# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr yong xing' _publ_contact_author_email yhxing2000@yahoo.com _publ_section_title ; A Novel Family of 3D Photoluminescent Lanthanide-Bta-Flexible MOFs Constructed from 1,2,4,5-Benzenetetracarboxylic Acid and Different Spanning of Dicarboxylate Acid Ligands ; loop_ _publ_author_name y.xing K.-L.Hou Bai, Feng-Ying' J.-L.Wang Z.Shi # Attachment '- 1.cif' data_1a _database_code_depnum_ccdc_archive 'CCDC 761941' #TrackingRef '- 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H10 Eu2 O16' _chemical_formula_weight 714.12 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' Eu Eu -0.1578 3.6682 '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' 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 6.2301(12) _cell_length_b 8.6277(17) _cell_length_c 8.9610(18) _cell_angle_alpha 110.70(3) _cell_angle_beta 110.27(3) _cell_angle_gamma 91.49(3) _cell_volume 416.58(14) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3909 _cell_measurement_theta_min 3.515 _cell_measurement_theta_max 27.415 _exptl_crystal_description block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.847 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 336 _exptl_absorpt_coefficient_mu 7.553 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2974 _exptl_absorpt_correction_T_max 0.6277 _exptl_absorpt_process_details 'Higashi, T. (1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID IP' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 4095 _diffrn_reflns_av_R_equivalents 0.0218 _diffrn_reflns_av_sigmaI/netI 0.0278 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.51 _diffrn_reflns_theta_max 27.42 _reflns_number_total 1871 _reflns_number_gt 1804 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Rgaku R-AXIS RAPID' _computing_cell_refinement 'Rgaku R-AXIS RAPID' _computing_data_reduction 'Rgaku R-AXIS RAPID' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXP-97 _computing_publication_material SHELXP-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.6318P] 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 1871 _refine_ls_number_parameters 152 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0164 _refine_ls_R_factor_gt 0.0155 _refine_ls_wR_factor_ref 0.0352 _refine_ls_wR_factor_gt 0.0350 _refine_ls_goodness_of_fit_ref 1.111 _refine_ls_restrained_S_all 1.111 _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 H1WA H 1.275(8) 0.285(6) 0.304(6) 0.043(15) Uiso 1 1 d . . . H1WB H 1.255(7) 0.341(5) 0.434(6) 0.029(11) Uiso 1 1 d . . . H2WA H 1.135(8) 0.272(6) 0.022(6) 0.042(14) Uiso 1 1 d . . . H2WB H 0.986(6) 0.328(5) -0.084(5) 0.020(9) Uiso 1 1 d . . . C2 C 0.5074(5) 0.1557(3) 0.6267(3) 0.0096(5) Uani 1 1 d . . . Eu1 Eu 0.80927(2) 0.355009(16) 0.186951(16) 0.00916(5) Uani 1 1 d . . . C1 C 0.6457(5) 0.1426(3) 0.5298(3) 0.0104(5) Uani 1 1 d . . . C3 C 0.6363(5) -0.0123(3) 0.4043(3) 0.0121(5) Uani 1 1 d . . . H3 H 0.7280 -0.0201 0.3401 0.014 Uiso 1 1 calc R . . C4 C 0.8149(5) 0.2924(3) 0.5638(4) 0.0117(5) Uani 1 1 d . . . C5 C 0.4963(5) 0.3214(3) 0.7579(3) 0.0104(5) Uani 1 1 d . . . C6 C 0.6074(5) -0.0373(4) -0.0111(4) 0.0127(6) Uani 1 1 d . . . O1W O 1.1943(4) 0.3113(3) 0.3381(3) 0.0234(5) Uani 1 1 d . . . O1 O 0.8179(4) 0.3248(3) 0.4393(3) 0.0212(5) Uani 1 1 d . . . O2W O 1.0289(4) 0.3183(3) 0.0087(3) 0.0253(5) Uani 1 1 d . . . O2 O 0.9472(4) 0.3754(3) 0.7177(3) 0.0175(4) Uani 1 1 d . . . O3 O 0.4064(4) 0.4291(3) 0.7004(3) 0.0159(4) Uani 1 1 d . . . O4 O 0.5638(4) 0.3379(3) 0.9107(3) 0.0204(5) Uani 1 1 d . . . O5 O 0.7968(4) 0.0568(3) 0.0663(3) 0.0225(5) Uani 1 1 d . . . O6 O 0.4304(4) 0.1918(3) 0.1061(3) 0.0185(4) 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 C2 0.0123(13) 0.0056(12) 0.0083(12) 0.0005(10) 0.0035(10) -0.0001(11) Eu1 0.01123(8) 0.00743(7) 0.00846(7) 0.00219(5) 0.00431(5) 0.00037(5) C1 0.0137(13) 0.0079(12) 0.0088(12) 0.0027(10) 0.0038(10) 0.0005(11) C3 0.0163(14) 0.0114(13) 0.0134(13) 0.0052(11) 0.0108(11) 0.0019(12) C4 0.0134(13) 0.0104(13) 0.0137(13) 0.0051(11) 0.0074(11) 0.0032(11) C5 0.0070(12) 0.0112(13) 0.0109(12) 0.0014(10) 0.0040(10) -0.0006(11) C6 0.0150(15) 0.0100(13) 0.0157(13) 0.0050(11) 0.0088(11) 0.0027(12) O1W 0.0188(12) 0.0368(15) 0.0139(12) 0.0078(11) 0.0068(10) 0.0122(11) O1 0.0315(12) 0.0194(11) 0.0159(10) 0.0081(9) 0.0118(9) -0.0015(10) O2W 0.0259(13) 0.0431(15) 0.0220(12) 0.0223(12) 0.0157(10) 0.0198(12) O2 0.0216(11) 0.0127(10) 0.0130(10) 0.0025(8) 0.0037(8) -0.0056(9) O3 0.0202(11) 0.0110(9) 0.0155(10) 0.0047(8) 0.0060(8) 0.0061(9) O4 0.0277(12) 0.0214(11) 0.0101(10) 0.0044(8) 0.0062(9) 0.0110(10) O5 0.0131(10) 0.0120(10) 0.0350(13) 0.0013(9) 0.0086(9) 0.0001(9) O6 0.0156(10) 0.0107(10) 0.0255(11) 0.0006(8) 0.0102(9) 0.0021(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C2 C3 1.391(4) 2_656 ? C2 C1 1.402(4) . ? C2 C5 1.518(4) . ? Eu1 O1 2.348(2) . ? Eu1 O4 2.365(2) 1_554 ? Eu1 O2W 2.388(2) . ? Eu1 O5 2.400(2) . ? Eu1 O1W 2.426(3) . ? Eu1 O2 2.440(2) 2_766 ? Eu1 O6 2.449(2) . ? Eu1 O3 2.456(2) 2_666 ? C1 C3 1.393(4) . ? C1 C4 1.518(4) . ? C3 C2 1.391(4) 2_656 ? C4 O1 1.249(3) . ? C4 O2 1.256(4) . ? C5 O4 1.238(3) . ? C5 O3 1.268(3) . ? C6 O5 1.232(4) . ? C6 O6 1.265(4) 2_655 ? C6 C6 1.543(5) 2_655 ? O2 Eu1 2.440(2) 2_766 ? O3 Eu1 2.456(2) 2_666 ? O4 Eu1 2.365(2) 1_556 ? O6 C6 1.265(4) 2_655 ? 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 C3 C2 C1 118.9(2) 2_656 . ? C3 C2 C5 118.0(2) 2_656 . ? C1 C2 C5 123.0(2) . . ? O1 Eu1 O4 144.40(8) . 1_554 ? O1 Eu1 O2W 141.36(9) . . ? O4 Eu1 O2W 70.70(8) 1_554 . ? O1 Eu1 O5 87.33(8) . . ? O4 Eu1 O5 88.74(9) 1_554 . ? O2W Eu1 O5 75.63(9) . . ? O1 Eu1 O1W 71.29(9) . . ? O4 Eu1 O1W 140.92(8) 1_554 . ? O2W Eu1 O1W 70.89(9) . . ? O5 Eu1 O1W 75.05(9) . . ? O1 Eu1 O2 105.90(8) . 2_766 ? O4 Eu1 O2 98.44(8) 1_554 2_766 ? O2W Eu1 O2 72.54(9) . 2_766 ? O5 Eu1 O2 142.76(7) . 2_766 ? O1W Eu1 O2 76.64(9) . 2_766 ? O1 Eu1 O6 74.79(8) . . ? O4 Eu1 O6 71.20(8) 1_554 . ? O2W Eu1 O6 125.96(9) . . ? O5 Eu1 O6 66.67(8) . . ? O1W Eu1 O6 129.25(8) . . ? O2 Eu1 O6 150.01(8) 2_766 . ? O1 Eu1 O3 76.44(8) . 2_666 ? O4 Eu1 O3 85.92(8) 1_554 2_666 ? O2W Eu1 O3 135.40(8) . 2_666 ? O5 Eu1 O3 143.05(7) . 2_666 ? O1W Eu1 O3 127.80(9) . 2_666 ? O2 Eu1 O3 74.15(7) 2_766 2_666 ? O6 Eu1 O3 77.03(7) . 2_666 ? C3 C1 C2 119.8(3) . . ? C3 C1 C4 118.8(2) . . ? C2 C1 C4 121.3(2) . . ? C2 C3 C1 121.3(2) 2_656 . ? O1 C4 O2 123.9(3) . . ? O1 C4 C1 119.0(3) . . ? O2 C4 C1 117.2(2) . . ? O4 C5 O3 125.0(3) . . ? O4 C5 C2 117.9(2) . . ? O3 C5 C2 117.0(2) . . ? O5 C6 O6 126.6(3) . 2_655 ? O5 C6 C6 117.7(3) . 2_655 ? O6 C6 C6 115.7(3) 2_655 2_655 ? C4 O1 Eu1 173.9(2) . . ? C4 O2 Eu1 123.63(18) . 2_766 ? C5 O3 Eu1 129.61(17) . 2_666 ? C5 O4 Eu1 160.8(2) . 1_556 ? C6 O5 Eu1 119.33(19) . . ? C6 O6 Eu1 117.66(18) 2_655 . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.42 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.713 _refine_diff_density_min -0.783 _refine_diff_density_rms 0.114 # Attachment '- 3.cif' data_xa _database_code_depnum_ccdc_archive 'CCDC 761942' #TrackingRef '- 3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H10 Dy2 O16' _chemical_formula_weight 735.20 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.2071(8) _cell_length_b 8.5862(18) _cell_length_c 8.8891(11) _cell_angle_alpha 110.938(2) _cell_angle_beta 110.025(2) _cell_angle_gamma 91.761(2) _cell_volume 409.34(11) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1497 _cell_measurement_theta_min 2.58 _cell_measurement_theta_max 28.99 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.982 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 342 _exptl_absorpt_coefficient_mu 9.152 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2174 _exptl_absorpt_correction_T_max 0.5317 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 2197 _diffrn_reflns_av_R_equivalents 0.0211 _diffrn_reflns_av_sigmaI/netI 0.0401 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.58 _diffrn_reflns_theta_max 25.75 _reflns_number_total 1542 _reflns_number_gt 1429 _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^)+(0.0360P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1542 _refine_ls_number_parameters 136 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0295 _refine_ls_R_factor_gt 0.0267 _refine_ls_wR_factor_ref 0.0674 _refine_ls_wR_factor_gt 0.0658 _refine_ls_goodness_of_fit_ref 1.120 _refine_ls_restrained_S_all 1.120 _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 Dy1 Dy 0.30965(5) 0.35305(3) 0.18479(3) 0.01092(12) Uani 1 1 d . . . O1 O 0.5523(8) 0.6202(5) 0.2840(6) 0.0181(10) Uani 1 1 d . . . O2 O 0.6835(8) 0.6747(6) 0.5649(6) 0.0211(11) Uani 1 1 d . . . O1W O 0.6879(9) 0.3102(6) 0.3367(6) 0.0259(11) Uani 1 1 d . . . H1A H 0.7821 0.2785 0.2912 0.039 Uiso 1 1 d R . . H1B H 0.7661 0.3592 0.4409 0.039 Uiso 1 1 d R . . O2W O 0.5283(8) 0.3167(6) 0.0079(6) 0.0259(11) Uani 1 1 d . . . H2A H 0.4895 0.3535 -0.0691 0.039 Uiso 1 1 d R . . H2B H 0.6589 0.2924 0.0251 0.039 Uiso 1 1 d R . . O3 O 0.9033(8) 1.4326(5) 0.7026(5) 0.0142(9) Uani 1 1 d . . . O4 O 1.0738(8) 1.3444(6) 0.9158(6) 0.0207(10) Uani 1 1 d . . . O5 O 0.2974(8) 0.0574(6) 0.0631(6) 0.0230(11) Uani 1 1 d . . . O6 O 0.0685(8) -0.1950(5) -0.1039(6) 0.0189(10) Uani 1 1 d . . . C1 C 0.6832(11) 0.7062(7) 0.4388(8) 0.0127(13) Uani 1 1 d . . . C2 C 0.8526(11) 0.8567(8) 0.4708(8) 0.0130(13) Uani 1 1 d . . . C3 C 0.8615(11) 1.0131(8) 0.5973(8) 0.0144(13) Uani 1 1 d . . . H3 H 0.7698 1.0220 0.6627 0.017 Uiso 1 1 calc