# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Xintao Wu' _publ_contact_author_address ; Fuzhou 350002 ; _publ_contact_author_email wxt@fjirsm.ac.cn loop_ _publ_author_name 'Ning Yuan' 'Xintao Wu' # Attachment '- Complex 1.CIF' data_a _database_code_depnum_ccdc_archive 'CCDC 801417' #TrackingRef '- Complex 1.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H49 Gd9 N12 O44' _chemical_formula_weight 3201.48 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' 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 R-3c 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+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' '-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+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' _cell_length_a 17.0151(3) _cell_length_b 17.0151(3) _cell_length_c 56.2326(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 14099.0(6) _cell_formula_units_Z 6 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 12486 _cell_measurement_theta_min 3.1215 _cell_measurement_theta_max 27.4797 _exptl_crystal_description Prism _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.2000 _exptl_crystal_size_mid 0.2000 _exptl_crystal_size_min 0.2000 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.262 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8958 _exptl_absorpt_coefficient_mu 6.350 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7891 _exptl_absorpt_correction_T_max 1.0000 _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 Mercury70 _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 14.6306 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34641 _diffrn_reflns_av_R_equivalents 0.0254 _diffrn_reflns_av_sigmaI/netI 0.0131 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -72 _diffrn_reflns_limit_l_max 72 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3601 _reflns_number_gt 3551 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _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^)+(0.0472P)^2^+668.8796P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment geom _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3601 _refine_ls_number_parameters 201 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0330 _refine_ls_R_factor_gt 0.0325 _refine_ls_wR_factor_ref 0.0938 _refine_ls_wR_factor_gt 0.0934 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd1 Gd 0.861589(17) 0.879694(17) 0.034394(4) 0.01125(9) Uani 1 1 d . . . Gd2 Gd 0.6667 0.80722(2) 0.0833 0.01426(11) Uani 1 2 d S . . C1 C 0.6396(4) 0.8210(4) 0.03041(10) 0.0182(11) Uani 1 1 d . . . C2 C 0.6375(4) 0.8464(5) 0.00671(12) 0.0241(13) Uani 1 1 d . . . C3 C 0.5554(5) 0.8344(7) -0.00169(15) 0.045(2) Uani 1 1 d . . . H3A H 0.5511 0.8494 -0.0173 0.054 Uiso 1 1 calc R . . C4 C 0.4803(5) 0.8006(8) 0.01283(16) 0.052(3) Uani 1 1 d . . . H4A H 0.4241 0.7881 0.0069 0.062 Uiso 1 1 calc R . . C5 C 0.4910(5) 0.7858(6) 0.03645(15) 0.0401(19) Uani 1 1 d . . . H5A H 0.4421 0.7681 0.0467 0.048 Uiso 1 1 calc R . . C6 C 0.7207(4) 0.8918(4) -0.00834(10) 0.0192(11) Uani 1 1 d . . . C7 C 0.8237(4) 0.7738(4) 0.08497(11) 0.0190(11) Uani 1 1 d . . . C8 C 0.8937(4) 0.7523(5) 0.08352(12) 0.0247(13) Uani 1 1 d . . . C9 C 0.8855(6) 0.6821(6) 0.09778(18) 0.047(2) Uani 1 1 d . . . H9A H 0.9312 0.6673 