 . . . ? O1 Eu1 N1 C2 1.9(2) . . . . ? O1 Eu1 N1 C2 -145.8(2) 6 . . . ? O1 Eu1 N1 C2 -178.1(2) 5_655 . . . ? O1 Eu1 N1 C2 88.8(2) 3_665 . . . ? O1 Eu1 N1 C2 34.2(2) 2_655 . . . ? N1 Eu1 N1 C2 -47.0(2) 2_655 . . . ? N1 Eu1 N1 C2 133.0(2) 3_665 . . . ? O1 Eu1 N1 C2 88.8(2) 4_665 . . 5_655 ? O1 Eu1 N1 C2 -178.1(2) . . . 5_655 ? O1 Eu1 N1 C2 34.2(2) 6 . . 5_655 ? O1 Eu1 N1 C2 1.9(2) 5_655 . . 5_655 ? O1 Eu1 N1 C2 -91.2(2) 3_665 . . 5_655 ? O1 Eu1 N1 C2 -145.8(2) 2_655 . . 5_655 ? N1 Eu1 N1 C2 133.0(2) 2_655 . . 5_655 ? N1 Eu1 N1 C2 -47.0(2) 3_665 . . 5_655 ? N2 Cu1 N2 C3 47.3(2) 2_545 . . 5_655 ? N2 Cu1 N2 C3 -132.7(2) 3_655 . . 5_655 ? N2 Cu1 N2 C3 -132.7(2) 2_545 . . . ? N2 Cu1 N2 C3 47.3(2) 3_655 . . . ? Eu1 O1 C1 O2 -178.4(4) . . . . ? Eu1 O1 C1 C2 3.5(6) . . . . ? Eu3 O2 C1 O1 60.4(7) 7_755 . . . ? Eu3 O2 C1 O1 111.5(5) 3_765 . . . ? Eu3 O2 C1 C2 -121.6(4) 7_755 . . . ? Eu3 O2 C1 C2 -70.5(5) 3_765 . . . ? C2 N1 C2 C3 0.3(3) 5_655 . . . ? Eu1 N1 C2 C3 -179.7(3) . . . . ? C2 N1 C2 C1 178.9(4) 5_655 . . . ? Eu1 N1 C2 C1 -1.1(4) . . . . ? O1 C1 C2 N1 -1.4(5) . . . . ? O2 C1 C2 N1 -179.6(4) . . . . ? O1 C1 C2 C3 177.2(4) . . . . ? O2 C1 C2 C3 -1.0(7) . . . . ? C3 N2 C3 C2 0.3(3) 5_655 . . . ? Cu1 N2 C3 C2 -179.7(3) . . . . ? N1 C2 C3 N2 -0.6(6) . . . . ? C1 C2 C3 N2 -179.1(4) . . . . ? O4 Eu2 O4 O41 -52.0(16) 5_755 . . . ? O4 Eu2 O4 O41 154.1(16) 2_645 . . . ? O4 Eu2 O4 O41 17.6(15) 4_665 . . . ? O4 Eu2 O4 O41 83.7(16) 6_545 . . . ? O4 Eu2 O4 O41 -127.2(17) 3_765 . . . ? O41 Eu2 O4 O41 -79(2) 5_755 . . . ? O41 Eu2 O4 O41 128.3(12) 2_645 . . . ? O41 Eu2 O4 O41 128(2) 6_545 . . . ? O41 Eu2 O4 O41 -112.9(9) 3_765 . . . ? O41 Eu2 O4 O41 29(2) 4_665 . . . ? Eu2 O4 O41 O41 -57(2) . . . 4_665 ? O4 Eu2 O41 O4 143.2(12) 5_755 . . . ? O4 Eu2 O41 O4 -26.1(16) 2_645 . . . ? O4 Eu2 O41 O4 -159.2(18) 4_665 . . . ? O4 Eu2 O41 O4 -128.7(12) 6_545 . . . ? O4 Eu2 O41 O4 51.0(15) 3_765 . . . ? O41 Eu2 O41 O4 110.1(17) 5_755 . . . ? O41 Eu2 O41 O4 -59.7(18) 2_645 . . . ? O41 Eu2 O41 O4 -84.7(14) 6_545 . . . ? O41 Eu2 O41 O4 79.2(16) 3_765 . . . ? O41 Eu2 O41 O4 -130(4) 4_665 . . . ? O4 Eu2 O41 O41 -87(3) 5_755 . . 4_665 ? O4 Eu2 O41 O41 104(3) 2_645 . . 4_665 ? O4 Eu2 O41 O41 -29(3) 4_665 . . 4_665 ? O4 Eu2 O41 O41 130(4) . . . 4_665 ? O4 Eu2 O41 O41 1(4) 6_545 . . 4_665 ? O4 Eu2 O41 O41 -179(3) 3_765 . . 4_665 ? O41 Eu2 O41 O41 -120(3) 5_755 . . 4_665 ? O41 Eu2 O41 O41 70(4) 2_645 . . 4_665 ? O41 Eu2 O41 O41 45(3) 6_545 . . 4_665 ? O41 Eu2 O41 O41 -151(2) 3_765 . . 4_665 ? O4 Eu2 O5 Eu3 175.2(3) 5_755 . . 