R . . C4 C 1.0094(11) 1.1582(7) 0.6264(8) 0.0127(13) Uani 1 1 d . . . C5 C 0.9978(10) 1.3259(7) 0.7589(8) 0.0113(12) Uani 1 1 d . . . C6 C 0.1078(11) -0.0373(8) -0.0116(8) 0.0161(14) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.01192(17) 0.00978(17) 0.01077(18) 0.00409(12) 0.00400(12) 0.00089(11) O1 0.018(2) 0.018(2) 0.013(2) 0.0036(19) 0.0036(19) -0.0034(19) O2 0.026(3) 0.020(2) 0.018(2) 0.007(2) 0.008(2) -0.005(2) O1W 0.028(3) 0.034(3) 0.016(2) 0.009(2) 0.010(2) 0.016(2) O2W 0.018(3) 0.047(3) 0.026(3) 0.023(2) 0.014(2) 0.017(2) O3 0.023(2) 0.011(2) 0.013(2) 0.0066(17) 0.0098(19) 0.0071(18) O4 0.027(3) 0.024(2) 0.012(2) 0.0068(19) 0.008(2) 0.009(2) O5 0.015(2) 0.015(2) 0.036(3) 0.003(2) 0.012(2) 0.0012(19) O6 0.014(2) 0.012(2) 0.029(3) 0.0033(19) 0.012(2) 0.0039(18) C1 0.015(3) 0.013(3) 0.011(3) 0.004(3) 0.007(3) 0.006(2) C2 0.012(3) 0.014(3) 0.011(3) 0.005(2) 0.002(2) -0.001(2) C3 0.015(3) 0.015(3) 0.017(3) 0.006(3) 0.010(3) 0.007(2) C4 0.015(3) 0.008(3) 0.011(3) 0.003(2) 0.002(2) -0.003(2) C5 0.007(3) 0.013(3) 0.014(3) 0.004(3) 0.006(2) 0.000(2) C6 0.019(3) 0.015(3) 0.019(3) 0.010(3) 0.009(3) 0.002(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 O2 2.308(4) 2_666 ? Dy1 O4 2.310(4) 1_444 ? Dy1 O2W 2.355(5) . ? Dy1 O5 2.364(4) . ? Dy1 O1W 2.389(5) . ? Dy1 O1 2.396(4) . ? Dy1 O6 2.412(4) 2 ? Dy1 O3 2.424(4) 2_676 ? O1 C1 1.253(7) . ? O2 C1 1.243(7) . ? O2 Dy1 2.308(4) 2_666 ? O1W H1A 0.8200 . ? O1W H1B 0.8200 . ? O2W H2A 0.8200 . ? O2W H2B 0.8200 . ? O3 C5 1.262(7) . ? O3 Dy1 2.424(4) 2_676 ? O4 C5 1.257(7) . ? O4 Dy1 2.310(4) 1_666 ? O5 C6 1.228(8) . ? O6 C6 1.271(7) . ? O6 Dy1 2.412(4) 2 ? C1 C2 1.518(8) . ? C2 C3 1.394(9) . ? C2 C4 1.390(9) 2_776 ? C3 C4 1.414(8) . ? C3 H3 0.9300 . ? C4 C2 1.390(9) 2_776 ? C4 C5 1.523(8) . ? C6 C6 1.546(13) 2 ? 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 O2 Dy1 O4 145.07(17) 2_666 1_444 ? O2 Dy1 O2W 141.51(17) 2_666 . ? O4 Dy1 O2W 70.69(16) 1_444 . ? O2 Dy1 O5 87.94(17) 2_666 . ? O4 Dy1 O5 90.32(17) 1_444 . ? O2W Dy1 O5 75.34(17) . . ? O2 Dy1 O1W 70.86(17) 2_666 . ? O4 Dy1 O1W 141.67(17) 1_444 . ? O2W Dy1 O1W 71.38(16) . . ? O5 Dy1 O1W 74.98(16) . . ? O2 Dy1 O1 104.90(15) 2_666 . ? O4 Dy1 O1 97.46(16) 1_444 . ? O2W Dy1 O1 73.01(17) . . ? O5 Dy1 O1 142.62(16) . . ? O1W Dy1 O1 76.47(16) . . ? O2 Dy1 O6 75.18(16) 2_666 2 ? O4 Dy1 O6 71.91(16) 1_444 2 ? O2W Dy1 O6 126.37(17) . 2 ? O5 Dy1 O6 67.86(15) . 2 ? O1W Dy1 O6 129.80(16) . 2 ? O1 Dy1 O6 149.06(16) . 2 ? O2 Dy1 O3 76.18(16) 2_666 2_676 ? O4 Dy1 O3 84.83(15) 1_444 2_676 ? O2W Dy1 O3 135.36(16) . 2_676 ? O5 Dy1 O3 143.34(15) . 2_676 ? O1W Dy1 O3 127.52(15) . 2_676 ? O1 Dy1 O3 73.97(15) . 2_676 ? O6 Dy1 O3 76.14(15) 2 2_676 ? C1 O1 Dy1 125.0(4) . . ? C1 O2 Dy1 173.9(4) . 2_666 ? Dy1 O1W H1A 123.7 . . ? Dy1 O1W H1B 126.4 . . ? H1A O1W H1B 105.2 . . ? Dy1 O2W H2A 118.6 . . ? Dy1 O2W H2B 128.6 . . ? H2A O2W H2B 111.0 . . ? C5 O3 Dy1 131.0(4) . 2_676 ? C5 O4 Dy1 162.7(4) . 1_666 ? C6 O5 Dy1 119.0(4) . . ? C6 O6 Dy1 117.7(4) . 2 ? O2 C1 O1 124.2(6) . . ? O2 C1 C2 119.0(5) . . ? O1 C1 C2 116.8(5) . . ? C3 C2 C4 120.4(6) . 2_776 ? C3 C2 C1 118.2(6) . . ? C4 C2 C1 121.4(5) 2_776 . ? C2 C3 C4 120.2(6) . . ? C2 C3 H3 119.9 . . ? C4 C3 H3 119.9 . . ? C2 C4 C3 119.5(6) 2_776 . ? C2 C4 C5 123.6(5) 2_776 . ? C3 C4 C5 116.9(5) . . ? O4 C5 O3 124.9(5) . . ? O4 C5 C4 117.2(5) . . ? O3 C5 C4 117.8(5) . . ? O5 C6 O6 126.7(6) . . ? O5 C6 C6 118.2(7) . 2 ? O6 C6 C6 115.1(7) . 2 ? 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 O2 Dy1 O1 C1 11.3(5) 2_666 . . . ? O4 Dy1 O1 C1 164.2(5) 1_444 . . . ? O2W Dy1 O1 C1 -128.7(5) . . . . ? O5 Dy1 O1 C1 -95.4(5) . . . . ? O1W Dy1 O1 C1 -54.3(5) . . . . ? O6 Dy1 O1 C1 97.2(5) 2 . . . ? O3 Dy1 O1 C1 81.8(5) 2_676 . . . ? O2 Dy1 O5 C6 87.5(5) 2_666 . . . ? O4 Dy1 O5 C6 -57.6(5) 1_444 . . . ? O2W Dy1 O5 C6 -127.5(5) . . . . ? O1W Dy1 O5 C6 158.3(5) . . . . ? O1 Dy1 O5 C6 -160.3(4) . . . . ? O6 Dy1 O5 C6 12.7(5) 2 . . . ? O3 Dy1 O5 C6 24.2(6) 2_676 . . . ? Dy1 O2 C1 O1 -142(4) 2_666 . . . ? Dy1 O2 C1 C2 39(4) 2_666 . . . ? Dy1 O1 C1 O2 -9.2(9) . . . . ? Dy1 O1 C1 C2 170.0(4) . . . . ? O2 C1 C2 C3 -50.9(8) . . . . ? O1 C1 C2 C3 129.9(6) . . . . ? O2 C1 C2 C4 131.2(6) . . . 2_776 ? O1 C1 C2 C4 -48.1(8) . . . 2_776 ? C4 C2 C3 C4 0.7(10) 2_776 . . . ? C1 C2 C3 C4 -177.3(6) . . . . ? C2 C3 C4 C2 -0.7(10) . . . 2_776 ? C2 C3 C4 C5 176.3(6) . . . . ? Dy1 O4 C5 O3 -131.7(12) 1_666 . . . ? Dy1 O4 C5 C4 51.7(16) 1_666 . . . ? Dy1 O3 C5 O4 -26.9(8) 2_676 . . . ? Dy1 O3 C5 C4 149.6(4) 2_676 . . . ? C2 C4 C5 O4 -114.6(7) 2_776 . . . ? C3 C4 C5 O4 68.6(7) . . . . ? C2 C4 C5 O3 68.6(8) 2_776 . . . ? C3 C4 C5 O3 -108.3(6) . . . . ? Dy1 O5 C6 O6 169.5(5) . . . . ? Dy1 O5 C6 C6 -13.0(10) . . . 2 ? Dy1 O6 C6 O5 168.2(5) 2 . . . ? Dy1 O6 C6 C6 -9.4(9) 2 . . 2 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1A O6 0.82 2.10 2.884(7) 161.2 2_655 O1W H1B O3 0.82 2.02 2.822(6) 164.5 1_545 O2W H2A O1 0.82 1.93 2.722(6) 160.9 2_665 O2W H2B O6 0.82 1.94 2.724(6) 160.9 2_655 _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.75 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.592 _refine_diff_density_min -1.565 _refine_diff_density_rms 0.215 # Attachment '- 4.cif' data_1b _database_code_depnum_ccdc_archive 'CCDC 761943' #TrackingRef '- 4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H10 Ho2 O16' _chemical_formula_weight 740.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 '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' 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 6.1931(12) _cell_length_b 8.5776(17) _cell_length_c 8.8684(18) _cell_angle_alpha 111.03(3) _cell_angle_beta 109.97(3) _cell_angle_gamma 91.82(3) _cell_volume 406.84(14) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3883 _cell_measurement_theta_min 3.545 _cell_measurement_theta_max 27.445 _exptl_crystal_description block _exptl_crystal_colour rosiness _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.021 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 344 _exptl_absorpt_coefficient_mu 9.749 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2340 _exptl_absorpt_correction_T_max 0.5056 _exptl_absorpt_process_details 'Higashi, T. (1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID IP' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 3251 _diffrn_reflns_av_R_equivalents 0.0233 _diffrn_reflns_av_sigmaI/netI 0.0278 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.54 _diffrn_reflns_theta_max 24.99 _reflns_number_total 1437 _reflns_number_gt 1413 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Rgaku R-AXIS RAPID' _computing_cell_refinement 'Rgaku R-AXIS RAPID' _computing_data_reduction 'Rgaku R-AXIS RAPID' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXP-97 _computing_publication_material SHELXP-97 _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^)+(0.0166P)^2^+0.7930P] 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 1437 _refine_ls_number_parameters 152 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0179 _refine_ls_R_factor_gt 0.0173 _refine_ls_wR_factor_ref 0.0447 _refine_ls_wR_factor_gt 0.0445 _refine_ls_goodness_of_fit_ref 1.237 _refine_ls_restrained_S_all 1.234 _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 H1WB H 0.204(8) 0.730(8) 0.695(7) 0.05(2) Uiso 1 1 d D . . H2WB H 0.494(10) 0.670(8) 1.085(5) 0.043(19) Uiso 1 1 d D . . H2WA H 0.342(6) 0.715(7) 0.960(7) 0.029(16) Uiso 1 1 d D . . H1WA H 0.254(9) 0.639(7) 0.554(3) 0.033(17) Uiso 1 1 d D . . Ho1 Ho 0.69031(3) 0.64753(2) 0.81595(2) 0.00697(9) Uani 1 1 d . . . C1 C 1.1466(7) 0.1437(5) 0.5288(5) 0.0084(8) Uani 1 1 d . . . C2 C 1.0065(7) 0.1587(5) 0.6273(5) 0.0079(8) Uani 1 1 d . . . C3 C 1.1378(8) -0.0136(5) 0.4028(6) 0.0097(8) Uani 1 1 d . . . H3 H 1.2299 -0.0219 0.3375 0.012 Uiso 1 1 calc R . . C4 C 1.3143(7) 0.2935(5) 0.5599(5) 0.0094(8) Uani 1 1 d . . . C5 C 0.9981(7) 0.3265(5) 0.7605(5) 0.0083(8) Uani 1 1 d . . . C6 C 1.1067(8) 0.9622(5) 0.9892(6) 0.0118(9) Uani 1 1 d . . . O1 O 1.4491(6) 0.3808(4) 0.7156(4) 0.0162(7) Uani 1 1 d . . . O1W O 0.3118(6) 0.6905(5) 0.6641(4) 0.0203(7) Uani 1 1 d D . . O2W O 0.4725(6) 0.6829(5) 0.9921(5) 0.0222(8) Uani 1 1 d D . . O2 O 1.3144(6) 0.3253(4) 0.4338(4) 0.0193(7) Uani 1 1 d . . . O3 O 1.0741(6) 0.3461(4) 0.9163(4) 0.0182(7) Uani 1 1 d . . . O4 O 0.9010(5) 0.4319(4) 0.7032(4) 0.0123(6) Uani 1 1 d . . . O5 O 1.0683(5) 0.8050(4) 0.8965(4) 0.0168(7) Uani 1 1 d . . . O6 O 0.7036(5) 0.9422(4) 0.9379(5) 0.0198(7) 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 Ho1 0.00840(12) 0.00580(12) 0.00610(12) 0.00176(8) 0.00275(9) 0.00034(8) C1 0.009(2) 0.007(2) 0.009(2) 0.0030(16) 0.0028(17) 0.0018(16) C2 0.009(2) 0.0037(19) 0.007(2) 0.0000(16) 0.0011(17) -0.0011(16) C3 0.014(2) 0.010(2) 0.010(2) 0.0048(17) 0.0097(18) 0.0002(17) C4 0.012(2) 0.009(2) 0.010(2) 0.0031(17) 0.0069(18) 0.0038(17) C5 0.0036(19) 0.010(2) 0.008(2) 0.0013(17) 0.0013(17) -0.0014(16) C6 0.016(2) 0.008(2) 0.012(2) 0.0032(18) 0.0065(19) 0.0008(18) O1 0.0191(17) 0.0135(16) 0.0129(16) 0.0049(13) 0.0033(14) -0.0044(13) O1W 0.0154(17) 0.034(2) 0.0085(16) 0.0051(15) 0.0035(14) 0.0093(15) O2W 0.0211(19) 0.038(2) 0.0211(19) 0.0206(17) 0.0139(16) 0.0157(16) O2 0.0275(19) 0.0194(17) 0.0146(17) 0.0085(14) 0.0107(15) -0.0003(14) O3 0.0229(18) 0.0211(17) 0.0071(16) 0.0038(13) 0.0028(14) 0.0094(14) O4 0.0186(17) 0.0077(15) 0.0126(15) 0.0044(12) 0.0076(13) 0.0068(12) O5 0.0140(16) 0.0070(16) 0.0251(18) 0.0000(13) 0.0092(14) 0.0025(12) O6 0.0092(16) 0.0122(16) 0.0307(19) 0.0018(14) 0.0064(15) -0.0015(13) _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 Ho1 O2 2.300(3) 2_766 ? Ho1 O3 2.304(3) 2_767 ? Ho1 O2W 2.341(3) . ? Ho1 O6 2.351(3) . ? Ho1 O1 2.382(3) 1_455 ? Ho1 O1W 2.387(3) . ? Ho1 O5 2.404(3) . ? Ho1 O4 2.417(3) . ? C1 C3 1.394(6) . ? C1 C2 1.406(6) . ? C1 C4 1.507(6) . ? C2 C3 1.396(6) 2_756 ? C2 C5 1.515(6) . ? C3 C2 1.396(6) 2_756 ? C4 O2 1.242(5) . ? C4 O1 1.263(5) . ? C5 O3 1.242(5) . ? C5 O4 1.262(5) . ? C6 O6 1.229(6) 2_777 ? C6 O5 1.266(5) . ? C6 C6 1.530(8) 2_777 ? O1 Ho1 2.382(3) 1_655 ? O2 Ho1 2.299(3) 2_766 ? O3 Ho1 2.304(3) 2_767 ? O6 C6 1.229(6) 2_777 ? 