# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Feng Luo' _publ_contact_author_email ecitluofeng@163.com _publ_author_name 'Feng Luo' data_1 _database_code_depnum_ccdc_archive 'CCDC 821188' #TrackingRef '- CEC-R2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_absolute_configuration 0 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H19 Gd O7' _chemical_formula_weight 432.51 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 Hexagonal _symmetry_space_group_name_H-M P6(5) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+2/3' '-x+y, -x, z+1/3' '-x, -y, z+1/2' 'y, -x+y, z+1/6' 'x-y, x, z+5/6' _cell_length_a 10.9374(2) _cell_length_b 10.9374(2) _cell_length_c 21.0837(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2184.27(10) _cell_formula_units_Z 6 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 8726 _cell_measurement_theta_min 2.89 _cell_measurement_theta_max 27.38 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.964 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1254 _exptl_absorpt_coefficient_mu 4.581 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4610 _exptl_absorpt_correction_T_max 0.5466 _exptl_absorpt_process_details ; Higashi, T. . Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10783 _diffrn_reflns_av_R_equivalents 0.0228 _diffrn_reflns_av_sigmaI/netI 0.0246 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1952 _reflns_number_gt 1919 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0146P)^2^+1.6629P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.014(16) _refine_ls_number_reflns 1952 _refine_ls_number_parameters 189 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0197 _refine_ls_R_factor_gt 0.0191 _refine_ls_wR_factor_ref 0.0404 _refine_ls_wR_factor_gt 0.0400 _refine_ls_goodness_of_fit_ref 1.136 _refine_ls_restrained_S_all 1.135 _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 C1 C 1.0446(7) 0.9681(6) 0.2353(3) 0.0347(14) Uani 1 1 d . . . C2 C 0.9607(7) 0.8350(6) 0.1990(3) 0.0486(17) Uani 1 1 d . . . H2A H 1.0228 0.8176 0.1732 0.073 Uiso 1 1 calc R . . H2B H 0.8941 0.8434 0.1724 0.073 Uiso 1 1 calc R . . H2C H 0.9109 0.7579 0.2280 0.073 Uiso 1 1 calc R . . C3 C 0.6381(5) 0.9259(5) 0.1295(3) 0.0280(13) Uani 1 1 d . . . C4 C 0.4960(5) 0.8543(5) 0.1634(3) 0.0288(12) Uani 1 1 d . . . C5 C 0.3699(6) 0.8239(6) 0.1226(3) 0.0503(18) Uani 1 1 d . . . H5A H 0.3923 0.8264 0.0780 0.060 Uiso 1 1 calc R . . H5B H 0.3398 0.8922 0.1306 0.060 Uiso 1 1 calc R . . C6 C 0.2532(6) 0.6730(7) 0.1427(4) 0.0568(17) Uani 1 1 d . . . H6A H 0.1646 0.6710 0.1497 0.068 Uiso 1 1 calc R . . H6B H 0.2393 0.6054 0.1097 0.068 Uiso 1 1 calc R . . C7 C 0.3023(5) 0.6363(5) 0.2036(3) 0.0282(12) Uani 1 1 d . . . C8 C 0.2628(8) 0.6981(7) 0.2604(4) 0.059(2) Uani 1 1 d . . . H8A H 0.1621 0.6494 0.2652 0.088 Uiso 1 1 calc R . . H8B H 0.2969 0.7966 0.2533 0.088 Uiso 1 1 calc R . . H8C H 0.3050 0.6868 0.2983 0.088 Uiso 1 1 calc R . . C9 C 0.4663(6) 0.7123(6) 0.1948(3) 0.0398(15) Uani 1 1 d . . . C10 C 0.5060(7) 0.6283(6) 0.1501(5) 0.067(2) Uani 1 1 d . . . H10A H 0.6033 0.6849 0.1381 0.100 Uiso 1 1 calc R . . H10B H 0.4477 0.6026 0.1129 0.100 Uiso 1 1 calc R . . H10C H 0.4921 0.5445 0.1712 0.100 Uiso 1 1 calc R . . C11 C 0.5494(8) 0.7378(8) 0.2562(4) 0.076(3) Uani 1 1 d . . . H11A H 0.5315 0.6491 0.2733 0.114 Uiso 1 1 calc R . . H11B H 0.5205 0.7844 0.2863 0.114 Uiso 1 1 calc R . . H11C H 0.6484 0.7961 0.2476 0.114 Uiso 1 1 calc R . . C12 C 0.2428(6) 0.4794(6) 0.2165(3) 0.0350(14) Uani 1 1 d . . . Gd1 Gd 0.96708(2) 1.19133(2) 0.14637(3) 0.02265(8) Uani 1 1 d . . . H1M H 0.485(4) 0.895(4) 0.208(2) 0.013(11) Uiso 1 1 d . . . O1 O 1.0908(4) 1.3358(4) 0.0486(2) 0.0444(11) Uani 1 1 d . . . O2 O 1.0219(4) 1.0714(3) 0.2282(2) 0.0307(9) Uani 1 1 d . . . O3 O 1.1364(5) 0.9800(4) 0.2753(2) 0.0439(11) Uani 1 1 d . . . O4 O 0.6394(4) 0.9139(4) 0.0705(2) 0.0415(10) Uani 1 1 d . . . O5 O 0.7460(4) 0.9939(4) 0.1632(2) 0.0398(10) Uani 1 1 d . . . O6 O 0.1777(4) 0.3923(4) 0.1724(2) 0.0542(13) Uani 1 1 d . . . O7 O 0.2622(5) 0.4439(4) 0.2690(2) 0.0502(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 C1 0.047(4) 0.029(3) 0.033(3) -0.003(3) 0.002(3) 0.023(3) C2 0.058(4) 0.035(4) 0.051(4) -0.009(3) -0.013(3) 0.023(3) C3 0.029(3) 0.019(3) 0.033(4) 0.008(2) 0.001(2) 0.010(2) C4 0.026(3) 0.024(3) 0.030(3) 0.005(2) 0.007(2) 0.008(2) C5 0.034(3) 0.051(4) 0.059(5) 0.013(3) -0.005(3) 0.016(3) C6 0.042(3) 0.056(4) 0.060(4) 0.015(4) -0.007(4) 0.015(3) C7 0.020(3) 0.022(3) 0.036(3) 0.002(2) 0.002(2) 0.006(2) C8 0.071(5) 0.043(4) 0.062(5) 0.004(3) 0.023(4) 0.029(4) C9 0.031(3) 0.036(3) 0.043(4) 0.014(3) 0.001(3) 0.009(3) C10 0.058(4) 0.032(3) 0.118(7) 0.014(4) 0.043(5) 0.028(3) C11 0.052(4) 0.068(5) 0.071(6) 0.040(4) -0.018(4) 0.003(4) C12 0.022(3) 0.036(3) 0.037(4) 0.001(3) 0.008(3) 0.008(3) Gd1 0.02185(13) 0.02114(13) 0.02316(12) -0.00116(11) -0.00165(12) 0.00939(11) O1 0.050(3) 0.028(2) 0.038(3) 0.0062(19) 0.007(2) 0.0073(19) O2 0.033(2) 0.0257(18) 0.033(2) 0.004(2) -0.0034(16) 0.0141(18) O3 0.059(3) 0.045(2) 0.040(3) -0.008(2) -0.016(2) 0.035(2) O4 0.041(2) 0.046(2) 0.027(2) -0.0009(19) 0.0076(19) 0.0145(19) O5 0.028(2) 0.035(2) 0.037(3) 0.0052(18) -0.0013(18) 0.0017(19) O6 0.033(2) 0.034(2) 0.068(3) -0.022(2) 0.001(2) -0.0038(19) O7 0.070(3) 0.032(2) 0.043(3) 0.012(2) 0.015(2) 0.022(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 C1 O3 1.266(7) . ? C1 O2 1.281(6) . ? C1 C2 1.488(8) . ? C1 Gd1 2.935(6) 5_565 ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 O4 1.252(6) . ? C3 O5 1.255(6) . ? C3 C4 1.524(7) . ? C4 C5 1.514(8) . ? C4 C9 1.565(8) . ? C4 H1M 1.07(4) . ? C5 C6 1.557(8) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C7 1.520(9) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C12 1.525(7) . ? C7 C8 1.541(8) . ? C7 C9 1.566(7) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 C10 1.523(9) . ? C9 C11 1.525(9) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 O7 1.228(7) . ? C12 O6 1.264(7) . ? Gd1 O4 2.315(4) 5_565 ? Gd1 O7 2.317(4) 6_664 ? Gd1 O6 2.319(4) 1_665 ? Gd1 O5 2.327(4) . ? Gd1 O2 2.418(4) . ? Gd1 O2 2.515(4) 6_654 ? Gd1 O1 2.538(4) . ? Gd1 O3 2.554(4) 6_654 ? Gd1 C1 2.935(6) 6_654 ? O2 Gd1 2.515(4) 5_565 ? O3 Gd1 2.554(4) 5_565 ? O4 Gd1 2.315(4) 6_654 ? O6 Gd1 2.319(4) 1_445 ? O7 Gd1 2.317(4) 5_455 ? 