0.0978 0.056 Uiso 1 1 calc R . . C10 C 0.8095(8) 0.6338(8) 0.1121(2) 0.077(4) Uani 1 1 d . . . H10A H 0.8037 0.5867 0.1217 0.093 Uiso 1 1 calc R . . C11 C 0.7430(7) 0.6572(7) 0.1117(2) 0.061(3) Uani 1 1 d . . . H11A H 0.6912 0.6238 0.1209 0.073 Uiso 1 1 calc R . . C12 C 0.9758(4) 0.8029(4) 0.06846(10) 0.0166(11) Uani 1 1 d . . . O1 O 0.7990(3) 0.9124(3) 0.00004(7) 0.0196(8) Uani 1 1 d . . . O2 O 0.7153(3) 0.9151(4) -0.02912(8) 0.0274(10) Uani 1 1 d . . . O3 O 0.7078(3) 0.8196(3) 0.04010(7) 0.0198(9) Uani 1 1 d . . . O4 O 0.9793(3) 0.8600(3) 0.05281(7) 0.0172(8) Uani 1 1 d . . . O5 O 1.0382(3) 0.7868(3) 0.07169(9) 0.0243(9) Uani 1 1 d . . . O6 O 0.8226(3) 0.8397(3) 0.07368(7) 0.0180(8) Uani 1 1 d . . . O7 O 1.0000 1.0000 0.02244(11) 0.0111(12) Uani 1 3 d S . . H7 H 1.0000 1.0000 0.0000 0.013 Uiso 1 6 d S . . O8 O 0.9511(8) 0.5557(8) 0.1418(2) 0.100 Uiso 1 1 d . . . N1 N 0.5678(4) 0.7956(4) 0.04519(9) 0.0267(12) Uani 1 1 d . . . N2 N 0.7493(4) 0.7255(5) 0.09871(11) 0.0335(14) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.01126(14) 0.01250(14) 0.00942(14) 0.00067(9) 0.00103(8) 0.00552(10) Gd2 0.01149(18) 0.01655(16) 0.01305(18) 0.00168(6) 0.00336(13) 0.00575(9) C1 0.010(2) 0.020(3) 0.018(3) -0.001(2) 0.001(2) 0.003(2) C2 0.014(3) 0.029(3) 0.024(3) 0.007(2) -0.002(2) 0.007(3) C3 0.022(4) 0.073(6) 0.034(4) 0.023(4) -0.001(3) 0.019(4) C4 0.019(4) 0.089(7) 0.043(5) 0.019(5) 0.000(3) 0.024(4) C5 0.020(3) 0.063(6) 0.037(4) 0.014(4) 0.009(3) 0.021(4) C6 0.017(3) 0.019(3) 0.017(3) 0.005(2) 0.002(2) 0.006(2) C7 0.018(3) 0.021(3) 0.020(3) 0.004(2) 0.004(2) 0.010(2) C8 0.020(3) 0.028(3) 0.027(3) 0.011(3) 0.004(2) 0.013(3) C9 0.043(5) 0.047(5) 0.068(6) 0.037(4) 0.028(4) 0.036(4) C10 0.069(7) 0.080(8) 0.110(9) 0.082(7) 0.060(7) 0.058(6) C11 0.051(5) 0.069(7) 0.081(7) 0.058(6) 0.047(5) 0.043(5) C12 0.017(3) 0.017(3) 0.017(3) 0.002(2) -0.001(2) 0.009(2) O1 0.0138(19) 0.026(2) 0.0175(19) 0.0057(17) 0.0005(15) 0.0091(17) O2 0.018(2) 0.039(3) 0.020(2) 0.0100(19) 0.0000(17) 0.011(2) O3 0.0119(19) 0.028(2) 0.0142(18) 0.0050(16) 0.0003(15) 0.0063(18) O4 0.016(2) 0.019(2) 0.018(2) 0.0073(15) 0.0023(15) 0.0093(16) O5 0.015(2) 0.027(2) 0.032(2) 0.0077(19) -0.0004(18) 0.0110(18) O6 0.021(2) 0.024(2) 0.0140(18) 0.0042(16) 0.0033(16) 0.0150(18) O7 0.0100(18) 0.0100(18) 0.013(3) 0.000 0.000 0.0050(9) N1 0.017(3) 0.036(3) 0.023(3) 0.005(2) 0.006(2) 0.010(2) N2 0.029(3) 0.039(3) 0.037(3) 0.022(3) 0.018(3) 0.021(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 O3 2.306(4) . ? Gd1 O6 2.309(4) . ? Gd1 O7 2.3168(18) . ? Gd1 O1 2.402(4) . ? Gd1 O4 2.423(4) . ? Gd1 O2 2.466(5) 21_655 ? Gd1 O4 2.481(4) 3_675 ? Gd1 O1 2.530(4) 21_655 ? Gd1 C6 2.875(6) 21_655 ? Gd1 Gd1 3.8402(4) 2_765 ? Gd1 Gd1 3.8402(4) 3_675 ? Gd1 Gd2 4.0005(3) . ? Gd2 O5 2.371(4) 3_675 ? Gd2 O5 2.371(4) 17_564 ? Gd2 O6 2.485(4) . ? Gd2 O6 2.485(4) 18_654 ? Gd2 O3 2.510(4) . ? Gd2 O3 2.509(4) 18_654 ? Gd2 N2 2.572(6) 18_654 ? Gd2 N2 2.572(6) . ? Gd2 N1 2.671(6) . ? Gd2 N1 2.671(6) 18_654 ? Gd2 C7 2.998(6) . ? Gd2 C7 2.998(6) 18_654 ? C1 O3 1.293(7) . ? C1 N1 1.357(7) . ? C1 C2 1.407(8) . ? C2 C3 1.390(9) . ? C2 C6 1.491(8) . ? C3 C4 1.377(11) . ? C3 H3A 0.9300 . ? C4 C5 1.381(12) . ? C4 H4A 0.9300 . ? C5 N1 1.327(9) . ? C5 H5A 0.9300 . ? C6 O2 1.252(7) . ? C6 O1 