data_c:complex_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H12 Eu O10' _chemical_formula_weight 468.18 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' '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 'monoclinic' _symmetry_space_group_name_H-M 'P21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.821(5) _cell_length_b 18.955(9) _cell_length_c 9.288(5) _cell_angle_alpha 90.00 _cell_angle_beta 109.557(8) _cell_angle_gamma 90.00 _cell_volume 1463.3(13) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 1555 _cell_measurement_theta_min 2.1488 _cell_measurement_theta_max 27.3756 _exptl_crystal_description 'plate' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.125 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 908 _exptl_absorpt_coefficient_mu 4.338 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_min 0.5622 _exptl_absorpt_correction_T_max 0.6709 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 Mercury2_(2x2_bin_mode) _diffrn_measurement_method 'CCD_Profile_fitting' _diffrn_detector_area_resol_mean 13.6612 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11268 _diffrn_reflns_av_R_equivalents 0.0480 _diffrn_reflns_av_sigmaI/netI 0.0506 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.68 _diffrn_reflns_theta_max 27.47 _reflns_number_total 3332 _reflns_number_gt 2825 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _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^)+(0.0423P)^2^+3.0832P] 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 3332 _refine_ls_number_parameters 198 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0489 _refine_ls_R_factor_gt 0.0394 _refine_ls_wR_factor_ref 0.0948 _refine_ls_wR_factor_gt 0.0888 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Eu1 Eu 0.28973(3) 0.553215(13) 0.01552(3) 0.01880(11) Uani 1 1 d . . . O1 O 0.2333(7) 0.6199(3) 0.2189(6) 0.0576(15) Uani 1 1 d . . . H1A H 0.1647 0.6136 0.2651 0.069 Uiso 1 1 d R . . H1B H 0.2424 0.6667 0.2290 0.069 Uiso 1 1 d R . . O2 O 0.1970(5) 0.4443(2) -0.1319(5) 0.0356(11) Uani 1 1 d . . . H2A H 0.2716 0.4184 -0.1447 0.043 Uiso 1 1 d R . . H2B H 0.1157 0.4496 -0.2151 0.043 Uiso 1 1 d R . . O3 O 0.4943(5) 0.5362(2) -0.1212(4) 0.0223(8) Uani 1 1 d . . . O4 O 0.2609(5) 0.5749(2) -0.2723(5) 0.0354(10) Uani 1 1 d . . . O5 O 0.3481(5) 0.8172(2) -0.5026(5) 0.0355(11) Uani 1 1 d . . . O6 O 0.5372(5) 0.88129(19) -0.3448(5) 0.0283(9) Uani 1 1 d . . . O7 O 1.0311(5) 0.5915(2) -0.1129(5) 0.0307(10) Uani 1 1 d . . . O8 O 0.8250(5) 0.5170(2) -0.1616(5) 0.0281(9) Uani 1 1 d . . . O9 O 0.0375(11) 0.5910(5) -0.5780(10) 0.109(3) Uiso 1 1 d . . . C1 C 0.3944(6) 0.5489(3) -0.2551(6) 0.0195(11) Uani 1 1 d . . . C2 C 0.4449(6) 0.5258(3) -0.3883(6) 0.0182(10) Uani 1 1 d . . . C3 C 0.5663(6) 0.5619(3) -0.4218(6) 0.0194(11) Uani 1 1 d . . . C4 C 0.6212(7) 0.5356(3) -0.5346(6) 0.0216(11) Uani 1 1 d . . . H4 H 0.7023 0.5590 -0.5586 0.026 Uiso 1 1 calc R . . C5 C 0.6265(6) 0.6324(3) -0.3456(6) 0.0189(10) Uani 1 1 d . . . C6 C 0.5343(7) 0.6911(3) -0.4013(6) 0.0232(12) Uani 1 1 d . . . H6 H 0.4384 0.6865 -0.4826 0.028 Uiso 1 1 calc R . . C7 C 0.5824(7) 0.7573(3) -0.3378(6) 0.0249(12) Uani 1 1 d . . . C8 C 0.7241(8) 0.7639(3) -0.2145(8) 0.0361(15) Uani 1 1 d . . . H8 H 0.7552 0.8077 -0.1691 0.043 Uiso 1 1 calc R . . C9 C 0.8181(8) 0.7055(3) -0.1598(8) 0.0346(15) Uani 1 1 d . . . H9 H 0.9139 0.7103 -0.0785 0.042 Uiso 1 1 calc R . . C10 C 0.7716(7) 0.6389(3) -0.2250(6) 0.0229(11) Uani 1 1 d . . . C11 C 0.8837(7) 0.5774(3) -0.1605(6) 0.0240(12) Uani 1 1 d . . . C12 C 0.4823(7) 0.8219(3) -0.4005(7) 0.0258(12) Uani 1 1 d . . . O10 O 0.1439(14) 0.7659(6) 0.1961(12) 0.152(4) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Eu1 0.01662(16) 0.01506(15) 0.02360(17) 0.00028(10) 0.00524(11) 0.00011(9) O1 0.075(4) 0.054(3) 0.061(4) -0.022(3) 0.046(3) -0.021(3) O2 0.027(2) 0.032(2) 0.043(3) -0.008(2) 0.006(2) 0.0037(17) O3 0.022(2) 0.0250(19) 0.0184(19) 0.0032(16) 0.0054(15) 0.0028(15) O4 0.025(2) 0.051(3) 0.028(2) -0.001(2) 0.0064(18) 0.014(2) O5 0.033(2) 0.023(2) 0.041(3) -0.0063(19) 0.000(2) 0.0046(17) O6 0.030(2) 0.0142(19) 0.037(2) 0.0059(17) 0.0065(18) 0.0039(15) O7 0.017(2) 0.026(2) 0.045(3) 0.0056(19) 0.0058(18) 0.0028(16) O8 0.030(2) 0.0171(19) 0.038(2) 0.0066(17) 0.0113(18) 0.0014(16) C1 0.020(3) 0.016(2) 0.022(3) -0.001(2) 0.005(2) -0.0042(19) C2 0.022(3) 0.012(2) 0.019(3) 0.002(2) 0.006(2) 0.0025(19) C3 0.022(3) 0.015(2) 0.020(3) 0.002(2) 0.004(2) 0.001(2) C4 0.020(3) 0.020(3) 0.023(3) 0.000(2) 0.005(2) -0.005(2) C5 0.018(3) 0.020(3) 0.018(3) -0.002(2) 0.006(2) -0.002(2) C6 0.020(3) 0.020(3) 0.028(3) -0.004(2) 0.005(2) -0.001(2) C7 0.028(3) 0.016(3) 0.028(3) 0.003(2) 0.006(2) 0.005(2) C8 0.035(4) 0.020(3) 0.043(4) -0.005(3) 0.000(3) -0.003(3) C9 0.029(3) 0.023(3) 0.039(4) 0.000(3) -0.007(3) 0.002(2) C10 0.021(3) 0.021(3) 0.027(3) 0.002(2) 0.008(2) 0.002(2) C11 0.023(3) 0.026(3) 0.023(3) 0.002(2) 0.007(2) 0.003(2) C12 0.030(3) 0.018(3) 0.028(3) 0.001(2) 0.007(2) 0.005(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu1 O7 2.309(4) 1_455 ? Eu1 O8 2.356(4) 3_665 ? Eu1 O1 2.459(5) . ? Eu1 O2 2.462(4) . ? Eu1 O6 2.469(4) 4_576 ? Eu1 O3 2.492(4) 3_665 ? Eu1 O5 2.526(4) 4_576 ? Eu1 O3 2.551(4) . ? Eu1 O4 2.631(5) . ? Eu1 C12 2.865(5) 4_576 ? Eu1 C1 2.955(6) . ? Eu1 Eu1 4.3161(18) 3_665 ? O1 H1A 0.8586 . ? O1 H1B 0.8926 . ? O2 H2A 0.8591 . ? O2 H2B 0.8665 . ? O3 C1 1.284(6) . ? O3 Eu1 2.492(4) 3_665 ? O4 C1 1.236(7) . ? O5 C12 1.248(7) . ? O5 Eu1 2.526(4) 4_575 ? O6 C12 1.265(7) . ? O6 Eu1 2.469(4) 4_575 ? O7 C11 1.254(7) . ? O7 Eu1 2.309(4) 1_655 ? O8 C11 1.256(7) . ? O8 Eu1 2.356(4) 3_665 ? C1 C2 1.512(7) . ? C2 C4 1.389(7) 3_664 ? C2 C3 1.392(8) . ? C3 C4 1.386(8) . ? C3 C5 1.521(7) . ? C4 C2 1.389(7) 3_664 ? C4 H4 0.9300 . ? C5 C6 1.374(7) . ? C5 C10 1.396(7) . ? C6 C7 1.392(7) . ? C6 H6 0.9300 . ? C7 C8 1.390(8) . ? C7 C12 1.507(7) . ? C8 C9 1.374(8) . ? C8 H8 0.9300 . ? C9 C10 1.400(8) . ? C9 H9 0.9300 . ? C10 C11 1.516(7) . ? C12 Eu1 2.865(5) 4_575 ? 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 O7 Eu1 O8 86.23(15) 1_455 3_665 ? O7 Eu1 O1 79.41(19) 1_455 . ? O8 Eu1 O1 67.14(16) 3_665 . ? O7 Eu1 O2 83.64(15) 1_455 . ? O8 Eu1 O2 73.73(15) 3_665 . ? O1 Eu1 O2 138.05(17) . . ? O7 Eu1 O6 131.35(14) 1_455 4_576 ? O8 Eu1 O6 117.13(14) 3_665 4_576 ? O1 Eu1 O6 73.06(17) . 4_576 ? O2 Eu1 O6 141.71(14) . 4_576 ? O7 Eu1 O3 155.46(13) 1_455 3_665 ? O8 Eu1 O3 78.95(14) 3_665 3_665 ? O1 Eu1 O3 111.82(17) . 3_665 ? O2 Eu1 O3 73.53(14) . 3_665 ? O6 Eu1 O3 73.15(13) 4_576 3_665 ? O7 Eu1 O5 81.28(14) 1_455 4_576 ? O8 Eu1 O5 136.35(15) 3_665 4_576 ? O1 Eu1 O5 69.50(17) . 4_576 ? O2 Eu1 O5 144.64(15) . 4_576 ? O6 Eu1 O5 51.84(13) 4_576 4_576 ? O3 Eu1 O5 122.77(14) 3_665 4_576 ? O7 Eu1 O3 121.60(14) 1_455 . ? O8 Eu1 O3 136.60(13) 3_665 . ? O1 Eu1 O3 143.77(15) . . ? O2 Eu1 O3 77.02(14) . . ? O6 Eu1 O3 71.14(14) 4_576 . ? O3 Eu1 O3 62.29(15) 3_665 . ? O5 Eu1 O3 84.04(14) 4_576 . ? O7 Eu1 O4 71.55(14) 1_455 . ? O8 Eu1 O4 139.36(15) 3_665 . ? O1 Eu1 O4 136.45(17) . . ? O2 Eu1 O4 70.42(15) . . ? O6 Eu1 O4 102.88(14) 4_576 . ? O3 Eu1 O4 107.91(13) 3_665 . ? O5 Eu1 O4 74.51(15) 4_576 . ? O3 Eu1 O4 50.06(12) . . ? O7 Eu1 C12 105.93(16) 1_455 4_576 ? O8 Eu1 C12 129.75(16) 3_665 4_576 ? O1 Eu1 C12 67.68(18) . 4_576 ? O2 Eu1 C12 154.27(17) . 4_576 ? O6 Eu1 C12 26.11(14) 4_576 4_576 ? O3 Eu1 C12 98.57(15) 3_665 4_576 ? O5 Eu1 C12 25.81(14) 4_576 4_576 ? O3 Eu1 C12 77.67(15) . 4_576 ? O4 Eu1 C12 89.68(16) . 4_576 ? O7 Eu1 C1 96.04(16) 1_455 . ? O8 Eu1 C1 142.25(14) 3_665 . ? O1 Eu1 C1 150.37(16) . . ? O2 Eu1 C1 69.13(15) . . ? O6 Eu1 C1 89.30(15) 4_576 . ? O3 Eu1 C1 84.32(14) 3_665 . ? O5 Eu1 C1 80.88(15) 4_576 . ? O3 Eu1 C1 25.65(13) . . ? O4 Eu1 C1 24.71(14) . . ? C12 Eu1 C1 85.93(16) 4_576 . ? O7 Eu1 Eu1 146.61(12) 1_455 3_665 ? O8 Eu1 Eu1 108.59(10) 3_665 3_665 ? O1 Eu1 Eu1 133.74(15) . 3_665 ? O2 Eu1 Eu1 72.76(11) . 3_665 ? O6 Eu1 Eu1 68.99(10) 4_576 3_665 ? O3 Eu1 Eu1 31.55(9) 3_665 3_665 ? O5 Eu1 Eu1 104.54(11) 4_576 3_665 ? O3 Eu1 Eu1 30.74(8) . 3_665 ? O4 Eu1 Eu1 78.35(9) . 3_665 ? C12 Eu1 Eu1 87.70(13) 4_576 3_665 ? C1 Eu1 Eu1 53.84(10) . 3_665 ? Eu1 O1 H1A 132.0 . . ? Eu1 O1 H1B 123.8 . . ? H1A O1 H1B 98.1 . . ? Eu1 O2 H2A 115.3 . . ? Eu1 O2 H2B 114.8 . . ? H2A O2 H2B 112.7 . . ? C1 O3 Eu1 134.1(3) . 3_665 ? C1 O3 Eu1 95.0(3) . . ? Eu1 O3 Eu1 117.71(15) 3_665 . ? C1 O4 Eu1 92.5(3) . . ? C12 O5 Eu1 92.4(3) . 4_575 ? C12 O6 Eu1 94.7(3) . 4_575 ? C11 O7 Eu1 147.6(4) . 1_655 ? C11 O8 Eu1 140.0(4) . 3_665 ? O4 C1 O3 121.0(5) . . ? O4 C1 C2 122.6(5) . . ? O3 C1 C2 116.3(5) . . ? O4 C1 Eu1 62.8(3) . . ? O3 C1 Eu1 59.3(3) . . ? C2 C1 Eu1 164.7(3) . . ? C4 C2 C3 121.2(5) 3_664 . ? C4 C2 C1 118.5(5) 3_664 . ? C3 C2 C1 120.0(5) . . ? C4 C3 C2 118.8(5) . . ? C4 C3 C5 120.8(5) . . ? C2 C3 C5 120.2(5) . . ? C3 C4 C2 120.0(5) . 