8_665 ? O4 Eu2 O5 Eu3 23.5(5) 2_645 . . 8_665 ? O4 Eu2 O5 Eu3 10(3) 4_665 . . 8_665 ? O4 Eu2 O5 Eu3 -47.9(4) . . . 8_665 ? O4 Eu2 O5 Eu3 95.4(4) 6_545 . . 8_665 ? O4 Eu2 O5 Eu3 -120.2(6) 3_765 . . 8_665 ? O41 Eu2 O5 Eu3 -158.5(9) 5_755 . . 8_665 ? O41 Eu2 O5 Eu3 51.0(9) 2_645 . . 8_665 ? O41 Eu2 O5 Eu3 84.7(9) 6_545 . . 8_665 ? O41 Eu2 O5 Eu3 -158.7(11) 3_765 . . 8_665 ? O41 Eu2 O5 Eu3 -24.5(14) 4_665 . . 8_665 ? O41 Eu2 O5 Eu3 -55.2(10) . . . 8_665 ? O4 Eu2 O5 Eu3 -85.7(4) 5_755 . . 9_545 ? O4 Eu2 O5 Eu3 122.6(6) 2_645 . . 9_545 ? O4 Eu2 O5 Eu3 109(3) 4_665 . . 9_545 ? O4 Eu2 O5 Eu3 51.2(4) . . . 9_545 ? O4 Eu2 O5 Eu3 -165.6(3) 6_545 . . 9_545 ? O4 Eu2 O5 Eu3 -21.2(5) 3_765 . . 9_545 ? O41 Eu2 O5 Eu3 -59.5(9) 5_755 . . 9_545 ? O41 Eu2 O5 Eu3 150.0(10) 2_645 . . 9_545 ? O41 Eu2 O5 Eu3 -176.3(9) 6_545 . . 9_545 ? O41 Eu2 O5 Eu3 -59.6(10) 3_765 . . 9_545 ? O41 Eu2 O5 Eu3 74.6(14) 4_665 . . 9_545 ? O41 Eu2 O5 Eu3 43.8(10) . . . 9_545 ? O4 Eu2 O5 Eu3 -97.6(3) 5_755 . . 2_645 ? O4 Eu2 O5 Eu3 110.7(5) 2_645 . . 2_645 ? O4 Eu2 O5 Eu3 97(3) 4_665 . . 2_645 ? O4 Eu2 O5 Eu3 39.3(3) . . . 2_645 ? O4 Eu2 O5 Eu3 -177.4(3) 6_545 . . 2_645 ? O4 Eu2 O5 Eu3 -33.1(5) 3_765 . . 2_645 ? O41 Eu2 O5 Eu3 -71.3(9) 5_755 . . 2_645 ? O41 Eu2 O5 Eu3 138.1(9) 2_645 . . 2_645 ? O41 Eu2 O5 Eu3 171.9(9) 6_545 . . 2_645 ? O41 Eu2 O5 Eu3 -71.5(10) 3_765 . . 2_645 ? O41 Eu2 O5 Eu3 62.7(14) 4_665 . . 2_645 ? O41 Eu2 O5 Eu3 31.9(10) . . . 2_645 ? O4 Eu2 O5 Eu3 -172.9(3) 5_755 . . 3_765 ? O4 Eu2 O5 Eu3 35.4(6) 2_645 . . 3_765 ? O4 Eu2 O5 Eu3 22(3) 4_665 . . 3_765 ? O4 Eu2 O5 Eu3 -36.0(3) . . . 3_765 ? O4 Eu2 O5 Eu3 107.3(3) 6_545 . . 3_765 ? O4 Eu2 O5 Eu3 -108.4(4) 3_765 . . 3_765 ? O41 Eu2 O5 Eu3 -146.6(9) 5_755 . . 3_765 ? O41 Eu2 O5 Eu3 62.8(9) 2_645 . . 3_765 ? O41 Eu2 O5 Eu3 96.6(9) 6_545 . . 3_765 ? O41 Eu2 O5 Eu3 -146.8(10) 3_765 . . 3_765 ? O41 Eu2 O5 Eu3 -12.6(14) 4_665 . . 3_765 ? O41 Eu2 O5 Eu3 -43.4(10) . . . 3_765 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.41 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.458 _refine_diff_density_min -0.686 _refine_diff_density_rms 0.104 #===END data_complex 3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H22.50 Cu Gd1.50 N6 O20' _chemical_formula_weight 942.34 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 trigonal _symmetry_space_group_name_H-M P-31c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-y, -x, -z+1/2' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'y, x, z-1/2' 'x-y, -y, z-1/2' '-x, -x+y, z-1/2' _cell_length_a 12.6203(11) _cell_length_b 12.6203(11) _cell_length_c 9.4547(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1304.