1.285(7) . ? C6 Gd1 2.875(6) 20_565 ? C7 O6 1.296(7) . ? C7 N2 1.354(8) . ? C7 C8 1.413(9) . ? C8 C9 1.386(9) . ? C8 C12 1.485(8) . ? C9 C10 1.390(12) . ? C9 H9A 0.9300 . ? C10 C11 1.376(13) . ? C10 H10A 0.9300 . ? C11 N2 1.329(10) . ? C11 H11A 0.9300 . ? C12 O5 1.236(7) . ? C12 O4 1.290(7) . ? O1 Gd1 2.530(4) 20_565 ? O2 Gd1 2.466(5) 20_565 ? O4 Gd1 2.481(4) 2_765 ? O5 Gd2 2.371(4) 2_765 ? O7 Gd1 2.3168(18) 2_765 ? O7 Gd1 2.3168(18) 3_675 ? O7 H7 1.262(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Gd1 O6 68.98(15) . . ? O3 Gd1 O7 149.17(12) . . ? O6 Gd1 O7 123.60(18) . . ? O3 Gd1 O1 71.24(14) . . ? O6 Gd1 O1 137.95(14) . . ? O7 Gd1 O1 86.25(16) . . ? O3 Gd1 O4 135.44(14) . . ? O6 Gd1 O4 71.68(14) . . ? O7 Gd1 O4 72.58(13) . . ? O1 Gd1 O4 150.34(14) . . ? O3 Gd1 O2 76.77(17) . 21_655 ? O6 Gd1 O2 83.35(15) . 21_655 ? O7 Gd1 O2 129.34(13) . 21_655 ? O1 Gd1 O2 100.42(16) . 21_655 ? O4 Gd1 O2 78.75(16) . 21_655 ? O3 Gd1 O4 86.65(15) . 3_675 ? O6 Gd1 O4 76.42(14) . 3_675 ? O7 Gd1 O4 71.51(12) . 3_675 ? O1 Gd1 O4 88.32(15) . 3_675 ? O4 Gd1 O4 103.7(2) . 3_675 ? O2 Gd1 O4 157.45(14) 21_655 3_675 ? O3 Gd1 O1 109.11(15) . 21_655 ? O6 Gd1 O1 132.34(14) . 21_655 ? O7 Gd1 O1 83.39(15) . 21_655 ? O1 Gd1 O1 74.01(6) . 21_655 ? O4 Gd1 O1 82.93(14) . 21_655 ? O2 Gd1 O1 51.90(14) 21_655 21_655 ? O4 Gd1 O1 150.25(13) 3_675 21_655 ? O3 Gd1 C6 90.63(17) . 21_655 ? O6 Gd1 C6 108.54(16) . 21_655 ? O7 Gd1 C6 108.44(16) . 21_655 ? O1 Gd1 C6 84.75(16) . 21_655 ? O4 Gd1 C6 82.65(16) . 21_655 ? O2 Gd1 C6 25.66(16) 21_655 21_655 ? O4 Gd1 C6 173.06(16) 3_675 21_655 ? O1 Gd1 C6 26.53(15) 21_655 21_655 ? O3 Gd1 Gd1 172.00(10) . 2_765 ? O6 Gd1 Gd1 103.23(11) . 2_765 ? O7 Gd1 Gd1 34.03(7) . 2_765 ? O1 Gd1 Gd1 115.83(10) . 2_765 ? O4 Gd1 Gd1 38.99(9) . 2_765 ? O2 Gd1 Gd1 104.64(12) 21_655 2_765 ? O4 Gd1 Gd1 89.76(9) 3_675 2_765 ? O1 Gd1 Gd1 77.29(10) 21_655 2_765 ? C6 Gd1 Gd1 93.71(13) 21_655 2_765 ? O3 Gd1 Gd1 119.40(12) . 3_675 ? O6 Gd1 Gd1 105.69(11) . 3_675 ? O7 Gd1 Gd1 34.03(7) . 3_675 ? O1 Gd1 Gd1 82.42(11) . 3_675 ? O4 Gd1 Gd1 90.63(10) . 3_675 ? O2 Gd1 Gd1 163.30(12) 21_655 3_675 ? O4 Gd1 Gd1 37.91(9) 3_675 3_675 ? O1 Gd1 Gd1 114.44(9) 21_655 3_675 ? C6 Gd1 Gd1 140.84(12) 21_655 3_675 ? Gd1 Gd1 Gd1 60.0 2_765 3_675 ? O3 Gd1 Gd2 35.49(10) . . ? O6 Gd1 Gd2 34.85(10) . . ? O7 Gd1 Gd2 142.35(12) . . ? O1 Gd1 Gd2 103.26(10) . . ? O4 Gd1 Gd2 106.18(10) . . ? O2 Gd1 Gd2 85.28(11) 21_655 . ? O4 Gd1 Gd2 72.45(9) 3_675 . ? O1 Gd1 Gd2 134.25(9) 21_655 . ? C6 Gd1 Gd2 108.66(12) 21_655 . ? Gd1 Gd1 Gd2 136.514(4) 2_765 . ? Gd1 Gd1 Gd2 110.255(9) 3_675 . ? O5 Gd2 O5 70.7(2) 3_675 17_564 ? O5 Gd2 O6 73.94(15) 3_675 . ? O5 Gd2 O6 141.73(15) 17_564 . ? O5 Gd2 O6 141.73(15) 3_675 18_654 ? O5 Gd2 O6 73.94(15) 17_564 18_654 ? O6 Gd2 O6 143.7(2) . 18_654 ? O5 Gd2 O3 69.81(15) 3_675 . ? O5 Gd2 O3 115.82(15) 17_564 . ? O6 Gd2 O3 63.11(13) . . ? O6 Gd2 O3 114.69(14) 18_654 . ? O5 Gd2 O3 115.82(15) 3_675 18_654 ? O5 Gd2 O3 69.82(15) 17_564 18_654 ? O6 Gd2 O3 114.69(13) . 18_654 ? O6 Gd2 O3 63.11(13) 18_654 18_654 ? O3 Gd2 O3 173.6(2) . 18_654 ? O5 Gd2 N2 144.28(18) 3_675 18_654 ? O5 Gd2 N2 121.03(18) 17_564 18_654 ? O6 Gd2 N2 96.36(17) . 18_654 ? O6 Gd2 N2 51.81(16) 18_654 18_654 ? O3 Gd2 N2 75.14(17) . 