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 O2 Ho1 O3 144.80(13) 2_766 2_767 ? O2 Ho1 O2W 141.87(12) 2_766 . ? O3 Ho1 O2W 70.80(12) 2_767 . ? O2 Ho1 O6 88.04(12) 2_766 . ? O3 Ho1 O6 90.75(13) 2_767 . ? O2W Ho1 O6 75.55(13) . . ? O2 Ho1 O1 104.74(12) 2_766 1_455 ? O3 Ho1 O1 97.18(12) 2_767 1_455 ? O2W Ho1 O1 73.18(13) . 1_455 ? O6 Ho1 O1 142.98(11) . 1_455 ? O2 Ho1 O1W 71.13(12) 2_766 . ? O3 Ho1 O1W 141.89(11) 2_767 . ? O2W Ho1 O1W 71.44(12) . . ? O6 Ho1 O1W 75.02(12) . . ? O1 Ho1 O1W 76.62(12) 1_455 . ? O2 Ho1 O5 74.90(12) 2_766 . ? O3 Ho1 O5 72.13(12) 2_767 . ? O2W Ho1 O5 126.56(13) . . ? O6 Ho1 O5 67.85(11) . . ? O1 Ho1 O5 148.75(11) 1_455 . ? O1W Ho1 O5 129.78(12) . . ? O2 Ho1 O4 76.20(11) 2_766 . ? O3 Ho1 O4 84.36(11) 2_767 . ? O2W Ho1 O4 134.83(11) . . ? O6 Ho1 O4 143.65(11) . . ? O1 Ho1 O4 73.30(11) 1_455 . ? O1W Ho1 O4 127.45(11) . . ? O5 Ho1 O4 76.41(10) . . ? C3 C1 C2 120.0(4) . . ? C3 C1 C4 118.5(4) . . ? C2 C1 C4 121.5(4) . . ? C3 C2 C1 118.6(4) 2_756 . ? C3 C2 C5 118.3(4) 2_756 . ? C1 C2 C5 123.1(4) . . ? C1 C3 C2 121.4(4) . 2_756 ? O2 C4 O1 123.4(4) . . ? O2 C4 C1 119.4(4) . . ? O1 C4 C1 117.2(4) . . ? O3 C5 O4 124.9(4) . . ? O3 C5 C2 117.8(4) . . ? O4 C5 C2 117.2(4) . . ? O6 C6 O5 126.4(4) 2_777 . ? O6 C6 C6 117.8(5) 2_777 2_777 ? O5 C6 C6 115.7(5) . 2_777 ? C4 O1 Ho1 125.8(3) . 1_655 ? C4 O2 Ho1 173.7(3) . 2_766 ? C5 O3 Ho1 162.4(3) . 2_767 ? C5 O4 Ho1 131.3(3) . . ? C6 O5 Ho1 117.3(3) . . ? C6 O6 Ho1 119.3(3) 2_777 . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.622 _refine_diff_density_min -1.764 _refine_diff_density_rms 0.181 # Attachment '- 5.cif' data_xb _database_code_depnum_ccdc_archive 'CCDC 761944' #TrackingRef '- 5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H18 O17 Tb2' _chemical_formula_weight 788.13 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 18.833(3) _cell_length_b 7.7766(12) _cell_length_c 14.755(2) _cell_angle_alpha 90.00 _cell_angle_beta 113.696(2) _cell_angle_gamma 90.00 _cell_volume 1978.8(5) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2237 _cell_measurement_theta_min 2.99 _cell_measurement_theta_max 29.00 _exptl_crystal_description prismatic _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.646 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1496 _exptl_absorpt_coefficient_mu 7.184 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3035 _exptl_absorpt_correction_T_max 0.5425 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 'Bruker SMART APEX' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 5451 _diffrn_reflns_av_R_equivalents 0.0291 _diffrn_reflns_av_sigmaI/netI 0.0356 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 26.74 _reflns_number_total 2087 _reflns_number_gt 1824 _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^)+(0.0200P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2087 _refine_ls_number_parameters 156 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0287 _refine_ls_R_factor_gt 0.0232 _refine_ls_wR_factor_ref 0.0495 _refine_ls_wR_factor_gt 0.0477 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _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 Tb1 Tb 0.253737(10) 0.36633(2) 0.384331(14) 0.01272(7) Uani 1 1 d . . . O1 O 0.11446(16) 0.4497(4) 0.3518(2) 0.0266(8) Uani 1 1 d . . . O2 O 0.19268(15) 0.3780(4) 0.5030(2) 0.0187(6) Uani 1 1 d . . . O1W O 0.34760(17) 0.5429(4) 0.3509(2) 0.0238(7) Uani 1 1 d . . . H1A H 0.3479 0.5324 0.2958 0.036 Uiso 1 1 d R . . H1B H 0.3895 0.4985 0.3846 0.036 Uiso 1 1 d R . . O2W O 0.2372(2) 0.6862(4) 0.4019(3) 0.0346(8) Uani 1 1 d . . . H2A H 0.2298 0.7244 0.4492 0.052 Uiso 0.50 1 d PR A 1 H2B H 0.2162 0.7456 0.3524 0.052 Uiso 0.50 1 d PR A 1 H2C H 0.2714 0.7171 0.3845 0.052 Uiso 0.50 1 d PR A 2 H2D H 0.2010 0.6637 0.3493 0.052 Uiso 0.50 1 d PR A 2 O3W O 0.5000 0.5000 0.5000 0.120(3) Uani 1 2 d S . . O3 O 0.17857(16) 0.3081(4) 0.6822(2) 0.0199(7) Uani 1 1 d . . . O4 O 0.18507(16) 0.5906(4) 0.7101(2) 0.0213(7) Uani 1 1 d . . . O5 O 0.17141(16) 0.1162(4) 0.3356(2) 0.0216(7) Uani 1 1 d . . . O6 O 0.14763(17) 0.0359(4) 0.4664(2) 0.0264(8) Uani 1 1 d . . . C1 C 0.0622(2) 0.4616(5) 0.4742(3) 0.0161(9) Uani 1 1 d . . . C2 C 0.0757(2) 0.4834(5) 0.5741(3) 0.0150(9) Uani 1 1 d . . . C3 C 0.0133(2) 0.5197(5) 0.5983(3) 0.0165(9) Uani 1 1 d . . . H3 H 0.0218 0.5320 0.6645 0.020 Uiso 1 1 calc R . . C4 C 0.1257(2) 0.4290(6) 0.4397(3) 0.0176(9) Uani 1 1 d . . . C5 C 0.1530(2) 0.4589(6) 0.6605(3) 0.0172(9) Uani 1 1 d . . . C6 C 0.1351(2) 0.0297(6) 0.3760(3) 0.0182(9) Uani 1 1 d . . . C7 C 0.0701(2) -0.0862(5) 0.3104(3) 0.0189(9) Uani 1 1 d . . . H7A H 0.0563 -0.1669 0.3508 0.023 Uiso 1 1 calc R . . H7B H 0.0869 -0.1511 0.2665 0.023 Uiso 1 1 calc R . . C8 C 0.0000 0.0233(8) 0.2500 0.0203(14) Uani 1 2 d S . . H8A H -0.0130 0.0966 0.2943 0.024 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 Tb1 0.01120(11) 0.01800(12) 0.00897(11) 0.00022(9) 0.00408(8) 0.00106(8) O1 0.0159(16) 0.052(2) 0.0122(16) 0.0032(15) 0.0057(13) 0.0104(15) O2 0.0135(14) 0.0266(17) 0.0162(16) 0.0037(13) 0.0063(13) 0.0030(13) O1W 0.0247(17) 0.0326(18) 0.0129(16) 0.0029(14) 0.0064(14) 0.0006(14) O2W 0.043(2) 0.0295(19) 0.034(2) 0.0003(16) 0.0188(18) 0.0066(16) O3W 0.029(4) 0.230(11) 0.094(6) 0.040(7) 0.016(4) 0.001(5) O3 0.0192(16) 0.0205(16) 0.0194(17) 0.0032(13) 0.0074(14) 0.0060(13) O4 0.0189(16) 0.0274(17) 0.0132(16) -0.0038(14) 0.0019(13) -0.0053(13) O5 0.0206(16) 0.0314(18) 0.0140(16) -0.0020(14) 0.0081(13) -0.0058(14) O6 0.0207(17) 0.042(2) 0.0147(17) -0.0022(15) 0.0050(14) -0.0091(15) C1 0.012(2) 0.023(2) 0.013(2) 0.0008(18) 0.0047(18) 0.0040(17) C2 0.012(2) 0.016(2) 0.018(2) 0.0002(18) 0.0066(18) 0.0022(16) C3 0.015(2) 0.022(2) 0.012(2) -0.0003(18) 0.0050(18) 0.0032(17) C4 0.015(2) 0.023(2) 0.017(2) -0.0018(19) 0.0080(19) 0.0019(18) C5 0.014(2) 0.030(3) 0.007(2) -0.0003(18) 0.0042(18) 0.0024(19) C6 0.011(2) 0.022(2) 0.017(2) 0.0002(19) 0.0014(19) 0.0015(18) C7 0.019(2) 0.020(2) 0.014(2) -0.0002(18) 0.0024(19) -0.0015(18) C8 0.013(3) 0.028(4) 0.018(3) 0.000 0.005(3) 0.000 _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 O3 2.331(3) 7_556 ? Tb1 O6 2.364(3) 7_556 ? Tb1 O4 2.393(3) 6_565 ? Tb1 O5 2.410(3) . ? Tb1 O1W 2.440(3) . ? Tb1 O2 2.453(3) . ? Tb1 O2 2.459(3) 7_556 ? Tb1 O2W 2.533(3) . ? Tb1 O1 2.553(3) . ? Tb1 C4 2.881(4) . ? Tb1 Tb1 3.9154(6) 7_556 ? Tb1 H2D 2.4874 . ? O1 C4 1.238(5) . ? O2 C4 1.294(5) . ? O2 Tb1 2.459(3) 7_556 ? O1W H1A 0.8199 . ? O1W H1B 0.8200 . ? O2W H2A 0.8198 . ? O2W H2B 0.8200 . ? O2W H2C 0.8203 . ? O2W H2D 0.8199 . ? O3 C5 1.260(5) . ? O3 Tb1 2.331(3) 7_556 ? O4 C5 1.262(5) . ? O4 Tb1 2.393(3) 6_566 ? O5 C6 1.266(5) . ? O6 C6 1.259(5) . ? O6 Tb1 2.364(3) 7_556 ? C1 C3 1.400(5) 5_566 ? C1 C2 1.402(6) . ? C1 C4 1.498(5) . ? C2 C3 1.387(5) . ? C2 C5 1.514(5) . ? C3 C1 1.400(5) 5_566 ? C3 H3 0.9300 . ? C6 C7 1.515(6) . ? C7 C8 1.522(5) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C7 1.522(5) 2 ? C8 H8A 0.9700 . ? 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 Tb1 O6 102.79(11) 7_556 7_556 ? O3 Tb1 O4 77.27(10) 7_556 6_565 ? O6 Tb1 O4 147.04(11) 7_556 6_565 ? O3 Tb1 O5 78.47(10) 7_556 . ? O6 Tb1 O5 135.04(11) 7_556 . ? O4 Tb1 O5 77.73(10) 6_565 . ? O3 Tb1 O1W 71.28(10) 7_556 . ? O6 Tb1 O1W 69.24(10) 7_556 . ? O4 Tb1 O1W 80.01(10) 6_565 . ? O5 Tb1 O1W 145.63(10) . . ? O3 Tb1 O2 144.58(10) 7_556 . ? O6 Tb1 O2 75.01(10) 7_556 . ? O4 Tb1 O2 123.80(10) 6_565 . ? O5 Tb1 O2 79.21(9) . . ? O1W Tb1 O2 135.15(10) . . ? O3 Tb1 O2 71.92(10) 7_556 7_556 ? O6 Tb1 O2 70.33(10) 7_556 7_556 ? O4 Tb1 O2 137.10(10) 6_565 7_556 ? O5 Tb1 O2 67.53(10) . 7_556 ? O1W Tb1 O2 115.96(10) . 7_556 ? O2 Tb1 O2 74.27(10) . 7_556 ? O3 Tb1 O2W 136.47(11) 7_556 . ? O6 Tb1 O2W 70.84(11) 7_556 . ? O4 Tb1 O2W 86.40(11) 6_565 . ? O5 Tb1 O2W 137.08(10) . . ? O1W Tb1 O2W 66.23(11) . . ? O2 Tb1 O2W 77.18(10) . . ? O2 Tb1 O2W 136.36(10) 7_556 . ? O3 Tb1 O1 139.71(10) 7_556 . ? O6 Tb1 O1 117.19(10) 7_556 . ? O4 Tb1 O1 72.04(10) 6_565 . ? O5 Tb1 O1 70.10(10) . . ? O1W Tb1 O1 126.30(10) . . ? O2 Tb1 O1 51.97(9) . . ? O2 Tb1 O1 115.78(10) 7_556 . ? O2W Tb1 O1 67.09(11) . . ? O3 Tb1 C4 151.57(11) 7_556 . ? O6 Tb1 C4 96.63(11) 7_556 . ? O4 Tb1 C4 97.39(11) 6_565 . ? O5 Tb1 C4 73.12(11) . . ? O1W Tb1 C4 135.96(11) . . ? O2 Tb1 C4 26.55(10) . . ? O2 Tb1 C4 95.86(11) 7_556 . ? O2W Tb1 C4 69.72(12) . . ? O1 Tb1 C4 25.42(10) . . ? O3 Tb1 Tb1 108.40(7) 7_556 7_556 ? O6 Tb1 Tb1 68.08(8) 7_556 7_556 ? O4 Tb1 Tb1 143.94(7) 6_565 7_556 ? O5 Tb1 Tb1 69.07(7) . 7_556 ? O1W Tb1 Tb1 135.97(7) . 7_556 ? O2 Tb1 Tb1 37.18(7) . 7_556 ? O2 Tb1 Tb1 37.08(6) 7_556 7_556 ? O2W Tb1 Tb1 108.39(8) . 7_556 ? O1 Tb1 Tb1 83.52(7) . 7_556 ? C4 Tb1 Tb1 60.25(9) . 