3_664 ? C3 C4 H4 120.0 . . ? C2 C4 H4 120.0 3_664 . ? C6 C5 C10 119.9(5) . . ? C6 C5 C3 117.7(5) . . ? C10 C5 C3 122.4(5) . . ? C5 C6 C7 120.9(5) . . ? C5 C6 H6 119.6 . . ? C7 C6 H6 119.6 . . ? C8 C7 C6 119.5(5) . . ? C8 C7 C12 119.6(5) . . ? C6 C7 C12 120.9(5) . . ? C9 C8 C7 119.9(6) . . ? C9 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? C8 C9 C10 120.8(5) . . ? C8 C9 H9 119.6 . . ? C10 C9 H9 119.6 . . ? C5 C10 C9 119.0(5) . . ? C5 C10 C11 123.3(5) . . ? C9 C10 C11 117.7(5) . . ? O7 C11 O8 124.9(5) . . ? O7 C11 C10 116.0(5) . . ? O8 C11 C10 119.1(5) . . ? O5 C12 O6 120.7(5) . . ? O5 C12 C7 121.3(5) . . ? O6 C12 C7 118.0(5) . . ? O5 C12 Eu1 61.8(3) . 4_575 ? O6 C12 Eu1 59.2(3) . 4_575 ? C7 C12 Eu1 173.3(4) . 4_575 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.645 _refine_diff_density_min -1.427 _refine_diff_density_rms 0.170 ###END data_c:complex_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H12 O10 Tb' _chemical_formula_weight 475.14 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Tb' 'Tb' -0.1723 4.1537 '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/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.728(5) _cell_length_b 18.911(10) _cell_length_c 9.289(6) _cell_angle_alpha 90.00 _cell_angle_beta 109.307(9) _cell_angle_gamma 90.00 _cell_volume 1447.0(15) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 1649 _cell_measurement_theta_min 2.5613 _cell_measurement_theta_max 27.4256 _exptl_crystal_description 'plate' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.181 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 916 _exptl_absorpt_coefficient_mu 4.940 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_min 0.5245 _exptl_absorpt_correction_T_max 0.6379 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 Mercury2_(2x2_bin_mode) _diffrn_measurement_method 'CCD_Profile_fitting' _diffrn_detector_area_resol_mean 13.6612 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11044 _diffrn_reflns_av_R_equivalents 0.0426 _diffrn_reflns_av_sigmaI/netI 0.0408 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 27.39 _reflns_number_total 3270 _reflns_number_gt 2895 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _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^)+(0.0633P)^2^+4.6094P] 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 3270 _refine_ls_number_parameters 198 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0479 _refine_ls_R_factor_gt 0.0428 _refine_ls_wR_factor_ref 0.1152 _refine_ls_wR_factor_gt 0.1099 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _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 Tb1 Tb 0.20942(3) 0.446837(13) 0.48394(3) 0.02128(12) Uani 1 1 d . . . O1 O 0.2652(8) 0.3803(3) 0.2826(7) 0.0565(16) Uani 1 1 d . . . H1A H 0.3233 0.4070 0.2507 0.068 Uiso 1 1 d R . . H1B H 0.3342 0.3413 0.3308 0.068 Uiso 1 1 d R . . O2 O 0.3039(6) 0.5539(2) 0.6294(6) 0.0362(11) Uani 1 1 d . . . H2A H 0.3972 0.5605 0.7123 0.043 Uiso 1 1 d R . . H2B H 0.2155 0.5858 0.6290 0.043 Uiso 1 1 d R . . O3 O 0.0060(5) 0.4646(2) 0.6206(5) 0.0268(8) Uani 1 1 d . . . O4 O 0.2396(6) 0.4248(3) 0.7708(5) 0.0391(11) Uani 1 1 d . . . O5 O -0.3251(5) 0.4833(2) 0.6603(5) 0.0318(9) Uani 1 1 d . . . O6 O -0.5328(5) 0.4090(2) 0.6085(5) 0.0339(10) Uani 1 1 d . . . O7 O -0.0379(5) 0.1180(2) 0.8455(5) 0.0303(9) Uani 1 1 d . . . O8 O 0.1524(6) 0.1819(2) 1.0044(5) 0.0381(11) Uani 1 1 d . . . C1 C 0.1049(7) 0.4521(3) 0.7545(7) 0.0216(11) Uani 1 1 d . . . C2 C 0.0547(6) 0.4744(3) 0.8861(6) 0.0219(10) Uani 1 1 d . . . C3 C -0.0660(7) 0.4376(3) 0.9224(7) 0.0217(11) Uani 1 1 d . . . C4 C -0.1214(7) 0.4638(3) 1.0357(6) 0.0236(11) Uani 1 1 d . . . H4 H -0.2032 0.4402 1.0597 0.028 Uiso 1 1 calc R . . C5 C -0.1284(7) 0.3676(3) 0.8448(6) 0.0217(10) Uani 1 1 d . . . C6 C -0.2729(7) 0.3613(3) 0.7249(7) 0.0264(12) Uani 1 1 d . . . C7 C -0.3184(8) 0.2947(3) 0.6596(8) 0.0375(15) Uani 1 1 d . . . H7 H -0.4140 0.2902 0.5774 0.045 Uiso 1 1 calc R . . C8 C -0.2249(8) 0.2357(3) 0.7142(8) 0.0372(15) Uani 1 1 d . . . H8 H -0.2560 0.1919 0.6682 0.045 Uiso 1 1 calc R . . C9 C -0.0826(7) 0.2423(3) 0.8396(7) 0.0280(12) Uani 1 1 d . . . C10 C -0.0353(7) 0.3081(3) 0.9030(7) 0.0259(11) Uani 1 1 d . . . H10 H 0.0599 0.3127 0.9856 0.031 Uiso 1 1 calc R . . C11 C 0.0166(7) 0.1773(3) 0.9009(7) 0.0281(12) Uani 1 1 d . . . C12 C -0.3840(7) 0.4231(3) 0.6590(7) 0.0263(11) Uani 1 1 d . . . O10 O 0.5387(13) 0.5903(6) 0.9213(11) 0.116(3) Uiso 1 1 d . . . O9 O 0.3543(16) 0.2360(6) 0.2991(13) 0.144(4) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tb1 0.02134(18) 0.01566(17) 0.02529(19) 0.00003(8) 0.00563(13) -0.00010(8) O1 0.076(4) 0.053(3) 0.054(4) -0.018(3) 0.040(3) -0.018(3) O2 0.031(2) 0.031(3) 0.041(3) -0.0096(18) 0.004(2) -0.0004(17) O3 0.031(2) 0.027(2) 0.020(2) -0.0003(16) 0.0058(17) 0.0014(17) O4 0.036(2) 0.052(3) 0.029(2) 0.001(2) 0.011(2) 0.015(2) O5 0.036(2) 0.018(2) 0.043(3) 0.0072(17) 0.015(2) 0.0006(17) O6 0.023(2) 0.026(2) 0.050(3) 0.0065(19) 0.0068(19) 0.0048(17) O7 0.032(2) 0.0142(19) 0.041(3) 0.0032(16) 0.0065(19) 0.0028(16) O8 0.037(2) 0.022(2) 0.043(3) -0.0055(18) -0.002(2) 0.0055(18) C1 0.026(3) 0.018(3) 0.022(3) -0.0012(19) 0.009(2) -0.0006(19) C2 0.024(3) 0.019(3) 0.020(3) 0.000(2) 0.004(2) 0.003(2) C3 0.026(3) 0.017(2) 0.021(3) 0.0010(19) 0.006(2) 0.002(2) C4 0.027(3) 0.020(3) 0.023(3) 0.000(2) 0.007(2) -0.002(2) C5 0.025(3) 0.024(3) 0.016(2) -0.003(2) 0.006(2) -0.002(2) C6 0.025(3) 0.023(3) 0.030(3) 0.000(2) 0.006(2) 0.002(2) C7 0.033(3) 0.023(3) 0.041(4) 0.001(3) -0.010(3) -0.004(2) C8 0.036(3) 0.018(3) 0.046(4) -0.008(3) -0.001(3) 0.000(3) C9 0.034(3) 0.017(3) 0.030(3) -0.001(2) 0.008(2) -0.001(2) C10 0.027(3) 0.022(3) 0.025(3) -0.001(2) 0.002(2) 0.000(2) C11 0.032(3) 0.022(3) 0.029(3) 0.000(2) 0.007(2) 0.005(2) C12 0.029(3) 0.022(3) 0.026(3) 0.002(2) 0.008(2) 0.004(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tb1 O6 2.278(4) 1_655 ? Tb1 O5 2.336(4) 3_566 ? Tb1 O2 2.423(4) . ? Tb1 O1 2.434(5) . ? Tb1 O7 2.445(4) 4_565 ? Tb1 O3 2.464(4) 3_566 ? Tb1 O8 2.506(4) 4_565 ? Tb1 O3 2.524(4) . ? Tb1 O4 2.623(5) . ? Tb1 C11 2.842(6) 4_565 ? Tb1 C1 2.945(6) . ? O1 H1A 0.8372 . ? O1 H1B 0.9627 . ? O2 H2A 0.9254 . ? O2 H2B 0.9784 . ? O3 C1 1.280(7) . ? O3 Tb1 2.464(4) 3_566 ? O4 C1 1.245(8) . ? O5 C12 1.247(7) . ? O5 Tb1 2.336(4) 3_566 ? O6 C12 1.256(7) . ? O6 Tb1 2.278(4) 1_455 ? O7 C11 1.259(7) . ? O7 Tb1 2.445(4) 4_566 ? O8 C11 1.258(8) . ? O8 Tb1 2.506(4) 4_566 ? C1 C2 1.490(7) . ? C2 C3 1.394(8) . ? C2 C4 1.397(8) 3_567 ? C3 C4 1.386(8) . ? C3 C5 1.520(7) . ? C4 C2 1.397(8) 3_567 ? C4 H4 0.9300 . ? C5 C6 1.384(8) . ? C5 C10 1.388(8) . ? C6 C7 1.396(8) . ? C6 C12 1.513(8) . ? C7 C8 1.376(9) . ? C7 H7 0.9300 . ? C8 C9 1.400(9) . ? C8 H8 0.9300 . ? C9 C10 1.381(8) . ? C9 C11 1.503(8) . ? C10 H10 0.9300 . ? C11 Tb1 2.842(6) 4_566 ? 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 O6 Tb1 O5 85.84(16) 1_655 3_566 ? O6 Tb1 O2 83.24(17) 1_655 . ? O5 Tb1 O2 73.46(17) 3_566 . ? O6 Tb1 O1 79.2(2) 1_655 . ? O5 Tb1 O1 67.51(18) 3_566 . ? O2 Tb1 O1 138.02(18) . . ? O6 Tb1 O7 131.40(15) 1_655 4_565 ? O5 Tb1 O7 117.11(16) 3_566 4_565 ? O2 Tb1 O7 142.26(15) . 4_565 ? O1 Tb1 O7 72.71(18) . 4_565 ? O6 Tb1 O3 155.51(15) 1_655 3_566 ? O5 Tb1 O3 78.92(15) 3_566 3_566 ? O2 Tb1 O3 74.14(16) . 3_566 ? O1 Tb1 O3 111.66(19) . 3_566 ? O7 Tb1 O3 73.00(14) 4_565 3_566 ? O6 Tb1 O8 81.01(15) 1_655 4_565 ? O5 Tb1 O8 136.70(16) 3_566 4_565 ? O2 Tb1 O8 144.05(16) . 4_565 ? O1 Tb1 O8 69.56(18) . 4_565 ? O7 Tb1 O8 52.39(14) 4_565 4_565 ? O3 Tb1 O8 123.05(15) 3_566 4_565 ? O6 Tb1 O3 121.82(16) 1_655 . ? O5 Tb1 O3 136.29(14) 3_566 . ? O2 Tb1 O3 76.96(16) . . ? O1 Tb1 O3 143.95(17) . . ? O7 Tb1 O3 71.69(15) 4_565 . ? O3 Tb1 O3 62.34(16) 3_566 . ? O8 Tb1 O3 84.31(16) 4_565 . ? O6 Tb1 O4 71.56(16) 1_655 . ? O5 Tb1 O4 139.07(17) 3_566 . ? O2 Tb1 O4 70.41(17) . . ? O1 Tb1 O4 136.07(18) . . ? O7 Tb1 O4 103.25(16) 4_565 . ? O3 Tb1 O4 108.39(14) 3_566 . ? O8 Tb1 O4 74.00(16) 4_565 . ? O3 Tb1 O4 50.28(14) . . ? O6 Tb1 C11 105.97(17) 1_655 4_565 ? O5 Tb1 C11 129.85(17) 3_566 4_565 ? O2 Tb1 C11 154.61(17) . 4_565 ? O1 Tb1 C11 67.36(18) . 4_565 ? O7 Tb1 C11 26.21(15) 4_565 4_565 ? O3 Tb1 C11 98.51(16) 3_566 4_565 ? O8 Tb1 C11 26.26(16) 4_565 4_565 ? O3 Tb1 C11 78.15(16) . 4_565 ? O4 Tb1 C11 89.78(17) . 4_565 ? O6 Tb1 C1 96.29(17) 1_655 . ? O5 Tb1 C1 141.74(15) 3_566 . ? O2 Tb1 C1 68.92(16) . . ? O1 Tb1 C1 150.49(17) . . ? O7 Tb1 C1 89.83(16) 4_565 . ? O3 Tb1 C1 84.40(15) 3_566 . ? O8 Tb1 C1 80.93(16) 4_565 . ? O3 Tb1 C1 25.62(15) . . ? O4 Tb1 C1 25.00(16) . . ? C11 Tb1 C1 86.37(16) 4_565 . ? Tb1 O1 H1A 104.9 . . ? Tb1 O1 H1B 107.0 . . ? H1A O1 H1B 105.6 . . ? Tb1 O2 H2A 128.3 . . ? Tb1 O2 H2B 113.0 . . ? H2A O2 H2B 113.3 . . ? C1 O3 Tb1 133.7(3) . 