18_654 ? O3 Gd2 N2 99.57(17) 18_654 18_654 ? O5 Gd2 N2 121.03(18) 3_675 . ? O5 Gd2 N2 144.29(18) 17_564 . ? O6 Gd2 N2 51.81(16) . . ? O6 Gd2 N2 96.36(17) 18_654 . ? O3 Gd2 N2 99.56(17) . . ? O3 Gd2 N2 75.14(17) 18_654 . ? N2 Gd2 N2 71.0(3) 18_654 . ? O5 Gd2 N1 81.94(18) 3_675 . ? O5 Gd2 N1 75.40(17) 17_564 . ? O6 Gd2 N1 113.82(15) . . ? O6 Gd2 N1 75.29(15) 18_654 . ? O3 Gd2 N1 50.74(15) . . ? O3 Gd2 N1 131.26(15) 18_654 . ? N2 Gd2 N1 70.6(2) 18_654 . ? N2 Gd2 N1 136.4(2) . . ? O5 Gd2 N1 75.40(17) 3_675 18_654 ? O5 Gd2 N1 81.94(18) 17_564 18_654 ? O6 Gd2 N1 75.29(15) . 18_654 ? O6 Gd2 N1 113.82(15) 18_654 18_654 ? O3 Gd2 N1 131.26(15) . 18_654 ? O3 Gd2 N1 50.74(15) 18_654 18_654 ? N2 Gd2 N1 136.4(2) 18_654 18_654 ? N2 Gd2 N1 70.6(2) . 18_654 ? N1 Gd2 N1 152.2(3) . 18_654 ? O5 Gd2 C7 97.68(16) 3_675 . ? O5 Gd2 C7 154.45(17) 17_564 . ? O6 Gd2 C7 25.18(15) . . ? O6 Gd2 C7 120.59(15) 18_654 . ? O3 Gd2 C7 78.93(15) . . ? O3 Gd2 C7 96.98(15) 18_654 . ? N2 Gd2 C7 81.88(19) 18_654 . ? N2 Gd2 C7 26.76(17) . . ? N1 Gd2 C7 126.75(17) . . ? N1 Gd2 C7 72.98(17) 18_654 . ? O5 Gd2 C7 154.44(17) 3_675 18_654 ? O5 Gd2 C7 97.68(16) 17_564 18_654 ? O6 Gd2 C7 120.59(15) . 18_654 ? O6 Gd2 C7 25.18(15) 18_654 18_654 ? O3 Gd2 C7 96.97(15) . 18_654 ? O3 Gd2 C7 78.94(15) 18_654 18_654 ? N2 Gd2 C7 26.76(17) 18_654 18_654 ? N2 Gd2 C7 81.88(19) . 18_654 ? N1 Gd2 C7 72.98(17) . 18_654 ? N1 Gd2 C7 126.75(17) 18_654 18_654 ? C7 Gd2 C7 101.1(2) . 18_654 ? O3 C1 N1 114.1(5) . . ? O3 C1 C2 124.4(5) . . ? N1 C1 C2 121.4(6) . . ? O3 C1 Gd2 54.1(3) . . ? N1 C1 Gd2 61.5(3) . . ? C2 C1 Gd2 168.4(5) . . ? C3 C2 C1 117.0(6) . . ? C3 C2 C6 120.5(6) . . ? C1 C2 C6 122.2(5) . . ? C4 C3 C2 121.0(7) . . ? C4 C3 H3A 119.5 . . ? C2 C3 H3A 119.5 . . ? C3 C4 C5 117.8(7) . . ? C3 C4 H4A 121.1 . . ? C5 C4 H4A 121.1 . . ? N1 C5 C4 123.0(7) . . ? N1 C5 H5A 118.5 . . ? C4 C5 H5A 118.5 . . ? O2 C6 O1 119.1(5) . . ? O2 C6 C2 119.5(6) . . ? O1 C6 C2 121.3(5) . . ? O2 C6 Gd1 58.6(3) . 20_565 ? O1 C6 Gd1 61.6(3) . 20_565 ? C2 C6 Gd1 166.2(5) . 20_565 ? O6 C7 N2 113.1(5) . . ? O6 C7 C8 125.0(6) . . ? N2 C7 C8 121.9(6) . . ? O6 C7 Gd2 54.7(3) . . ? N2 C7 Gd2 58.8(3) . . ? C8 C7 Gd2 173.8(5) . . ? C9 C8 C7 117.1(6) . . ? C9 C8 C12 119.3(6) . . ? C7 C8 C12 123.6(6) . . ? C8 C9 C10 120.4(7) . . ? C8 C9 H9A 119.8 . . ? C10 C9 H9A 119.8 . . ? C11 C10 C9 118.5(8) . . ? C11 C10 H10A 120.8 . . ? C9 C10 H10A 120.8 . . ? N2 C11 C10 122.9(7) . . ? N2 C11 H11A 118.6 . . ? C10 C11 H11A 118.6 . . ? O5 C12 O4 123.1(5) . . ? O5 C12 C8 116.8(5) . . ? O4 C12 C8 120.1(5) . . ? C6 O1 Gd1 138.7(4) . . ? C6 O1 Gd1 91.9(3) . 20_565 ? Gd1 O1 Gd1 129.38(17) . 20_565 ? C6 O2 Gd1 95.8(4) . 20_565 ? C1 O3 Gd1 139.7(4) . . ? C1 O3 Gd2 101.2(3) . . ? Gd1 O3 Gd2 112.27(16) . . ? C12 O4 Gd1 131.7(4) . . ? C12 O4 Gd1 125.2(4) . 2_765 ? Gd1 O4 Gd1 103.10(15) . 2_765 ? C12 O5 Gd2 141.0(4) . 2_765 ? C7 O6 Gd1 126.7(4) . . ? C7 O6 Gd2 100.1(3) . . ? Gd1 O6 Gd2 113.08(16) . . ? Gd1 O7 Gd1 111.95(13) 2_765 . ? Gd1 O7 Gd1 111.95(13) 2_765 3_675 ? Gd1 O7 Gd1 111.95(13) . 