7_556 ? O3 Tb1 H2D 133.9 7_556 . ? O6 Tb1 H2D 89.6 7_556 . ? O4 Tb1 H2D 69.4 6_565 . ? O5 Tb1 H2D 122.2 . . ? O1W Tb1 H2D 72.3 . . ? O2 Tb1 H2D 81.4 . . ? O2 Tb1 H2D 151.7 7_556 . ? O2W Tb1 H2D 18.8 . . ? O1 Tb1 H2D 55.3 . . ? C4 Tb1 H2D 65.9 . . ? Tb1 Tb1 H2D 117.4 7_556 . ? C4 O1 Tb1 92.3(2) . . ? C4 O2 Tb1 95.5(2) . . ? C4 O2 Tb1 137.8(3) . 7_556 ? Tb1 O2 Tb1 105.73(10) . 7_556 ? Tb1 O1W H1A 116.0 . . ? Tb1 O1W H1B 103.8 . . ? H1A O1W H1B 99.8 . . ? Tb1 O2W H2A 120.9 . . ? Tb1 O2W H2B 119.8 . . ? H2A O2W H2B 111.6 . . ? Tb1 O2W H2C 96.4 . . ? H2A O2W H2C 125.7 . . ? H2B O2W H2C 73.4 . . ? Tb1 O2W H2D 77.5 . . ? H2A O2W H2D 121.5 . . ? H2B O2W H2D 49.9 . . ? H2C O2W H2D 103.0 . . ? C5 O3 Tb1 130.7(3) . 7_556 ? C5 O4 Tb1 131.5(3) . 6_566 ? C6 O5 Tb1 133.9(3) . . ? C6 O6 Tb1 137.9(3) . 7_556 ? C3 C1 C2 119.3(4) 5_566 . ? C3 C1 C4 117.5(4) 5_566 . ? C2 C1 C4 123.1(4) . . ? C3 C2 C1 118.7(4) . . ? C3 C2 C5 115.9(4) . . ? C1 C2 C5 125.2(4) . . ? C2 C3 C1 122.0(4) . 5_566 ? C2 C3 H3 119.0 . . ? C1 C3 H3 119.0 5_566 . ? O1 C4 O2 120.2(4) . . ? O1 C4 C1 120.7(4) . . ? O2 C4 C1 119.1(4) . . ? O1 C4 Tb1 62.3(2) . . ? O2 C4 Tb1 57.9(2) . . ? C1 C4 Tb1 176.9(3) . . ? O3 C5 O4 124.3(4) . . ? O3 C5 C2 118.1(4) . . ? O4 C5 C2 117.4(4) . . ? O6 C6 O5 124.9(4) . . ? O6 C6 C7 117.3(4) . . ? O5 C6 C7 117.8(4) . . ? C6 C7 C8 109.2(4) . . ? C6 C7 H7A 109.8 . . ? C8 C7 H7A 109.8 . . ? C6 C7 H7B 109.8 . . ? C8 C7 H7B 109.8 . . ? H7A C7 H7B 108.3 . . ? C7 C8 C7 112.0(5) 2 . ? C7 C8 H8A 109.3 2 . ? C7 C8 H8A 109.2 . . ? 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 O3 Tb1 O1 C4 133.3(3) 7_556 . . . ? O6 Tb1 O1 C4 -38.9(3) 7_556 . . . ? O4 Tb1 O1 C4 175.5(3) 6_565 . . . ? O5 Tb1 O1 C4 92.4(3) . . . . ? O1W Tb1 O1 C4 -122.1(3) . . . . ? O2 Tb1 O1 C4 0.7(2) . . . . ? O2 Tb1 O1 C4 41.2(3) 7_556 . . . ? O2W Tb1 O1 C4 -90.7(3) . . . . ? Tb1 Tb1 O1 C4 22.4(3) 7_556 . . . ? O3 Tb1 O2 C4 -125.5(3) 7_556 . . . ? O6 Tb1 O2 C4 143.4(3) 7_556 . . . ? O4 Tb1 O2 C4 -6.6(3) 6_565 . . . ? O5 Tb1 O2 C4 -73.8(2) . . . . ? O1W Tb1 O2 C4 105.6(3) . . . . ? O2 Tb1 O2 C4 -143.2(3) 7_556 . . . ? O2W Tb1 O2 C4 70.1(3) . . . . ? O1 Tb1 O2 C4 -0.7(2) . . . . ? Tb1 Tb1 O2 C4 -143.2(3) 7_556 . . . ? O3 Tb1 O2 Tb1 17.7(2) 7_556 . . 7_556 ? O6 Tb1 O2 Tb1 -73.35(12) 7_556 . . 7_556 ? O4 Tb1 O2 Tb1 136.65(11) 6_565 . . 7_556 ? O5 Tb1 O2 Tb1 69.48(11) . . . 7_556 ? O1W Tb1 O2 Tb1 -111.20(13) . . . 7_556 ? O2 Tb1 O2 Tb1 0.0 7_556 . . 7_556 ? O2W Tb1 O2 Tb1 -146.63(12) . . . 7_556 ? O1 Tb1 O2 Tb1 142.57(17) . . . 7_556 ? C4 Tb1 O2 Tb1 143.2(3) . . . 7_556 ? O3 Tb1 O5 C6 137.2(4) 7_556 . . . ? O6 Tb1 O5 C6 40.6(4) 7_556 . . . ? O4 Tb1 O5 C6 -143.5(4) 6_565 . . . ? O1W Tb1 O5 C6 165.7(3) . . . . ? O2 Tb1 O5 C6 -15.1(4) . . . . ? O2 Tb1 O5 C6 62.2(4) 7_556 . . . ? O2W Tb1 O5 C6 -72.7(4) . . . . ? O1 Tb1 O5 C6 -68.4(4) . . . . ? C4 Tb1 O5 C6 -41.8(4) . . . . ? Tb1 Tb1 O5 C6 22.2(3) 7_556 . . . ? C3 C1 C2 C3 1.3(7) 5_566 . . . ? C4 C1 C2 C3 177.5(4) . . . . ? C3 C1 C2 C5 176.9(4) 5_566 . . . ? C4 C1 C2 C5 -6.9(7) . . . . ? C1 C2 C3 C1 -1.3(7) . . . 5_566 ? C5 C2 C3 C1 -177.3(4) . . . 5_566 ? Tb1 O1 C4 O2 -1.2(4) . . . . ? Tb1 O1 C4 C1 179.1(4) . . . . ? Tb1 O2 C4 O1 1.2(4) . . . . ? Tb1 O2 C4 O1 -119.6(4) 7_556 . . . ? Tb1 O2 C4 C1 -179.1(3) . . . . ? Tb1 O2 C4 C1 60.1(6) 7_556 . . . ? Tb1 O2 C4 Tb1 -120.8(4) 7_556 . . . ? C3 C1 C4 O1 13.1(6) 5_566 . . . ? C2 C1 C4 O1 -163.2(4) . . . . ? C3 C1 C4 O2 -166.6(4) 5_566 . . . ? C2 C1 C4 O2 17.1(6) . . . . ? C3 C1 C4 Tb1 179(100) 5_566 . . . ? C2 C1 C4 Tb1 3(6) . . . . ? O3 Tb1 C4 O1 -81.2(4) 7_556 . . . ? O6 Tb1 C4 O1 145.8(3) 7_556 . . . ? O4 Tb1 C4 O1 -4.3(3) 6_565 . . . ? O5 Tb1 C4 O1 -79.0(3) . . . . ? O1W Tb1 C4 O1 79.0(3) . . . . ? O2 Tb1 C4 O1 -178.8(4) . . . . ? O2 Tb1 C4 O1 -143.4(3) 7_556 . . . ? O2W Tb1 C4 O1 79.1(3) . . . . ? Tb1 Tb1 C4 O1 -154.2(3) 7_556 . . . ? O3 Tb1 C4 O2 97.6(3) 7_556 . . . ? O6 Tb1 C4 O2 -35.4(3) 7_556 . . . ? O4 Tb1 C4 O2 174.5(2) 6_565 . . . ? O5 Tb1 C4 O2 99.8(2) . . . . ? O1W Tb1 C4 O2 -102.3(3) . . . . ? O2 Tb1 C4 O2 35.4(3) 7_556 . . . ? O2W Tb1 C4 O2 -102.1(3) . . . . ? O1 Tb1 C4 O2 178.8(4) . . . . ? Tb1 Tb1 C4 O2 24.6(2) 7_556 . . . ? O3 Tb1 C4 C1 113(6) 7_556 . . . ? O6 Tb1 C4 C1 -20(6) 7_556 . . . ? O4 Tb1 C4 C1 -170(6) 6_565 . . . ? O5 Tb1 C4 C1 115(6) . . . . ? O1W Tb1 C4 C1 -87(6) . . . . ? O2 Tb1 C4 C1 15(6) . . . . ? O2 Tb1 C4 C1 50(6) 7_556 . . . ? O2W Tb1 C4 C1 -87(6) . . . . ? O1 Tb1 C4 C1 -166(6) . . . . ? Tb1 Tb1 C4 C1 40(6) 7_556 . . . ? Tb1 O3 C5 O4 -102.3(4) 7_556 . . . ? Tb1 O3 C5 C2 82.7(4) 7_556 . . . ? Tb1 O4 C5 O3 -35.7(6) 6_566 . . . ? Tb1 O4 C5 C2 139.3(3) 6_566 . . . ? C3 C2 C5 O3 104.2(5) . . . . ? C1 C2 C5 O3 -71.6(6) . . . . ? C3 C2 C5 O4 -71.1(5) . . . . ? C1 C2 C5 O4 113.1(5) . . . . ? Tb1 O6 C6 O5 -16.5(7) 7_556 . . . ? Tb1 O6 C6 C7 165.4(3) 7_556 . . . ? Tb1 O5 C6 O6 -16.5(6) . . . . ? Tb1 O5 C6 C7 161.7(3) . . . . ? O6 C6 C7 C8 103.6(4) . . . . ? O5 C6 C7 C8 -74.7(4) . . . . ? C6 C7 C8 C7 -174.6(4) . . . 2 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.74 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.724 _refine_diff_density_min -0.623 _refine_diff_density_rms 0.149 # Attachment '- 7.cif' data_1c _database_code_depnum_ccdc_archive 'CCDC 761945' #TrackingRef '- 7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H18 Dy2 O17' _chemical_formula_weight 795.29 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 Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 18.805(4) _cell_length_b 7.7577(16) _cell_length_c 14.724(3) _cell_angle_alpha 90.00 _cell_angle_beta 113.70(3) _cell_angle_gamma 90.00 _cell_volume 1966.7(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8505 _cell_measurement_theta_min 2.995 _cell_measurement_theta_max 27.405 _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.686 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1504 _exptl_absorpt_coefficient_mu 7.634 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3063 _exptl_absorpt_correction_T_max 0.5664 _exptl_absorpt_process_details ;Higashi, T. (1995). Program for Absorption Correction. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID IP' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 9064 _diffrn_reflns_av_R_equivalents 0.0263 _diffrn_reflns_av_sigmaI/netI 0.0241 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 27.40 _reflns_number_total 2239 _reflns_number_gt 2150 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Rgaku R-AXIS RAPID diffractometer Control Software' _computing_cell_refinement 'Rgaku R-AXIS RAPID diffractometer Control Software' _computing_data_reduction 'Rgaku R-AXIS RAPID diffractometer Control Software' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXP-97 _computing_publication_material SHELXTL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+11.0824P] 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 2239 _refine_ls_number_parameters 172 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.0192 _refine_ls_R_factor_gt 0.0175 _refine_ls_wR_factor_ref 0.0382 _refine_ls_wR_factor_gt 0.0377 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.077 _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 O3W O 0.0000 1.0000 0.0000 0.130(3) Uani 1 2 d S . . H2WA H 0.2508(19) 1.279(3) 0.117(3) 0.031(4) Uiso 1 1 d DU . . H1WB H 0.156(2) 1.049(5) 0.2072(16) 0.029(4) Uiso 1 1 d DU . . H1WA H 0.168(2) 1.132(3) 0.133(3) 0.033(4) Uiso 1 1 d DU . . H2WB H 0.3050(14) 1.180(5) 0.098(3) 0.031(4) Uiso 1 1 d DU . . Dy1 Dy 0.246511(7) 0.866296(17) 0.115480(9) 0.01140(5) Uani 1 1 d . . . C1 C 0.57552(16) 1.0172(4) 0.0740(2) 0.0149(6) Uani 1 1 d . . . C2 C 0.43776(16) 0.9620(4) 0.0261(2) 0.0153(6) Uani 1 1 d . . . C3 C 0.51330(16) 0.9803(4) 0.0990(2) 0.0162(6) Uani 1 1 d . . . H3 H 0.5220 0.9674 0.1654 0.019 Uiso 1 1 calc RU . . C5 C 0.37426(17) 0.9272(4) 0.0604(2) 0.0163(6) Uani 1 1 d . . . C6 C 0.36459(16) 0.5289(4) 0.1240(2) 0.0171(6) Uani 1 1 d . . . C7 C 0.42989(17) 0.4143(4) 0.1897(2) 0.0204(6) Uani 1 1 d . . . H7A H 0.4438 0.3333 0.1494 0.024 Uiso 1 1 calc RU . . H7B H 0.4133 0.3492 0.2340 0.024 Uiso 1 1 calc RU . . C8 C 0.5000 0.5256(6) 0.2500 0.0214(9) Uani 1 2 d S . . H8A H 0.5129 0.5991 0.2055 0.026 Uiso 0.50 1 calc PRU . . H8B H 0.4871 0.5991 0.2945 0.026 Uiso 0.50 1 calc PRU . . O1W O 0.15205(13) 1.0392(3) 0.14866(17) 0.0231(5) Uani 1 1 d D . . O2W O 0.26256(17) 1.1841(4) 0.0994(2) 0.0344(6) Uani 1 1 d D . . O3 O 0.38521(13) 0.9493(3) 0.14828(16) 0.0273(5) Uani 1 1 d . . . O4 O 0.30737(11) 0.8778(3) -0.00293(15) 0.0185(4) Uani 1 1 d . . . O6 O 0.32857(12) 0.6169(3) 0.16449(16) 0.0202(5) Uani 1 1 d . . . O5 O 0.35181(13) 0.5353(3) 0.03357(16) 0.0259(5) Uani 1 1 d . . . C4 C 0.65387(15) 1.0409(4) 0.1607(2) 0.0135(6) Uani 1 1 d . . . O1 O 0.67932(12) 1.1923(3) 0.18184(16) 0.0191(4) Uani 1 1 d . . . O2 O 0.68527(12) 0.9105(3) 0.21095(16) 0.0198(4) 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 O3W 0.036(3) 0.246(11) 0.101(6) -0.031(6) 0.021(3) 0.006(5) Dy1 0.00923(7) 0.01641(8) 0.00874(7) -0.00022(5) 0.00379(5) -0.00119(5) C1 0.0099(12) 0.0188(14) 0.0150(14) 0.0005(11) 0.0040(11) -0.0013(11) C2 0.0117(13) 0.0201(15) 0.0149(14) 0.0012(11) 0.0063(11) -0.0026(11) C3 0.0119(13) 0.0253(16) 0.0119(13) 0.0016(11) 0.0051(11) -0.0034(12) C5 0.0136(13) 0.0210(15) 0.0148(14) 0.0012(11) 0.0064(11) -0.0025(12) C6 0.0119(13) 0.0238(16) 0.0147(14) -0.0011(11) 0.0044(11) -0.0038(12) C7 0.0154(14) 0.0217(15) 0.0205(16) -0.0015(12) 0.0034(12) 0.0001(12) C8 0.0133(19) 0.025(2) 0.021(2) 0.000 0.0017(17) 0.000 O1W 0.0251(12) 0.0295(13) 0.0182(11) -0.0019(9) 0.0123(10) 0.0029(10) O2W 0.0441(16) 0.0255(13) 0.0389(16) -0.0003(11) 