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 C1 O2 118.7(6) . . ? O3 C1 C2 120.8(5) . . ? O2 C1 C2 120.4(5) . . ? O3 C1 Gd1 60.2(3) . 5_565 ? O2 C1 Gd1 58.5(3) . 5_565 ? C2 C1 Gd1 175.7(5) . 5_565 ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? O4 C3 O5 124.7(5) . . ? O4 C3 C4 118.3(5) . . ? O5 C3 C4 117.0(5) . . ? C5 C4 C3 115.5(5) . . ? C5 C4 C9 107.9(4) . . ? C3 C4 C9 111.1(4) . . ? C5 C4 H1M 108(2) . . ? C3 C4 H1M 120(2) . . ? C9 C4 H1M 91(2) . . ? C4 C5 C6 104.6(5) . . ? C4 C5 H5A 110.8 . . ? C6 C5 H5A 110.8 . . ? C4 C5 H5B 110.8 . . ? C6 C5 H5B 110.8 . . ? H5A C5 H5B 108.9 . . ? C7 C6 C5 107.4(5) . . ? C7 C6 H6A 110.2 . . ? C5 C6 H6A 110.2 . . ? C7 C6 H6B 110.2 . . ? C5 C6 H6B 110.2 . . ? H6A C6 H6B 108.5 . . ? C6 C7 C12 116.1(5) . . ? C6 C7 C8 109.1(5) . . ? C12 C7 C8 107.4(5) . . ? C6 C7 C9 102.8(5) . . ? C12 C7 C9 110.5(4) . . ? C8 C7 C9 110.9(5) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 C11 108.1(6) . . ? C10 C9 C4 110.9(5) . . ? C11 C9 C4 111.6(5) . . ? C10 C9 C7 110.4(5) . . ? C11 C9 C7 114.6(5) . . ? C4 C9 C7 101.0(4) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? O7 C12 O6 123.1(6) . . ? O7 C12 C7 118.2(5) . . ? O6 C12 C7 118.7(6) . . ? O4 Gd1 O7 80.97(15) 5_565 6_664 ? O4 Gd1 O6 75.94(15) 5_565 1_665 ? O7 Gd1 O6 108.00(16) 6_664 1_665 ? O4 Gd1 O5 83.68(15) 5_565 . ? O7 Gd1 O5 78.11(15) 6_664 . ? O6 Gd1 O5 157.26(16) 1_665 . ? O4 Gd1 O2 78.59(14) 5_565 . ? O7 Gd1 O2 150.84(15) 6_664 . ? O6 Gd1 O2 86.94(15) 1_665 . ? O5 Gd1 O2 79.15(14) . . ? O4 Gd1 O2 159.65(14) 5_565 6_654 ? O7 Gd1 O2 99.08(14) 6_664 6_654 ? O6 Gd1 O2 122.57(14) 1_665 6_654 ? O5 Gd1 O2 76.48(14) . 6_654 ? O2 Gd1 O2 93.09(10) . 6_654 ? O4 Gd1 O1 125.96(14) 5_565 . ? O7 Gd1 O1 73.23(14) 6_664 . ? O6 Gd1 O1 68.58(15) 1_665 . ? O5 Gd1 O1 133.25(14) . . ? O2 Gd1 O1 135.91(14) . . ? O2 Gd1 O1 72.60(14) 6_654 . ? O4 Gd1 O3 137.95(14) 5_565 6_654 ? O7 Gd1 O3 137.84(15) 6_664 6_654 ? O6 Gd1 O3 76.05(14) 1_665 6_654 ? O5 Gd1 O3 114.67(15) . 6_654 ? O2 Gd1 O3 69.19(14) . 6_654 ? O2 Gd1 O3 51.21(12) 6_654 6_654 ? O1 Gd1 O3 69.58(14) . 6_654 ? O4 Gd1 C1 158.11(16) 5_565 6_654 ? O7 Gd1 C1 120.39(17) 6_664 6_654 ? O6 Gd1 C1 99.63(15) 1_665 6_654 ? O5 Gd1 C1 95.53(15) . 6_654 ? O2 Gd1 C1 79.77(16) . 6_654 ? O2 Gd1 C1 25.74(12) 6_654 6_654 ? O1 Gd1 C1 69.56(16) . 6_654 ? O3 Gd1 C1 25.49(13) 6_654 6_654 ? C1 O2 Gd1 140.5(4) . . ? C1 O2 Gd1 95.8(4) . 5_565 ? Gd1 O2 Gd1 116.55(12) . 5_565 ? C1 O3 Gd1 94.3(3) . 5_565 ? C3 O4 Gd1 146.6(4) . 6_654 ? C3 O5 Gd1 134.2(3) . . ? C12 O6 Gd1 143.8(4) . 1_445 ? C12 O7 Gd1 131.9(4) . 5_455 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 C3 C4 C5 -22.5(7) . . . . ? O5 C3 C4 C5 156.9(5) . . . . ? O4 C3 C4 C9 100.8(6) . . . . ? O5 C3 C4 C9 -79.7(6) . . . . ? C3 C4 C5 C6 137.9(5) . . . . ? C9 C4 C5 C6 12.9(7) . . . . ? C4 C5 C6 C7 13.1(7) . . . . ? C5 C6 C7 C12 -154.3(5) . . . . ? C5 C6 C7 C8 84.2(6) . . . . ? C5 C6 C7 C9 -33.5(7) . . . . ? C5 C4 C9 C10 84.2(6) . . . . ? C3 C4 C9 C10 -43.3(7) . . . . ? C5 C4 C9 C11 -155.1(6) . . . . ? C3 C4 C9 C11 77.3(7) . . . . ? C5 C4 C9 C7 -32.9(6) . . . . ? C3 C4 C9 C7 -160.4(5) . . . . ? C6 C7 C9 C10 -77.7(6) . . . . ? C12 C7 C9 C10 46.8(7) . . . . ? C8 C7 C9 C10 165.8(6) . . . . ? C6 C7 C9 C11 159.9(6) . . . . ? C12 C7 C9 C11 -75.6(7) . . . . ? C8 C7 C9 C11 43.4(7) . . . . ? C6 C7 C9 C4 39.7(6) . . . . ? C12 C7 C9 C4 164.2(5) . . . . ? C8 C7 C9 C4 -76.8(6) . . . . ? C6 C7 C12 O7 -169.2(5) . . . . ? C8 C7 C12 O7 -46.8(7) . . . . ? C9 C7 C12 O7 74.3(7) . . . . ? C6 C7 C12 O6 11.7(8) . . . . ? C8 C7 C12 O6 134.1(6) . . . . ? C9 C7 C12 O6 -104.8(6) . . . . ? O3 C1 O2 Gd1 143.4(5) . . . . ? C2 C1 O2 Gd1 -39.0(10) . . . . ? Gd1 C1 O2 Gd1 146.0(6) 5_565 . . . ? O3 C1 O2 Gd1 -2.6(6) . . . 5_565 ? C2 C1 O2 Gd1 175.1(6) . . . 5_565 ? O4 Gd1 O2 C1 164.4(7) 5_565 . . . ? O7 Gd1 O2 C1 118.1(7) 6_664 . . . ? O6 Gd1 O2 C1 -119.3(7) 1_665 . . . ? O5 Gd1 O2 C1 78.8(6) . . . . ? O2 Gd1 O2 C1 3.2(7) 6_654 . . . ? O1 Gd1 O2 C1 -64.8(7) . . . . ? O3 Gd1 O2 C1 -43.1(6) 6_654 . . . ? C1 Gd1 O2 C1 -19.0(6) 6_654 . . . ? O4 Gd1 O2 Gd1 -54.09(18) 5_565 . . 5_565 ? O7 Gd1 O2 Gd1 -100.4(3) 6_664 . . 5_565 ? O6 Gd1 O2 Gd1 22.18(19) 1_665 . . 5_565 ? O5 Gd1 O2 Gd1 -139.7(2) . . . 5_565 ? O2 Gd1 O2 Gd1 144.65(9) 6_654 . . 5_565 ? O1 Gd1 O2 Gd1 76.7(3) . . . 5_565 ? O3 Gd1 O2 Gd1 98.4(2) 6_654 . . 5_565 ? C1 Gd1 O2 Gd1 122.5(2) 6_654 . . 5_565 ? O2 C1 O3 Gd1 2.5(6) . . . 5_565 ? C2 C1 O3 Gd1 -175.1(6) . . . 5_565 ? O5 C3 O4 Gd1 2.1(10) . . . 6_654 ? C4 C3 O4 Gd1 -178.5(4) . . . 6_654 ? O4 C3 O5 Gd1 29.8(8) . . . . ? C4 C3 O5 Gd1 -149.6(4) . . . . ? O4 Gd1 O5 C3 127.2(5) 5_565 . . . ? O7 Gd1 O5 C3 45.2(5) 6_664 . . . ? O6 Gd1 O5 C3 153.5(5) 1_665 . . . ? O2 Gd1 O5 C3 -153.2(5) . . . . ? O2 Gd1 O5 C3 -57.3(5) 6_654 . . . ? O1 Gd1 O5 C3 -7.8(6) . . . . ? O3 Gd1 O5 C3 -92.3(5) 6_654 . . . ? C1 Gd1 O5 C3 -74.8(5) 6_654 . . . ? O7 C12 O6 Gd1 55.6(10) . . . 1_445 ? C7 C12 O6 Gd1 -125.4(6) . . . 1_445 ? O6 C12 O7 Gd1 -2.6(9) . . . 5_455 ? C7 C12 O7 Gd1 178.4(3) . . . 