3_566 ? C1 O3 Tb1 95.9(3) . . ? Tb1 O3 Tb1 117.66(16) 3_566 . ? C1 O4 Tb1 92.1(4) . . ? C12 O5 Tb1 139.9(4) . 3_566 ? C12 O6 Tb1 148.1(4) . 1_455 ? C11 O7 Tb1 94.8(4) . 4_566 ? C11 O8 Tb1 91.9(3) . 4_566 ? O4 C1 O3 120.1(5) . . ? O4 C1 C2 122.6(5) . . ? O3 C1 C2 117.2(5) . . ? O4 C1 Tb1 62.9(3) . . ? O3 C1 Tb1 58.5(3) . . ? C2 C1 Tb1 165.4(4) . . ? C3 C2 C4 120.7(5) . 3_567 ? C3 C2 C1 120.5(5) . . ? C4 C2 C1 118.6(5) 3_567 . ? C4 C3 C2 119.0(5) . . ? C4 C3 C5 120.8(5) . . ? C2 C3 C5 120.1(5) . . ? C3 C4 C2 120.3(5) . 3_567 ? C3 C4 H4 119.9 . . ? C2 C4 H4 119.9 3_567 . ? C6 C5 C10 120.3(5) . . ? C6 C5 C3 123.0(5) . . ? C10 C5 C3 116.7(5) . . ? C5 C6 C7 118.7(5) . . ? C5 C6 C12 123.4(5) . . ? C7 C6 C12 117.9(5) . . ? C8 C7 C6 121.5(6) . . ? C8 C7 H7 119.3 . . ? C6 C7 H7 119.3 . . ? C7 C8 C9 119.3(6) . . ? C7 C8 H8 120.3 . . ? C9 C8 H8 120.3 . . ? C10 C9 C8 119.5(5) . . ? C10 C9 C11 121.5(5) . . ? C8 C9 C11 119.0(5) . . ? C9 C10 C5 120.7(5) . . ? C9 C10 H10 119.7 . . ? C5 C10 H10 119.7 . . ? O8 C11 O7 120.5(5) . . ? O8 C11 C9 120.7(5) . . ? O7 C11 C9 118.8(5) . . ? O8 C11 Tb1 61.8(3) . 4_566 ? O7 C11 Tb1 59.0(3) . 4_566 ? C9 C11 Tb1 173.5(4) . 4_566 ? O5 C12 O6 124.7(6) . . ? O5 C12 C6 119.6(5) . . ? O6 C12 C6 115.6(5) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.39 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.499 _refine_diff_density_min -2.362 _refine_diff_density_rms 0.204 ###END data_c:complex_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H12 Gd O10' _chemical_formula_weight 473.47 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' '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 'monoclinic' _symmetry_space_group_name_H-M 'p21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.783(5) _cell_length_b 18.952(9) _cell_length_c 9.285(5) _cell_angle_alpha 90.00 _cell_angle_beta 109.398(9) _cell_angle_gamma 90.00 _cell_volume 1457.8(13) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 1601 _cell_measurement_theta_min 2.5621 _cell_measurement_theta_max 27.4797 _exptl_crystal_description 'plate' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.157 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 912 _exptl_absorpt_coefficient_mu 4.602 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_min 0.5453 _exptl_absorpt_correction_T_max 0.6561 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 Mercury2_(2x2_bin_mode) _diffrn_measurement_method 'CCD_Profile_fitting' _diffrn_detector_area_resol_mean 13.6612 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11282 _diffrn_reflns_av_R_equivalents 0.0407 _diffrn_reflns_av_sigmaI/netI 0.0432 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.68 _diffrn_reflns_theta_max 27.49 _reflns_number_total 3332 _reflns_number_gt 2847 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _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^)+(0.0455P)^2^+5.7985P] 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 3332 _refine_ls_number_parameters 198 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0469 _refine_ls_R_factor_gt 0.0392 _refine_ls_wR_factor_ref 0.1005 _refine_ls_wR_factor_gt 0.0935 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _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 -0.21026(3) 0.446883(13) 0.51511(3) 0.01944(11) Uani 1 1 d . . . O1 O -0.2678(7) 0.3809(3) 0.7168(6) 0.0552(15) Uani 1 1 d . . . H1B H -0.2343 0.3344 0.7050 0.066 Uiso 1 1 d R . . H1A H -0.2546 0.4093 0.8071 0.066 Uiso 1 1 d R . . C1 C -0.1037(7) 0.4514(3) 0.2449(6) 0.0197(11) Uani 1 1 d . . . O2 O -0.3032(6) 0.5546(2) 0.3672(6) 0.0362(11) Uani 1 1 d . . . H2A H -0.3614 0.5624 0.2609 0.043 Uiso 1 1 d R . . H2B H -0.2462 0.5801 0.4399 0.043 Uiso 1 1 d R . . C2 C -0.0561(6) 0.4741(3) 0.1130(6) 0.0198(11) Uani 1 1 d . . . O3 O -0.0052(5) 0.4646(2) 0.3784(4) 0.0239(8) Uani 1 1 d . . . C3 C -0.1203(7) 0.5354(3) 0.0347(6) 0.0206(11) Uani 1 1 d . . . H3 H -0.2014 0.5589 0.0591 0.025 Uiso 1 1 calc R . . O4 O -0.2391(5) 0.4250(3) 0.2288(5) 0.0366(11) Uani 1 1 d . . . C4 C 0.0673(7) 0.4374(3) 0.0785(7) 0.0213(11) Uani 1 1 d . . . O5 O -0.1518(6) 0.1826(2) -0.0027(5) 0.0363(11) Uani 1 1 d . . . C5 C 0.1278(6) 0.3684(3) 0.1551(6) 0.0202(11) Uani 1 1 d . . . O6 O 0.0369(5) 0.1182(2) 0.1551(5) 0.0289(9) Uani 1 1 d . . . C6 C 0.0342(7) 0.3085(3) 0.0978(7) 0.0260(12) Uani 1 1 d . . . H6 H -0.0615 0.3129 0.0163 0.031 Uiso 1 1 calc R . . O7 O 0.3255(5) 0.4833(2) 0.3400(5) 0.0309(10) Uani 1 1 d . . . C7 C 0.0827(7) 0.2424(3) 0.1614(7) 0.0249(12) Uani 1 1 d . . . O8 O 0.5320(5) 0.4080(2) 0.3883(5) 0.0327(10) Uani 1 1 d . . . C8 C 0.2235(8) 0.2357(3) 0.2859(8) 0.0351(15) Uani 1 1 d . . . H8 H 0.2549 0.1918 0.3310 0.042 Uiso 1 1 calc R . . O9 O 0.3554(17) 0.7645(7) 0.3009(14) 0.160(5) Uiso 1 1 d . . . C9 C 0.3165(8) 0.2949(3) 0.3421(8) 0.0365(16) Uani 1 1 d . . . H9 H 0.4103 0.2905 0.4259 0.044 Uiso 1 1 calc R . . O10 O 0.5378(12) 0.4105(5) 0.9229(11) 0.111(3) Uiso 1 1 d . . . C10 C 0.2722(7) 0.3610(3) 0.2752(7) 0.0244(12) Uani 1 1 d . . . C11 C 0.3836(7) 0.4226(3) 0.3400(7) 0.0237(12) Uani 1 1 d . . . C12 C -0.0178(7) 0.1782(3) 0.0994(7) 0.0249(12) 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 0.01808(16) 0.01397(15) 0.02488(18) -0.00001(9) 0.00526(12) 0.00009(9) O1 0.075(4) 0.049(3) 0.058(3) 0.018(3) 0.044(3) 0.020(3) C1 0.022(3) 0.014(2) 0.023(3) 0.0025(19) 0.008(2) 0.0009(19) O2 0.031(2) 0.032(3) 0.039(3) 0.0078(19) 0.003(2) -0.0017(18) C2 0.019(2) 0.017(3) 0.020(3) 0.000(2) 0.003(2) -0.001(2) O3 0.024(2) 0.028(2) 0.0190(19) -0.0013(16) 0.0058(16) -0.0037(16) C3 0.024(3) 0.016(2) 0.022(3) 0.003(2) 0.010(2) 0.002(2) O4 0.029(2) 0.048(3) 0.030(2) 0.000(2) 0.007(2) -0.012(2) C4 0.023(3) 0.015(2) 0.024(3) -0.001(2) 0.004(2) -0.001(2) O5 0.036(2) 0.020(2) 0.042(3) 0.0033(19) -0.001(2) -0.0054(18) C5 0.020(3) 0.019(3) 0.023(3) 0.004(2) 0.009(2) 0.000(2) O6 0.028(2) 0.017(2) 0.036(2) -0.0031(17) 0.0038(19) -0.0037(16) C6 0.022(3) 0.023(3) 0.027(3) 0.000(2) 0.001(2) -0.001(2) O7 0.032(2) 0.019(2) 0.043(3) -0.0081(18) 0.014(2) -0.0023(17) C7 0.028(3) 0.017(3) 0.028(3) 0.001(2) 0.007(2) -0.003(2) O8 0.019(2) 0.028(2) 0.046(3) -0.0086(19) 0.0031(19) -0.0035(17) C8 0.037(4) 0.016(3) 0.040(4) 0.008(3) -0.002(3) 0.001(3) C9 0.032(3) 0.019(3) 0.042(4) 0.002(3) -0.011(3) 0.000(2) C10 0.021(3) 0.020(3) 0.029(3) 0.000(2) 0.004(2) -0.003(2) C11 0.025(3) 0.020(3) 0.024(3) -0.003(2) 0.006(2) -0.004(2) C12 0.027(3) 0.018(3) 0.029(3) -0.002(2) 0.008(2) -0.005(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 O8 2.298(4) 1_455 ? Gd1 O7 2.344(4) 3_566 ? Gd1 O1 2.441(5) . ? Gd1 O2 2.445(4) . ? Gd1 O6 2.460(4) 4_566 ? Gd1 O3 2.476(4) 3_566 ? Gd1 O5 2.524(4) 4_566 ? Gd1 O3 2.547(4) . ? Gd1 O4 2.618(5) . ? Gd1 C12 2.866(6) 4_566 ? Gd1 C1 2.955(6) . ? O1 H1B 0.9472 . ? O1 H1A 0.9696 . ? C1 O4 1.253(7) . ? C1 O3 1.278(7) . ? C1 C2 1.483(8) . ? O2 H2A 0.9605 . ? O2 H2B 0.8454 . ? C2 C3 1.387(7) . ? C2 C4 1.410(8) . ? O3 Gd1 2.476(4) 3_566 ? C3 C4 1.382(8) 3_565 ? C3 H3 0.9300 . ? C4 C3 1.382(8) 3_565 ? C4 C5 1.500(7) . ? O5 C12 1.245(7) . ? O5 Gd1 2.524(4) 4_565 ? C5 C10 1.390(8) . ? C5 C6 1.399(8) . ? O6 C12 1.275(7) . ? O6 Gd1 2.460(4) 4_565 ? C6 C7 1.389(8) . ? C6 H6 0.9300 . ? O7 C11 1.258(7) . ? O7 Gd1 2.344(4) 3_566 ? C7 C8 1.390(8) . ? C7 C12 1.501(7) . ? O8 C11 1.260(7) . ? O8 Gd1 2.298(4) 1_655 ? C8 C9 1.384(9) . ? C8 H8 0.9300 . ? C9 C10 1.395(8) . ? C9 H9 0.9300 . ? C10 C11 1.513(8) . ? C12 Gd1 2.866(6) 4_565 ? 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 O8 Gd1 O7 86.30(16) 1_455 3_566 ? O8 Gd1 O1 79.0(2) 1_455 . ? O7 Gd1 O1 67.03(18) 3_566 . ? O8 Gd1 O2 83.78(16) 1_455 . ? O7 Gd1 O2 73.93(16) 3_566 . ? O1 Gd1 O2 138.01(18) . . ? O8 Gd1 O6 131.01(15) 1_455 4_566 ? O7 Gd1 O6 116.98(15) 3_566 4_566 ? O1 Gd1 O6 73.09(17) . 4_566 ? O2 Gd1 O6 141.92(15) . 4_566 ? O8 Gd1 O3 156.03(15) 1_455 3_566 ? O7 Gd1 O3 78.83(14) 3_566 3_566 ? O1 Gd1 O3 111.49(18) . 3_566 ? O2 Gd1 O3 74.13(15) . 3_566 ? O6 Gd1 O3 72.88(14) 4_566 3_566 ? O8 Gd1 O5 80.91(15) 1_455 4_566 ? O7 Gd1 O5 136.29(16) 3_566 4_566 ? O1 Gd1 O5 69.54(18) . 4_566 ? O2 Gd1 O5 144.36(16) . 4_566 ? O6 Gd1 O5 51.96(14) 4_566 4_566 ? O3 Gd1 O5 122.68(15) 3_566 4_566 ? O8 Gd1 O3 121.74(15) 1_455 . ? O7 Gd1 O3 136.35(14) 3_566 . ? O1 Gd1 O3 144.20(16) . . ? O2 Gd1 O3 76.68(15) . . ? O6 Gd1 O3 71.53(14) 4_566 . ? O3 Gd1 O3 62.40(16) 3_566 . ? O5 Gd1 O3 84.41(15) 4_566 . ? O8 Gd1 O4 71.49(15) 1_455 . ? O7 Gd1 O4 139.28(16) 3_566 . ? O1 Gd1 O4 136.30(18) . . ? O2 Gd1 O4 70.17(17) . . ? O6 Gd1 O4 103.15(15) 4_566 . ? O3 Gd1 O4 108.44(14) 3_566 . ? O5 Gd1 O4 74.49(16) 4_566 . ? O3 Gd1 O4 50.27(13) . . ? O8 Gd1 C12 105.43(16) 1_455 4_566 ? O7 Gd1 C12 129.69(16) 3_566 4_566 ? O1 Gd1 C12 67.69(18) . 