0.0223(14) -0.0030(12) O3 0.0183(11) 0.0509(16) 0.0148(11) -0.0038(10) 0.0088(9) -0.0122(11) O4 0.0103(9) 0.0308(12) 0.0145(10) -0.0032(9) 0.0049(8) -0.0052(9) O6 0.0172(10) 0.0283(12) 0.0147(11) 0.0022(9) 0.0061(9) 0.0051(9) O5 0.0215(11) 0.0412(14) 0.0136(11) 0.0003(9) 0.0055(9) 0.0082(10) C4 0.0073(12) 0.0238(15) 0.0117(13) 0.0020(11) 0.0063(10) -0.0011(11) O1 0.0177(10) 0.0221(11) 0.0179(11) -0.0031(8) 0.0076(9) -0.0072(9) O2 0.0175(10) 0.0247(11) 0.0147(10) 0.0048(9) 0.0037(8) 0.0032(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 O1 2.316(2) 3_445 ? Dy1 O5 2.357(2) 7_565 ? Dy1 O2 2.379(2) 2_655 ? Dy1 O6 2.398(2) . ? Dy1 O1W 2.427(2) . ? Dy1 O4 2.442(2) . ? Dy1 O4 2.451(2) 7_565 ? Dy1 O2W 2.506(3) . ? Dy1 O3 2.537(2) . ? Dy1 C5 2.867(3) . ? Dy1 Dy1 3.8981(7) 7_565 ? C1 C3 1.390(4) . ? C1 C2 1.403(4) 5_675 ? C1 C4 1.524(4) . ? C2 C3 1.401(4) . ? C2 C1 1.403(4) 5_675 ? C2 C5 1.496(4) . ? C5 O3 1.238(4) . ? C5 O4 1.286(4) . ? C6 O5 1.255(4) . ? C6 O6 1.267(4) . ? C6 C7 1.510(4) . ? C7 C8 1.527(4) . ? C8 C7 1.527(4) 2_655 ? O4 Dy1 2.451(2) 7_565 ? O5 Dy1 2.357(2) 7_565 ? C4 O2 1.252(4) . ? C4 O1 1.259(4) . ? O1 Dy1 2.317(2) 3 ? O2 Dy1 2.379(2) 2_655 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Dy1 O5 103.00(8) 3_445 7_565 ? O1 Dy1 O2 77.35(8) 3_445 2_655 ? O5 Dy1 O2 146.72(8) 7_565 2_655 ? O1 Dy1 O6 78.29(8) 3_445 . ? O5 Dy1 O6 135.29(8) 7_565 . ? O2 Dy1 O6 77.83(8) 2_655 . ? O1 Dy1 O1W 70.72(8) 3_445 . ? O5 Dy1 O1W 69.19(8) 7_565 . ? O2 Dy1 O1W 80.00(8) 2_655 . ? O6 Dy1 O1W 145.08(8) . . ? O1 Dy1 O4 144.51(8) 3_445 . ? O5 Dy1 O4 74.97(8) 7_565 . ? O2 Dy1 O4 123.82(7) 2_655 . ? O6 Dy1 O4 79.32(7) . . ? O1W Dy1 O4 135.61(8) . . ? O1 Dy1 O4 71.80(7) 3_445 7_565 ? O5 Dy1 O4 70.40(8) 7_565 7_565 ? O2 Dy1 O4 137.35(8) 2_655 7_565 ? O6 Dy1 O4 67.75(8) . 7_565 ? O1W Dy1 O4 115.21(8) . 7_565 ? O4 Dy1 O4 74.37(8) . 7_565 ? O1 Dy1 O2W 136.04(9) 3_445 . ? O5 Dy1 O2W 70.89(9) 7_565 . ? O2 Dy1 O2W 85.76(9) 2_655 . ? O6 Dy1 O2W 137.28(9) . . ? O1W Dy1 O2W 66.48(9) . . ? O4 Dy1 O2W 77.75(8) . . ? O4 Dy1 O2W 136.78(8) 7_565 . ? O1 Dy1 O3 139.54(8) 3_445 . ? O5 Dy1 O3 117.17(8) 7_565 . ? O2 Dy1 O3 71.93(8) 2_655 . ? O6 Dy1 O3 70.09(8) . . ? O1W Dy1 O3 126.94(8) . . ? O4 Dy1 O3 52.09(7) . . ? O4 Dy1 O3 116.01(8) 7_565 . ? O2W Dy1 O3 67.35(9) . . ? O1 Dy1 C5 151.22(8) 3_445 . ? O5 Dy1 C5 96.66(8) 7_565 . ? O2 Dy1 C5 97.40(8) 2_655 . ? O6 Dy1 C5 72.96(8) . . ? O1W Dy1 C5 136.90(9) . . ? O4 Dy1 C5 26.53(8) . . ? O4 Dy1 C5 95.83(8) 7_565 . ? O2W Dy1 C5 70.42(9) . . ? O3 Dy1 C5 25.56(8) . . ? O1 Dy1 Dy1 108.27(6) 3_445 7_565 ? O5 Dy1 Dy1 68.08(6) 7_565 7_565 ? O2 Dy1 Dy1 144.21(5) 2_655 7_565 ? O6 Dy1 Dy1 69.25(5) . 7_565 ? O1W Dy1 Dy1 135.68(6) . 7_565 ? O4 Dy1 Dy1 37.27(5) . 7_565 ? O4 Dy1 Dy1 37.10(5) 7_565 7_565 ? O2W Dy1 Dy1 108.99(7) . 7_565 ? O3 Dy1 Dy1 83.74(6) . 7_565 ? C5 Dy1 Dy1 60.23(6) . 7_565 ? C3 C1 C2 119.3(3) . 5_675 ? C3 C1 C4 115.9(2) . . ? C2 C1 C4 124.8(3) 5_675 . ? C3 C2 C1 119.4(3) . 5_675 ? C3 C2 C5 117.5(3) . . ? C1 C2 C5 123.1(3) 5_675 . ? C1 C3 C2 121.4(3) . . ? O3 C5 O4 120.1(3) . . ? O3 C5 C2 120.5(3) . . ? O4 C5 C2 119.3(3) . . ? O3 C5 Dy1 62.17(16) . . ? O4 C5 Dy1 57.97(14) . . ? C2 C5 Dy1 176.8(2) . . ? O5 C6 O6 124.6(3) . . ? O5 C6 C7 117.6(3) . . ? O6 C6 C7 117.8(3) . . ? C6 C7 C8 109.2(3) . . ? C7 C8 C7 111.1(4) 2_655 . ? C5 O3 Dy1 92.27(18) . . ? C5 O4 Dy1 95.50(17) . . ? C5 O4 Dy1 137.55(19) . 7_565 ? Dy1 O4 Dy1 105.63(8) . 7_565 ? C6 O6 Dy1 134.0(2) . . ? C6 O5 Dy1 138.1(2) . 7_565 ? O2 C4 O1 124.4(3) . . ? O2 C4 C1 117.7(3) . . ? O1 C4 C1 117.6(3) . . ? C4 O1 Dy1 131.06(19) . 3 ? C4 O2 Dy1 132.4(2) . 2_655 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.40 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.520 _refine_diff_density_min -1.198 _refine_diff_density_rms 0.112 # Attachment '- 8.cif' data_1d _database_code_depnum_ccdc_archive 'CCDC 761946' #TrackingRef '- 8.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H18 Ho2 O17' _chemical_formula_weight 800.15 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' Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 18.7825(18) _cell_length_b 7.7434(8) _cell_length_c 14.6995(14) _cell_angle_alpha 90.00 _cell_angle_beta 113.7770(10) _cell_angle_gamma 90.00 _cell_volume 1956.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 2869 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 28.67 _exptl_crystal_description prismatic _exptl_crystal_colour pink _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.717 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1512 _exptl_absorpt_coefficient_mu 8.124 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2152 _exptl_absorpt_correction_T_max 0.6457 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 'Bruker SMART APEX' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 4715 _diffrn_reflns_av_R_equivalents 0.0235 _diffrn_reflns_av_sigmaI/netI 0.0272 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1710 _reflns_number_gt 1583 _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^)+(0.0192P)^2^+0.5901P] 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 1710 _refine_ls_number_parameters 172 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0211 _refine_ls_R_factor_gt 0.0187 _refine_ls_wR_factor_ref 0.0421 _refine_ls_wR_factor_gt 0.0412 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.062 _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 H1WB H 0.113(3) 0.466(6) 0.109(4) 0.028(4) Uiso 1 1 d U . . H1WA H 0.158(3) 0.435(6) 0.211(3) 0.027(4) Uiso 1 1 d U . . H2WB H 0.235(3) 0.262(7) 0.117(3) 0.029(4) Uiso 1 1 d U . . H2WA H 0.290(3) 0.308(8) 0.089(4) 0.027(4) Uiso 1 1 d U . . O4 O 0.32011(16) 0.6923(4) -0.18184(19) 0.0189(6) Uani 1 1 d . . . O3 O 0.31486(16) 0.4101(4) -0.2116(2) 0.0187(6) Uani 1 1 d . . . Ho1 Ho 0.246496(10) 0.63449(2) 0.115349(12) 0.01214(8) Uani 1 1 d . . . C1 C 0.4380(2) 0.5376(5) 0.0258(3) 0.0136(8) Uani 1 1 d . . . C2 C 0.4244(2) 0.5172(5) -0.0743(3) 0.0157(9) Uani 1 1 d . . . C3 C 0.5131(2) 0.5213(5) 0.0984(3) 0.0172(9) Uani 1 1 d . . . H3 H 0.5217 0.5367 0.1647 0.021 Uiso 1 1 calc RU . . C4 C 0.3740(2) 0.5730(5) 0.0607(3) 0.0156(9) Uani 1 1 d . . . C5 C 0.3462(2) 0.5409(6) -0.1608(3) 0.0161(9) Uani 1 1 d . . . C6 C 0.3642(2) 0.9708(5) 0.1232(3) 0.0187(9) Uani 1 1 d . . . C7 C 0.4299(2) 1.0856(5) 0.1900(3) 0.0205(9) Uani 1 1 d . . . H7A H 0.4131 1.1499 0.2345 0.025 Uiso 1 1 calc RU . . H7B H 0.4437 1.1676 0.1500 0.025 Uiso 1 1 calc RU . . C8 C 0.5000 0.9754(8) 0.2500 0.0195(13) Uani 1 2 d S . . H8A H 0.5127 0.9017 0.2053 0.023 Uiso 0.50 1 calc PRU . . H8B H 0.4873 0.9017 0.2947 0.023 Uiso 0.50 1 calc PRU . . O1 O 0.38552(17) 0.5516(4) 0.1488(2) 0.0266(7) Uani 1 1 d . . . O1W O 0.15329(18) 0.4604(4) 0.1493(2) 0.0229(7) Uani 1 1 d . . . O2W O 0.2632(2) 0.3170(5) 0.0994(3) 0.0338(9) Uani 1 1 d . . . O2 O 0.30709(16) 0.6225(3) -0.0027(2) 0.0175(6) Uani 1 1 d . . . O3W O 0.0000 0.5000 0.0000 0.113(3) Uani 1 2 d S . . O5 O 0.35173(17) 0.9650(4) 0.0333(2) 0.0236(7) Uani 1 1 d . . . O6 O 0.32834(16) 0.8826(3) 0.1643(2) 0.0201(7) 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 O4 0.0174(15) 0.0211(16) 0.0179(15) 0.0021(13) 0.0069(13) 0.0051(13) O3 0.0144(15) 0.0224(16) 0.0162(15) -0.0045(13) 0.0029(13) -0.0036(12) Ho1 0.01033(11) 0.01650(12) 0.00951(11) 0.00029(7) 0.00393(8) 0.00121(7) C1 0.010(2) 0.015(2) 0.017(2) -0.0008(16) 0.0072(17) 0.0019(16) C2 0.014(2) 0.016(2) 0.015(2) -0.0010(17) 0.0033(17) 0.0009(16) C3 0.013(2) 0.025(2) 0.011(2) -0.0033(17) 0.0027(17) 0.0035(17) C4 0.015(2) 0.017(2) 0.014(2) 0.0004(17) 0.0050(18) 0.0053(17) C5 0.012(2) 0.027(2) 0.013(2) -0.0005(18) 0.0091(18) 0.0005(18) C6 0.012(2) 0.020(2) 0.022(2) -0.0005(18) 0.0047(19) 0.0089(17) C7 0.015(2) 0.021(2) 0.020(2) -0.0004(18) 0.0020(19) -0.0015(18) C8 0.015(3) 0.025(3) 0.017(3) 0.000 0.004(3) 0.000 O1 0.0178(17) 0.050(2) 0.0119(15) 0.0068(14) 0.0059(13) 0.0137(15) O1W 0.0219(18) 0.0320(19) 0.0133(16) 0.0023(14) 0.0056(14) -0.0024(15) O2W 0.038(3) 0.032(2) 0.040(2) 0.0001(16) 0.0254(19) 0.0021(18) O2 0.0112(15) 0.0266(17) 0.0142(15) 0.0027(12) 0.0044(12) 0.0058(12) O3W 0.038(4) 0.209(9) 0.087(5) 0.029(6) 0.020(4) 0.000(5) O5 0.0213(17) 0.0354(19) 0.0140(15) -0.0024(13) 0.0069(13) -0.0085(14) O6 0.0171(16) 0.0282(17) 0.0151(15) -0.0031(12) 0.0067(13) -0.0064(13) _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 O4 C5 1.260(5) . ? O4 Ho1 2.303(3) 7_565 ? O3 C5 1.256(5) . ? O3 Ho1 2.367(3) 6_565 ? Ho1 O4 2.303(3) 7_565 ? Ho1 O5 2.349(3) 7_565 ? Ho1 O3 2.367(3) 6_566 ? Ho1 O6 2.383(3) . ? Ho1 O1W 2.416(3) . ? Ho1 O2 2.430(3) . ? Ho1 O2 2.440(3) 7_565 ? Ho1 O2W 2.501(4) . ? Ho1 O1 2.537(3) . ? Ho1 C4 2.856(4) . ? Ho1 Ho1 3.8829(4) 7_565 ? C1 C3 1.390(5) . ? C1 C2 1.398(5) . ? C1 C4 1.510(5) . ? C2 C3 1.387(5) 5_665 ? C2 C5 1.517(5) . ? C3 C2 1.387(5) 5_665 ? C4 O1 1.235(5) . ? C4 O2 1.284(5) . ? C6 O5 1.247(5) . ? C6 O6 1.271(5) . ? C6 C7 1.516(6) . ? C7 C8 1.518(5) . ? C8 C7 1.518(5) 2_655 ? O2 Ho1 2.440(3) 7_565 ? O5 Ho1 2.349(3) 7_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 C5 O4 Ho1 131.4(2) . 7_565 ? C5 O3 Ho1 132.7(3) . 6_565 ? O4 Ho1 O5 103.20(10) 7_565 7_565 ? O4 Ho1 O3 77.36(9) 7_565 6_566 ? O5 Ho1 O3 146.48(10) 7_565 6_566 ? O4 Ho1 O6 78.30(10) 7_565 . ? O5 Ho1 O6 135.57(10) 7_565 . ? O3 Ho1 O6 77.80(9) 6_566 . ? O4 Ho1 O1W 71.00(11) 7_565 . ? O5 Ho1 O1W 69.29(10) 7_565 . ? O3 Ho1 O1W 79.69(10) 6_566 . ? O6 Ho1 O1W 145.13(10) . . ? O4 Ho1 O2 144.68(9) 7_565 . ? O5 Ho1 O2 75.04(9) 7_565 . ? O3 Ho1 O2 123.65(9) 6_566 . ? O6 Ho1 O2 79.36(9) . . ? O1W Ho1 O2 135.50(10) . . ? O4 Ho1 O2 72.12(9) 7_565 7_565 ? O5 Ho1 O2 70.57(10) 7_565 7_565 ? O3 Ho1 O2 137.60(9) 6_566 7_565 ? O6 Ho1 O2 67.83(9) . 