3_675 ? Gd1 O7 H7 106.87(15) 2_765 . ? Gd1 O7 H7 106.87(15) . . ? Gd1 O7 H7 106.87(15) 3_675 . ? C5 N1 C1 119.1(6) . . ? C5 N1 Gd2 148.3(5) . . ? C1 N1 Gd2 92.0(4) . . ? C11 N2 C7 119.1(6) . . ? C11 N2 Gd2 146.0(5) . . ? C7 N2 Gd2 94.4(4) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.793 _refine_diff_density_min -6.033 _refine_diff_density_rms 0.215 # Attachment '- Complex 2.CIF' data_a2 _database_code_depnum_ccdc_archive 'CCDC 801418' #TrackingRef '- Complex 2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H49 Eu9 N12 O44' _chemical_formula_weight 3153.87 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' 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 R-3c 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+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' '-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+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' _cell_length_a 17.0615(4) _cell_length_b 17.0615(4) _cell_length_c 56.505(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 14244.7(10) _cell_formula_units_Z 6 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 11604 _cell_measurement_theta_min 3.1115 _cell_measurement_theta_max 27.4797 _exptl_crystal_description Prism _exptl_crystal_colour White _exptl_crystal_size_max 0.2000 _exptl_crystal_size_mid 0.2000 _exptl_crystal_size_min 0.1500 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.206 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8904 _exptl_absorpt_coefficient_mu 5.944 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8591 _exptl_absorpt_correction_T_max 1.0000 _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 Mercury70 _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 14.6306 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35328 _diffrn_reflns_av_R_equivalents 0.0363 _diffrn_reflns_av_sigmaI/netI 0.0197 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -63 _diffrn_reflns_limit_l_max 70 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3617 _reflns_number_gt 3503 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _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^)+(0.0740P)^2^+656.2661P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment geom _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3617 _refine_ls_number_parameters 201 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0446 _refine_ls_R_factor_gt 0.0432 _refine_ls_wR_factor_ref 0.1237 _refine_ls_wR_factor_gt 0.1224 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _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 Eu1 Eu 0.21277(2) 0.52782(2) 0.132281(5) 0.01340(12) Uani 1 1 d . . . Eu2 Eu 0.14042(3) 0.3333 0.0833 0.01649(14) Uani 1 2 d S . . C1 C 0.1535(5) 0.3060(4) 0.13621(12) 0.0213(14) Uani 1 1 d . . . C2 C 0.1805(5) 0.3047(5) 0.15986(14) 0.0268(16) Uani 1 1 d . . . C3 C 0.1667(8) 0.2214(6) 0.16830(18) 0.048(3) Uani 1 1 d . . . H3A H 0.1787 0.2162 0.1841 0.057 Uiso 1 1 calc R . . C4 C 0.1358(9) 0.1473(6) 0.1538(2) 0.058(3) Uani 1 1 d . . . H4A H 0.1257 0.0920 0.1596 0.070 Uiso 1 1 calc R . . C5 C 0.1201(7) 0.1574(6) 0.13024(18) 0.041(2) Uani 1 1 d . . . H5A H 0.1033 0.1088 0.1200 0.049 Uiso 1 1 calc R . . C6 C 0.2246(5) 0.3861(5) 0.17485(13) 0.0200(13) Uani 1 1 d . . . C7 C 0.1068(5) 0.4904(5) 0.08179(13) 0.0211(14) Uani 1 1 d . . . C8 C 0.0852(5) 0.5605(5) 0.08302(14) 0.0256(15) Uani 1 1 d . . . C9 C 0.0186(7) 0.5541(7) 0.0686(2) 0.053(3) Uani 1 1 d . . . H9A H 0.0070 0.6018 0.0677 0.064 Uiso 1 1 calc R . . C10 C -0.0339(10) 0.4747(10) 0.0547(3) 0.086(6) Uani 1 1 d . . . H10A