4_566 ? O2 Gd1 C12 154.30(17) . 4_566 ? O6 Gd1 C12 26.32(15) 4_566 4_566 ? O3 Gd1 C12 98.53(16) 3_566 4_566 ? O5 Gd1 C12 25.71(15) 4_566 4_566 ? O3 Gd1 C12 78.13(16) . 4_566 ? O4 Gd1 C12 89.73(16) . 4_566 ? O8 Gd1 C1 96.32(17) 1_455 . ? O7 Gd1 C1 142.15(15) 3_566 . ? O1 Gd1 C1 150.58(17) . . ? O2 Gd1 C1 68.88(15) . . ? O6 Gd1 C1 89.45(15) 4_566 . ? O3 Gd1 C1 84.48(14) 3_566 . ? O5 Gd1 C1 81.05(15) 4_566 . ? O3 Gd1 C1 25.51(14) . . ? O4 Gd1 C1 25.05(15) . . ? C12 Gd1 C1 86.08(16) 4_566 . ? Gd1 O1 H1B 103.6 . . ? Gd1 O1 H1A 112.5 . . ? H1B O1 H1A 131.6 . . ? O4 C1 O3 120.3(5) . . ? O4 C1 C2 122.3(5) . . ? O3 C1 C2 117.3(5) . . ? O4 C1 Gd1 62.2(3) . . ? O3 C1 Gd1 59.1(3) . . ? C2 C1 Gd1 164.8(4) . . ? Gd1 O2 H2A 132.0 . . ? Gd1 O2 H2B 91.7 . . ? H2A O2 H2B 134.8 . . ? C3 C2 C4 120.1(5) . . ? C3 C2 C1 119.9(5) . . ? C4 C2 C1 119.6(5) . . ? C1 O3 Gd1 134.5(3) . 3_566 ? C1 O3 Gd1 95.4(3) . . ? Gd1 O3 Gd1 117.60(16) 3_566 . ? C4 C3 C2 122.0(5) 3_565 . ? C4 C3 H3 119.0 3_565 . ? C2 C3 H3 119.0 . . ? C1 O4 Gd1 92.7(4) . . ? C3 C4 C2 117.9(5) 3_565 . ? C3 C4 C5 122.0(5) 3_565 . ? C2 C4 C5 120.0(5) . . ? C12 O5 Gd1 92.7(3) . 4_565 ? C10 C5 C6 119.2(5) . . ? C10 C5 C4 123.6(5) . . ? C6 C5 C4 117.2(5) . . ? C12 O6 Gd1 94.9(3) . 4_565 ? C7 C6 C5 120.8(5) . . ? C7 C6 H6 119.6 . . ? C5 C6 H6 119.6 . . ? C11 O7 Gd1 140.2(4) . 3_566 ? C6 C7 C8 119.9(5) . . ? C6 C7 C12 120.6(5) . . ? C8 C7 C12 119.4(5) . . ? C11 O8 Gd1 147.0(4) . 1_655 ? C9 C8 C7 119.3(6) . . ? C9 C8 H8 120.4 . . ? C7 C8 H8 120.4 . . ? C8 C9 C10 121.2(6) . . ? C8 C9 H9 119.4 . . ? C10 C9 H9 119.4 . . ? C5 C10 C9 119.5(5) . . ? C5 C10 C11 122.6(5) . . ? C9 C10 C11 117.9(5) . . ? O7 C11 O8 124.8(5) . . ? O7 C11 C10 119.7(5) . . ? O8 C11 C10 115.4(5) . . ? O5 C12 O6 120.1(5) . . ? O5 C12 C7 121.7(5) . . ? O6 C12 C7 118.2(5) . . ? O5 C12 Gd1 61.6(3) . 4_565 ? O6 C12 Gd1 58.8(3) . 4_565 ? C7 C12 Gd1 173.6(4) . 4_565 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.551 _refine_diff_density_min -1.172 _refine_diff_density_rms 0.181 ###END data_c:complex_4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H18 Eu N0 O16' _chemical_formula_weight 714.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Eu' 'Eu' -8.9294 11.1857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 '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' _symmetry_cell_setting 'triclinic' _symmetry_space_group_name_H-M 'p-1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.0981(4) _cell_length_b 12.3000(5) _cell_length_c 13.3240(6) _cell_angle_alpha 77.141(4) _cell_angle_beta 77.071(3) _cell_angle_gamma 79.576(3) _cell_volume 1711.71(12) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8700 _cell_measurement_theta_min 3.4540 _cell_measurement_theta_max 73.3740 _exptl_crystal_description 'block' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.386 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 706 _exptl_absorpt_coefficient_mu 13.674 _exptl_absorpt_correction_type sphere _exptl_absorpt_correction_T_min 0.1707 _exptl_absorpt_correction_T_max 0.1707 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type 'CuK\a' _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator 'mirror' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.5594 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12804 _diffrn_reflns_av_R_equivalents 0.0238 _diffrn_reflns_av_sigmaI/netI 0.0320 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.47 _diffrn_reflns_theta_max 71.00 _reflns_number_total 6548 _reflns_number_gt 6250 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlisPro, Agilent Technologies' _computing_cell_refinement 'CrysAlisPro, Agilent Technologies' _computing_data_reduction 'CrysAlisPro, Agilent Technologies' _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^)+(0.0656P)^2^+4.9504P] 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 6548 _refine_ls_number_parameters 388 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0453 _refine_ls_R_factor_gt 0.0441 _refine_ls_wR_factor_ref 0.1159 _refine_ls_wR_factor_gt 0.1148 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.086 _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 0.32950(2) 0.382998(18) 0.703022(19) 0.01604(10) Uani 1 1 d . . . O1 O 1.0773(3) -0.1310(3) 0.3749(3) 0.0233(7) Uani 1 1 d . . . O2 O 1.1836(3) 0.0154(3) 0.3381(2) 0.0194(6) Uani 1 1 d . . . H2 H 1.2473 -0.0352 0.3349 0.029 Uiso 1 1 d R . . O3 O 0.9657(4) 0.4037(3) 0.3206(4) 0.0522(13) Uani 1 1 d . . . O4 O 0.7591(3) 0.4286(3) 0.3375(3) 0.0274(7) Uani 1 1 d U . . O5 O 0.4633(3) 0.2525(3) 0.6106(3) 0.0297(8) Uani 1 1 d . . . O6 O 0.6343(3) 0.1464(3) 0.6528(2) 0.0230(7) Uani 1 1 d . . . O7 O 0.4649(3) 0.2771(2) 0.8322(2) 0.0174(6) Uani 1 1 d . . . O8 O 0.3071(3) 0.1985(2) 0.8218(3) 0.0217(7) Uani 1 1 d . . . O9 O 0.0573(3) 0.4035(3) 1.0245(3) 0.0309(8) Uani 1 1 d . . . O10 O -0.1276(3) 0.3491(3) 1.1014(3) 0.0311(8) Uani 1 1 d . . . O11 O -0.1736(3) -0.0454(3) 1.1718(2) 0.0193(6) Uani 1 1 d . . . H11 H -0.2146 -0.1001 1.1785 0.029 Uiso 1 1 d R . . O12 O -0.0081(3) -0.1798(2) 1.1536(3) 0.0234(7) Uani 1 1 d . . . O13 O 0.5100(4) 0.4721(4) 0.6436(6) 0.088(2) Uani 1 1 d . . . O14 O 0.1102(4) 0.3748(3) 0.7577(5) 0.0648(16) Uani 1 1 d . . . O15 O 0.2832(5) 0.4598(4) 0.8628(4) 0.0551(13) Uani 1 1 d . . . O16A O 0.3721(11) 0.4703(10) 0.5137(9) 0.030(2) Uani 0.30 1 d PU . . O16B O 0.2720(7) 0.3826(7) 0.5404(6) 0.0355(16) Uani 0.50 1 d PU . . O16C O 0.2267(14) 0.3012(15) 0.5937(12) 0.024(3) Uani 0.20 1 d P . . C1 C 1.0798(4) -0.0304(3) 0.3632(3) 0.0150(8) Uani 1 1 d . . . C2 C 0.8500(4) 0.0117(3) 0.4128(3) 0.0135(8) Uani 1 1 d . . . H2A H 0.8476 -0.0671 0.4261 0.016 Uiso 1 1 calc R . . C3 C 0.9640(4) 0.0521(3) 0.3764(3) 0.0135(8) Uani 1 1 d . . . C4 C 0.9690(4) 0.1679(3) 0.3547(3) 0.0161(8) Uani 1 1 d . . . H4 H 1.0470 0.1955 0.3306 0.019 Uiso 1 1 calc R . . C5 C 0.8599(4) 0.2419(3) 0.3683(3) 0.0167(8) Uani 1 1 d . . . C6 C 0.7450(4) 0.2010(3) 0.4070(3) 0.0149(8) Uani 1 1 d . . . H6 H 0.6704 0.2524 0.4174 0.018 Uiso 1 1 calc R . . C7 C 0.7390(4) 0.0847(3) 0.4304(3) 0.0142(8) Uani 1 1 d . . . C8 C 0.6170(4) 0.0412(3) 0.4695(3) 0.0146(8) Uani 1 1 d . . . C9 C 0.5239(4) 0.0827(3) 0.5474(3) 0.0148(8) Uani 1 1 d . . . C10 C 0.5435(4) 0.1663(3) 0.6082(3) 0.0160(8) Uani 1 1 d . . . C11 C 0.4089(4) 0.0424(3) 0.5755(3) 0.0151(8) Uani 1 1 d . . . H11A H 0.3461 0.0728 0.6270 0.018 Uiso 1 1 calc R . . C12 C 0.8617(4) 0.3680(4) 0.3396(4) 0.0248(10) Uani 1 1 d . . . C13 C -0.0523(4) -0.0816(4) 1.1503(3) 0.0163(8) Uani 1 1 d . . . C14 C 0.1542(4) -0.0151(3) 1.0873(3) 0.0127(7) Uani 1 1 d . . . H14 H 0.1897 -0.0918 1.0898 0.015 Uiso 1 1 calc R . . C15 C 0.0258(4) 0.0119(3) 1.1180(3) 0.0131(7) Uani 1 1 d . . . C16 C -0.0264(4) 0.1241(3) 1.1133(3) 0.0127(7) Uani 1 1 d . . . H16 H -0.1141 0.1426 1.1342 0.015 Uiso 1 1 calc R . . C17 C 0.0476(4) 0.2090(3) 1.0787(3) 0.0147(8) Uani 1 1 d . . . C18 C 0.1762(4) 0.1816(3) 1.0492(3) 0.0135(8) Uani 1 1 d . . . H18 H 0.2271 0.2401 1.0263 0.016 Uiso 1 1 calc R . . C19 C 0.2320(4) 0.0695(3) 1.0526(3) 0.0124(7) Uani 1 1 d . . . C20 C 0.3684(4) 0.0368(3) 1.0220(3) 0.0129(7) Uani 1 1 d . . . C21 C 0.4470(4) 0.0952(3) 0.9368(3) 0.0139(8) Uani 1 1 d . . . C22 C 0.4036(4) 0.1966(3) 0.8601(3) 0.0150(8) Uani 1 1 d . . . C23 C 0.5746(4) 0.0581(3) 0.9166(3) 0.0141(8) Uani 1 1 d . . . H23 H 0.6255 0.0988 0.8586 0.017 Uiso 1 1 calc R . . C24 C -0.0145(4) 0.3284(3) 1.0688(3) 0.0181(8) 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 0.01706(14) 0.00357(13) 0.02277(15) 0.00082(9) -0.00161(9) 0.00383(9) O1 0.0171(15) 0.0135(15) 0.0404(19) -0.0095(13) -0.0084(13) 0.0044(12) O2 0.0147(14) 0.0176(15) 0.0218(15) 0.0008(12) -0.0030(11) 0.0028(12) O3 0.037(2) 0.0130(17) 0.106(4) 0.013(2) -0.031(2) -0.0086(16) O4 0.0257(13) 0.0136(13) 0.0369(14) 0.0026(11) -0.0043(12) 0.0012(11) O5 0.0383(19) 0.0166(16) 0.0361(19) -0.0152(14) -0.0160(15) 0.0151(14) O6 0.0231(16) 0.0222(16) 0.0259(16) -0.0116(13) -0.0083(13) 0.0047(13) O7 0.0186(14) 0.0068(13) 0.0235(15) 0.0035(11) -0.0047(12) 0.0000(11) O8 0.0179(15) 0.0098(14) 0.0353(17) 0.0101(12) -0.0141(13) -0.0029(11) O9 0.0207(16) 0.0091(15) 0.051(2) 0.0021(14) 0.0058(15) 0.0026(13) O10 0.0152(16) 0.0143(16) 0.057(2) -0.0077(15) 0.0015(15) 0.0055(12) O11 0.0141(14) 0.0168(15) 0.0268(15) -0.0028(12) -0.0004(12) -0.0075(11) O12 0.0222(16) 0.0110(15) 0.0360(18) 0.0004(13) -0.0054(13) -0.0061(12) O13 0.033(2) 0.022(2) 0.187(7) 0.004(3) 0.001(3) -0.0039(19) O14 0.030(2) 0.022(2) 0.125(5) 0.020(2) -0.014(2) -0.0031(17) O15 0.077(3) 0.036(2) 0.053(3) -0.029(2) -0.032(2) 0.039(2) O16A 0.029(3) 0.028(3) 0.029(3) -0.0040(19) -0.0020(19) -0.0006(19) O16B 0.034(2) 0.040(2) 0.032(2) -0.0060(17) -0.0125(17) 0.0036(17) O16C 0.016(7) 0.038(9) 