7_565 ? O1W Ho1 O2 115.82(10) . 7_565 ? O2 Ho1 O2 74.25(10) . 7_565 ? O4 Ho1 O2W 136.24(10) 7_565 . ? O5 Ho1 O2W 70.82(12) 7_565 . ? O3 Ho1 O2W 85.61(12) 6_566 . ? O6 Ho1 O2W 136.94(11) . . ? O1W Ho1 O2W 66.40(11) . . ? O2 Ho1 O2W 77.47(10) . . ? O2 Ho1 O2W 136.66(11) 7_565 . ? O4 Ho1 O1 139.27(10) 7_565 . ? O5 Ho1 O1 117.27(10) 7_565 . ? O3 Ho1 O1 71.63(9) 6_566 . ? O6 Ho1 O1 69.95(10) . . ? O1W Ho1 O1 126.43(10) . . ? O2 Ho1 O1 52.20(9) . . ? O2 Ho1 O1 115.93(9) 7_565 . ? O2W Ho1 O1 67.14(12) . . ? O4 Ho1 C4 151.26(11) 7_565 . ? O5 Ho1 C4 96.70(10) 7_565 . ? O3 Ho1 C4 97.18(10) 6_566 . ? O6 Ho1 C4 72.98(10) . . ? O1W Ho1 C4 136.45(11) . . ? O2 Ho1 C4 26.58(10) . . ? O2 Ho1 C4 95.78(10) 7_565 . ? O2W Ho1 C4 70.05(11) . . ? O1 Ho1 C4 25.62(10) . . ? O4 Ho1 Ho1 108.53(7) 7_565 7_565 ? O5 Ho1 Ho1 68.25(7) 7_565 7_565 ? O3 Ho1 Ho1 144.17(7) 6_566 7_565 ? O6 Ho1 Ho1 69.35(6) . 7_565 ? O1W Ho1 Ho1 136.06(7) . 7_565 ? O2 Ho1 Ho1 37.21(6) . 7_565 ? O2 Ho1 Ho1 37.04(6) 7_565 7_565 ? O2W Ho1 Ho1 108.73(8) . 7_565 ? O1 Ho1 Ho1 83.75(6) . 7_565 ? C4 Ho1 Ho1 60.23(8) . 7_565 ? C3 C1 C2 119.7(3) . . ? C3 C1 C4 117.2(3) . . ? C2 C1 C4 123.1(3) . . ? C3 C2 C1 118.6(4) 5_665 . ? C3 C2 C5 116.4(3) 5_665 . ? C1 C2 C5 124.9(3) . . ? C2 C3 C1 121.7(3) 5_665 . ? O1 C4 O2 120.5(3) . . ? O1 C4 C1 120.3(3) . . ? O2 C4 C1 119.2(3) . . ? O1 C4 Ho1 62.6(2) . . ? O2 C4 Ho1 57.89(19) . . ? C1 C4 Ho1 176.6(3) . . ? O3 C5 O4 124.2(4) . . ? O3 C5 C2 117.7(4) . . ? O4 C5 C2 117.9(4) . . ? O5 C6 O6 125.1(4) . . ? O5 C6 C7 117.7(4) . . ? O6 C6 C7 117.1(4) . . ? C6 C7 C8 109.6(3) . . ? C7 C8 C7 111.6(5) . 2_655 ? C4 O1 Ho1 91.8(2) . . ? C4 O2 Ho1 95.5(2) . . ? C4 O2 Ho1 137.5(2) . 7_565 ? Ho1 O2 Ho1 105.75(10) . 7_565 ? C6 O5 Ho1 137.7(3) . 7_565 ? C6 O6 Ho1 133.7(3) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.667 _refine_diff_density_min -0.652 _refine_diff_density_rms 0.122 # Attachment '- 9.cif' data_2b _database_code_depnum_ccdc_archive 'CCDC 761947' #TrackingRef '- 9.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H14 O14 Tb2' _chemical_formula_weight 748.11 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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.7740(10) _cell_length_b 7.2219(10) _cell_length_c 17.336(2) _cell_angle_alpha 90.00 _cell_angle_beta 91.540(2) _cell_angle_gamma 90.00 _cell_volume 973.0(2) _cell_formula_units_Z 2 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 2699 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 28.86 _exptl_crystal_description spicule _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.554 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 704 _exptl_absorpt_coefficient_mu 7.287 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3490 _exptl_absorpt_correction_T_max 0.6038 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 'Bruker SMART APEX' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 4634 _diffrn_reflns_av_R_equivalents 0.0220 _diffrn_reflns_av_sigmaI/netI 0.0252 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -3 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1719 _reflns_number_gt 1544 _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^)+(0.0173P)^2^+0.8172P] 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 1719 _refine_ls_number_parameters 153 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0222 _refine_ls_R_factor_gt 0.0187 _refine_ls_wR_factor_ref 0.0422 _refine_ls_wR_factor_gt 0.0409 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _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 Tb Tb 0.85033(2) 0.51185(2) 0.244809(9) 0.01230(7) Uani 1 1 d . . . C1 C 0.9074(5) 0.2449(5) 0.12401(19) 0.0135(8) Uani 1 1 d . . . C2 C 0.9513(5) 0.1136(5) 0.06117(19) 0.0148(8) Uani 1 1 d . . . C3 C 0.9705(5) -0.0770(5) 0.0728(2) 0.0150(8) Uani 1 1 d . . . C4 C 1.0186(5) -0.1871(5) 0.01144(19) 0.0164(8) Uani 1 1 d . . . H4 H 1.0312 -0.3139 0.0191 0.020 Uiso 1 1 calc R . . C5 C 0.9418(5) 0.8194(5) 0.14657(19) 0.0153(8) Uani 1 1 d . . . C6 C 0.4913(5) 0.3490(5) 0.1455(2) 0.0182(8) Uani 1 1 d . . . C7 C 0.3614(5) 0.4102(6) 0.0843(2) 0.0266(10) Uani 1 1 d . . . H7A H 0.2655 0.4693 0.1091 0.032 Uiso 1 1 calc R . . H7B H 0.3175 0.3019 0.0572 0.032 Uiso 1 1 calc R . . C8 C 0.4356(6) 0.5449(7) 0.0255(3) 0.0361(11) Uani 1 1 d . . . H8A H 0.3422 0.5949 -0.0064 0.043 Uiso 1 1 calc R . . H8B H 0.4902 0.6473 0.0528 0.043 Uiso 1 1 calc R . . H1W H 1.175(8) 0.335(8) 0.308(3) 0.07(2) Uiso 1 1 d . . . H2W H 1.056(8) 0.219(8) 0.295(3) 0.07(2) Uiso 1 1 d . . . O1 O 0.9222(4) 0.4149(3) 0.11433(14) 0.0215(6) Uani 1 1 d . . . O1W O 1.0853(5) 0.3234(5) 0.2889(2) 0.0385(9) Uani 1 1 d . . . O2 O 0.8583(3) 0.1826(3) 0.18905(13) 0.0170(6) Uani 1 1 d . . . O3 O 1.0639(3) 0.7354(4) 0.17804(14) 0.0212(6) Uani 1 1 d . . . O4 O 0.7880(3) 0.8018(3) 0.17149(13) 0.0153(6) Uani 1 1 d . . . O5 O 0.5775(4) 0.4724(3) 0.18107(15) 0.0205(6) Uani 1 1 d . . . O6 O 0.9935(4) 0.6785(4) 0.34126(15) 0.0256(7) 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 Tb 0.01708(11) 0.00933(11) 0.01066(11) -0.00056(7) 0.00341(7) -0.00012(7) C1 0.0147(19) 0.017(2) 0.0085(17) -0.0008(15) 0.0027(14) -0.0027(16) C2 0.019(2) 0.0143(19) 0.0109(18) 0.0000(15) 0.0048(15) 0.0001(16) C3 0.016(2) 0.0171(19) 0.0121(18) 0.0005(15) 0.0038(15) 0.0003(16) C4 0.023(2) 0.0111(18) 0.016(2) 0.0000(15) 0.0064(16) -0.0014(15) C5 0.025(2) 0.0111(18) 0.0105(18) -0.0058(14) 0.0030(16) -0.0027(16) C6 0.017(2) 0.026(2) 0.0113(18) 0.0004(16) 0.0040(15) -0.0005(18) C7 0.024(2) 0.031(2) 0.024(2) 0.0044(19) -0.0062(18) 0.0009(19) C8 0.040(3) 0.039(3) 0.029(2) 0.009(2) -0.004(2) 0.014(2) O1 0.0362(18) 0.0091(13) 0.0197(14) -0.0012(11) 0.0096(12) -0.0018(12) O1W 0.028(2) 0.026(2) 0.061(2) -0.0037(17) -0.0143(18) 0.0023(16) O2 0.0220(15) 0.0167(13) 0.0125(13) -0.0016(10) 0.0059(11) -0.0034(11) O3 0.0217(15) 0.0216(14) 0.0200(14) 0.0040(11) -0.0016(12) 0.0038(12) O4 0.0183(15) 0.0135(13) 0.0142(13) 0.0002(10) 0.0046(11) -0.0026(11) O5 0.0221(15) 0.0172(14) 0.0219(14) -0.0004(11) -0.0031(12) -0.0013(12) O6 0.0363(18) 0.0179(15) 0.0223(15) -0.0035(12) -0.0079(13) 0.0019(13) _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 Tb O6 2.320(3) . ? Tb O2 2.359(2) 2_655 ? Tb O4 2.377(2) 2_645 ? Tb O5 2.382(3) . ? Tb O1W 2.387(3) . ? Tb O1 2.447(2) . ? Tb O4 2.491(2) . ? Tb O2 2.568(2) . ? Tb O3 2.609(3) . ? Tb C1 2.889(3) . ? Tb C5 2.899(4) . ? Tb Tb 3.9395(5) 2_655 ? C1 O1 1.245(4) . ? C1 O2 1.282(4) . ? C1 C2 1.491(5) . ? C2 C4 1.391(5) 3_755 ? C2 C3 1.399(5) . ? C3 C4 1.388(5) . ? C3 C5 1.503(5) 1_545 ? C4 C2 1.391(5) 3_755 ? C5 O3 1.241(4) . ? C5 O4 1.288(4) . ? C5 C3 1.503(5) 1_565 ? C6 O6 1.257(4) 2_645 ? C6 O5 1.266(4) . ? C6 C7 1.512(5) . ? C7 C8 1.532(6) . ? C8 C8 1.501(9) 3_665 ? O2 Tb 2.359(2) 2_645 ? O4 Tb 2.376(2) 2_655 ? O6 C6 1.257(4) 2_655 ? 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 Tb O2 72.63(9) . 2_655 ? O6 Tb O4 96.16(9) . 2_645 ? O2 Tb O4 73.04(9) 2_655 2_645 ? O6 Tb O5 143.16(9) . . ? O2 Tb O5 70.90(9) 2_655 . ? O4 Tb O5 78.17(9) 2_645 . ? O6 Tb O1W 73.56(12) . . ? O2 Tb O1W 132.27(11) 2_655 . ? O4 Tb O1W 78.21(12) 2_645 . ? O5 Tb O1W 138.11(11) . . ? O6 Tb O1 134.24(10) . . ? O2 Tb O1 140.89(9) 2_655 . ? O4 Tb O1 120.01(8) 2_645 . ? O5 Tb O1 76.08(9) . . ? O1W Tb O1 86.62(11) . . ? O6 Tb O4 90.84(8) . . ? O2 Tb O4 71.45(8) 2_655 . ? O4 Tb O4 139.76(4) 2_645 . ? O5 Tb O4 72.86(8) . . ? O1W Tb O4 141.21(11) . . ? O1 Tb O4 79.33(8) . . ? O6 Tb O2 137.35(9) . . ? O2 Tb O2 133.68(6) 2_655 . ? O4 Tb O2 69.80(8) 2_645 . ? O5 Tb O2 75.22(8) . . ? O1W Tb O2 64.31(11) . . ? O1 Tb O2 51.59(8) . . ? O4 Tb O2 126.36(8) . . ? O6 Tb O3 72.55(9) . . ? O2 Tb O3 110.27(8) 2_655 . ? O4 Tb O3 165.89(8) 2_645 . ? O5 Tb O3 115.95(8) . . ? O1W Tb O3 90.24(11) . . ? O1 Tb O3 66.61(8) . . ? O4 Tb O3 50.99(8) . . ? O2 Tb O3 112.57(8) . . ? O6 Tb C1 142.04(10) . . ? O2 Tb C1 145.27(10) 2_655 . ? O4 Tb C1 95.60(9) 2_645 . ? O5 Tb C1 74.69(10) . . ? O1W Tb C1 73.78(12) . . ? O1 Tb C1 25.27(9) . . ? O4 Tb C1 102.86(9) . . ? O2 Tb C1 26.33(8) . . ? O3 Tb C1 88.82(9) . . ? O6 Tb C5 84.58(9) . . ? O2 Tb C5 93.89(9) 2_655 . ? O4 Tb C5 165.91(9) 2_645 . ? O5 Tb C5 92.78(10) . . ? O1W Tb C5 115.29(13) . . ? O1 Tb C5 67.07(9) . . ? O4 Tb C5 26.28(9) . . ? O2 Tb C5 118.65(8) . . ? O3 Tb C5 25.34(9) . . ? C1 Tb C5 92.32(10) . . ? O6 Tb Tb 71.01(7) . 2_655 ? O2 Tb Tb 38.79(6) 2_655 2_655 ? O4 Tb Tb 111.77(6) 2_645 2_655 ? O5 Tb Tb 77.42(6) . 2_655 ? O1W Tb Tb 143.96(9) . 2_655 ? O1 Tb Tb 113.89(6) . 2_655 ? O4 Tb Tb 35.00(5) . 2_655 ? O2 Tb Tb 151.58(6) . 2_655 ? O3 Tb Tb 73.18(6) . 2_655 ? C1 Tb Tb 135.50(7) . 2_655 ? C5 Tb Tb 55.13(7) . 2_655 ? O1 C1 O2 119.7(3) . . ? O1 C1 C2 120.3(3) . . ? O2 C1 C2 119.9(3) . . ? O1 C1 Tb 57.07(17) . . ? O2 C1 Tb 62.73(17) . . ? C2 C1 Tb 175.3(3) . . ? C4 C2 C3 119.1(3) 3_755 . ? C4 C2 C1 117.8(3) 3_755 . ? C3 C2 C1 123.1(3) . . ? C4 C3 C2 118.9(3) . . ? C4 C3 C5 114.6(3) . 1_545 ? C2 C3 C5 126.5(3) . 1_545 ? C3 C4 C2 122.0(4) . 3_755 ? O3 C5 O4 120.7(3) . . ? O3 C5 C3 119.2(3) . 1_565 ? O4 C5 C3 119.6(3) . 1_565 ? O3 C5 Tb 64.15(19) . . ? O4 C5 Tb 58.88(17) . . ? C3 C5 Tb 157.7(2) 1_565 . ? O6 C6 O5 123.7(4) 2_645 . ? O6 C6 C7 118.2(4) 2_645 . ? O5 C6 C7 118.1(3) . . ? C6 C7 C8 113.4(3) . . ? C8 C8 C7 112.7(5) 3_665 . ? C1 O1 Tb 97.7(2) . . ? C1 O2 Tb 146.7(2) . 