5_455 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.458 _refine_diff_density_min -0.383 _refine_diff_density_rms 0.077 #================================================================end data_2 _database_code_depnum_ccdc_archive 'CCDC 821189' #TrackingRef '- CEC-R2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_absolute_configuration 0 _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H19 O7 Tb' _chemical_formula_weight 434.18 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' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M P6(5) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+2/3' '-x+y, -x, z+1/3' '-x, -y, z+1/2' 'y, -x+y, z+1/6' 'x-y, x, z+5/6' _cell_length_a 10.9106(2) _cell_length_b 10.9106(2) _cell_length_c 20.9713(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2161.99(9) _cell_formula_units_Z 6 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 8817 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 27.58 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.992 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1260 _exptl_absorpt_coefficient_mu 4.933 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4387 _exptl_absorpt_correction_T_max 0.5249 _exptl_absorpt_process_details ; Higashi, T. . Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10565 _diffrn_reflns_av_R_equivalents 0.0398 _diffrn_reflns_av_sigmaI/netI 0.0306 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1917 _reflns_number_gt 1877 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0213P)^2^+0.9549P] 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 refu _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.010(17) _refine_ls_number_reflns 1917 _refine_ls_number_parameters 185 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0209 _refine_ls_R_factor_gt 0.0203 _refine_ls_wR_factor_ref 0.0469 _refine_ls_wR_factor_gt 0.0465 _refine_ls_goodness_of_fit_ref 1.074 _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 C1 C 0.6398(6) 0.7127(6) 0.0798(3) 0.0277(13) Uani 1 1 d . . . C2 C 0.4973(6) 0.6421(6) 0.0454(3) 0.0296(13) Uani 1 1 d . . . C3 C 0.4669(6) 0.7544(7) 0.0150(3) 0.0339(15) Uani 1 1 d . . . C4 C 0.5050(7) 0.8771(6) 0.0600(5) 0.059(2) Uani 1 1 d . . . H4A H 0.6034 0.9207 0.0711 0.089 Uiso 1 1 calc R . . H4B H 0.4485 0.8429 0.0980 0.089 Uiso 1 1 calc R . . H4C H 0.4873 0.9453 0.0395 0.089 Uiso 1 1 calc R . . C5 C 0.3026(6) 0.6655(6) 0.0054(3) 0.0282(13) Uani 1 1 d . . . C6 C 0.2412(6) 0.7613(6) -0.0055(3) 0.0307(14) Uani 1 1 d . . . C7 C 0.2635(9) 0.5672(8) -0.0523(4) 0.057(2) Uani 1 1 d . . . H7A H 0.1634 0.5220 -0.0596 0.086 Uiso 1 1 calc R . . H7B H 0.2896 0.4966 -0.0443 0.086 Uiso 1 1 calc R . . H7C H 0.3131 0.6213 -0.0892 0.086 Uiso 1 1 calc R . . C8 C 0.2527(6) 0.5771(7) 0.0667(4) 0.0514(18) Uani 1 1 d . . . H8A H 0.2377 0.6296 0.1002 0.062 Uiso 1 1 calc R . . H8B H 0.1644 0.4899 0.0593 0.062 Uiso 1 1 calc R . . C9 C 0.3686(7) 0.5448(7) 0.0861(4) 0.0452(17) Uani 1 1 d . . . H9A H 0.3389 0.4464 0.0779 0.054 Uiso 1 1 calc R . . H9B H 0.3905 0.5640 0.1311 0.054 Uiso 1 1 calc R . . C10 C 1.0456(7) 1.0748(6) -0.0252(3) 0.0346(15) Uani 1 1 d . . . C11 C 0.9638(8) 1.1260(7) 0.0125(3) 0.0474(18) Uani 1 1 d . . . H11A H 1.0267 1.2006 0.0406 0.071 Uiso 1 1 calc R . . H11B H 0.8925 1.0493 0.0372 0.071 Uiso 1 1 calc R . . H11C H 0.9195 1.1610 -0.0160 0.071 Uiso 1 1 calc R . . C12 C 0.5496(9) 0.8142(11) -0.0468(4) 0.074(3) Uani 1 1 d . . . H12A H 0.5252 0.8798 -0.0651 0.110 Uiso 1 1 calc R . . H12B H 0.5264 0.7384 -0.0763 0.110 Uiso 1 1 calc R . . H12C H 0.6492 0.8621 -0.0379 0.110 Uiso 1 1 calc R . . H1M H 0.5045 0.5856 0.0072 0.088 Uiso 1 1 d R . . O1 O 1.0901(5) 0.7533(5) 0.1616(2) 0.0480(12) Uani 1 1 d . . . O2 O 1.0241(5) 0.9506(4) -0.0181(2) 0.0298(9) Uani 1 1 d . . . O3 O 1.1386(5) 1.1559(5) -0.0642(2) 0.0426(12) Uani 1 1 d . . . O4 O 0.7492(5) 0.7532(5) 0.0467(2) 0.0384(11) Uani 1 1 d . . . O5 O 0.6401(4) 0.7248(4) 0.1396(2) 0.0374(10) Uani 1 1 d . . . O6 O 0.2587(5) 0.8181(5) -0.0586(2) 0.0489(13) Uani 1 1 d . . . O7 O 0.1762(5) 0.7827(5) 0.0384(2) 0.0474(13) Uani 1 1 d . . . Tb1 Tb 0.96756(2) 0.77574(2) 0.06344(3) 0.02213(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 C1 0.032(3) 0.028(3) 0.029(4) 0.000(3) -0.008(3) 0.020(3) C2 0.031(3) 0.031(3) 0.028(3) -0.004(2) -0.006(3) 0.016(3) C3 0.030(3) 0.040(3) 0.033(3) 0.010(3) 0.001(3) 0.018(3) C4 0.057(4) 0.034(4) 0.095(6) -0.024(4) -0.035(5) 0.029(3) C5 0.022(3) 0.033(3) 0.028(3) 0.000(3) -0.006(3) 0.013(3) C6 0.024(3) 0.037(3) 0.028(3) -0.008(3) -0.010(3) 0.013(3) C7 0.074(6) 0.061(5) 0.055(5) -0.025(4) -0.022(4) 0.048(5) C8 0.033(3) 0.064(5) 0.056(4) 0.028(4) 0.015(4) 0.024(3) C9 0.035(4) 0.044(4) 0.053(4) 0.016(4) 0.006(3) 0.017(3) C10 0.048(4) 0.035(3) 0.025(3) 0.001(3) 0.002(3) 0.023(3) C11 0.068(5) 0.050(4) 0.044(4) 0.001(4) 0.006(4) 0.044(4) C12 0.052(5) 0.118(8) 0.062(6) 0.046(6) 0.016(4) 0.051(5) O1 0.052(3) 0.066(3) 0.036(3) 0.001(2) -0.006(2) 0.037(3) O2 0.036(2) 0.030(2) 0.029(2) 0.0074(19) 0.0063(18) 0.0202(18) O3 0.059(3) 0.036(3) 0.037(3) 0.007(2) 0.014(3) 0.027(2) O4 0.032(2) 0.055(3) 0.030(3) 0.003(2) -0.001(2) 0.023(2) O5 0.037(2) 0.051(3) 0.023(2) -0.005(2) -0.004(2) 0.021(2) O6 0.063(3) 0.060(3) 0.040(3) 0.002(3) -0.007(3) 0.043(3) O7 0.036(2) 0.067(3) 0.052(3) -0.016(3) 0.002(2) 0.036(2) Tb1 0.02220(14) 0.02433(15) 0.02080(13) 0.00034(12) 0.00156(13) 0.01234(11) _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 C1 O4 1.255(7) . ? C1 O5 1.260(7) . ? C1 C2 1.528(8) . ? C2 C9 1.529(8) . ? C2 C3 1.556(8) . ? C2 H1M 1.0354 . ? C3 C4 1.516(9) . ? C3 C12 1.527(9) . ? C3 C5 1.567(8) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 C6 1.515(8) . ? C5 C7 1.529(9) . ? C5 C8 1.535(9) . ? C6 O6 