0.022(8) -0.006(7) -0.014(6) -0.002(7) C1 0.016(2) 0.015(2) 0.0130(18) -0.0011(15) -0.0070(15) 0.0023(16) C2 0.018(2) 0.0071(18) 0.0136(18) -0.0027(14) -0.0038(15) 0.0036(15) C3 0.019(2) 0.0103(18) 0.0110(17) -0.0015(14) -0.0056(15) 0.0021(15) C4 0.017(2) 0.013(2) 0.0160(19) 0.0043(15) -0.0073(15) -0.0004(16) C5 0.023(2) 0.0076(19) 0.018(2) 0.0013(15) -0.0086(16) 0.0022(16) C6 0.021(2) 0.0062(18) 0.0149(18) -0.0001(14) -0.0036(15) 0.0025(15) C7 0.019(2) 0.0092(18) 0.0133(18) -0.0005(14) -0.0045(15) 0.0019(15) C8 0.0165(19) 0.0074(18) 0.0158(19) -0.0004(14) -0.0015(15) 0.0044(15) C9 0.0164(19) 0.0068(18) 0.0194(19) -0.0020(15) -0.0040(16) 0.0031(15) C10 0.019(2) 0.0080(18) 0.0178(19) -0.0023(15) 0.0002(16) 0.0004(15) C11 0.0160(19) 0.0082(18) 0.0173(19) -0.0015(15) -0.0011(15) 0.0046(15) C12 0.026(2) 0.009(2) 0.036(3) 0.0033(18) -0.011(2) 0.0023(17) C13 0.020(2) 0.015(2) 0.0139(18) -0.0002(15) -0.0051(15) -0.0032(16) C14 0.0163(19) 0.0058(17) 0.0155(18) -0.0008(14) -0.0064(15) 0.0027(15) C15 0.0164(19) 0.0097(18) 0.0134(18) -0.0029(14) -0.0034(15) -0.0006(15) C16 0.0083(17) 0.015(2) 0.0123(17) -0.0021(15) -0.0004(14) 0.0016(15) C17 0.0155(19) 0.0072(18) 0.0197(19) -0.0001(15) -0.0040(15) 0.0009(15) C18 0.0142(19) 0.0064(18) 0.0183(19) 0.0011(15) -0.0031(15) -0.0016(15) C19 0.0121(18) 0.0065(17) 0.0175(18) 0.0010(14) -0.0054(15) 0.0008(14) C20 0.0133(18) 0.0054(17) 0.0197(19) -0.0008(15) -0.0058(15) 0.0007(14) C21 0.0133(19) 0.0066(17) 0.021(2) -0.0004(15) -0.0049(15) 0.0001(14) C22 0.0156(19) 0.0077(18) 0.0189(19) 0.0001(15) -0.0028(15) 0.0017(15) C23 0.0137(19) 0.0074(18) 0.0197(19) 0.0004(15) -0.0025(15) -0.0020(15) C24 0.018(2) 0.0085(19) 0.024(2) -0.0019(16) -0.0017(17) 0.0037(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 Eu1 O4 2.342(3) 2_666 ? Eu1 O5 2.344(3) . ? Eu1 O13 2.354(5) . ? Eu1 O14 2.393(4) . ? Eu1 O16B 2.393(7) . ? Eu1 O15 2.432(4) . ? Eu1 O8 2.479(3) . ? Eu1 O16A 2.487(11) . ? Eu1 O16C 2.499(15) . ? Eu1 O7 2.523(3) . ? Eu1 C22 2.876(4) . ? O1 C1 1.217(5) . ? O2 C1 1.317(5) . ? O2 H2 0.8534 . ? O3 C12 1.263(6) . ? O4 C12 1.245(6) . ? O4 Eu1 2.342(3) 2_666 ? O5 C10 1.256(5) . ? O6 C10 1.242(5) . ? O7 C22 1.245(5) . ? O8 C22 1.280(5) . ? O9 C24 1.285(5) . ? O10 C24 1.232(5) . ? O11 C13 1.327(5) . ? O11 H11 0.8566 . ? O12 C13 1.213(5) . ? O16A O16B 1.616(14) . ? O16B O16C 1.210(18) . ? C1 C3 1.490(5) . ? C2 C3 1.389(6) . ? C2 C7 1.394(6) . ? C2 H2A 0.9500 . ? C3 C4 1.397(6) . ? C4 C5 1.379(6) . ? C4 H4 0.9500 . ? C5 C6 1.403(6) . ? C5 C12 1.515(6) . ? C6 C7 1.405(5) . ? C6 H6 0.9500 . ? C7 C8 1.487(6) . ? C8 C11 1.400(6) 2_656 ? C8 C9 1.404(6) . ? C9 C11 1.395(6) . ? C9 C10 1.514(6) . ? C11 C8 1.400(6) 2_656 ? C11 H11A 0.9500 . ? C13 C15 1.494(6) . ? C14 C15 1.392(6) . ? C14 C19 1.406(5) . ? C14 H14 0.9500 . ? C15 C16 1.390(6) . ? C16 C17 1.380(6) . ? C16 H16 0.9500 . ? C17 C18 1.392(6) . ? C17 C24 1.496(5) . ? C18 C19 1.401(5) . ? C18 H18 0.9500 . ? C19 C20 1.481(5) . ? C20 C23 1.404(5) 2_657 ? C20 C21 1.410(6) . ? C21 C23 1.391(6) . ? C21 C22 1.505(5) . ? C23 C20 1.404(5) 2_657 ? C23 H23 0.9500 . ? 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 O4 Eu1 O5 136.13(12) 2_666 . ? O4 Eu1 O13 79.17(14) 2_666 . ? O5 Eu1 O13 78.83(18) . . ? O4 Eu1 O14 76.74(13) 2_666 . ? O5 Eu1 O14 122.21(16) . . ? O13 Eu1 O14 155.57(16) . . ? O4 Eu1 O16B 80.2(2) 2_666 . ? O5 Eu1 O16B 67.5(2) . . ? O13 Eu1 O16B 101.1(3) . . ? O14 Eu1 O16B 78.8(2) . . ? O4 Eu1 O15 72.21(13) 2_666 . ? O5 Eu1 O15 144.93(12) . . ? O13 Eu1 O15 90.4(2) . . ? O14 Eu1 O15 78.5(2) . . ? O16B Eu1 O15 147.5(2) . . ? O4 Eu1 O8 145.75(11) 2_666 . ? O5 Eu1 O8 75.66(12) . . ? O13 Eu1 O8 127.74(15) . . ? O14 Eu1 O8 73.51(12) . . ? O16B Eu1 O8 109.8(2) . . ? O15 Eu1 O8 85.46(14) . . ? O4 Eu1 O16A 65.0(3) 2_666 . ? O5 Eu1 O16A 71.2(3) . . ? O13 Eu1 O16A 63.8(3) . . ? O14 Eu1 O16A 108.6(3) . . ? O16B Eu1 O16A 38.6(3) . . ? O15 Eu1 O16A 133.0(3) . . ? O8 Eu1 O16A 141.5(3) . . ? O4 Eu1 O16C 98.8(4) 2_666 . ? O5 Eu1 O16C 65.8(4) . . ? O13 Eu1 O16C 126.0(4) . . ? O14 Eu1 O16C 62.5(4) . . ? O16B Eu1 O16C 28.5(4) . . ? O15 Eu1 O16C 141.0(4) . . ? O8 Eu1 O16C 82.3(4) . . ? O16A Eu1 O16C 66.7(5) . . ? O4 Eu1 O7 133.64(11) 2_666 . ? O5 Eu1 O7 77.15(11) . . ? O13 Eu1 O7 78.34(18) . . ? O14 Eu1 O7 116.21(15) . . ? O16B Eu1 O7 143.92(19) . . ? O15 Eu1 O7 67.98(11) . . ? O8 Eu1 O7 51.95(9) . . ? O16A Eu1 O7 134.2(3) . . ? O16C Eu1 O7 127.1(4) . . ? O4 Eu1 C22 147.89(12) 2_666 . ? O5 Eu1 C22 74.34(12) . . ? O13 Eu1 C22 102.67(17) . . ? O14 Eu1 C22 95.63(14) . . ? O16B Eu1 C22 129.5(2) . . ? O15 Eu1 C22 75.72(12) . . ? O8 Eu1 C22 26.35(11) . . ? O16A Eu1 C22 144.8(3) . . ? O16C Eu1 C22 105.2(4) . . ? O7 Eu1 C22 25.60(10) . . ? C1 O2 H2 110.7 . . ? C12 O4 Eu1 141.8(3) . 2_666 ? C10 O5 Eu1 150.6(3) . . ? C22 O7 Eu1 93.2(2) . . ? C22 O8 Eu1 94.4(2) . . ? C13 O11 H11 109.3 . . ? O16B O16A Eu1 67.5(5) . . ? O16C O16B O16A 151.9(10) . . ? O16C O16B Eu1 80.6(8) . . ? O16A O16B Eu1 73.8(5) . . ? O16B O16C Eu1 70.9(8) . . ? O1 C1 O2 123.7(4) . . ? O1 C1 C3 122.3(4) . . ? O2 C1 C3 114.0(3) . . ? C3 C2 C7 121.2(4) . . ? C3 C2 H2A 119.4 . . ? C7 C2 H2A 119.4 . . ? C2 C3 C4 120.2(4) . . ? C2 C3 C1 118.6(4) . . ? C4 C3 C1 121.2(4) . . ? C5 C4 C3 119.6(4) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? C4 C5 C6 120.2(4) . . ? C4 C5 C12 120.8(4) . . ? C6 C5 C12 119.0(4) . . ? C5 C6 C7 120.7(4) . . ? C5 C6 H6 119.7 . . ? C7 C6 H6 119.7 . . ? C2 C7 C6 118.1(4) . . ? C2 C7 C8 121.1(4) . . ? C6 C7 C8 120.8(4) . . ? C11 C8 C9 117.9(4) 2_656 . ? C11 C8 C7 118.9(4) 2_656 . ? C9 C8 C7 123.1(4) . . ? C11 C9 C8 119.8(4) . . ? C11 C9 C10 116.9(4) . . ? C8 C9 C10 123.2(4) . . ? O6 C10 O5 124.2(4) . . ? O6 C10 C9 119.6(4) . . ? O5 C10 C9 116.2(4) . . ? C9 C11 C8 122.3(4) . 2_656 ? C9 C11 H11A 118.9 . . ? C8 C11 H11A 118.9 2_656 . ? O4 C12 O3 125.0(4) . . ? O4 C12 C5 116.9(4) . . ? O3 C12 C5 118.1(4) . . ? O12 C13 O11 124.3(4) . . ? O12 C13 C15 122.8(4) . . ? O11 C13 C15 112.9(3) . . ? C15 C14 C19 120.9(3) . . ? C15 C14 H14 119.6 . . ? C19 C14 H14 119.6 . . ? C16 C15 C14 119.6(4) . . ? C16 C15 C13 122.1(4) . . ? C14 C15 C13 118.2(4) . . ? C17 C16 C15 120.8(4) . . ? C17 C16 H16 119.6 . . ? C15 C16 H16 119.6 . . ? C16 C17 C18 119.5(4) . . ? C16 C17 C24 118.3(4) . . ? C18 C17 C24 122.1(4) . . ? C17 C18 C19 121.3(4) . . ? C17 C18 H18 119.3 . . ? C19 C18 H18 119.3 . . ? C18 C19 C14 117.9(4) . . ? C18 C19 C20 123.0(3) . . ? C14 C19 C20 119.0(3) . . ? C23 C20 C21 116.8(4) 2_657 . ? C23 C20 C19 118.1(4) 2_657 . ? C21 C20 C19 125.1(4) . . ? C23 C21 C20 120.1(4) . . ? C23 C21 C22 115.0(4) . . ? C20 C21 C22 124.9(4) . . ? O7 C22 O8 120.4(4) . . ? O7 C22 C21 119.1(4) . . ? O8 C22 C21 120.4(3) . . ? O7 C22 Eu1 61.2(2) . . ? O8 C22 Eu1 59.3(2) . . ? C21 C22 Eu1 176.3(3) . . ? C21 C23 C20 123.1(4) . 2_657 ? C21 C23 H23 118.5 . . ? C20 C23 H23 118.5 2_657 . ? O10 C24 O9 124.5(4) . . ? O10 C24 C17 120.0(4) . . ? O9 C24 C17 115.5(4) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 71.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 4.920 _refine_diff_density_min -1.089 _refine_diff_density_rms 0.113 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.097 0.500 0.597 577.2 159.5 _platon_squeeze_details ; ; ###END data_c:complex_5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H18 N0 O16 Tb' _chemical_formula_weight 721.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Tb' 'Tb' -9.1472 9.1891 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 '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' _symmetry_cell_setting 'triclinic' _symmetry_space_group_name_H-M 'p-1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.1102(3) _cell_length_b 12.2579(4) _cell_length_c 13.2870(5) _cell_angle_alpha 77.034(3) _cell_angle_beta 76.785(3) _cell_angle_gamma 79.413(3) _cell_volume 1699.88(10) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8881 _cell_measurement_theta_min 3.4790 _cell_measurement_theta_max 74.7560 _exptl_crystal_description 'block' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.409 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 710 _exptl_absorpt_coefficient_mu 10.793 _exptl_absorpt_correction_type sphere _exptl_absorpt_correction_T_min 0.2214 _exptl_absorpt_correction_T_max 0.2214 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type 'CuK\a' _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator 'mirror' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.5594 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13166 _diffrn_reflns_av_R_equivalents 0.0289 _diffrn_reflns_av_sigmaI/netI 0.0402 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.48 _diffrn_reflns_theta_max 74.79 _reflns_number_total 6755 _reflns_number_gt 6365 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlisPro, Agilent