2_645 ? C1 O2 Tb 90.9(2) . . ? Tb O2 Tb 106.08(9) 2_645 . ? C5 O3 Tb 90.5(2) . . ? C5 O4 Tb 125.5(2) . 2_655 ? C5 O4 Tb 94.8(2) . . ? Tb O4 Tb 108.06(9) 2_655 . ? C6 O5 Tb 139.8(2) . . ? C6 O6 Tb 132.9(2) 2_655 . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.573 _refine_diff_density_min -0.696 _refine_diff_density_rms 0.112 # Attachment '- 12.cif' data_xd _database_code_depnum_ccdc_archive 'CCDC 761949' #TrackingRef '- 12.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H14 Er2 O14' _chemical_formula_weight 764.79 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' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.7489(8) _cell_length_b 7.1601(7) _cell_length_c 17.2940(18) _cell_angle_alpha 90.00 _cell_angle_beta 91.1650(10) _cell_angle_gamma 90.00 _cell_volume 959.32(17) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2271 _cell_measurement_theta_min 2.356 _cell_measurement_theta_max 28.894 _exptl_crystal_description spicule _exptl_crystal_colour Pink _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.648 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 716 _exptl_absorpt_coefficient_mu 8.766 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2521 _exptl_absorpt_correction_T_max 0.5026 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 'Bruker SMART APEX' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 5281 _diffrn_reflns_av_R_equivalents 0.0283 _diffrn_reflns_av_sigmaI/netI 0.0346 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 26.73 _reflns_number_total 2035 _reflns_number_gt 1748 _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^)+(0.0200P)^2^+0.4000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0095(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2035 _refine_ls_number_parameters 146 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0284 _refine_ls_R_factor_gt 0.0231 _refine_ls_wR_factor_ref 0.0524 _refine_ls_wR_factor_gt 0.0501 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.062 _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 Er1 Er 0.34753(2) 0.48793(2) 0.244532(10) 0.01228(10) Uani 1 1 d . . . O1W O 0.5820(4) 0.6710(4) 0.2864(2) 0.0348(9) Uani 1 1 d . . . H1A H 0.6819 0.6694 0.3029 0.052 Uiso 1 1 d R . . H1B H 0.5516 0.7803 0.2824 0.052 Uiso 1 1 d R . . O1 O 0.2884(4) 0.1994(4) 0.17294(17) 0.0153(7) Uani 1 1 d . . . O2 O 0.5658(4) 0.2664(4) 0.17850(18) 0.0202(7) Uani 1 1 d . . . O3 O 0.3578(4) -0.1825(4) 0.18950(17) 0.0160(7) Uani 1 1 d . . . O4 O 0.4202(4) -0.4178(4) 0.11527(17) 0.0201(7) Uani 1 1 d . . . O5 O 0.0100(4) 0.8235(4) 0.15970(19) 0.0234(8) Uani 1 1 d . . . O6 O 0.0779(4) 0.5266(4) 0.18223(19) 0.0202(7) Uani 1 1 d . . . C1 C 0.4426(6) 0.1814(5) 0.1477(2) 0.0135(9) Uani 1 1 d U . . C2 C 0.4703(5) 0.0777(6) 0.0727(2) 0.0136(9) Uani 1 1 d . . . C3 C 0.4502(6) -0.1150(6) 0.0612(2) 0.0146(9) Uani 1 1 d . . . C4 C 0.5199(5) 0.1889(6) 0.0113(2) 0.0153(10) Uani 1 1 d . . . H4A H 0.5335 0.3167 0.0190 0.018 Uiso 1 1 calc R . . C5 C 0.4059(5) -0.2468(6) 0.1250(2) 0.0142(9) Uani 1 1 d . . . C6 C -0.0074(6) 0.6518(6) 0.1462(3) 0.0182(10) Uani 1 1 d . . . C7 C -0.1371(6) 0.5921(7) 0.0859(3) 0.0253(11) Uani 1 1 d . . . H7A H -0.1808 0.7020 0.0592 0.030 Uiso 1 1 calc R . . H7B H -0.2334 0.5329 0.1112 0.030 Uiso 1 1 calc R . . C8 C -0.0643(7) 0.4568(7) 0.0264(3) 0.0315(12) Uani 1 1 d . . . H8A H -0.0097 0.3533 0.0536 0.038 Uiso 1 1 calc R . . H8B H -0.1591 0.4066 -0.0046 0.038 Uiso 1 1 calc 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 Er1 0.01780(14) 0.00980(13) 0.00937(13) 0.00045(7) 0.00375(8) 0.00011(7) O1W 0.026(2) 0.0252(19) 0.053(3) 0.0026(17) -0.0154(18) -0.0043(15) O1 0.0188(17) 0.0133(15) 0.0139(16) 0.0004(12) 0.0054(13) 0.0015(12) O2 0.0196(17) 0.0236(17) 0.0174(18) -0.0030(13) 0.0022(14) -0.0010(14) O3 0.0239(17) 0.0129(15) 0.0115(16) 0.0013(12) 0.0071(13) 0.0007(12) O4 0.035(2) 0.0102(15) 0.0152(16) 0.0002(13) 0.0093(14) 0.0018(13) O5 0.036(2) 0.0144(16) 0.0199(18) -0.0024(13) -0.0059(15) 0.0021(14) O6 0.0228(18) 0.0160(16) 0.0217(18) -0.0007(13) -0.0004(14) 0.0006(13) C1 0.026(2) 0.0075(19) 0.008(2) 0.0058(16) 0.0055(18) 0.0027(16) C2 0.014(2) 0.017(2) 0.010(2) -0.0033(17) 0.0037(17) 0.0010(17) C3 0.017(2) 0.015(2) 0.012(2) 0.0018(17) 0.0028(18) 0.0013(17) C4 0.022(2) 0.008(2) 0.017(3) 0.0001(16) 0.006(2) 0.0010(16) C5 0.017(2) 0.012(2) 0.013(2) 0.0018(17) 0.0041(18) -0.0016(17) C6 0.023(2) 0.021(2) 0.011(2) -0.0002(18) 0.0035(19) 0.0012(19) C7 0.022(3) 0.034(3) 0.020(3) -0.006(2) -0.007(2) -0.002(2) C8 0.034(3) 0.037(3) 0.024(3) -0.011(2) -0.002(2) -0.009(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 Er1 O5 2.297(3) 2_545 ? Er1 O3 2.323(3) 2 ? Er1 O1W 2.343(3) . ? Er1 O1 2.345(3) 2 ? Er1 O6 2.348(3) . ? Er1 O4 2.413(3) 1_565 ? Er1 O1 2.447(3) . ? Er1 O3 2.547(3) 1_565 ? Er1 O2 2.600(3) . ? Er1 C5 2.850(4) 1_565 ? Er1 C1 2.866(4) . ? Er1 Er1 3.8921(4) 2 ? O1W H1A 0.8200 . ? O1W H1B 0.8200 . ? O1 C1 1.287(5) . ? O1 Er1 2.345(3) 2_545 ? O2 C1 1.242(5) . ? O3 C5 1.270(5) . ? O3 Er1 2.323(3) 2_545 ? O3 Er1 2.547(3) 1_545 ? O4 C5 1.242(5) . ? O4 Er1 2.413(3) 1_545 ? O5 C6 1.258(5) . ? O5 Er1 2.297(3) 2 ? O6 C6 1.270(5) . ? C1 C2 1.513(6) . ? C2 C4 1.389(6) . ? C2 C3 1.402(6) . ? C3 C4 1.385(6) 3_655 ? C3 C5 1.497(6) . ? C4 C3 1.385(6) 3_655 ? C4 H4A 0.9300 . ? C5 Er1 2.850(4) 1_545 ? C6 C7 1.495(6) . ? C7 C8 1.530(7) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C8 1.499(10) 3_565 ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? 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 Er1 O3 72.59(11) 2_545 2 ? O5 Er1 O1W 72.86(12) 2_545 . ? O3 Er1 O1W 132.57(12) 2 . ? O5 Er1 O1 96.17(11) 2_545 2 ? O3 Er1 O1 73.72(10) 2 2 ? O1W Er1 O1 78.78(11) . 2 ? O5 Er1 O6 143.30(11) 2_545 . ? O3 Er1 O6 71.04(11) 2 . ? O1W Er1 O6 138.87(10) . . ? O1 Er1 O6 78.27(10) 2 . ? O5 Er1 O4 133.92(11) 2_545 1_565 ? O3 Er1 O4 141.00(11) 2 1_565 ? O1W Er1 O4 86.33(12) . 1_565 ? O1 Er1 O4 119.97(10) 2 1_565 ? O6 Er1 O4 76.36(11) . 1_565 ? O5 Er1 O1 90.82(10) 2_545 . ? O3 Er1 O1 71.46(10) 2 . ? O1W Er1 O1 139.89(11) . . ? O1 Er1 O1 140.46(5) 2 . ? O6 Er1 O1 73.23(10) . . ? O4 Er1 O1 79.17(10) 1_565 . ? O5 Er1 O3 136.58(10) 2_545 1_565 ? O3 Er1 O3 134.21(7) 2 1_565 ? O1W Er1 O3 64.35(11) . 1_565 ? O1 Er1 O3 69.33(9) 2 1_565 ? O6 Er1 O3 75.74(10) . 1_565 ? O4 Er1 O3 52.04(9) 1_565 1_565 ? O1 Er1 O3 126.89(10) . 1_565 ? O5 Er1 O2 72.32(11) 2_545 . ? O3 Er1 O2 110.70(10) 2 . ? O1W Er1 O2 88.29(11) . . ? O1 Er1 O2 164.90(10) 2 . ? O6 Er1 O2 116.81(10) . . ? O4 Er1 O2 66.26(10) 1_565 . ? O1 Er1 O2 51.63(9) . . ? O3 Er1 O2 112.07(9) 1_565 . ? O5 Er1 C5 141.59(12) 2_545 1_565 ? O3 Er1 C5 145.75(12) 2 1_565 ? O1W Er1 C5 73.62(13) . 1_565 ? O1 Er1 C5 95.22(11) 2 1_565 ? O6 Er1 C5 75.02(11) . 1_565 ? O4 Er1 C5 25.60(10) 1_565 1_565 ? O1 Er1 C5 103.09(11) . 1_565 ? O3 Er1 C5 26.45(10) 1_565 1_565 ? O2 Er1 C5 88.50(11) . 1_565 ? O5 Er1 C1 84.43(11) 2_545 . ? O3 Er1 C1 94.10(10) 2 . ? O1W Er1 C1 113.72(12) . . ? O1 Er1 C1 166.89(11) 2 . ? O6 Er1 C1 93.40(12) . . ? O4 Er1 C1 66.76(10) 1_565 . ? O1 Er1 C1 26.56(11) . . ? O3 Er1 C1 118.76(10) 1_565 . ? O2 Er1 C1 25.68(10) . . ? C5 Er1 C1 92.31(11) 1_565 . ? O5 Er1 Er1 128.17(8) 2_545 2 ? O3 Er1 Er1 100.87(7) 2 2 ? O1W Er1 Er1 76.69(8) . 2 ? O1 Er1 Er1 36.57(7) 2 2 ? O6 Er1 Er1 64.60(7) . 2 ? O4 Er1 Er1 83.46(7) 1_565 2 ? O1 Er1 Er1 137.08(7) . 2 ? O3 Er1 Er1 35.00(6) 1_565 2 ? O2 Er1 Er1 147.07(7) . 2 ? C5 Er1 Er1 59.32(8) 1_565 2 ? C1 Er1 Er1 146.89(8) . 2 ? Er1 O1W H1A 145.1 . . ? Er1 O1W H1B 106.8 . . ? H1A O1W H1B 108.1 . . ? C1 O1 Er1 125.0(2) . 2_545 ? C1 O1 Er1 95.2(2) . . ? Er1 O1 Er1 108.60(11) 2_545 . ? C1 O2 Er1 89.2(2) . . ? C5 O3 Er1 146.9(3) . 2_545 ? C5 O3 Er1 90.2(2) . 1_545 ? Er1 O3 Er1 106.04(10) 2_545 1_545 ? C5 O4 Er1 97.3(2) . 1_545 ? C6 O5 Er1 133.1(3) . 2 ? C6 O6 Er1 139.3(3) . . ? O2 C1 O1 121.1(4) . . ? O2 C1 C2 119.1(4) . . ? O1 C1 C2 119.2(4) . . ? O2 C1 Er1 65.1(2) . . ? O1 C1 Er1 58.2(2) . . ? C2 C1 Er1 156.7(3) . . ? C4 C2 C3 119.1(4) . . ? C4 C2 C1 114.9(4) . . ? C3 C2 C1 126.0(4) . . ? C4 C3 C2 119.0(4) 3_655 . ? C4 C3 C5 118.1(4) 3_655 . ? C2 C3 C5 122.8(4) . . ? C3 C4 C2 121.9(4) 3_655 . ? C3 C4 H4A 119.1 3_655 . ? C2 C4 H4A 119.1 . . ? O4 C5 O3 120.4(4) . . ? O4 C5 C3 120.0(4) . . ? O3 C5 C3 119.6(4) . . ? O4 C5 Er1 57.1(2) . 1_545 ? O3 C5 Er1 63.3(2) . 1_545 ? C3 C5 Er1 175.4(3) . 1_545 ? O5 C6 O6 123.1(4) . . ? O5 C6 C7 118.5(4) . . ? O6 C6 C7 118.4(4) . . ? C6 C7 C8 113.5(4) . . ? C6 C7 H7A 108.9 . . ? C8 C7 H7A 108.9 . . ? C6 C7 H7B 108.9 . . ? C8 C7 H7B 108.9 . . ? H7A C7 H7B 107.7 . . ? C8 C8 C7 114.0(5) 3_565 . ? C8 C8 H8A 108.7 3_565 . ? C7 C8 H8A 108.7 . . ? C8 C8 H8B 108.7 3_565 . ? C7 C8 H8B 108.7 . . ? H8A C8 H8B 107.6 . . ? 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 Er1 O1 C1 -75.8(2) 2_545 . . . ? O3 Er1 O1 C1 -147.1(3) 2 . . . ? O1W Er1 O1 C1 -11.9(3) . . . . ? O1 Er1 O1 C1 -176.5(2) 2 . . . ? O6 Er1 O1 C1 137.8(2) . . . . ? O4 Er1 O1 C1 58.9(2) 1_565 . . . ? O3 Er1 O1 C1 81.0(2) 1_565 . . . ? O2 Er1 O1 C1 -9.3(2) . . . . ? C5 Er1 O1 C1 68.1(2) 1_565 . . . ? Er1 Er1 O1 C1 126.9(2) 2 . . . ? O5 Er1 O1 Er1 53.84(13) 2_545 . . 2_545 ? O3 Er1 O1 Er1 -17.46(11) 2 . . 2_545 ? O1W Er1 O1 Er1 117.71(16) . . . 2_545 ? O1 Er1 O1 Er1 -46.89(15) 2 . . 2_545 ? O6 Er1 O1 Er1 -92.58(13) . . . 2_545 ? O4 Er1 O1 Er1 -171.45(13) 1_565 . . 2_545 ? O3 Er1 O1 Er1 -149.36(10) 1_565 . . 2_545 ? O2 Er1 O1 Er1 120.35(16) . . . 2_545 ? C5 Er1 O1 Er1 -162.26(12) 1_565 . . 