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 1732 _cell_measurement_theta_min 2.85 _cell_measurement_theta_max 26.09 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 2.400 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 915 _exptl_absorpt_coefficient_mu 4.696 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.551492 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(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 7141 _diffrn_reflns_av_R_equivalents 0.0590 _diffrn_reflns_av_sigmaI/netI 0.0319 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 26.30 _reflns_number_total 894 _reflns_number_gt 661 _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 ? _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0290P)^2^+3.1261P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0020(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 894 _refine_ls_number_parameters 90 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0488 _refine_ls_R_factor_gt 0.0303 _refine_ls_wR_factor_ref 0.0755 _refine_ls_wR_factor_gt 0.0688 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.099 _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 0.6667 0.3333 0.2500 0.0155(2) Uani 1 6 d S . . Cu1 Cu 0.3333 -0.3333 0.2500 0.0214(3) Uani 1 6 d S . . O1 O 0.7296(3) 0.2328(3) 0.0771(4) 0.0256(8) Uani 1 1 d . . . O2 O 0.7209(3) 0.0671(3) -0.0227(4) 0.0329(9) Uani 1 1 d . . . N1 N 0.5508(2) 0.1017(5) 0.2500 0.0153(12) Uani 1 2 d S . . N2 N 0.4245(2) -0.1510(5) 0.2500 0.0200(13) Uani 1 2 d S . . C1 C 0.6869(4) 0.1192(4) 0.0630(5) 0.0211(11) Uani 1 1 d . . . C2 C 0.5812(4) 0.0399(4) 0.1613(5) 0.0170(10) Uani 1 1 d . . . C3 C 0.5184(4) -0.0874(4) 0.1608(5) 0.0186(10) Uani 1 1 d . . . H3 H 0.5416 -0.1289 0.0981 0.025(14) Uiso 1 1 calc R . . Gd2 Gd 1.0000 0.0000 0.2500 0.0194(3) Uani 0.50 6 d SP . . O3 O 0.7601(6) -0.1199(3) 0.2500 0.062(2) Uani 1 2 d S A 1 O4 O 0.9256(10) 0.0850(10) 0.0745(11) 0.054(3) Uani 0.50 1 d P A 1 O5 O 1.0669(16) -0.0902(14) 0.036(2) 0.078(6) Uani 0.33 1 d P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.0155(2) 0.0155(2) 0.0156(3) 0.000 0.000 0.00774(12) Cu1 0.0164(4) 0.0164(4) 0.0314(8) 0.000 0.000 0.0082(2) O1 0.0256(19) 0.0195(19) 0.026(2) 0.0015(15) 0.0126(16) 0.0069(16) O2 0.036(2) 0.031(2) 0.030(2) -0.0035(17) 0.0143(17) 0.0158(18) N1 0.019(2) 0.014(3) 0.012(3) 0.000 -0.0015(19) 0.0068(13) N2 0.021(2) 0.014(3) 0.022(3) 