1.241(7) . ? C6 O7 1.253(7) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 C9 1.527(9) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 O3 1.259(7) . ? C10 O2 1.263(6) . ? C10 C11 1.494(9) . ? C10 Tb1 2.909(7) 6_654 ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? O1 Tb1 2.533(4) . ? O2 Tb1 2.402(4) . ? O2 Tb1 2.497(4) 6_654 ? O3 Tb1 2.534(4) 6_654 ? O4 Tb1 2.297(4) . ? O5 Tb1 2.297(4) 5_565 ? O6 Tb1 2.293(4) 6_554 ? O7 Tb1 2.299(4) 1_455 ? Tb1 O6 2.293(4) 5 ? Tb1 O5 2.297(4) 6_654 ? Tb1 O7 2.299(4) 1_655 ? Tb1 O2 2.497(4) 5_565 ? Tb1 O3 2.534(4) 5_565 ? Tb1 C10 2.909(7) 5_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 O4 C1 O5 124.2(5) . . ? O4 C1 C2 117.7(5) . . ? O5 C1 C2 118.1(5) . . ? C1 C2 C9 115.8(5) . . ? C1 C2 C3 111.1(5) . . ? C9 C2 C3 106.9(5) . . ? C1 C2 H1M 107.8 . . ? C9 C2 H1M 109.6 . . ? C3 C2 H1M 105.2 . . ? C4 C3 C12 107.9(6) . . ? C4 C3 C2 111.6(5) . . ? C12 C3 C2 111.8(5) . . ? C4 C3 C5 110.5(5) . . ? C12 C3 C5 113.8(6) . . ? C2 C3 C5 101.2(5) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C5 C7 107.5(5) . . ? C6 C5 C8 114.8(5) . . ? C7 C5 C8 109.6(6) . . ? C6 C5 C3 110.9(5) . . ? C7 C5 C3 111.6(5) . . ? C8 C5 C3 102.6(5) . . ? O6 C6 O7 121.7(6) . . ? O6 C6 C5 118.0(6) . . ? O7 C6 C5 120.3(5) . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 C5 107.0(5) . . ? C9 C8 H8A 110.3 . . ? C5 C8 H8A 110.3 . . ? C9 C8 H8B 110.3 . . ? C5 C8 H8B 110.3 . . ? H8A C8 H8B 108.6 . . ? C8 C9 C2 105.7(5) . . ? C8 C9 H9A 110.6 . . ? C2 C9 H9A 110.6 . . ? C8 C9 H9B 110.6 . . ? C2 C9 H9B 110.6 . . ? H9A C9 H9B 108.7 . . ? O3 C10 O2 118.8(6) . . ? O3 C10 C11 120.3(6) . . ? O2 C10 C11 120.9(6) . . ? O3 C10 Tb1 60.3(3) . 6_654 ? O2 C10 Tb1 58.6(3) . 6_654 ? C11 C10 Tb1 176.9(5) . 6_654 ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C3 C12 H12A 109.5 . . ? C3 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C3 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C10 O2 Tb1 140.6(4) . . ? C10 O2 Tb1 95.8(4) . 6_654 ? Tb1 O2 Tb1 117.08(13) . 6_654 ? C10 O3 Tb1 94.1(4) . 6_654 ? C1 O4 Tb1 134.9(4) . . ? C1 O5 Tb1 146.2(4) . 5_565 ? C6 O6 Tb1 134.2(4) . 6_554 ? C6 O7 Tb1 143.6(4) . 1_455 ? O6 Tb1 O4 77.68(17) 5 . ? O6 Tb1 O5 81.65(16) 5 6_654 ? O4 Tb1 O5 83.92(16) . 6_654 ? O6 Tb1 O7 108.07(17) 5 1_655 ? O4 Tb1 O7 157.68(17) . 1_655 ? O5 Tb1 O7 75.84(16) 6_654 1_655 ? O6 Tb1 O2 151.22(17) 5 . ? O4 Tb1 O2 79.43(16) . . ? O5 Tb1 O2 78.80(15) 6_654 . ? O7 Tb1 O2 87.38(16) 1_655 . ? O6 Tb1 O2 97.90(15) 5 5_565 ? O4 Tb1 O2 76.43(16) . 5_565 ? O5 Tb1 O2 159.93(15) 6_654 5_565 ? O7 Tb1 O2 122.66(15) 1_655 5_565 ? O2 Tb1 O2 93.41(11) . 5_565 ? O6 Tb1 O1 72.93(16) 5 . ? O4 Tb1 O1 133.11(15) . . ? O5 Tb1 O1 125.67(15) 6_654 . ? O7 Tb1 O1 68.15(16) 1_655 . ? O2 Tb1 O1 135.84(15) . . ? O2 Tb1 O1 72.46(15) 5_565 . ? O6 Tb1 O3 136.74(16) 5 5_565 ? O4 Tb1 O3 114.77(17) . 5_565 ? O5 Tb1 O3 138.41(14) 6_654 5_565 ? O7 Tb1 O3 76.40(16) 1_655 5_565 ? O2 Tb1 O3 69.56(16) . 5_565 ? O2 Tb1 O3 51.13(14) 5_565 5_565 ? O1 Tb1 O3 69.24(15) . 5_565 ? O6 Tb1 C10 119.32(18) 5 5_565 ? O4 Tb1 C10 95.20(17) . 5_565 ? O5 Tb1 C10 158.43(17) 6_654 5_565 ? O7 Tb1 C10 100.14(17) 1_655 5_565 ? O2 Tb1 C10 79.85(17) . 5_565 ? O2 Tb1 C10 25.59(13) 5_565 5_565 ? O1 Tb1 C10 69.71(18) . 5_565 ? O3 Tb1 C10 25.57(15) 5_565 5_565 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 C1 C2 C9 156.9(5) . . . . ? O5 C1 C2 C9 -22.1(7) . . . . ? O4 C1 C2 C3 -80.9(6) . . . . ? O5 C1 C2 C3 100.1(6) . . . . ? C1 C2 C3 C4 -43.1(7) . . . . ? C9 C2 C3 C4 84.1(6) . . . . ? C1 C2 C3 C12 77.9(7) . . . . ? C9 C2 C3 C12 -154.9(6) . . . . ? C1 C2 C3 C5 -160.7(5) . . . . ? C9 C2 C3 C5 -33.4(6) . . . . ? C4 C3 C5 C6 44.9(7) . . . . ? C12 C3 C5 C6 -76.7(7) . . . . ? C2 C3 C5 C6 163.3(5) . . . . ? C4 C3 C5 C7 164.6(6) . . . . ? C12 C3 C5 C7 43.0(8) . . . . ? C2 C3 C5 C7 -77.0(6) . . . . ? C4 C3 C5 C8 -78.1(6) . . . . ? C12 C3 C5 C8 160.3(6) . . . . ? C2 C3 C5 C8 40.3(6) . . . . ? C7 C5 C6 O6 -46.4(7) . . . . ? C8 C5 C6 O6 -168.6(6) . . . . ? C3 C5 C6 O6 75.7(7) . . . . ? C7 C5 C6 O7 134.3(6) . . . . ? C8 C5 C6 O7 12.1(8) . . . . ? C3 C5 C6 O7 -103.6(6) . . . . ? C6 C5 C8 C9 -153.9(5) . . . . ? C7 C5 C8 C9 85.1(7) . . . . ? C3 C5 C8 C9 -33.5(7) . . . . ? C5 C8 C9 C2 12.8(8) . . . . ? C1 C2 C9 C8 137.8(6) . . . . ? C3 C2 C9 C8 13.4(7) . . . . ? O3 C10 O2 Tb1 143.2(5) . . . . ? C11 C10 O2 Tb1 -36.2(11) . . . . ? Tb1 C10 O2 Tb1 147.4(7) 6_654 . . . ? O3 C10 O2 Tb1 -4.3(7) . . . 6_654 ? C11 C10 O2 Tb1 176.4(6) . . . 6_654 ? O2 C10 O3 Tb1 4.2(6) . . . 6_654 ? C11 C10 O3 Tb1 -176.4(6) . . . 6_654 ? O5 C1 O4 Tb1 29.9(9) . . . . ? C2 C1 O4 Tb1 -149.1(4) . . . . ? O4 C1 O5 Tb1 3.3(11) . . . 5_565 ? C2 C1 O5 Tb1 -177.8(4) . . . 5_565 ? O7 C6 O6 Tb1 -1.3(9) . . . 6_554 ? C5 C6 O6 Tb1 179.4(4) . . . 6_554 ? O6 C6 O7 Tb1 53.7(10) . . . 1_455 ? C5 C6 O7 Tb1 -127.0(6) . . . 1_455 ? C1 O4 Tb1 O6 43.8(6) . . . 5 ? C1 O4 Tb1 O5 126.6(6) . . . 6_654 ? C1 O4 Tb1 O7 151.5(5) . . . 1_655 ? C1 O4 Tb1 O2 -153.7(6) . . . . ? C1 O4 Tb1 O2 -57.6(6) . . . 5_565 ? C1 O4 Tb1 O1 -8.2(7) . . . . ? C1 O4 Tb1 O3 -92.3(6) . . . 5_565 ? C1 O4 Tb1 C10 -75.1(6) . . . 5_565 ? C10 O2 Tb1 O6 115.3(8) . . . 5 ? Tb1 O2 Tb1 O6 -101.7(3) 6_654 . . 5 ? C10 O2 Tb1 O4 77.5(7) . . . . ? Tb1 O2 Tb1 O4 -139.4(2) 6_654 . . . ? C10 O2 Tb1 O5 163.4(8) . . . 6_654 ? Tb1 O2 Tb1 O5 -53.61(19) 6_654 . . 6_654 ? C10 O2 Tb1 O7 -120.5(7) . . . 1_655 ? Tb1 O2 Tb1 O7 22.5(2) 6_654 . . 1_655 ? C10 O2 Tb1 O2 2.0(8) . . . 5_565 ? Tb1 O2 Tb1 O2 145.06(10) 6_654 . . 5_565 ? C10 O2 Tb1 O1 -66.1(8) . . . . ? Tb1 O2 Tb1 O1 76.9(3) 6_654 . . . ? C10 O2 Tb1 O3 -44.1(7) . . . 5_565 ? Tb1 O2 Tb1 O3 98.9(2) 6_654 . . 5_565 ? C10 O2 Tb1 C10 -19.8(7) . . . 