Technologies' _computing_cell_refinement 'CrysAlisPro, Agilent Technologies' _computing_data_reduction 'CrysAlisPro, Agilent Technologies' _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^)+(0.0662P)^2^+0.4696P] 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 6755 _refine_ls_number_parameters 388 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0390 _refine_ls_R_factor_gt 0.0374 _refine_ls_wR_factor_ref 0.1040 _refine_ls_wR_factor_gt 0.1025 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.123 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tb1 Tb 0.329972(17) 0.382949(14) 0.703537(15) 0.01425(8) Uani 1 1 d U . . O1 O 1.0781(2) -0.1318(2) 0.3738(2) 0.0219(6) Uani 1 1 d . . . C1 C 1.0799(3) -0.0308(3) 0.3625(3) 0.0144(6) Uani 1 1 d . . . O2 O 1.1844(2) 0.0155(2) 0.33765(19) 0.0181(5) Uani 1 1 d . . . C2 C 0.8501(3) 0.0116(3) 0.4127(2) 0.0122(6) Uani 1 1 d . . . H2 H 0.8479 -0.0676 0.4258 0.015 Uiso 1 1 calc R . . O3 O 0.9639(3) 0.4055(2) 0.3229(3) 0.0444(9) Uani 1 1 d . . . C3 C 0.9641(3) 0.0524(3) 0.3767(2) 0.0129(6) Uani 1 1 d . . . O4 O 0.7571(3) 0.4306(2) 0.3382(2) 0.0259(6) Uani 1 1 d U . . C4 C 0.9689(3) 0.1687(3) 0.3550(3) 0.0143(6) Uani 1 1 d . . . H4 H 1.0469 0.1966 0.3310 0.017 Uiso 1 1 calc R . . O5 O 0.4619(3) 0.2533(2) 0.6109(2) 0.0268(6) Uani 1 1 d . . . C5 C 0.8588(3) 0.2429(3) 0.3689(3) 0.0156(7) Uani 1 1 d . . . O6 O 0.6331(2) 0.1472(2) 0.6530(2) 0.0214(5) Uani 1 1 d . . . C6 C 0.7449(3) 0.2013(3) 0.4073(3) 0.0142(7) Uani 1 1 d . . . H6 H 0.6701 0.2527 0.4181 0.017 Uiso 1 1 calc R . . O7 O 0.4652(2) 0.27753(19) 0.83018(19) 0.0161(5) Uani 1 1 d . . . C7 C 0.7390(3) 0.0852(3) 0.4300(3) 0.0135(6) Uani 1 1 d . . . O8 O 0.3068(2) 0.19959(19) 0.8213(2) 0.0195(5) Uani 1 1 d . . . C8 C 0.6175(3) 0.0410(3) 0.4690(3) 0.0133(6) Uani 1 1 d . . . O9 O 0.0569(3) 0.4039(2) 1.0261(3) 0.0318(7) Uani 1 1 d . . . C9 C 0.5236(3) 0.0833(3) 0.5470(3) 0.0129(6) Uani 1 1 d . . . O10 O -0.1290(3) 0.3497(2) 1.1016(3) 0.0297(7) Uani 1 1 d . . . C10 C 0.4086(3) 0.0426(3) 0.5759(3) 0.0145(6) Uani 1 1 d . . . H10 H 0.3459 0.0729 0.6280 0.017 Uiso 1 1 calc R . . O11 O -0.1741(2) -0.0468(2) 1.1727(2) 0.0178(5) Uani 1 1 d . . . C11 C 0.5424(3) 0.1673(3) 0.6082(3) 0.0157(7) Uani 1 1 d . . . O12 O -0.0080(2) -0.1816(2) 1.1537(2) 0.0212(5) Uani 1 1 d . . . C12 C 0.8608(4) 0.3687(3) 0.3414(3) 0.0232(8) Uani 1 1 d . . . O13 O 0.5075(3) 0.4727(3) 0.6348(5) 0.0826(18) Uani 1 1 d . . . C13 C -0.0523(3) -0.0830(3) 1.1505(3) 0.0151(7) Uani 1 1 d . . . O14 O 0.2869(4) 0.4605(3) 0.8597(3) 0.0525(11) Uani 1 1 d . . . C14 C 0.1536(3) -0.0157(3) 1.0872(2) 0.0119(6) Uani 1 1 d . . . H14 H 0.1894 -0.0926 1.0893 0.014 Uiso 1 1 calc R . . O15 O 0.1136(3) 0.3747(3) 0.7554(4) 0.0562(12) Uani 1 1 d . . . C15 C 0.0257(3) 0.0105(3) 1.1184(2) 0.0111(6) Uani 1 1 d . . . C16 C -0.0278(3) 0.1233(3) 1.1142(2) 0.0116(6) Uani 1 1 d . . . H16 H -0.1154 0.1414 1.1360 0.014 Uiso 1 1 calc R . . C17 C 0.0461(3) 0.2087(3) 1.0787(3) 0.0136(6) Uani 1 1 d . . . C18 C 0.1753(3) 0.1813(3) 1.0494(3) 0.0128(6) Uani 1 1 d . . . H18 H 0.2261 0.2401 1.0269 0.015 Uiso 1 1 calc R . . C19 C 0.2313(3) 0.0690(3) 1.0524(2) 0.0113(6) Uani 1 1 d . . . C20 C 0.3685(3) 0.0362(3) 1.0218(3) 0.0127(6) Uani 1 1 d . . . C21 C 0.4256(3) -0.0587(3) 1.0834(3) 0.0125(6) Uani 1 1 d . . . H21 H 0.3745 -0.0998 1.1415 0.015 Uiso 1 1 calc R . . C22 C 0.4037(3) 0.1970(3) 0.8591(3) 0.0131(6) Uani 1 1 d . . . C23 C 0.4475(3) 0.0953(3) 0.9362(3) 0.0129(6) Uani 1 1 d . . . C24 C -0.0154(3) 0.3287(3) 1.0690(3) 0.0181(7) Uani 1 1 d . . . O16B O 0.2709(5) 0.3817(5) 0.5411(4) 0.0223(11) Uani 0.50 1 d PU . . O16C O 0.3728(11) 0.4679(10) 0.5172(9) 0.046(3) Uani 0.30 1 d PU . . O16A O 0.2276(17) 0.3186(17) 0.5890(15) 0.047(4) Uani 0.20 1 d PU . . 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 Tb1 0.01541(13) 0.00229(11) 0.02050(13) 0.00141(7) -0.00105(8) 0.00280(7) O1 0.0186(13) 0.0105(12) 0.0363(15) -0.0081(11) -0.0065(11) 0.0049(10) C1 0.0175(17) 0.0140(16) 0.0103(15) 0.0006(12) -0.0064(13) 0.0022(13) O2 0.0173(12) 0.0148(12) 0.0189(12) 0.0003(9) -0.0025(10) 0.0005(9) C2 0.0185(16) 0.0060(14) 0.0111(15) -0.0011(11) -0.0044(12) 0.0018(12) O3 0.0330(17) 0.0121(14) 0.086(3) 0.0077(15) -0.0223(17) -0.0052(12) C3 0.0209(17) 0.0089(15) 0.0075(14) 0.0004(11) -0.0060(12) 0.0026(13) O4 0.0226(12) 0.0098(10) 0.0374(13) 0.0055(9) -0.0018(10) 0.0004(9) C4 0.0179(17) 0.0083(15) 0.0142(15) 0.0041(12) -0.0057(13) -0.0001(12) O5 0.0338(15) 0.0150(13) 0.0322(15) -0.0119(11) -0.0142(12) 0.0136(11) C5 0.0218(18) 0.0073(15) 0.0153(16) 0.0021(12) -0.0055(13) 0.0009(13) O6 0.0218(13) 0.0178(12) 0.0262(14) -0.0103(10) -0.0084(11) 0.0052(10) C6 0.0199(17) 0.0065(15) 0.0131(15) 0.0006(12) -0.0034(13) 0.0031(12) O7 0.0197(12) 0.0044(10) 0.0227(12) 0.0014(9) -0.0051(10) -0.0019(9) C7 0.0194(17) 0.0075(15) 0.0114(15) -0.0008(11) -0.0029(13) 0.0023(12) O8 0.0161(12) 0.0085(11) 0.0316(14) 0.0102(10) -0.0130(11) -0.0029(9) C8 0.0185(17) 0.0045(14) 0.0133(15) 0.0001(11) -0.0014(13) 0.0035(12) O9 0.0219(14) 0.0081(12) 0.0521(19) 0.0029(12) 0.0072(13) 0.0027(10) C9 0.0149(16) 0.0065(14) 0.0158(16) -0.0022(12) -0.0032(13) 0.0029(12) O10 0.0179(14) 0.0113(13) 0.0530(19) -0.0062(12) 0.0006(13) 0.0061(10) C10 0.0163(16) 0.0077(14) 0.0150(16) 0.0000(12) -0.0008(12) 0.0041(12) O11 0.0147(12) 0.0150(12) 0.0221(13) -0.0023(10) 0.0002(10) -0.0043(9) C11 0.0205(17) 0.0061(14) 0.0161(16) 0.0005(12) 0.0011(13) 0.0000(12) O12 0.0213(13) 0.0088(11) 0.0322(14) 0.0007(10) -0.0048(11) -0.0048(10) C12 0.025(2) 0.0094(16) 0.032(2) 0.0046(14) -0.0078(16) -0.0011(14) O13 0.0256(19) 0.0210(18) 0.180(6) -0.007(2) 0.010(2) -0.0047(14) C13 0.0192(17) 0.0124(16) 0.0135(16) 0.0000(12) -0.0038(13) -0.0038(13) O14 0.072(3) 0.0341(19) 0.054(2) -0.0280(17) -0.033(2) 0.0364(18) C14 0.0146(16) 0.0060(14) 0.0140(15) -0.0011(11) -0.0043(12) 0.0026(12) O15 0.0270(17) 0.0171(15) 0.111(3) 0.0194(18) -0.0161(19) -0.0047(13) C15 0.0143(16) 0.0077(14) 0.0099(14) -0.0009(11) -0.0014(12) -0.0006(12) C16 0.0094(15) 0.0121(15) 0.0106(15) -0.0033(12) 0.0003(12) 0.0035(12) C17 0.0151(16) 0.0065(15) 0.0165(16) -0.0002(12) -0.0031(13) 0.0027(12) C18 0.0148(16) 0.0047(14) 0.0169(16) 0.0020(12) -0.0027(13) -0.0019(12) C19 0.0141(16) 0.0061(14) 0.0131(15) 0.0003(11) -0.0045(12) -0.0005(12) C20 0.0138(16) 0.0049(14) 0.0187(16) -0.0010(12) -0.0043(13) 0.0000(12) C21 0.0144(16) 0.0055(14) 0.0163(16) -0.0002(12) -0.0020(12) -0.0018(12) C22 0.0122(15) 0.0060(14) 0.0186(16) 0.0006(12) -0.0027(13) 0.0013(11) C23 0.0149(16) 0.0045(14) 0.0190(16) 0.0011(12) -0.0072(13) 0.0002(11) C24 0.0196(18) 0.0072(15) 0.0236(18) -0.0025(13) -0.0017(14) 0.0046(13) O16B 0.0180(17) 0.0276(18) 0.0187(17) -0.0029(15) -0.0084(14) 0.0075(15) O16C 0.047(3) 0.043(3) 0.044(3) -0.007(2) -0.006(2) -0.002(2) O16A 0.047(5) 0.049(5) 0.047(5) -0.010(2) -0.012(2) -0.005(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tb1 O4 2.309(3) 2_666 ? Tb1 O5 2.321(2) . ? Tb1 O13 2.336(4) . ? Tb1 O15 2.359(3) . ? Tb1 O14 2.387(3) . ? Tb1 O16B 2.399(5) . ? Tb1 O16A 2.427(18) . ? Tb1 O16C 2.435(12) . ? Tb1 O8 2.453(2) . ? Tb1 O7 2.495(2) . ? Tb1 C22 2.848(3) . ? O1 C1 1.216(4) . ? C1 O2 1.327(4) . ? C1 C3 1.492(4) . ? C2 C3 1.389(5) . ? C2 C7 1.395(4) . ? C2 H2 0.9500 . ? O3 C12 1.260(5) . ? C3 C4 1.399(4) . ? O4 C12 1.261(5) . ? O4 Tb1 2.309(3) 2_666 ? C4 C5 1.387(5) . ? C4 H4 0.9500 . ? O5 C11 1.253(4) . ? C5 C6 1.395(5) . ? C5 C12 1.506(5) . ? O6 C11 1.244(4) . ? C6 C7 1.398(4) . ? C6 H6 0.9500 . ? O7 C22 1.243(4) . ? C7 C8 1.486(5) . ? O8 C22 1.280(4) . ? C8 C10 1.398(5) 2_656 ? C8 C9 1.406(5) . ? O9 C24 1.283(5) . ? C9 C10 1.397(5) . ? C9 C11 1.515(5) . ? O10 C24 1.236(5) . ? C10 C8 1.398(5) 2_656 ? C10 H10 0.9500 . ? O11 C13 1.331(4) . ? O12 C13 1.213(4) . ? C13 C15 1.491(4) . ? C14 C15 1.384(5) . ? C14 C19 1.403(4) . ? C14 H14 0.9500 . ? C15 C16 1.395(4) . ? C16 C17 1.382(5) . ? C16 H16 0.9500 . ? C17 C18 1.397(5) . ? C17 C24 1.494(4) . ? C18 C19 1.399(4) . ? C18 H18 0.9500 . ? C19 C20 1.489(5) . ? C20 C21 1.402(4) . ? C20 C23 1.412(5) . ? C21 C23 1.382(5) 2_657 ? C21 H21 0.9500 . ? C22 C23 1.508(4) . ? C23 C21 1.382(5) 2_657 ? O16B O16A 1.00(2) . ? O16B O16C 1.621(14) . ? 