0.000 -0.001(2) 0.0071(14) C1 0.022(3) 0.026(3) 0.015(2) 0.000(2) 0.000(2) 0.012(2) C2 0.018(2) 0.019(2) 0.014(2) 0.002(2) 0.0011(19) 0.009(2) C3 0.021(3) 0.019(2) 0.019(3) 0.000(2) 0.001(2) 0.012(2) Gd2 0.0179(4) 0.0179(4) 0.0224(7) 0.000 0.000 0.0089(2) O3 0.047(4) 0.078(4) 0.052(4) -0.010(3) 0.000 0.024(2) O4 0.056(7) 0.060(7) 0.039(6) 0.006(5) -0.004(5) 0.024(5) O5 0.066(12) 0.039(9) 0.141(19) -0.001(11) 0.031(13) 0.037(9) _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 2.433(3) . ? Gd1 O1 2.433(3) 4_665 ? Gd1 O1 2.433(3) 3_665 ? Gd1 O1 2.433(3) 2_655 ? Gd1 O1 2.433(3) 6 ? Gd1 O1 2.433(3) 5_655 ? Gd1 N1 2.532(5) . ? Gd1 N1 2.532(5) 2_655 ? Gd1 N1 2.532(5) 3_665 ? Cu1 N2 1.993(5) . ? Cu1 N2 1.993(5) 2_545 ? Cu1 N2 1.993(5) 3_655 ? O1 C1 1.262(6) . ? O2 C1 1.247(6) . ? N1 C2 1.326(5) . ? N1 C2 1.326(5) 5_655 ? N2 C3 1.345(5) . ? N2 C3 1.345(5) 5_655 ? C1 C2 1.520(6) . ? C2 C3 1.391(6) . ? C3 H3 0.9300 . ? Gd2 O4 2.407(10) 2_645 ? Gd2 O4 2.407(10) 5_755 ? Gd2 O4 2.407(10) 3_765 ? Gd2 O4 2.407(10) . ? Gd2 O4 2.407(10) 6_545 ? Gd2 O4 2.407(10) 4_665 ? Gd2 O3 2.622(6) 3_765 ? Gd2 O3 2.622(6) . ? Gd2 O3 2.622(6) 2_645 ? Gd2 O5 2.659(18) 3_765 ? Gd2 O5 2.659(18) 6_545 ? Gd2 O5 2.659(18) . ? 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 85.52(17) . 4_665 ? O1 Gd1 O1 79.79(13) . 3_665 ? O1 Gd1 O1 147.17(16) 4_665 3_665 ? O1 Gd1 O1 79.79(13) . 2_655 ? O1 Gd1 O1 126.31(15) 4_665 2_655 ? O1 Gd1 O1 79.79(13) 3_665 2_655 ? O1 Gd1 O1 147.17(16) . 6 ? O1 Gd1 O1 79.79(13) 4_665 6 ? O1 Gd1 O1 126.31(15) 3_665 6 ? O1 Gd1 O1 85.52(17) 2_655 6 ? O1 Gd1 O1 126.31(15) . 5_655 ? O1 Gd1 O1 79.79(13) 4_665 5_655 ? O1 Gd1 O1 85.52(17) 3_665 5_655 ? O1 Gd1 O1 147.17(16) 2_655 5_655 ? O1 Gd1 O1 79.79(13) 6 5_655 ? O1 Gd1 N1 63.16(8) . . ? O1 Gd1 N1 73.58(8) 4_665 . ? O1 Gd1 N1 73.58(8) 3_665 . ? O1 Gd1 N1 137.24(9) 2_655 . ? O1 Gd1 N1 137.24(9) 6 . ? O1 Gd1 N1 63.16(8) 5_655 . ? O1 Gd1 N1 73.58(8) . 2_655 ? O1 Gd1 N1 63.16(8) 4_665 2_655 ? O1 Gd1 N1 137.24(9) 3_665 2_655 ? O1 Gd1 N1 63.16(8) 2_655 2_655 ? O1 Gd1 N1 73.58(8) 6 2_655 ? O1 Gd1 N1 137.24(9) 5_655 2_655 ? N1 Gd1 N1 120.0 . 2_655 ? O1 Gd1 N1 137.24(9) . 3_665 ? O1 Gd1 N1 137.24(9) 4_665 3_665 ? O1 Gd1 N1 63.16(8) 3_665 3_665 ? O1 Gd1 N1 73.58(8) 2_655 3_665 ? O1 Gd1 N1 63.16(8) 6 3_665 ? O1 Gd1 N1 73.58(8) 5_655 3_665 ? N1 Gd1 N1 120.0 . 3_665 ? N1 Gd1 N1 120.0 2_655 3_665 ? N2 Cu1 N2 120.0 . 2_545 ? N2 Cu1 N2 120.0 . 3_655 ? N2 Cu1 N2 120.0 2_545 3_655 ? C1 O1 Gd1 126.8(3) . . ? C2 N1 C2 118.8(6) . 