5_565 ? Tb1 O2 Tb1 C10 123.3(2) 6_654 . . 5_565 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.535 _refine_diff_density_min -0.557 _refine_diff_density_rms 0.084 #================================================================end data_3 _database_code_depnum_ccdc_archive 'CCDC 821190' #TrackingRef '- CEC-R2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_absolute_configuration 0 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H19 Eu O7' _chemical_formula_weight 427.23 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 Hexagonal _symmetry_space_group_name_H-M P6(5) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+2/3' '-x+y, -x, z+1/3' '-x, -y, z+1/2' 'y, -x+y, z+1/6' 'x-y, x, z+5/6' _cell_length_a 10.94450(10) _cell_length_b 10.94450(10) _cell_length_c 21.1465(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2193.62(6) _cell_formula_units_Z 6 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9657 _cell_measurement_theta_min 2.89 _cell_measurement_theta_max 27.49 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.940 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1260 _exptl_absorpt_coefficient_mu 4.315 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4369 _exptl_absorpt_correction_T_max 0.4790 _exptl_absorpt_process_details ; Higashi, T. . Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10480 _diffrn_reflns_av_R_equivalents 0.0238 _diffrn_reflns_av_sigmaI/netI 0.0261 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 24.99 _reflns_number_total 2241 _reflns_number_gt 2197 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The H atoms on coordinated water molecule is firstly found and then fixed by O-H/0.85 and O-O/1.25. ; _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^)+(0.0152P)^2^+1.6038P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.008(16) _refine_ls_number_reflns 2241 _refine_ls_number_parameters 197 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0193 _refine_ls_R_factor_gt 0.0185 _refine_ls_wR_factor_ref 0.0424 _refine_ls_wR_factor_gt 0.0418 _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_restrained_S_all 1.103 _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 C1 C -0.0760(5) -0.0449(6) 0.2478(3) 0.0317(12) Uani 1 1 d . . . C2 C -0.1260(6) 0.0387(7) 0.2112(3) 0.0488(15) Uani 1 1 d . . . H12A H -0.2074 -0.0241 0.1867 0.073 Uiso 1 1 calc R . . H12B H -0.0523 0.1028 0.1834 0.073 Uiso 1 1 calc R . . H12C H -0.1503 0.0911 0.2399 0.073 Uiso 1 1 calc R . . C3 C 0.3628(5) 0.0729(5) 0.3081(2) 0.0293(12) Uani 1 1 d . . . C4 C 0.5047(5) 0.1454(5) 0.3421(2) 0.0295(11) Uani 1 1 d . . . C5 C 0.6306(5) 0.1767(6) 0.3018(3) 0.0490(16) Uani 1 1 d . . . H5A H 0.6084 0.1741 0.2573 0.059 Uiso 1 1 calc R . . H5B H 0.6612 0.1088 0.3098 0.059 Uiso 1 1 calc R . . C6 C 0.7460(5) 0.3265(6) 0.3217(4) 0.0564(16) Uani 1 1 d . . . H6A H 0.8348 0.3289 0.3285 0.068 Uiso 1 1 calc R . . H6B H 0.7594 0.3939 0.2888 0.068 Uiso 1 1 calc R . . C7 C 0.5330(5) 0.2863(5) 0.3735(3) 0.0373(13) Uani 1 1 d . . . C8 C 0.4931(7) 0.3702(6) 0.3287(5) 0.068(2) Uani 1 1 d . . . H8A H 0.3949 0.3150 0.3181 0.102 Uiso 1 1 calc R . . H8B H 0.5488 0.3925 0.2909 0.102 Uiso 1 1 calc R . . H8C H 0.5107 0.4560 0.3490 0.102 Uiso 1 1 calc R . . C9 C 0.4509(7) 0.2613(8) 0.4351(4) 0.079(3) Uani 1 1 d . . . H9A H 0.4774 0.3503 0.4546 0.118 Uiso 1 1 calc R . . H9B H 0.4720 0.2054 0.4631 0.118 Uiso 1 1 calc R . . H9C H 0.3516 0.2125 0.4261 0.118 Uiso 1 1 calc R . . C10 C 0.6972(5) 0.3635(5) 0.3828(2) 0.0296(11) Uani 1 1 d . . . C11 C 0.7375(8) 0.3027(6) 0.4392(3) 0.063(2) Uani 1 1 d . . . H11A H 0.8381 0.3533 0.4443 0.094 Uiso 1 1 calc R . . H11B H 0.7057 0.2048 0.4317 0.094 Uiso 1 1 calc R . . H11C H 0.6938 0.3119 0.4769 0.094 Uiso 1 1 calc R . . C12 C 0.7548(5) 0.5198(5) 0.3956(3) 0.0370(13) Uani 1 1 d . . . Eu1 Eu 0.22452(2) 0.03238(2) 0.15862(2) 0.02265(7) Uani 1 1 d . . . H1M H 0.513(4) 0.101(4) 0.385(2) 0.023(12) Uiso 1 1 d . . . H1W H 0.220(7) -0.086(6) 0.0236(15) 0.10(3) Uiso 1 1 d D . . H2W H 0.191(5) -0.1777(17) 0.065(3) 0.05(2) Uiso 1 1 d D . . O1 O 0.8212(4) 0.6077(4) 0.3519(2) 0.0552(12) Uani 1 1 d . . . O2 O 0.0494(4) -0.0210(4) 0.24006(19) 0.0309(8) Uani 1 1 d . . . O3 O 0.2469(5) -0.0899(4) 0.0609(2) 0.0489(11) Uani 1 1 d D . . O4 O 0.3607(4) 0.0840(4) 0.24944(19) 0.0422(9) Uani 1 1 d . . . O5 O 0.2544(4) 0.0047(4) 0.34181(18) 0.0374(9) Uani 1 1 d . . . O6 O 0.7353(5) 0.5546(4) 0.4477(2) 0.0520(11) Uani 1 1 d . . . O7 O -0.1557(4) -0.1354(4) 0.28744(19) 0.0425(10) 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 C1 0.031(3) 0.040(3) 0.026(3) 0.003(2) 0.002(2) 0.019(2) C2 0.053(4) 0.065(4) 0.046(4) 0.006(3) 0.001(3) 0.044(3) C3 0.034(3) 0.021(2) 0.032(3) -0.005(2) -0.004(2) 0.013(2) C4 0.026(3) 0.027(3) 0.033(3) -0.009(2) -0.008(2) 0.011(2) C5 0.029(3) 0.054(4) 0.060(4) -0.017(3) 0.001(3) 0.017(3) C6 0.035(3) 0.059(4) 0.062(4) -0.004(4) 0.013(3) 0.013(3) C7 0.029(3) 0.031(3) 0.042(3) -0.013(2) -0.003(2) 0.007(2) C8 0.063(4) 0.034(3) 0.111(6) -0.017(4) -0.047(5) 0.027(3) C9 0.056(4) 0.067(5) 0.072(6) -0.042(4) 0.019(4) -0.001(4) C10 0.023(3) 0.027(3) 0.032(3) -0.003(2) -0.004(2) 0.008(2) C11 0.081(5) 0.039(3) 0.070(5) 0.000(3) -0.026(4) 0.031(4) C12 0.028(3) 0.032(3) 0.037(4) 0.000(3) -0.011(2) 0.006(2) Eu1 0.02435(12) 0.02193(12) 0.02313(11) 0.00153(11) 0.00043(10) 0.01266(10) O1 0.033(2) 0.032(2) 0.073(3) 0.021(2) -0.001(2) -0.0039(18) O2 0.030(2) 0.035(2) 0.0309(19) 0.0035(14) 0.0047(16) 0.0188(15) O3 0.078(3) 0.052(3) 0.033(3) -0.0019(19) -0.001(2) 0.045(3) O4 0.041(2) 0.048(2) 0.029(2) -0.0005(18) -0.0076(17) 0.0162(18) O5 0.0263(18) 0.0332(19) 0.034(2) -0.0029(15) 0.0015(15) 0.0012(16) O6 0.068(3) 0.036(2) 0.044(3) -0.0158(19) -0.017(2) 