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 O4 Tb1 O5 135.39(10) 2_666 . ? O4 Tb1 O13 78.33(12) 2_666 . ? O5 Tb1 O13 77.76(13) . . ? O4 Tb1 O15 76.83(10) 2_666 . ? O5 Tb1 O15 121.33(13) . . ? O13 Tb1 O15 155.16(12) . . ? O4 Tb1 O14 72.46(11) 2_666 . ? O5 Tb1 O14 145.09(10) . . ? O13 Tb1 O14 92.00(19) . . ? O15 Tb1 O14 80.20(16) . . ? O4 Tb1 O16B 79.80(15) 2_666 . ? O5 Tb1 O16B 67.36(14) . . ? O13 Tb1 O16B 98.7(2) . . ? O15 Tb1 O16B 77.33(18) . . ? O14 Tb1 O16B 147.55(14) . . ? O4 Tb1 O16A 94.1(5) 2_666 . ? O5 Tb1 O16A 67.5(4) . . ? O13 Tb1 O16A 120.7(5) . . ? O15 Tb1 O16A 61.8(5) . . ? O14 Tb1 O16A 141.8(5) . . ? O16B Tb1 O16A 24.0(5) . . ? O4 Tb1 O16C 64.8(3) 2_666 . ? O5 Tb1 O16C 70.7(3) . . ? O13 Tb1 O16C 60.7(3) . . ? O15 Tb1 O16C 108.0(3) . . ? O14 Tb1 O16C 132.5(3) . . ? O16B Tb1 O16C 39.2(3) . . ? O16A Tb1 O16C 63.0(6) . . ? O4 Tb1 O8 146.01(9) 2_666 . ? O5 Tb1 O8 75.80(10) . . ? O13 Tb1 O8 129.82(13) . . ? O15 Tb1 O8 73.56(10) . . ? O14 Tb1 O8 86.28(11) . . ? O16B Tb1 O8 109.11(15) . . ? O16A Tb1 O8 86.5(5) . . ? O16C Tb1 O8 141.2(3) . . ? O4 Tb1 O7 134.25(9) 2_666 . ? O5 Tb1 O7 77.09(8) . . ? O13 Tb1 O7 80.48(15) . . ? O15 Tb1 O7 117.36(11) . . ? O14 Tb1 O7 68.28(9) . . ? O16B Tb1 O7 143.63(13) . . ? O16A Tb1 O7 131.5(5) . . ? O16C Tb1 O7 133.5(3) . . ? O8 Tb1 O7 52.46(8) . . ? O4 Tb1 C22 148.67(10) 2_666 . ? O5 Tb1 C22 74.40(9) . . ? O13 Tb1 C22 104.83(14) . . ? O15 Tb1 C22 96.23(11) . . ? O14 Tb1 C22 76.27(10) . . ? O16B Tb1 C22 129.08(15) . . ? O16A Tb1 C22 109.7(5) . . ? O16C Tb1 C22 144.3(3) . . ? O8 Tb1 C22 26.63(9) . . ? O7 Tb1 C22 25.84(8) . . ? O1 C1 O2 123.4(3) . . ? O1 C1 C3 122.8(3) . . ? O2 C1 C3 113.8(3) . . ? C3 C2 C7 120.9(3) . . ? C3 C2 H2 119.6 . . ? C7 C2 H2 119.6 . . ? C2 C3 C4 120.3(3) . . ? C2 C3 C1 118.3(3) . . ? C4 C3 C1 121.3(3) . . ? C12 O4 Tb1 142.0(2) . 2_666 ? C5 C4 C3 119.3(3) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? C11 O5 Tb1 150.3(2) . . ? C4 C5 C6 120.0(3) . . ? C4 C5 C12 120.4(3) . . ? C6 C5 C12 119.5(3) . . ? C5 C6 C7 121.1(3) . . ? C5 C6 H6 119.4 . . ? C7 C6 H6 119.4 . . ? C22 O7 Tb1 93.16(19) . . ? C2 C7 C6 118.2(3) . . ? C2 C7 C8 120.7(3) . . ? C6 C7 C8 121.1(3) . . ? C22 O8 Tb1 94.17(19) . . ? C10 C8 C9 117.7(3) 2_656 . ? C10 C8 C7 119.5(3) 2_656 . ? C9 C8 C7 122.8(3) . . ? C10 C9 C8 119.9(3) . . ? C10 C9 C11 116.6(3) . . ? C8 C9 C11 123.3(3) . . ? C9 C10 C8 122.4(3) . 2_656 ? C9 C10 H10 118.8 . . ? C8 C10 H10 118.8 2_656 . ? O6 C11 O5 124.3(3) . . ? O6 C11 C9 119.6(3) . . ? O5 C11 C9 116.1(3) . . ? O3 C12 O4 124.2(3) . . ? O3 C12 C5 119.0(3) . . ? O4 C12 C5 116.8(3) . . ? O12 C13 O11 124.1(3) . . ? O12 C13 C15 122.8(3) . . ? O11 C13 C15 113.2(3) . . ? C15 C14 C19 121.3(3) . . ? C15 C14 H14 119.3 . . ? C19 C14 H14 119.3 . . ? C14 C15 C16 119.7(3) . . ? C14 C15 C13 118.7(3) . . ? C16 C15 C13 121.6(3) . . ? C17 C16 C15 120.4(3) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C16 C17 C18 119.5(3) . . ? C16 C17 C24 118.8(3) . . ? C18 C17 C24 121.6(3) . . ? C17 C18 C19 121.3(3) . . ? C17 C18 H18 119.4 . . ? C19 C18 H18 119.4 . . ? C18 C19 C14 117.9(3) . . ? C18 C19 C20 122.9(3) . . ? C14 C19 C20 119.2(3) . . ? C21 C20 C23 116.7(3) . . ? C21 C20 C19 118.2(3) . . ? C23 C20 C19 125.0(3) . . ? C23 C21 C20 123.2(3) 2_657 . ? C23 C21 H21 118.4 2_657 . ? C20 C21 H21 118.4 . . ? O7 C22 O8 120.2(3) . . ? O7 C22 C23 119.0(3) . . ? O8 C22 C23 120.8(3) . . ? O7 C22 Tb1 61.00(17) . . ? O8 C22 Tb1 59.20(16) . . ? C23 C22 Tb1 176.6(2) . . ? C21 C23 C20 120.1(3) 2_657 . ? C21 C23 C22 115.2(3) 2_657 . ? C20 C23 C22 124.7(3) . . ? O10 C24 O9 124.5(3) . . ? O10 C24 C17 119.8(3) . . ? O9 C24 C17 115.7(3) . . ? O16A O16B O16C 150.2(12) . . ? O16A O16B Tb1 79.5(11) . . ? O16C O16B Tb1 71.6(5) . . ? O16B O16C Tb1 69.2(5) . . ? O16B O16A Tb1 76.4(11) . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 74.79 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 2.726 _refine_diff_density_min -1.064 _refine_diff_density_rms 0.108 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.096 0.500 0.596 598.1 169.3 _platon_squeeze_details ; ; ###END data_c:complex_6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H18 Gd N0 O16' _chemical_formula_weight 719.63 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Gd' 'Gd' -8.8380 11.9157 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 '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' _symmetry_cell_setting 'triclinic' _symmetry_space_group_name_H-M 'p-1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.1090(4) _cell_length_b 12.2814(5) _cell_length_c 13.3034(5) _cell_angle_alpha 77.155(4) _cell_angle_beta 77.056(3) _cell_angle_gamma 79.616(3) _cell_volume 1708.32(11) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9033 _cell_measurement_theta_min 3.4630 _cell_measurement_theta_max 73.4140 _exptl_crystal_description 'block' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.399 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 708 _exptl_absorpt_coefficient_mu 13.116 _exptl_absorpt_correction_type sphere _exptl_absorpt_correction_T_min 0.1790 _exptl_absorpt_correction_T_max 0.1790 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type 'CuK\a' _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator 'mirror' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.5594 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12810 _diffrn_reflns_av_R_equivalents 0.0346 _diffrn_reflns_av_sigmaI/netI 0.0412 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.47 _diffrn_reflns_theta_max 70.99 _reflns_number_total 6528 _reflns_number_gt 6283 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlisPro, Agilent Technologies' _computing_cell_refinement 'CrysAlisPro, Agilent Technologies' _computing_data_reduction 'CrysAlisPro, Agilent Technologies' _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^)+(0.0743P)^2^+1.6828P] 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 6528 _refine_ls_number_parameters 388 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0431 _refine_ls_R_factor_gt 0.0422 _refine_ls_wR_factor_ref 0.1138 _refine_ls_wR_factor_gt 0.1127 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.074 _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 0.170412(18) 0.617281(15) 0.296661(16) 0.01614(9) Uani 1 1 d . . . O1 O -0.5774(3) 1.1312(2) 0.6256(2) 0.0237(6) Uani 1 1 d . . . O2 O -0.6834(2) 0.9845(2) 0.6621(2) 0.0194(6) Uani 1 1 d . . . H2 H -0.7492 1.0309 0.6643 0.029 Uiso 1 1 d R . . O3 O -0.4646(3) 0.5957(3) 0.6785(4) 0.0475(10) Uani 1 1 d . . . O4 O -0.2577(3) 0.5707(2) 0.6621(3) 0.0274(7) Uani 1 1 d . . . O5 O 0.0368(3) 0.7478(3) 0.3882(2) 0.0291(7) Uani 1 1 d . . . O6 O -0.1350(3) 0.8533(2) 0.3472(2) 0.0227(6) Uani 1 1 d . . . O7 O 0.0350(2) 0.7228(2) 0.1682(2) 0.0168(5) Uani 1 1 d . . . O8 O 0.1934(3) 0.8010(2) 0.1782(2) 0.0215(6) Uani 1 1 d . . . O9 O 0.4430(3) 0.5964(2) -0.0252(3) 0.0322(8) Uani 1 1 d . . . O10 O 0.6272(3) 0.6508(3) -0.1016(3) 0.0313(8) Uani 1 1 d . . . O11 O 0.6730(2) 1.0458(2) -0.1720(2) 0.0201(6) Uani 1 1 d . . . H11 H 0.7151 1.0998 -0.1816 0.030 Uiso 1 1 d R . . O12 O 0.5079(3) 1.1807(2) -0.1532(2) 0.0231(6) Uani 1 1 d . . . O13 O 0.3883(4) 0.6252(3) 0.2437(4) 0.0626(14) Uani 1 1 d . . . O14 O 0.2161(4) 0.5404(3) 0.1382(3) 0.0535(12) Uani 1 1 d . . . O15 O -0.0085(4) 0.5278(4) 0.3576(6) 0.086(2) Uani 1 1 d . . . O16A O 0.2730(13) 0.6969(15) 0.4065(11) 0.027(3) Uani 0.20 1 d P . . O16B O 0.2263(6) 0.6175(6) 0.4587(5) 0.0353(17) Uani 0.50 1 d P . . O16C O 0.1278(10) 0.5292(10) 0.4853(9) 0.035(2) Uani 0.30 1 d PU . . C1 C -0.5792(3) 1.0305(3) 0.6368(3) 0.0158(7) Uani 1 1 d . . . C2 C -0.3498(3) 0.9884(3) 0.5866(3) 0.0136(7) Uani 1 1 d . . . H2A H -0.3474 1.0674 0.5726 0.016 Uiso 1 1 calc R . . C3 C -0.4642(3) 0.9475(3) 0.6238(3) 0.0136(7) Uani 1 1 d . . . C4 C -0.4688(4) 0.8317(3) 0.6450(3) 0.0160(7) Uani 1 1 d . . . H4 H -0.5466 0.8037 0.6688 0.019 Uiso 1 1 calc R . . C5 C -0.3588(4) 0.7579(3) 0.6310(3) 0.0165(7) Uani 1 1 d . . . C6 C -0.2447(4) 0.7989(3) 0.5928(3) 0.0153(7) Uani 1 1 d . . . H6 H -0.1702 0.7475 0.5822 0.018 Uiso 1 1 calc R . . C7 C -0.2389(4) 0.9149(3) 0.5698(3) 0.0147(7) Uani 1 1 d . . . C8 C -0.1167(4) 0.9590(3) 0.5304(3) 0.0148(7) Uani 1 1 d . . . C9 C -0.0239(3) 0.9172(3) 0.4519(3) 0.0141(7) Uani 1 1 d . . . C10 C -0.0432(4) 0.8335(3) 0.3916(3) 0.0173(8) Uani 1 1 d . . . C11 C 0.0908(4) 0.9583(3) 0.4238(3) 0.0155(7) Uani 1 1 d . . . H11A H 0.1534 0.9289 0.3716 0.019 Uiso 1 1 calc R . . C12 C -0.3613(4) 0.6315(3) 0.6597(4) 0.0254(9) Uani 1 1 d . . . C13 C 0.5516(4) 1.0822(3) -0.1501(3) 0.0164(7) Uani 1 1 d . . . C14 C 0.3456(3) 1.0152(3) -0.0868(3) 0.0133(7) Uani 1 1 d . . . H14 H 0.3100 1.0918 -0.0885 0.016 Uiso 1 1 calc R . . C15 C 0.4740(3) 0.9888(3) -0.1183(3) 0.0144(7) Uani 1 1 d . . . C16 C 0.5267(3) 0.8762(3) -0.1139(3) 0.0135(7) Uani 1 1 d . . . H16 H 0.6142 0.8580 -0.1354 0.016 Uiso 1 1 calc R . . C17 C 0.4523(3) 0.7901(3) -0.0781(3) 0.0148(7) Uani 1 1 d . . . C18 C 0.3239(4) 0.8186(3) -0.0495(3) 0.0143(7) Uani 1 1 d . . . H18 H 0.2727 0.7602 -0.0270 0.017 Uiso 1 1 calc R . . C19 C 0.2680(3) 0.9308(3) -0.0527(3) 0.0130(7) Uani 1 1 d . . . C20 C 0.1317(3) 0.9634(3) -0.0221(3) 0.0142(7) Uani 1 1 d . . . C21 C 0.0526(3) 0.9047(3) 0.0633(3) 0.0135(7) Uani 1 1 d . . . C22 C 0.0966(3) 0.8026(3) 0.1400(3) 