H -0.0837 0.4670 0.0460 0.103 Uiso 1 1 calc R . . C11 C -0.0087(9) 0.4112(8) 0.0546(2) 0.070(4) Uani 1 1 d . . . H11A H -0.0396 0.3614 0.0447 0.084 Uiso 1 1 calc R . . C12 C 0.1362(5) 0.6423(4) 0.09824(12) 0.0175(12) Uani 1 1 d . . . O1 O 0.2451(3) 0.4647(3) 0.16646(9) 0.0211(10) Uani 1 1 d . . . O2 O 0.2477(4) 0.3809(4) 0.19551(10) 0.0301(12) Uani 1 1 d . . . O3 O 0.1524(3) 0.3735(3) 0.12650(9) 0.0223(10) Uani 1 1 d . . . O4 O 0.1933(3) 0.6456(3) 0.11370(9) 0.0199(10) Uani 1 1 d . . . O5 O 0.1202(4) 0.7046(3) 0.09503(11) 0.0283(12) Uani 1 1 d . . . O6 O 0.1719(3) 0.4884(3) 0.09301(9) 0.0202(10) Uani 1 1 d . . . O7 O 0.3333 0.6667 0.14428(13) 0.0136(14) Uani 1 3 d S . . H7 H 0.3333 0.6667 0.1667 0.016 Uiso 1 6 d S . . O8 O -0.0714(9) 0.5476(9) -0.0002(2) 0.100 Uiso 1 1 d . . . N1 N 0.1281(5) 0.2349(4) 0.12136(11) 0.0285(14) Uani 1 1 d . . . N2 N 0.0583(5) 0.4163(5) 0.06790(13) 0.0346(17) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Eu1 0.01460(18) 0.01330(17) 0.0117(2) -0.00115(10) -0.00068(10) 0.00652(13) Eu2 0.01896(19) 0.0135(2) 0.0152(3) -0.00356(16) -0.00178(8) 0.00673(11) C1 0.026(3) 0.013(3) 0.019(3) 0.001(2) 0.001(3) 0.006(3) C2 0.033(4) 0.015(3) 0.028(4) 0.002(3) -0.005(3) 0.009(3) C3 0.081(7) 0.023(4) 0.035(5) 0.002(4) -0.024(5) 0.023(5) C4 0.100(9) 0.023(4) 0.054(7) -0.001(4) -0.024(6) 0.032(5) C5 0.061(6) 0.022(4) 0.038(5) -0.012(3) -0.012(4) 0.019(4) C6 0.019(3) 0.018(3) 0.020(3) 0.000(3) -0.001(3) 0.007(3) C7 0.023(3) 0.020(3) 0.022(4) -0.007(3) -0.007(3) 0.012(3) C8 0.028(4) 0.025(3) 0.027(4) -0.005(3) -0.009(3) 0.015(3) C9 0.056(6) 0.048(6) 0.077(8) -0.036(5) -0.046(6) 0.043(5) C10 0.099(10) 0.078(9) 0.117(12) -0.062(9) -0.089(10) 0.072(8) C11 0.083(9) 0.062(7) 0.090(9) -0.058(7) -0.069(8) 0.054(7) C12 0.019(3) 0.016(3) 0.018(3) 0.000(2) -0.005(2) 0.009(2) O1 0.026(3) 0.014(2) 0.021(2) -0.0041(18) -0.008(2) 0.0088(19) O2 0.044(3) 0.022(3) 0.019(3) 0.001(2) -0.010(2) 0.013(2) O3 0.029(3) 0.012(2) 0.019(2) 0.0004(18) -0.002(2) 0.005(2) O4 0.023(2) 0.018(2) 0.020(3) -0.0019(18) -0.0064(18) 0.0110(19) O5 0.029(3) 0.016(2) 0.041(3) -0.001(2) -0.009(2) 0.012(2) O6 0.027(3) 0.024(2) 0.014(2) -0.0027(19) -0.0050(19) 0.016(2) O7 0.012(2) 0.012(2) 0.017(4) 0.000 0.000 0.0061(10) N1 0.039(4) 0.019(3) 0.022(3) -0.003(2) -0.001(3) 0.010(3) N2 0.042(4) 0.030(3) 0.036(4) -0.019(3) -0.022(3) 0.022(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 O3 2.321(5) . ? Eu1 O6 2.323(5) . ? Eu1 O7 2.330(2) . ? Eu1 O1 2.406(5) . ? Eu1 O4 2.433(5) . ? Eu1 O2 2.488(5) 26_455 ? Eu1 O4 2.497(5) 2_665 ? Eu1 O1 2.555(5) 26_455 ? Eu1 C6 2.902(7) 26_455 ? Eu1 C7 3.265(7) . ? Eu1 Eu1 3.8615(5) 3_565 ? Eu1 Eu1 3.8615(5) 2_665 ? Eu2 O5 2.385(5) 18_544 ? Eu2 O5 2.385(5) 2_665 ? Eu2 O6 2.483(5) 17_554 ? Eu2 O6 2.483(5) . ? Eu2 O3 2.514(5) 17_554 ? Eu2 O3 2.514(5) . ? Eu2 N2 2.590(7) 17_554 ? Eu2 N2 2.590(7) . ? Eu2 N1 2.670(6) 17_554 ? Eu2 N1 2.670(6) . ? Eu2 C7 3.009(7) 17_554 ? Eu2 C7 3.009(7) . ? C1 O3 1.285(8) . ? C1 N1 1.355(9) . ? C1 C2 1.416(10) . ? C2 C3 1.404(10) . ? C2 C6 1.472(10) . ? C3 C4 1.372(14) . ? C3 H3A 0.9300 . ? C4 C5 1.384(15) . ? C4 H4A 0.9300 . ? C5 N1 1.355(11) . ? C5 H5A 0.9300 . ? C6 O2 1.249(9) . ? C6 O1 1.295(8) . ? C6 Eu1 2.902(7) 27 ? C7 O6 1.293(8) . ? C7 N2 1.361(9) . ? C7 C8 1.418(10) . ? C8 C9 1.359(11) . ? C8 C12 1.493(10) . ? C9 C10 1.428(14) . ? C9 H9A 0.9300 . ? C10 C11 1.351(15) . ? C10 H10A 0.9300 . ? C11 N2 1.335(12) . ? C11 H11A 0.9300 . ? C12 O5 1.236(8) . ? C12 O4 1.289(8) . ? O1 Eu1 2.555(5) 27 ? O2 Eu1 2.488(5) 27 ? O4 Eu1 2.497(5) 3_565 ? O5 Eu2 2.385(5) 3_565 ? O7 Eu1 2.330(2) 3_565 ? O7 Eu1 2.330(2) 2_665 ? O7 H7 1.265(8) . ? 