0.021(2) O7 0.031(2) 0.059(3) 0.041(3) 0.015(2) 0.0083(17) 0.0246(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O7 1.257(6) . ? C1 O2 1.274(5) . ? C1 C2 1.496(7) . ? C1 Eu1 2.932(6) 5 ? C3 O4 1.247(6) . ? C3 O5 1.260(6) . ? C3 C4 1.526(7) . ? C4 C5 1.506(7) . ? C4 C7 1.562(7) . ? C5 C6 1.545(8) . ? C6 C10 1.529(8) . ? C7 C9 1.526(9) . ? C7 C8 1.528(9) . ? C7 C10 1.569(7) . ? C10 C12 1.522(7) . ? C10 C11 1.534(8) . ? C12 O6 1.219(7) . ? C12 O1 1.269(6) . ? Eu1 O4 2.321(4) . ? Eu1 O1 2.322(3) 6_544 ? Eu1 O6 2.331(4) 2_654 ? Eu1 O5 2.331(3) 6_554 ? Eu1 O2 2.421(4) . ? Eu1 O2 2.538(4) 6_554 ? Eu1 O3 2.540(4) . ? Eu1 O7 2.557(3) 6_554 ? Eu1 C1 2.932(6) 6_554 ? Eu1 Eu1 4.20886(13) 6_554 ? Eu1 Eu1 4.20886(13) 5 ? O1 Eu1 2.322(3) 5_665 ? O2 Eu1 2.538(4) 5 ? O5 Eu1 2.331(3) 5 ? O6 Eu1 2.331(4) 3_665 ? O7 Eu1 2.557(3) 5 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 C1 O2 120.0(5) . . ? O7 C1 C2 120.4(5) . . ? O2 C1 C2 119.6(5) . . ? O7 C1 Eu1 60.4(3) . 5 ? O2 C1 Eu1 59.6(3) . 5 ? C2 C1 Eu1 176.1(4) . 5 ? O4 C3 O5 124.3(5) . . ? O4 C3 C4 118.8(4) . . ? O5 C3 C4 116.9(4) . . ? C5 C4 C3 115.5(4) . . ? C5 C4 C7 108.0(4) . . ? C3 C4 C7 111.3(4) . . ? C4 C5 C6 104.9(5) . . ? C10 C6 C5 107.6(4) . . ? C9 C7 C8 108.5(6) . . ? C9 C7 C4 112.2(5) . . ? C8 C7 C4 110.7(5) . . ? C9 C7 C10 113.8(5) . . ? C8 C7 C10 110.4(4) . . ? C4 C7 C10 101.1(4) . . ? C12 C10 C6 116.4(4) . . ? C12 C10 C11 107.6(4) . . ? C6 C10 C11 109.2(5) . . ? C12 C10 C7 110.3(4) . . ? C6 C10 C7 102.1(4) . . ? C11 C10 C7 111.3(5) . . ? O6 C12 O1 123.0(5) . . ? O6 C12 C10 118.2(5) . . ? O1 C12 C10 118.8(5) . . ? O4 Eu1 O1 75.49(14) . 6_544 ? O4 Eu1 O6 81.19(15) . 2_654 ? O1 Eu1 O6 108.06(15) 6_544 2_654 ? O4 Eu1 O5 84.00(14) . 6_554 ? O1 Eu1 O5 157.14(15) 6_544 6_554 ? O6 Eu1 O5 78.06(14) 2_654 6_554 ? O4 Eu1 O2 78.73(13) . . ? O1 Eu1 O2 86.95(14) 6_544 . ? O6 Eu1 O2 150.95(14) 2_654 . ? O5 Eu1 O2 79.15(13) 6_554 . ? O4 Eu1 O2 159.91(13) . 6_554 ? O1 Eu1 O2 122.63(13) 6_544 6_554 ? O6 Eu1 O2 99.17(14) 2_654 6_554 ? O5 Eu1 O2 76.49(13) 6_554 6_554 ? O2 Eu1 O2 92.75(9) . 6_554 ? O4 Eu1 O3 125.60(14) . . ? O1 Eu1 O3 69.11(15) 6_544 . ? O6 Eu1 O3 72.55(15) 2_654 . ? O5 Eu1 O3 132.75(13) 6_554 . ? O2 Eu1 O3 136.49(14) . . ? O2 Eu1 O3 72.75(13) 6_554 . ? O4 Eu1 O7 137.87(13) . 6_554 ? O1 Eu1 O7 76.26(13) 6_544 6_554 ? O6 Eu1 O7 137.66(14) 2_654 6_554 ? O5 Eu1 O7 114.61(14) 6_554 6_554 ? O2 Eu1 O7 69.16(13) . 6_554 ? O2 Eu1 O7 50.94(11) 6_554 6_554 ? O3 Eu1 O7 70.09(14) . 6_554 ? O4 Eu1 C1 158.03(14) . 6_554 ? O1 Eu1 C1 99.69(14) 6_544 6_554 ? O6 Eu1 C1 120.32(16) 2_654 6_554 ? O5 Eu1 C1 95.58(14) 6_554 6_554 ? O2 Eu1 C1 79.62(14) . 6_554 ? O2 Eu1 C1 25.65(11) 6_554 6_554 ? O3 Eu1 C1 69.89(16) . 6_554 ? O7 Eu1 C1 25.30(12) 6_554 6_554 ? O4 Eu1 Eu1 140.86(9) . 6_554 ? O1 Eu1 Eu1 136.42(11) 6_544 6_554 ? O6 Eu1 Eu1 68.44(12) 2_654 6_554 ? O5 Eu1 Eu1 66.44(9) 6_554 6_554 ? O2 Eu1 Eu1 117.52(8) . 6_554 ? O2 Eu1 Eu1 31.09(7) 6_554 6_554 ? O3 Eu1 Eu1 68.66(10) . 6_554 ? O7 Eu1 Eu1 79.87(8) 6_554 6_554 ? C1 Eu1 Eu1 55.44(10) 6_554 6_554 ? O4 Eu1 Eu1 61.43(9) . 5 ? O1 Eu1 Eu1 56.92(12) 6_544 5 ? O6 Eu1 Eu1 141.69(12) 2_654 5 ? O5 Eu1 Eu1 104.32(9) 6_554 5 ? O2 Eu1 Eu1 32.78(8) . 5 ? O2 Eu1 Eu1 118.76(7) 6_554 5 ? O3 Eu1 Eu1 121.71(10) . 5 ? O7 Eu1 Eu1 77.03(9) 6_554 5 ? C1 Eu1 Eu1 97.72(11) 6_554 5 ? Eu1 Eu1 Eu1 148.277(2) 6_554 5 ? C12 O1 Eu1 144.5(4) . 5_665 ? C1 O2 Eu1 141.6(3) . . ? C1 O2 Eu1 94.8(3) . 5 ? Eu1 O2 Eu1 116.14(11) . 5 ? C3 O4 Eu1 147.1(3) . . ? C3 O5 Eu1 134.4(3) . 5 ? C12 O6 Eu1 131.7(4) . 3_665 ? C1 O7 Eu1 94.3(3) . 5 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 C3 C4 C5 -22.4(7) . . . . ? O5 C3 C4 C5 157.4(5) . . . . ? O4 C3 C4 C7 101.1(5) . . . . ? O5 C3 C4 C7 -79.1(6) . . . . ? C3 C4 C5 C6 138.0(5) . . . . ? C7 C4 C5 C6 12.8(6) . . . . ? C4 C5 C6 C10 13.4(7) . . . . ? C5 C4 C7 C9 -154.6(5) . . . . ? C3 C4 C7 C9 77.7(6) . . . . ? C5 C4 C7 C8 84.0(6) . . . . ? C3 C4 C7 C8 -43.7(6) . . . . ? C5 C4 C7 C10 -33.0(6) . . . . ? C3 C4 C7 C10 -160.7(4) . . . . ? C5 C6 C10 C12 -153.7(5) . . . . ? C5 C6 C10 C11 84.3(6) . . . . ? C5 C6 C10 C7 -33.6(6) . . . . ? C9 C7 C10 C12 -75.6(6) . . . . ? C8 C7 C10 C12 46.6(6) . . . . ? C4 C7 C10 C12 163.9(4) . . . . ? C9 C7 C10 C6 160.1(5) . . . . ? C8 C7 C10 C6 -77.7(6) . . . . ? C4 C7 C10 C6 39.6(5) . . . . ? C9 C7 C10 C11 43.8(7) . . . . ? C8 C7 C10 C11 166.0(5) . . . . ? C4 C7 C10 C11 -76.8(6) . . . . ? C6 C10 C12 O6 -169.5(5) . . . . ? C11 C10 C12 O6 -46.7(7) . . . . ? C7 C10 C12 O6 74.9(6) . . . . ? C6 C10 C12 O1 10.3(7) . . . . ? C11 C10 C12 O1 133.1(5) . . . . ? C7 C10 C12 O1 -105.4(5) . . . . ? O6 C12 O1 Eu1 56.0(10) . . . 5_665 ? C10 C12 O1 Eu1 -123.8(6) . . . 5_665 ? O7 C1 O2 Eu1 142.4(4) . . . . ? C2 C1 O2 Eu1 -39.7(9) . . . . ? Eu1 C1 O2 Eu1 144.7(6) 5 . . . ? O7 C1 O2 Eu1 -2.3(6) . . . 5 ? C2 C1 O2 Eu1 175.6(5) . . . 5 ? O4 Eu1 O2 C1 166.1(6) . . . . ? O1 Eu1 O2 C1 -118.1(6) 6_544 . . . ? O6 Eu1 O2 C1 119.0(6) 2_654 . . . ? O5 Eu1 O2 C1 80.2(6) 6_554 . . . ? O2 Eu1 O2 C1 4.5(6) 6_554 . . . ? O3 Eu1 O2 C1 -63.1(6) . . . . ? O7 Eu1 O2 C1 -41.6(6) 6_554 . . . ? C1 Eu1 O2 C1 -17.6(5) 6_554 . . . ? Eu1 Eu1 O2 C1 24.2(6) 6_554 . . . ? Eu1 Eu1 O2 C1 -140.1(7) 5 . . . ? O4 Eu1 O2 Eu1 -53.75(16) . . . 5 ? O1 Eu1 O2 Eu1 22.05(17) 6_544 . . 5 ? O6 Eu1 O2 Eu1 -100.9(3) 2_654 . . 5 ? O5 Eu1 O2 Eu1 -139.72(19) 6_554 . . 5 ? O2 Eu1 O2 Eu1 144.60(8) 6_554 . . 5 ? O3 Eu1 O2 Eu1 77.0(2) . . . 5 ? O7 Eu1 O2 Eu1 98.50(18) 6_554 . . 5 ? C1 Eu1 O2 Eu1 122.48(18) 6_554 . . 5 ? Eu1 Eu1 O2 Eu1 164.26(10) 6_554 . . 