0.0149(7) Uani 1 1 d . . . C23 C -0.0743(3) 0.9419(3) 0.0833(3) 0.0130(7) Uani 1 1 d . . . H23 H -0.1251 0.9011 0.1414 0.016 Uiso 1 1 calc R . . C24 C 0.5151(4) 0.6714(3) -0.0689(3) 0.0180(8) 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 0.01866(14) 0.00455(12) 0.01991(14) 0.00188(8) 0.00025(9) 0.00190(8) O1 0.0220(14) 0.0137(14) 0.0350(17) -0.0074(12) -0.0068(12) 0.0035(11) O2 0.0174(13) 0.0176(13) 0.0181(13) 0.0021(11) -0.0020(10) 0.0026(11) O3 0.0373(19) 0.0133(16) 0.088(3) 0.0132(17) -0.024(2) -0.0076(14) O4 0.0264(16) 0.0065(13) 0.0417(18) 0.0075(12) -0.0067(13) 0.0027(11) O5 0.0378(17) 0.0193(15) 0.0312(16) -0.0152(13) -0.0126(14) 0.0146(13) O6 0.0238(14) 0.0195(14) 0.0247(15) -0.0101(12) -0.0053(12) 0.0058(11) O7 0.0166(12) 0.0079(12) 0.0219(13) 0.0030(10) -0.0035(10) 0.0007(10) O8 0.0187(13) 0.0112(13) 0.0304(15) 0.0121(11) -0.0102(12) -0.0049(10) O9 0.0230(15) 0.0092(14) 0.052(2) 0.0014(14) 0.0087(14) 0.0021(12) O10 0.0212(15) 0.0123(14) 0.052(2) -0.0042(14) 0.0038(14) 0.0029(12) O11 0.0180(13) 0.0160(13) 0.0249(14) -0.0022(11) 0.0019(11) -0.0085(11) O12 0.0244(14) 0.0102(13) 0.0326(16) 0.0014(11) -0.0030(12) -0.0068(11) O13 0.0311(19) 0.0204(19) 0.121(4) 0.021(2) -0.016(2) -0.0040(15) O14 0.078(3) 0.038(2) 0.046(2) -0.0266(18) -0.032(2) 0.037(2) O15 0.035(2) 0.022(2) 0.178(6) 0.005(3) 0.005(3) -0.0016(17) O16A 0.019(7) 0.046(10) 0.012(7) 0.007(7) -0.008(5) -0.003(7) O16B 0.031(3) 0.054(4) 0.015(3) -0.012(3) -0.013(3) 0.028(3) O16C 0.034(3) 0.031(3) 0.033(3) -0.0036(19) -0.0019(19) -0.0006(19) C1 0.0187(18) 0.0163(19) 0.0105(16) 0.0009(14) -0.0052(14) 0.0013(15) C2 0.0214(18) 0.0070(16) 0.0102(16) -0.0001(13) -0.0029(14) 0.0017(14) C3 0.0206(18) 0.0112(17) 0.0075(15) -0.0005(13) -0.0046(13) 0.0021(14) C4 0.0220(19) 0.0124(18) 0.0105(16) 0.0053(13) -0.0049(14) -0.0014(14) C5 0.0225(19) 0.0075(17) 0.0161(18) 0.0040(14) -0.0069(15) 0.0027(14) C6 0.0214(19) 0.0094(17) 0.0127(17) 0.0012(13) -0.0046(14) 0.0019(14) C7 0.0216(19) 0.0099(17) 0.0101(16) -0.0008(13) -0.0017(14) 0.0015(14) C8 0.0194(18) 0.0079(16) 0.0125(17) 0.0020(13) -0.0006(14) 0.0022(14) C9 0.0181(18) 0.0074(16) 0.0141(17) -0.0001(13) -0.0030(14) 0.0030(13) C10 0.0224(19) 0.0113(17) 0.0141(17) -0.0006(14) 0.0014(15) -0.0002(14) C11 0.0194(18) 0.0090(16) 0.0139(17) 0.0002(13) -0.0016(14) 0.0043(14) C12 0.028(2) 0.0110(19) 0.033(2) 0.0049(16) -0.0067(18) -0.0035(16) C13 0.0207(19) 0.0148(18) 0.0122(17) 0.0014(14) -0.0027(14) -0.0039(15) C14 0.0167(18) 0.0068(16) 0.0145(17) 0.0004(13) -0.0037(14) 0.0009(13) C15 0.0196(18) 0.0100(17) 0.0122(16) -0.0010(13) -0.0015(14) -0.0019(14) C16 0.0134(17) 0.0154(18) 0.0084(16) -0.0014(13) 0.0005(13) 0.0016(14) C17 0.0186(18) 0.0063(17) 0.0150(17) 0.0037(13) -0.0018(14) 0.0013(14) C18 0.0198(18) 0.0040(16) 0.0158(17) 0.0029(13) 0.0000(14) -0.0037(14) C19 0.0169(18) 0.0076(16) 0.0121(16) 0.0026(13) -0.0025(13) -0.0015(13) C20 0.0174(17) 0.0054(16) 0.0186(18) -0.0003(13) -0.0036(14) -0.0010(13) C21 0.0166(18) 0.0072(16) 0.0154(17) 0.0023(13) -0.0046(14) -0.0021(13) C22 0.0166(17) 0.0072(16) 0.0181(18) 0.0001(14) -0.0013(14) -0.0002(13) C23 0.0145(17) 0.0083(16) 0.0142(17) 0.0023(13) -0.0024(13) -0.0027(13) C24 0.0166(18) 0.0123(18) 0.0207(19) -0.0030(15) 0.0019(15) 0.0029(15) _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 O4 2.332(3) 2_566 ? Gd1 O5 2.336(3) . ? Gd1 O15 2.342(4) . ? Gd1 O16B 2.373(6) . ? Gd1 O13 2.378(4) . ? Gd1 O14 2.413(4) . ? Gd1 O8 2.467(3) . ? Gd1 O16C 2.477(11) . ? Gd1 O16A 2.485(15) . ? Gd1 O7 2.515(3) . ? Gd1 C22 2.860(4) . ? O1 C1 1.215(5) . ? O2 C1 1.322(5) . ? O2 H2 0.8418 . ? O3 C12 1.256(6) . ? O4 C12 1.257(5) . ? O4 Gd1 2.332(3) 2_566 ? O5 C10 1.251(5) . ? O6 C10 1.251(5) . ? O7 C22 1.238(4) . ? O8 C22 1.283(5) . ? O9 C24 1.284(5) . ? O10 C24 1.223(5) . ? O11 C13 1.330(5) . ? O11 H11 0.8491 . ? O12 C13 1.215(5) . ? O16A O16B 1.192(17) . ? O16B O16C 1.606(14) . ? C1 C3 1.487(5) . ? C2 C7 1.396(5) . ? C2 C3 1.397(5) . ? C2 H2A 0.9500 . ? C3 C4 1.395(5) . ? C4 C5 1.387(5) . ? C4 H4 0.9500 . ? C5 C6 1.395(6) . ? C5 C12 1.517(5) . ? C6 C7 1.400(5) . ? C6 H6 0.9500 . ? C7 C8 1.493(5) . ? C8 C11 1.394(5) 2_576 ? C8 C9 1.407(5) . ? C9 C11 1.397(6) . ? C9 C10 1.507(5) . ? C11 C8 1.394(5) 2_576 ? C11 H11A 0.9500 . ? C13 C15 1.489(5) . ? C14 C15 1.393(5) . ? C14 C19 1.400(5) . ? C14 H14 0.9500 . ? C15 C16 1.395(5) . ? C16 C17 1.394(5) . ? C16 H16 0.9500 . ? C17 C18 1.392(5) . ? C17 C24 1.490(5) . ? C18 C19 1.402(5) . ? C18 H18 0.9500 . ? C19 C20 1.482(5) . ? C20 C23 1.402(5) 2_575 ? C20 C21 1.414(5) . ? C21 C23 1.386(5) . ? C21 C22 1.512(5) . ? C23 C20 1.402(5) 2_575 ? C23 H23 0.9500 . ? 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 O4 Gd1 O5 136.05(12) 2_566 . ? O4 Gd1 O15 78.69(13) 2_566 . ? O5 Gd1 O15 78.68(16) . . ? O4 Gd1 O16B 80.04(19) 2_566 . ? O5 Gd1 O16B 67.65(16) . . ? O15 Gd1 O16B 100.2(3) . . ? O4 Gd1 O13 76.82(12) 2_566 . ? O5 Gd1 O13 122.12(15) . . ? O15 Gd1 O13 155.30(14) . . ? O16B Gd1 O13 78.6(2) . . ? O4 Gd1 O14 72.30(12) 2_566 . ? O5 Gd1 O14 144.72(12) . . ? O15 Gd1 O14 90.7(2) . . ? O16B Gd1 O14 147.62(16) . . ? O13 Gd1 O14 78.95(18) . . ? O4 Gd1 O8 145.91(10) 2_566 . ? O5 Gd1 O8 75.61(11) . . ? O15 Gd1 O8 128.33(14) . . ? O16B Gd1 O8 109.9(2) . . ? O13 Gd1 O8 73.63(11) . . ? O14 Gd1 O8 85.60(13) . . ? O4 Gd1 O16C 64.5(3) 2_566 . ? O5 Gd1 O16C 71.7(3) . . ? O15 Gd1 O16C 63.0(3) . . ? O16B Gd1 O16C 38.6(3) . . ? O13 Gd1 O16C 108.2(3) . . ? O14 Gd1 O16C 132.5(3) . . ? O8 Gd1 O16C 141.9(3) . . ? O4 Gd1 O16A 98.2(4) 2_566 . ? O5 Gd1 O16A 66.3(4) . . ? O15 Gd1 O16A 125.2(4) . . ? O16B Gd1 O16A 28.3(4) . . ? O13 Gd1 O16A 62.2(4) . . ? O14 Gd1 O16A 141.1(4) . . ? O8 Gd1 O16A 82.8(4) . . ? O16C Gd1 O16A 66.6(4) . . ? O4 Gd1 O7 133.73(10) 2_566 . ? O5 Gd1 O7 76.75(10) . . ? O15 Gd1 O7 78.70(17) . . ? O16B Gd1 O7 143.73(16) . . ? O13 Gd1 O7 116.84(13) . . ? O14 Gd1 O7 68.17(10) . . ? O8 Gd1 O7 52.20(9) . . ? O16C Gd1 O7 134.0(3) . . ? O16A Gd1 O7 127.7(4) . . ? O4 Gd1 C22 148.04(11) 2_566 . ? O5 Gd1 C22 74.16(11) . . ? O15 Gd1 C22 103.07(16) . . ? O16B Gd1 C22 129.7(2) . . ? O13 Gd1 C22 96.06(13) . . ? O14 Gd1 C22 75.77(11) . . ? O8 Gd1 C22 26.59(10) . . ? O16C Gd1 C22 145.1(3) . . ? O16A Gd1 C22 105.9(4) . . ? O7 Gd1 C22 25.62(10) . . ? C1 O2 H2 114.7 . . ? C12 O4 Gd1 141.4(3) . 2_566 ? C10 O5 Gd1 151.4(3) . . ? C22 O7 Gd1 92.9(2) . . ? C22 O8 Gd1 94.0(2) . . ? C13 O11 H11 110.5 . . ? O16B O16A Gd1 70.6(8) . . ? O16A O16B O16C 153.2(9) . . ? O16A O16B Gd1 81.1(7) . . ? O16C O16B Gd1 74.2(5) . . ? O16B O16C Gd1 67.2(4) . . ? O1 C1 O2 123.2(3) . . ? O1 C1 C3 123.0(4) . . ? O2 C1 C3 113.7(3) . . ? C7 C2 C3 120.9(3) . . ? C7 C2 H2A 119.6 . . ? C3 C2 H2A 119.6 . . ? C4 C3 C2 120.1(3) . . ? C4 C3 C1 121.7(3) . . ? C2 C3 C1 118.2(3) . . ? C5 C4 C3 119.4(4) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? C4 C5 C6 120.5(3) . . ? C4 C5 C12 120.2(4) . . ? C6 C5 C12 119.3(3) . . ? C5 C6 C7 120.7(3) . . ? C5 C6 H6 119.6 . . ? C7 C6 H6 119.6 . . ? C2 C7 C6 118.4(3) . . ? C2 C7 C8 120.8(3) . . ? C6 C7 C8 120.8(3) . . ? C11 C8 C9 118.3(4) 2_576 . ? C11 C8 C7 118.8(3) 2_576 . ? C9 C8 C7 122.8(3) . . ? C11 C9 C8 119.3(4) . . ? C11 C9 C10 117.2(3) . . ? C8 C9 C10 123.4(4) . . ? O6 C10 O5 123.9(4) . . ? O6 C10 C9 119.5(3) . . ? O5 C10 C9 116.6(3) . . ? C8 C11 C9 122.4(3) 2_576 . ? C8 C11 H11A 118.8 2_576 . ? C9 C11 H11A 118.8 . . ? O3 C12 O4 125.1(4) . . ? O3 C12 C5 118.5(4) . . ? O4 C12 C5 116.4(4) . . ? O12 C13 O11 124.0(4) . . ? O12 C13 C15 123.1(4) . . ? O11 C13 C15 112.8(3) . . ? C15 C14 C19 121.1(3) . . ? C15 C14 H14 119.4 . . ? C19 C14 H14 119.4 . . ? C14 C15 C16 119.6(3) . . ? C14 C15 C13 118.4(3) . . ? C16 C15 C13 121.9(3) . . ? C17 C16 C15 120.6(3) . . ? C17 C16 H16 119.7 . . ? C15 C16 H16 119.7 . . ? C18 C17 C16 118.8(3) . . ? C18 C17 C24 123.1(3) . . ? C16 C17 C24 118.0(3) . . ? C17 C18 C19 121.9(3) . . ? C17 C18 H18 119.0 . . ? C19 C18 H18 119.0 . . ? C14 C19 C18 117.9(3) . . ? C14 C19 C20 119.1(3) . . ? C18 C19 C20 123.0(3) . . ? C23 C20 C21 116.4(3) 2_575 . ? C23 C20 C19 118.3(3) 2_575 . ? C21 C20 C19 125.2(3) . . ? C23 C21 C20 120.1(3) . . ? C23 C21 C22 115.3(3) . . ? C20 C21 C22 124.5(3) . . ? O7 C22 O8 120.8(3) . . ? O7 C22 C21 118.9(3) . . ? O8 C22 C21 120.3(3) . . ? O7 C22 Gd1 61.45(19) . . ? O8 C22 Gd1 59.36(18) . . ? C21 C22 Gd1 176.0(3) . . ? C21 C23 C20 123.4(3) . 2_575 ? C21 C23 H23 118.3 . . ? C20 C23 H23 118.3 2_575 . ? O10 C24 O9 124.6(4) . . ? O10 C24 C17 120.5(4) . . ? O9 C24 C17 114.9(3) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 70.99 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 3.904 _refine_diff_density_min -0.972 _refine_diff_density_rms 0.115 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.027 0.500 0.027 577.0 169.1 _platon_squeeze_details ; ; ###END