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 Eu1 O6 68.79(18) . . ? O3 Eu1 O7 149.27(14) . . ? O6 Eu1 O7 123.9(2) . . ? O3 Eu1 O1 71.12(17) . . ? O6 Eu1 O1 137.76(16) . . ? O7 Eu1 O1 86.45(18) . . ? O3 Eu1 O4 135.23(17) . . ? O6 Eu1 O4 71.44(17) . . ? O7 Eu1 O4 72.62(15) . . ? O1 Eu1 O4 150.76(16) . . ? O3 Eu1 O2 76.94(19) . 26_455 ? O6 Eu1 O2 83.42(18) . 26_455 ? O7 Eu1 O2 129.01(15) . 26_455 ? O1 Eu1 O2 100.12(19) . 26_455 ? O4 Eu1 O2 78.92(19) . 26_455 ? O3 Eu1 O4 86.85(17) . 2_665 ? O6 Eu1 O4 76.57(17) . 2_665 ? O7 Eu1 O4 71.46(15) . 2_665 ? O1 Eu1 O4 88.61(17) . 2_665 ? O4 Eu1 O4 103.2(2) . 2_665 ? O2 Eu1 O4 157.82(17) 26_455 2_665 ? O3 Eu1 O1 109.15(17) . 26_455 ? O6 Eu1 O1 132.04(17) . 26_455 ? O7 Eu1 O1 83.36(18) . 26_455 ? O1 Eu1 O1 74.12(7) . 26_455 ? O4 Eu1 O1 83.18(17) . 26_455 ? O2 Eu1 O1 51.51(16) 26_455 26_455 ? O4 Eu1 O1 150.35(16) 2_665 26_455 ? O3 Eu1 C6 90.63(19) . 26_455 ? O6 Eu1 C6 108.30(19) . 26_455 ? O7 Eu1 C6 108.38(18) . 26_455 ? O1 Eu1 C6 84.68(19) . 26_455 ? O4 Eu1 C6 82.93(18) . 26_455 ? O2 Eu1 C6 25.34(19) 26_455 26_455 ? O4 Eu1 C6 173.28(18) 2_665 26_455 ? O1 Eu1 C6 26.48(17) 26_455 26_455 ? O3 Eu1 C7 76.52(18) . . ? O6 Eu1 C7 18.50(17) . . ? O7 Eu1 C7 125.0(2) . . ? O1 Eu1 C7 147.40(17) . . ? O4 Eu1 C7 59.58(17) . . ? O2 Eu1 C7 68.15(18) 26_455 . ? O4 Eu1 C7 93.58(18) 2_665 . ? O1 Eu1 C7 114.02(17) 26_455 . ? C6 Eu1 C7 91.89(19) 26_455 . ? O3 Eu1 Eu1 171.90(13) . 3_565 ? O6 Eu1 Eu1 103.31(12) . 3_565 ? O7 Eu1 Eu1 34.05(8) . 3_565 ? O1 Eu1 Eu1 116.08(11) . 3_565 ? O4 Eu1 Eu1 39.03(11) . 3_565 ? O2 Eu1 Eu1 104.45(14) 26_455 3_565 ? O4 Eu1 Eu1 89.56(11) 2_665 3_565 ? O1 Eu1 Eu1 77.27(11) 26_455 3_565 ? C6 Eu1 Eu1 93.70(14) 26_455 3_565 ? C7 Eu1 Eu1 96.48(12) . 3_565 ? O3 Eu1 Eu1 119.47(13) . 2_665 ? O6 Eu1 Eu1 105.98(13) . 2_665 ? O7 Eu1 Eu1 34.05(8) . 2_665 ? O1 Eu1 Eu1 82.59(12) . 2_665 ? O4 Eu1 Eu1 90.51(11) . 2_665 ? O2 Eu1 Eu1 163.00(13) 26_455 2_665 ? O4 Eu1 Eu1 37.86(11) 2_665 2_665 ? O1 Eu1 Eu1 114.45(11) 26_455 2_665 ? C6 Eu1 Eu1 140.80(14) 26_455 2_665 ? C7 Eu1 Eu1 117.78(13) . 2_665 ? Eu1 Eu1 Eu1 60.0 3_565 2_665 ? O5 Eu2 O5 71.0(3) 18_544 2_665 ? O5 Eu2 O6 74.12(17) 18_544 17_554 ? O5 Eu2 O6 142.13(18) 2_665 17_554 ? O5 Eu2 O6 142.13(18) 18_544 . ? O5 Eu2 O6 74.12(17) 2_665 . ? O6 Eu2 O6 143.1(2) 17_554 . ? O5 Eu2 O3 69.83(18) 18_544 17_554 ? O5 Eu2 O3 115.72(18) 2_665 17_554 ? O6 Eu2 O3 63.33(16) 17_554 17_554 ? O6 Eu2 O3 114.47(16) . 17_554 ? O5 Eu2 O3 115.73(18) 18_544 . ? O5 Eu2 O3 69.84(18) 2_665 . ? O6 Eu2 O3 114.47(16) 17_554 . ? O6 Eu2 O3 63.33(16) . . ? O3 Eu2 O3 173.7(2) 17_554 . ? O5 Eu2 N2 121.0(2) 18_544 17_554 ? O5 Eu2 N2 144.2(2) 2_665 17_554 ? O6 Eu2 N2 51.66(18) 17_554 17_554 ? O6 Eu2 N2 96.01(19) . 17_554 ? O3 Eu2 N2 99.8(2) 17_554 17_554 ? O3 Eu2 N2 74.96(19) . 