5 ? O5 C3 O4 Eu1 3.1(10) . . . . ? C4 C3 O4 Eu1 -177.1(4) . . . . ? O1 Eu1 O4 C3 -75.4(6) 6_544 . . . ? O6 Eu1 O4 C3 173.3(6) 2_654 . . . ? O5 Eu1 O4 C3 94.5(6) 6_554 . . . ? O2 Eu1 O4 C3 14.4(6) . . . . ? O2 Eu1 O4 C3 80.7(7) 6_554 . . . ? O3 Eu1 O4 C3 -125.7(6) . . . . ? O7 Eu1 O4 C3 -26.1(7) 6_554 . . . ? C1 Eu1 O4 C3 4.4(9) 6_554 . . . ? Eu1 Eu1 O4 C3 134.5(6) 6_554 . . . ? Eu1 Eu1 O4 C3 -15.4(6) 5 . . . ? O4 C3 O5 Eu1 29.3(8) . . . 5 ? C4 C3 O5 Eu1 -150.5(3) . . . 5 ? O1 C12 O6 Eu1 -2.6(8) . . . 3_665 ? C10 C12 O6 Eu1 177.2(3) . . . 3_665 ? O2 C1 O7 Eu1 2.3(6) . . . 5 ? C2 C1 O7 Eu1 -175.6(5) . . . 5 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.435 _refine_diff_density_min -0.404 _refine_diff_density_rms 0.069 #================================================================end data_4 _database_code_depnum_ccdc_archive 'CCDC 821191' #TrackingRef '- CEC-R2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_absolute_configuration 0 _chemical_formula_moiety ? _chemical_formula_sum 'C12 H19 Dy O7' _chemical_formula_weight 437.76 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' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M P6(5) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+2/3' '-x+y, -x, z+1/3' '-x, -y, z+1/2' 'y, -x+y, z+1/6' 'x-y, x, z+5/6' _cell_length_a 10.8956(2) _cell_length_b 10.8956(2) _cell_length_c 20.9289(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2151.69(14) _cell_formula_units_Z 6 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 5698 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 27.45 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.018 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1266 _exptl_absorpt_coefficient_mu 5.236 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.3789 _exptl_absorpt_correction_T_max 0.4207 _exptl_absorpt_process_details ; Higashi, T. . Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10352 _diffrn_reflns_av_R_equivalents 0.0316 _diffrn_reflns_av_sigmaI/netI 0.0377 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 24.99 _reflns_number_total 2501 _reflns_number_gt 2338 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0118P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment refu _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.009(12) _refine_ls_number_reflns 2501 _refine_ls_number_parameters 185 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0244 _refine_ls_R_factor_gt 0.0213 _refine_ls_wR_factor_ref 0.0379 _refine_ls_wR_factor_gt 0.0372 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _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 C1 C 0.2637(6) 0.5676(6) 0.3828(3) 0.0507(18) Uani 1 1 d . . . H1A H 0.1626 0.5157 0.3775 0.076 Uiso 1 1 calc R . . H1B H 0.2977 0.5025 0.3891 0.076 Uiso 1 1 calc R . . H1C H 0.3070 0.6236 0.3453 0.076 Uiso 1 1 calc R . . C2 C 0.2395(5) 0.7628(5) 0.4301(3) 0.0314(14) Uani 1 1 d . . . C3 C 0.3017(4) 0.6656(5) 0.4414(3) 0.0238(12) Uani 1 1 d . . . C4 C 0.2541(5) 0.5788(6) 0.5033(4) 0.0470(16) Uani 1 1 d . . . H4A H 0.2400 0.6321 0.5368 0.056 Uiso 1 1 calc R . . H4B H 0.1657 0.4911 0.4965 0.056 Uiso 1 1 calc R . . C5 C 0.4656(5) 0.7554(5) 0.4510(3) 0.0320(14) Uani 1 1 d . . . C6 C 0.5046(5) 0.8781(5) 0.4973(4) 0.0530(18) Uani 1 1 d . . . H6A H 0.6034 0.9219 0.5078 0.079 Uiso 1 1 calc R . . H6B H 0.4490 0.8428 0.5355 0.079 Uiso 1 1 calc R . . H6C H 0.4860 0.9466 0.4775 0.079 Uiso 1 1 calc R . . C7 C 0.5506(6) 0.8181(7) 0.3899(4) 0.065(2) Uani 1 1 d . . . H7A H 0.5239 0.8817 0.3710 0.098 Uiso 1 1 calc R . . H7B H 0.5314 0.7432 0.3604 0.098 Uiso 1 1 calc R . . H7C H 0.6499 0.8690 0.3998 0.098 Uiso 1 1 calc R . . C8 C 0.4992(5) 0.6460(5) 0.4815(3) 0.0249(13) Uani 1 1 d . . . C9 C 0.3714(5) 0.5477(5) 0.5220(3) 0.0447(18) Uani 1 1 d . . . H9A H 0.3935 0.5663 0.5671 0.054 Uiso 1 1 calc R . . H9B H 0.3425 0.4495 0.5134 0.054 Uiso 1 1 calc R . . C10 C 1.0479(5) 1.0760(5) 0.4110(3) 0.0248(12) Uani 1 1 d . . . C11 C 0.9628(6) 1.1258(6) 0.4485(3) 0.0453(17) Uani 1 1 d . . . H11A H 1.0254 1.2058 0.4742 0.068 Uiso 1 1 calc R . . H11B H 0.8968 1.0505 0.4756 0.068 Uiso 1 1 calc R . . H11C H 0.9119 1.1526 0.4196 0.068 Uiso 1 1 calc R . . C12 C 0.6396(5) 0.7139(5) 0.5169(3) 0.0219(12) Uani 1 1 d . . . Dy1 Dy 0.96718(2) 0.77661(2) 0.49958(3) 0.01892(6) Uani 1 1 d . . . O1 O 1.0241(4) 0.9499(3) 0.4184(2) 0.0247(9) Uani 1 1 d . . . O2 O 0.7494(3) 0.7555(4) 0.48284(19) 0.0332(10) Uani 1 1 d . . . O3 O 1.1386(4) 1.1559(4) 0.37138(19) 0.0361(10) Uani 1 1 d . . . O4 O 1.0885(4) 0.7528(4) 0.5977(2) 0.0426(11) Uani 1 1 d . . . O5 O 0.2576(4) 0.8181(4) 0.3774(2) 0.0425(11) Uani 1 1 d . . . O6 O 0.1740(3) 0.7823(4) 0.47458(19) 0.0414(11) Uani 1 1 d . . . O7 O 0.6412(3) 0.7284(4) 0.57595(19) 0.0329(9) Uani 1 1 d . . . H1M H 0.4961 0.5930 0.4436 0.049 Uiso 1 1 d R . . 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 C1 0.065(4) 0.050(4) 0.053(5) -0.018(4) -0.022(4) 0.041(3) C2 0.019(3) 0.033(3) 0.041(5) -0.010(3) -0.011(3) 0.013(2) C3 0.018(2) 0.027(3) 0.025(3) -0.001(2) -0.007(2) 0.011(2) C4 0.037(3) 0.052(3) 0.054(5) 0.021(4) 0.010(4) 0.024(3) C5 0.021(3) 0.037(3) 0.037(4) 0.014(3) -0.002(3) 0.014(2) C6 0.048(3) 0.034(3) 0.080(5) -0.023(4) -0.033(4) 0.023(3) C7 0.040(4) 0.104(6) 0.053(5) 0.041(4) 0.012(4) 0.036(4) C8 0.025(2) 0.025(2) 0.028(4) 0.007(2) 0.000(2) 0.015(2) C9 0.027(3) 0.040(3) 0.060(5) 0.018(3) 0.002(3) 0.011(2) C10 0.034(3) 0.023(2) 0.020(3) -0.003(3) -0.002(3) 0.015(2) C11 0.062(4) 0.047(3) 0.044(5) 0.002(3) 0.009(3) 0.040(3) C12 0.033(3) 0.022(2) 0.020(4) 0.002(2) -0.004(2) 0.020(2) Dy1 0.01840(11) 0.02065(11) 0.01876(11) 0.00044(11) 0.00164(12) 0.01055(9) O1 0.0253(18) 0.0233(19) 0.027(2) 0.0053(18) 0.0030(15) 0.0133(14) O2 0.0228(18) 0.054(2) 0.027(3) 0.005(2) 0.0046(17) 0.0217(16) O3 0.056(3) 0.029(2) 0.028(3) 0.0067(19) 0.015(2) 