5_655 ? C2 N1 Gd1 120.6(3) . . ? C2 N1 Gd1 120.6(3) 5_655 . ? C3 N2 C3 117.7(6) . 5_655 ? C3 N2 Cu1 121.1(3) . . ? C3 N2 Cu1 121.1(3) 5_655 . ? O2 C1 O1 127.1(4) . . ? O2 C1 C2 118.1(4) . . ? O1 C1 C2 114.8(4) . . ? N1 C2 C3 121.1(4) . . ? N1 C2 C1 114.6(4) . . ? C3 C2 C1 124.4(4) . . ? N2 C3 C2 120.7(4) . . ? N2 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? O4 Gd2 O4 140.5(5) 2_645 5_755 ? O4 Gd2 O4 77.7(4) 2_645 3_765 ? O4 Gd2 O4 87.3(5) 5_755 3_765 ? O4 Gd2 O4 77.7(4) 2_645 . ? O4 Gd2 O4 134.6(5) 5_755 . ? O4 Gd2 O4 77.7(4) 3_765 . ? O4 Gd2 O4 87.3(5) 2_645 6_545 ? O4 Gd2 O4 77.7(4) 5_755 6_545 ? O4 Gd2 O4 134.6(5) 3_765 6_545 ? O4 Gd2 O4 140.5(5) . 6_545 ? O4 Gd2 O4 134.6(5) 2_645 4_665 ? O4 Gd2 O4 77.7(4) 5_755 4_665 ? O4 Gd2 O4 140.5(5) 3_765 4_665 ? O4 Gd2 O4 87.3(5) . 4_665 ? O4 Gd2 O4 77.7(4) 6_545 4_665 ? O4 Gd2 O3 136.4(3) 2_645 3_765 ? O4 Gd2 O3 67.3(3) 5_755 3_765 ? O4 Gd2 O3 70.3(3) 3_765 3_765 ? O4 Gd2 O3 67.3(3) . 3_765 ? O4 Gd2 O3 136.4(3) 6_545 3_765 ? O4 Gd2 O3 70.3(3) 4_665 3_765 ? O4 Gd2 O3 67.3(3) 2_645 . ? O4 Gd2 O3 136.4(3) 5_755 . ? O4 Gd2 O3 136.4(3) 3_765 . ? O4 Gd2 O3 70.3(3) . . ? O4 Gd2 O3 70.3(3) 6_545 . ? O4 Gd2 O3 67.3(3) 4_665 . ? O3 Gd2 O3 120.0 3_765 . ? O4 Gd2 O3 70.3(3) 2_645 2_645 ? O4 Gd2 O3 70.3(3) 5_755 2_645 ? O4 Gd2 O3 67.3(3) 3_765 2_645 ? O4 Gd2 O3 136.4(3) . 2_645 ? O4 Gd2 O3 67.3(3) 6_545 2_645 ? O4 Gd2 O3 136.4(3) 4_665 2_645 ? O3 Gd2 O3 120.0 3_765 2_645 ? O3 Gd2 O3 120.0 . 2_645 ? O4 Gd2 O5 42.2(5) 2_645 3_765 ? O4 Gd2 O5 172.3(5) 5_755 3_765 ? O4 Gd2 O5 86.8(4) 3_765 3_765 ? O4 Gd2 O5 38.9(5) . 3_765 ? O4 Gd2 O5 110.0(4) 6_545 3_765 ? O4 Gd2 O5 104.0(4) 4_665 3_765 ? O3 Gd2 O5 106.0(4) 3_765 3_765 ? O3 Gd2 O5 49.8(4) . 3_765 ? O3 Gd2 O5 111.8(4) 2_645 3_765 ? O4 Gd2 O5 172.3(5) 2_645 6_545 ? O4 Gd2 O5 42.2(5) 5_755 6_545 ? O4 Gd2 O5 110.0(4) 3_765 6_545 ? O4 Gd2 O5 104.0(4) . 6_545 ? O4 Gd2 O5 86.8(4) 6_545 6_545 ? O4 Gd2 O5 38.9(5) 4_665 6_545 ? O3 Gd2 O5 49.8(4) 3_765 6_545 ? O3 Gd2 O5 106.0(4) . 6_545 ? O3 Gd2 O5 111.8(4) 2_645 6_545 ? O5 Gd2 O5 136.5(7) 3_765 6_545 ? O4 Gd2 O5 38.9(5) 2_645 . ? O4 Gd2 O5 110.0(4) 5_755 . ? O4 Gd2 O5 42.2(5) 3_765 . ? O4 Gd2 O5 86.8(4) . . ? O4 Gd2 O5 104.0(4) 6_545 . ? O4 Gd2 O5 172.3(5) 4_665 . ? O3 Gd2 O5 111.8(4) 3_765 . ? O3 Gd2 O5 106.0(4) . . ? O3 Gd2 O5 49.8(4) 2_645 . ? O5 Gd2 O5 68.3(7) 3_765 . ? O5 Gd2 O5 148.1(8) 6_545 . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.30 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.730 _refine_diff_density_min -0.671 _refine_diff_density_rms 0.117