17_554 ? O5 Eu2 N2 144.2(2) 18_544 . ? O5 Eu2 N2 121.0(2) 2_665 . ? O6 Eu2 N2 96.01(19) 17_554 . ? O6 Eu2 N2 51.66(18) . . ? O3 Eu2 N2 74.96(19) 17_554 . ? O3 Eu2 N2 99.8(2) . . ? N2 Eu2 N2 71.0(4) 17_554 . ? O5 Eu2 N1 82.1(2) 18_544 17_554 ? O5 Eu2 N1 75.7(2) 2_665 17_554 ? O6 Eu2 N1 113.58(17) 17_554 17_554 ? O6 Eu2 N1 75.47(18) . 17_554 ? O3 Eu2 N1 50.27(17) 17_554 17_554 ? O3 Eu2 N1 131.68(17) . 17_554 ? N2 Eu2 N1 136.1(2) 17_554 17_554 ? N2 Eu2 N1 70.3(2) . 17_554 ? O5 Eu2 N1 75.7(2) 18_544 . ? O5 Eu2 N1 82.1(2) 2_665 . ? O6 Eu2 N1 75.47(18) 17_554 . ? O6 Eu2 N1 113.59(17) . . ? O3 Eu2 N1 131.68(17) 17_554 . ? O3 Eu2 N1 50.28(17) . . ? N2 Eu2 N1 70.3(2) 17_554 . ? N2 Eu2 N1 136.1(2) . . ? N1 Eu2 N1 152.7(3) 17_554 . ? O5 Eu2 C7 97.61(19) 18_544 17_554 ? O5 Eu2 C7 154.6(2) 2_665 17_554 ? O6 Eu2 C7 24.96(17) 17_554 17_554 ? O6 Eu2 C7 120.27(18) . 17_554 ? O3 Eu2 C7 79.11(18) 17_554 17_554 ? O3 Eu2 C7 96.85(18) . 17_554 ? N2 Eu2 C7 26.83(19) 17_554 17_554 ? N2 Eu2 C7 81.8(2) . 17_554 ? N1 Eu2 C7 126.4(2) 17_554 17_554 ? N1 Eu2 C7 72.9(2) . 17_554 ? O5 Eu2 C7 154.6(2) 18_544 . ? O5 Eu2 C7 97.61(19) 2_665 . ? O6 Eu2 C7 120.27(18) 17_554 . ? O6 Eu2 C7 24.96(17) . . ? O3 Eu2 C7 96.85(18) 17_554 . ? O3 Eu2 C7 79.11(18) . . ? N2 Eu2 C7 81.8(2) 17_554 . ? N2 Eu2 C7 26.83(19) . . ? N1 Eu2 C7 72.9(2) 17_554 . ? N1 Eu2 C7 126.4(2) . . ? C7 Eu2 C7 101.1(3) 17_554 . ? O3 C1 N1 113.4(6) . . ? O3 C1 C2 124.5(6) . . ? N1 C1 C2 122.1(7) . . ? O3 C1 Eu2 53.8(3) . . ? N1 C1 Eu2 61.0(4) . . ? C2 C1 Eu2 167.3(5) . . ? C3 C2 C1 116.4(7) . . ? C3 C2 C6 120.5(7) . . ? C1 C2 C6 123.1(6) . . ? C4 C3 C2 121.5(9) . . ? C4 C3 H3A 119.3 . . ? C2 C3 H3A 119.3 . . ? C3 C4 C5 118.0(8) . . ? C3 C4 H4A 121.0 . . ? C5 C4 H4A 121.0 . . ? N1 C5 C4 123.1(8) . . ? N1 C5 H5A 118.5 . . ? C4 C5 H5A 118.5 . . ? O2 C6 O1 119.0(6) . . ? O2 C6 C2 120.1(6) . . ? O1 C6 C2 120.8(6) . . ? O2 C6 Eu1 58.5(4) . 27 ? O1 C6 Eu1 61.6(3) . 27 ? C2 C6 Eu1 165.9(5) . 27 ? O6 C7 N2 112.9(6) . . ? O6 C7 C8 125.9(6) . . ? N2 C7 C8 121.2(7) . . ? O6 C7 Eu2 54.1(3) . . ? N2 C7 Eu2 59.2(4) . . ? C8 C7 Eu2 174.3(6) . . ? O6 C7 Eu1 34.8(3) . . ? N2 C7 Eu1 134.9(5) . . ? C8 C7 Eu1 98.3(4) . . ? Eu2 C7 Eu1 79.37(16) . . ? C9 C8 C7 117.6(7) . . ? C9 C8 C12 119.6(7) . . ? C7 C8 C12 122.8(6) . . ? C8 C9 C10 120.6(8) . . ? C8 C9 H9A 119.7 . . ? C10 C9 H9A 119.7 . . ? C11 C10 C9 117.6(9) . . ? C11 C10 H10A 121.2 . . ? C9 C10 H10A 121.2 . . ? N2 C11 C10 123.5(9) . . ? N2 C11 H11A 118.3 . . ? C10 C11 H11A 118.3 . . ? O5 C12 O4 123.2(6) . . ? O5 C12 C8 116.4(6) . . ? O4 C12 C8 120.4(6) . . ? C6 O1 Eu1 138.9(4) . . ? C6 O1 Eu1 91.9(4) . 27 ? Eu1 O1 Eu1 129.12(19) . 27 ? C6 O2 Eu1 96.2(4) . 27 ? C1 O3 Eu1 139.5(5) . . ? C1 O3 Eu2 101.9(4) . . ? Eu1 O3 Eu2 112.1(2) . . ? C12 O4 Eu1 131.9(4) . . ? C12 O4 Eu1 125.0(4) . 3_565 ? Eu1 O4 Eu1 103.11(17) . 3_565 ? C12 O5 Eu2 141.1(5) . 3_565 ? C7 O6 Eu1 126.7(4) . . ? C7 O6 Eu2 100.9(4) . . ? Eu1 O6 Eu2 113.11(19) . . ? Eu1 O7 Eu1 111.90(16) 3_565 . ? Eu1 O7 Eu1 111.90(16) 3_565 2_665 ? Eu1 O7 Eu1 111.90(16) . 2_665 ? Eu1 O7 H7 106.91(18) 3_565 . ? Eu1 O7 H7 106.91(18) . . ? Eu1 O7 H7 106.91(18) 2_665 . ? C1 N1 C5 118.3(7) . . ? C1 N1 Eu2 92.6(4) . . ? C5 N1 Eu2 148.1(6) . . ? C11 N2 C7 119.3(7) . . ? C11 N2 Eu2 146.5(6) . . ? C7 N2 Eu2 94.0(4) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.959 _refine_diff_density_min -6.155 _refine_diff_density_rms 0.258