0.0243(19) O4 0.044(2) 0.060(2) 0.038(3) 0.009(2) 0.003(2) 0.037(2) O5 0.057(3) 0.050(2) 0.033(3) 0.005(2) -0.007(2) 0.036(2) O6 0.0282(19) 0.060(2) 0.047(3) -0.012(2) 0.0012(19) 0.0306(19) O7 0.0294(19) 0.050(2) 0.020(2) -0.003(2) -0.0018(18) 0.0204(18) _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 C1 C3 1.539(8) . ? C2 O5 1.226(7) . ? C2 O6 1.254(6) . ? C2 C3 1.534(6) . ? C3 C4 1.534(8) . ? C3 C5 1.562(6) . ? C4 C9 1.528(7) . ? C5 C7 1.526(8) . ? C5 C6 1.528(8) . ? C5 C8 1.549(6) . ? C8 C12 1.518(6) . ? C8 C9 1.521(7) . ? C10 O3 1.249(6) . ? C10 O1 1.274(5) . ? C10 C11 1.508(7) . ? C10 Dy1 2.887(6) 6_654 ? C12 O7 1.244(6) . ? C12 O2 1.267(6) . ? Dy1 O6 2.284(3) 1_655 ? Dy1 O5 2.285(4) 5 ? Dy1 O7 2.286(4) 6_654 ? Dy1 O2 2.293(3) . ? Dy1 O1 2.380(4) . ? Dy1 O1 2.487(4) 5_565 ? Dy1 O3 2.522(3) 5_565 ? Dy1 O4 2.525(4) . ? Dy1 C10 2.887(6) 5_565 ? O1 Dy1 2.487(4) 6_654 ? O3 Dy1 2.522(3) 6_654 ? O5 Dy1 2.285(4) 6_554 ? O6 Dy1 2.284(3) 1_455 ? O7 Dy1 2.286(4) 5_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 O5 C2 O6 123.3(5) . . ? O5 C2 C3 117.4(5) . . ? O6 C2 C3 119.2(5) . . ? C4 C3 C2 115.1(4) . . ? C4 C3 C1 110.7(5) . . ? C2 C3 C1 107.3(4) . . ? C4 C3 C5 101.8(4) . . ? C2 C3 C5 110.4(4) . . ? C1 C3 C5 111.4(4) . . ? C9 C4 C3 106.9(4) . . ? C7 C5 C6 107.3(5) . . ? C7 C5 C8 111.4(4) . . ? C6 C5 C8 110.0(5) . . ? C7 C5 C3 114.8(5) . . ? C6 C5 C3 111.2(4) . . ? C8 C5 C3 102.0(4) . . ? C12 C8 C9 114.6(5) . . ? C12 C8 C5 113.2(4) . . ? C9 C8 C5 106.6(4) . . ? C8 C9 C4 105.9(5) . . ? O3 C10 O1 119.8(5) . . ? O3 C10 C11 120.6(5) . . ? O1 C10 C11 119.6(5) . . ? O3 C10 Dy1 60.7(3) . 6_654 ? O1 C10 Dy1 59.2(3) . 6_654 ? C11 C10 Dy1 175.3(4) . 6_654 ? O7 C12 O2 124.2(5) . . ? O7 C12 C8 119.6(4) . . ? O2 C12 C8 116.1(5) . . ? O6 Dy1 O5 107.73(13) 1_655 5 ? O6 Dy1 O7 76.22(13) 1_655 6_654 ? O5 Dy1 O7 81.41(14) 5 6_654 ? O6 Dy1 O2 157.67(15) 1_655 . ? O5 Dy1 O2 78.01(14) 5 . ? O7 Dy1 O2 83.56(13) 6_654 . ? O6 Dy1 O1 87.30(12) 1_655 . ? O5 Dy1 O1 151.29(14) 5 . ? O7 Dy1 O1 78.62(12) 6_654 . ? O2 Dy1 O1 79.43(12) . . ? O6 Dy1 O1 122.90(12) 1_655 5_565 ? O5 Dy1 O1 97.65(13) 5 5_565 ? O7 Dy1 O1 159.53(12) 6_654 5_565 ? O2 Dy1 O1 76.28(13) . 5_565 ? O1 Dy1 O1 94.00(9) . 5_565 ? O6 Dy1 O3 76.39(13) 1_655 5_565 ? O5 Dy1 O3 136.97(14) 5 5_565 ? O7 Dy1 O3 138.45(12) 6_654 5_565 ? O2 Dy1 O3 114.69(14) . 5_565 ? O1 Dy1 O3 69.47(13) . 5_565 ? O1 Dy1 O3 51.65(11) 5_565 5_565 ? O6 Dy1 O4 68.21(14) 1_655 . ? O5 Dy1 O4 72.66(13) 5 . ? O7 Dy1 O4 125.88(12) 6_654 . ? O2 Dy1 O4 133.05(13) . . ? O1 Dy1 O4 136.04(12) . . ? O1 Dy1 O4 72.33(13) 5_565 . ? O3 Dy1 O4 69.55(12) 5_565 . ? O6 Dy1 C10 99.94(13) 1_655 5_565 ? O5 Dy1 C10 119.36(16) 5 5_565 ? O7 Dy1 C10 158.65(14) 6_654 5_565 ? O2 Dy1 C10 95.45(13) . 5_565 ? O1 Dy1 C10 80.24(15) . 5_565 ? O1 Dy1 C10 26.09(11) 5_565 5_565 ? O3 Dy1 C10 25.58(12) 5_565 5_565 ? O4 Dy1 C10 69.48(14) . 5_565 ? C10 O1 Dy1 140.8(3) . . ? C10 O1 Dy1 94.7(3) . 6_654 ? Dy1 O1 Dy1 117.67(10) . 6_654 ? C12 O2 Dy1 134.0(3) . . ? C10 O3 Dy1 93.7(3) . 6_654 ? C2 O5 Dy1 133.4(4) . 6_554 ? C2 O6 Dy1 143.4(4) . 1_455 ? C12 O7 Dy1 146.7(3) . 5_565 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O5 C2 C3 C4 -169.6(5) . . . . ? O6 C2 C3 C4 10.7(7) . . . . ? O5 C2 C3 C1 -45.7(6) . . . . ? O6 C2 C3 C1 134.5(5) . . . . ? O5 C2 C3 C5 75.8(6) . . . . ? O6 C2 C3 C5 -103.9(5) . . . . ? C2 C3 C4 C9 -153.6(4) . . . . ? C1 C3 C4 C9 84.4(5) . . . . ? C5 C3 C4 C9 -34.2(6) . . . . ? C4 C3 C5 C7 161.2(5) . . . . ? C2 C3 C5 C7 -76.1(6) . . . . ? C1 C3 C5 C7 43.1(6) . . . . ? C4 C3 C5 C6 -76.7(5) . . . . ? C2 C3 C5 C6 46.0(7) . . . . ? C1 C3 C5 C6 165.2(5) . . . . ? C4 C3 C5 C8 40.5(5) . . . . ? C2 C3 C5 C8 163.3(5) . . . . ? C1 C3 C5 C8 -77.6(6) . . . . ? C7 C5 C8 C12 77.1(6) . . . . ? C6 C5 C8 C12 -41.9(6) . . . . ? C3 C5 C8 C12 -159.9(4) . . . . ? C7 C5 C8 C9 -156.0(5) . . . . ? C6 C5 C8 C9 85.0(5) . . . . ? C3 C5 C8 C9 -33.0(6) . . . . ? C12 C8 C9 C4 138.4(5) . . . . ? C5 C8 C9 C4 12.3(6) . . . . ? C3 C4 C9 C8 14.0(6) . . . . ? C9 C8 C12 O7 -24.6(6) . . . . ? C5 C8 C12 O7 98.0(5) . . . . ? C9 C8 C12 O2 157.0(4) . . . . ? C5 C8 C12 O2 -80.5(5) . . . . ? O3 C10 O1 Dy1 143.9(4) . . . . ? C11 C10 O1 Dy1 -38.2(9) . . . . ? Dy1 C10 O1 Dy1 147.0(5) 6_654 . . . ? O3 C10 O1 Dy1 -3.2(6) . . . 6_654 ? C11 C10 O1 Dy1 174.8(5) . . . 6_654 ? O6 Dy1 O1 C10 -119.7(6) 1_655 . . . ? O5 Dy1 O1 C10 117.0(6) 5 . . . ? O7 Dy1 O1 C10 163.8(6) 6_654 . . . ? O2 Dy1 O1 C10 78.3(6) . . . . ? O1 Dy1 O1 C10 3.1(6) 5_565 . . . ? O3 Dy1 O1 C10 -43.3(5) 5_565 . . . ? O4 Dy1 O1 C10 -65.5(6) . . . . ? C10 Dy1 O1 C10 -19.2(5) 5_565 . . . ? O6 Dy1 O1 Dy1 22.50(17) 1_655 . . 6_654 ? O5 Dy1 O1 Dy1 -100.8(3) 5 . . 6_654 ? O7 Dy1 O1 Dy1 -53.97(16) 6_654 . . 6_654 ? O2 Dy1 O1 Dy1 -139.45(19) . . . 6_654 ? O1 Dy1 O1 Dy1 145.31(8) 5_565 . . 6_654 ? O3 Dy1 O1 Dy1 98.97(18) 5_565 . . 6_654 ? O4 Dy1 O1 Dy1 76.8(2) . . . 6_654 ? C10 Dy1 O1 Dy1 123.07(18) 5_565 . . 6_654 ? O7 C12 O2 Dy1 32.0(7) . . . . ? C8 C12 O2 Dy1 -149.6(3) . . . . ? O6 Dy1 O2 C12 151.0(4) 1_655 . . . ? O5 Dy1 O2 C12 43.4(4) 5 . . . ? O7 Dy1 O2 C12 125.9(4) 6_654 . . . ? O1 Dy1 O2 C12 -154.5(5) . . . . ? O1 Dy1 O2 C12 -57.7(4) 5_565 . . . ? O3 Dy1 O2 C12 -93.1(5) 5_565 . . . ? O4 Dy1 O2 C12 -8.6(5) . . . . ? C10 Dy1 O2 C12 -75.5(5) 5_565 . . . ? O1 C10 O3 Dy1 3.1(5) . . . 6_654 ? C11 C10 O3 Dy1 -174.8(5) . . . 6_654 ? O6 C2 O5 Dy1 -0.9(8) . . . 6_554 ? C3 C2 O5 Dy1 179.4(3) . . . 6_554 ? O5 C2 O6 Dy1 51.7(9) . . . 1_455 ? C3 C2 O6 Dy1 -128.6(5) . . . 1_455 ? O2 C12 O7 Dy1 -0.5(9) . . . 5_565 ? C8 C12 O7 Dy1 -178.8(4) . . . 5_565 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.430 _refine_diff_density_min -0.368 _refine_diff_density_rms 0.080