2_545 ? C1 Er1 O1 Er1 129.6(3) . . . 2_545 ? Er1 Er1 O1 Er1 -103.54(11) 2 . . 2_545 ? O5 Er1 O2 C1 115.3(3) 2_545 . . . ? O3 Er1 O2 C1 52.5(3) 2 . . . ? O1W Er1 O2 C1 -172.1(3) . . . . ? O1 Er1 O2 C1 156.9(3) 2 . . . ? O6 Er1 O2 C1 -26.1(3) . . . . ? O4 Er1 O2 C1 -85.4(3) 1_565 . . . ? O1 Er1 O2 C1 9.6(2) . . . . ? O3 Er1 O2 C1 -110.8(2) 1_565 . . . ? C5 Er1 O2 C1 -98.5(2) 1_565 . . . ? Er1 Er1 O2 C1 -110.2(2) 2 . . . ? O5 Er1 O6 C6 152.6(4) 2_545 . . . ? O3 Er1 O6 C6 144.7(5) 2 . . . ? O1W Er1 O6 C6 10.7(5) . . . . ? O1 Er1 O6 C6 68.0(4) 2 . . . ? O4 Er1 O6 C6 -57.1(4) 1_565 . . . ? O1 Er1 O6 C6 -139.7(5) . . . . ? O3 Er1 O6 C6 -3.3(4) 1_565 . . . ? O2 Er1 O6 C6 -111.2(4) . . . . ? C5 Er1 O6 C6 -30.7(4) 1_565 . . . ? C1 Er1 O6 C6 -122.2(4) . . . . ? Er1 Er1 O6 C6 32.1(4) 2 . . . ? Er1 O2 C1 O1 -16.8(4) . . . . ? Er1 O2 C1 C2 154.3(3) . . . . ? Er1 O1 C1 O2 -99.0(4) 2_545 . . . ? Er1 O1 C1 O2 18.0(4) . . . . ? Er1 O1 C1 C2 89.9(4) 2_545 . . . ? Er1 O1 C1 C2 -153.1(3) . . . . ? Er1 O1 C1 Er1 -117.0(3) 2_545 . . . ? O5 Er1 C1 O2 -59.9(2) 2_545 . . . ? O3 Er1 C1 O2 -132.0(2) 2 . . . ? O1W Er1 C1 O2 8.6(3) . . . . ? O1 Er1 C1 O2 -153.2(4) 2 . . . ? O6 Er1 C1 O2 156.8(2) . . . . ? O4 Er1 C1 O2 83.2(2) 1_565 . . . ? O1 Er1 C1 O2 -163.1(4) . . . . ? O3 Er1 C1 O2 81.2(3) 1_565 . . . ? C5 Er1 C1 O2 81.7(2) 1_565 . . . ? Er1 Er1 C1 O2 110.9(2) 2 . . . ? O5 Er1 C1 O1 103.1(2) 2_545 . . . ? O3 Er1 C1 O1 31.1(2) 2 . . . ? O1W Er1 C1 O1 171.7(2) . . . . ? O1 Er1 C1 O1 9.9(7) 2 . . . ? O6 Er1 C1 O1 -40.1(2) . . . . ? O4 Er1 C1 O1 -113.7(3) 1_565 . . . ? O3 Er1 C1 O1 -115.7(2) 1_565 . . . ? O2 Er1 C1 O1 163.1(4) . . . . ? C5 Er1 C1 O1 -115.2(2) 1_565 . . . ? Er1 Er1 C1 O1 -86.0(2) 2 . . . ? O5 Er1 C1 C2 -166.1(8) 2_545 . . . ? O3 Er1 C1 C2 121.9(8) 2 . . . ? O1W Er1 C1 C2 -97.6(8) . . . . ? O1 Er1 C1 C2 100.6(8) 2 . . . ? O6 Er1 C1 C2 50.7(8) . . . . ? O4 Er1 C1 C2 -22.9(7) 1_565 . . . ? O1 Er1 C1 C2 90.8(8) . . . . ? O3 Er1 C1 C2 -24.9(8) 1_565 . . . ? O2 Er1 C1 C2 -106.2(8) . . . . ? C5 Er1 C1 C2 -24.4(8) 1_565 . . . ? Er1 Er1 C1 C2 4.8(9) 2 . . . ? O2 C1 C2 C4 -61.3(5) . . . . ? O1 C1 C2 C4 109.9(4) . . . . ? Er1 C1 C2 C4 33.0(10) . . . . ? O2 C1 C2 C3 118.7(5) . . . . ? O1 C1 C2 C3 -70.1(6) . . . . ? Er1 C1 C2 C3 -147.0(6) . . . . ? C4 C2 C3 C4 -0.2(7) . . . 3_655 ? C1 C2 C3 C4 179.8(4) . . . 3_655 ? C4 C2 C3 C5 176.8(4) . . . . ? C1 C2 C3 C5 -3.2(7) . . . . ? C3 C2 C4 C3 0.2(7) . . . 3_655 ? C1 C2 C4 C3 -179.8(4) . . . 3_655 ? Er1 O4 C5 O3 -2.4(5) 1_545 . . . ? Er1 O4 C5 C3 175.8(3) 1_545 . . . ? Er1 O3 C5 O4 -118.6(5) 2_545 . . . ? Er1 O3 C5 O4 2.3(4) 1_545 . . . ? Er1 O3 C5 C3 63.2(7) 2_545 . . . ? Er1 O3 C5 C3 -176.0(4) 1_545 . . . ? Er1 O3 C5 Er1 -120.9(5) 2_545 . . 1_545 ? C4 C3 C5 O4 10.1(6) 3_655 . . . ? C2 C3 C5 O4 -166.9(4) . . . . ? C4 C3 C5 O3 -171.7(4) 3_655 . . . ? C2 C3 C5 O3 11.3(7) . . . . ? C4 C3 C5 Er1 60(4) 3_655 . . 1_545 ? C2 C3 C5 Er1 -117(4) . . . 1_545 ? Er1 O5 C6 O6 -9.9(7) 2 . . . ? Er1 O5 C6 C7 168.9(3) 2 . . . ? Er1 O6 C6 O5 -29.6(7) . . . . ? Er1 O6 C6 C7 151.6(3) . . . . ? O5 C6 C7 C8 129.6(5) . . . . ? O6 C6 C7 C8 -51.5(6) . . . . ? C6 C7 C8 C8 -68.9(7) . . . 3_565 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.73 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.876 _refine_diff_density_min -0.847 _refine_diff_density_rms 0.156 # Attachment '- 10.cif' data_1e _database_code_depnum_ccdc_archive 'CCDC 771319' #TrackingRef '- 10.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H14 Eu2 O14' _chemical_formula_weight 734.19 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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.7869(19) _cell_length_b 7.2672(18) _cell_length_c 17.370(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.799(3) _cell_angle_gamma 90.00 _cell_volume 982.5(4) _cell_formula_units_Z 2 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 2533 _cell_measurement_theta_min 2.83 _cell_measurement_theta_max 29.09 _exptl_crystal_description spicule _exptl_crystal_colour colorless _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.482 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 696 _exptl_absorpt_coefficient_mu 6.402 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4056 _exptl_absorpt_correction_T_max 0.6810 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 'Bruker SMART APEX' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 4760 _diffrn_reflns_av_R_equivalents 0.0275 _diffrn_reflns_av_sigmaI/netI 0.0318 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.83 _diffrn_reflns_theta_max 24.99 _reflns_number_total 1736 _reflns_number_gt 1526 _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^)+(0.0248P)^2^+0.1701P] 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 1736 _refine_ls_number_parameters 153 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0256 _refine_ls_R_factor_gt 0.0214 _refine_ls_wR_factor_ref 0.0539 _refine_ls_wR_factor_gt 0.0519 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _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 H1WB H 0.561(7) 0.788(7) 0.300(3) 0.058(15) Uiso 1 1 d U . . H1WA H 0.674(7) 0.664(8) 0.301(4) 0.054(15) Uiso 1 1 d U . . C7 C -0.1391(6) 0.5881(6) 0.0837(3) 0.0264(10) Uani 1 1 d . . . H7A H -0.1834 0.6955 0.0566 0.032 Uiso 1 1 calc RU . . H7B H -0.2348 0.5289 0.1082 0.032 Uiso 1 1 calc RU . . Eu1 Eu 0.35278(2) 0.48817(2) 0.245026(11) 0.01187(9) Uani 1 1 d . . . O5 O 0.0760(4) 0.5282(3) 0.18119(18) 0.0203(7) Uani 1 1 d . . . O2 O 0.3583(4) 0.8182(3) 0.18849(16) 0.0172(6) Uani 1 1 d . . . C4 C 0.4076(5) 0.7559(5) 0.1239(2) 0.0145(9) Uani 1 1 d . . . O3 O 0.2870(3) 0.1979(3) 0.17024(15) 0.0142(6) Uani 1 1 d . . . O4 O 0.5630(3) 0.2634(3) 0.17750(16) 0.0189(6) Uani 1 1 d . . . C6 C -0.0109(5) 0.6495(5) 0.1450(2) 0.0174(9) Uani 1 1 d . . . C2 C 0.4702(5) 0.0767(5) 0.0725(2) 0.0136(8) Uani 1 1 d . . . O1 O 0.4238(4) 0.5880(3) 0.11381(16) 0.0207(7) Uani 1 1 d . . . C5 C 0.4422(5) 0.1799(5) 0.1461(2) 0.0139(9) Uani 1 1 d . . . C1 C 0.4506(5) 0.8871(5) 0.0610(2) 0.0140(8) Uani 1 1 d . . . O1W O 0.5870(5) 0.6807(5) 0.2903(2) 0.0371(10) Uani 1 1 d . . . C3 C 0.5186(5) 0.1869(5) 0.0114(2) 0.0150(9) Uani 1 1 d . . . H3 H 0.5307 0.3130 0.0190 0.018 Uiso 1 1 calc RU . . C8 C -0.0645(7) 0.4551(7) 0.0254(3) 0.0331(12) Uani 1 1 d . . . H8A H -0.0097 0.3536 0.0528 0.040 Uiso 1 1 calc RU . . H8B H -0.1574 0.4049 -0.0067 0.040 Uiso 1 1 calc RU . . O6 O 0.0033(4) 0.8187(4) 0.15835(17) 0.0247(7) 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 C7 0.027(3) 0.030(2) 0.022(3) -0.006(2) -0.008(2) 0.000(2) Eu1 0.01686(15) 0.01005(13) 0.00891(14) 0.00052(8) 0.00377(9) 0.00013(7) O5 0.0220(17) 0.0201(14) 0.0186(18) 0.0007(12) -0.0031(14) 0.0018(12) O2 0.0269(17) 0.0159(13) 0.0093(16) 0.0010(12) 0.0066(13) 0.0036(12) C4 0.014(2) 0.019(2) 0.011(2) 0.0011(17) 0.0039(17) 0.0001(16) O3 0.0193(16) 0.0122(12) 0.0116(15) 0.0011(11) 0.0063(12) 0.0016(11) O4 0.0209(16) 0.0200(14) 0.0158(16) -0.0035(12) -0.0013(13) -0.0021(12) C6 0.016(2) 0.028(2) 0.009(2) -0.0031(17) 0.0025(17) -0.0003(17) C2 0.017(2) 0.0143(19) 0.009(2) -0.0015(16) 0.0021(17) 0.0013(16) O1 0.0387(19) 0.0100(13) 0.0142(16) 0.0015(12) 0.0122(14) 0.0004(12) C5 0.025(2) 0.0112(18) 0.006(2) 0.0048(15) 0.0052(18) 0.0027(16) C1 0.017(2) 0.0158(19) 0.009(2) -0.0002(16) 0.0045(17) 0.0023(16) O1W 0.025(2) 0.0255(17) 0.060(3) 0.0007(18) -0.017(2) -0.0027(16) C3 0.024(2) 0.0098(18) 0.012(2) 0.0002(15) 0.0054(18) 0.0021(15) C8 0.036(3) 0.038(3) 0.025(3) -0.009(2) -0.006(2) -0.013(2) O6 0.0383(19) 0.0163(14) 0.0190(17) -0.0033(13) -0.0073(14) 0.0021(13) _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 C7 C6 1.504(6) . ? C7 C8 1.529(6) . ? Eu1 O6 2.339(3) 2_545 ? Eu1 O2 2.383(3) 2_545 ? Eu1 O3 2.403(2) 2 ? Eu1 O5 2.410(3) . ? Eu1 O1W 2.411(4) . ? Eu1 O1 2.471(3) . ? Eu1 O3 2.522(3) . ? Eu1 O2 2.593(3) . ? Eu1 O4 2.616(3) . ? Eu1 C4 2.907(4) . ? Eu1 C5 2.921(4) . ? Eu1 Eu1 3.9765(9) 2 ? O5 C6 1.266(5) . ? O2 C4 1.279(5) . ? O2 Eu1 2.383(3) 2 ? C4 O1 1.240(4) . ? C4 C1 1.496(5) . ? O3 C5 1.298(5) . ? O3 Eu1 2.403(2) 2_545 ? O4 C5 1.232(5) . ? C6 O6 1.256(5) . ? C2 C3 1.391(5) . ? C2 C1 1.400(5) 1_545 ? C2 C5 1.505(5) . ? C1 C3 1.395(5) 3_665 ? C1 C2 1.400(5) 1_565 ? C3 C1 1.395(5) 3_665 ? C8 C8 1.507(10) 3_565 ? O6 Eu1 2.339(3) 2 ? 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 C6 C7 C8 113.5(4) . . ? O6 Eu1 O2 72.64(10) 2_545 2_545 ? O6 Eu1 O3 96.34(10) 2_545 2 ? O2 Eu1 O3 72.50(9) 2_545 2 ? O6 Eu1 O5 142.66(10) 2_545 . ? O2 Eu1 O5 70.44(10) 2_545 . ? O3 Eu1 O5 77.85(10) 2 . ? O6 Eu1 O1W 74.38(12) 2_545 . ? O2 Eu1 O1W 131.96(12) 2_545 . ? O3 Eu1 O1W 77.56(11) 2 . ? O5 Eu1 O1W 137.43(10) . . ? O6 Eu1 O1 134.45(10) 2_545 . ? O2 Eu1 O1 140.98(10) 2_545 . ? O3 Eu1 O1 119.84(8) 2 . ? O5 Eu1 O1 76.29(10) . . ? O1W Eu1 O1 86.66(12) . . ? O6 Eu1 O3 90.82(9) 2_545 . ? O2 Eu1 O3 71.59(9) 2_545 . ? O3 Eu1 O3 139.25(4) 2 . ? O5 Eu1 O3 72.53(9) . . ? O1W Eu1 O3 142.47(11) . . ? O1 Eu1 O3 79.52(9) . . ? O6 Eu1 O2 138.20(9) 2_545 . ? O2 Eu1 O2 133.07(6) 2_545 . ? O3 Eu1 O2 70.03(8) 2 . ? O5 Eu1 O2 74.89(9) . . ? O1W Eu1 O2 64.24(11) . . ? O1 Eu1 O2 51.11(8) . . ? O3 Eu1 O2 125.76(9) . . ? O6 Eu1 O4 72.58(10) 2_545 . ? O2 Eu1 O4 110.15(9) 2_545 . ? O3 Eu1 O4 166.52(9) 2 . ? O5 Eu1 O4 115.60(9) . . ? O1W Eu1 O4 91.78(11) . . ? O1 Eu1 O4 66.94(9) . . ? O3 Eu1 O4 50.69(8) . . ? O2 Eu1 O4 112.93(8) . . ? O6 Eu1 C4 142.53(11) 2_545 . ? O2 Eu1 C4 144.76(10) 2_545 . ? O3 Eu1 C4 95.64(10) 2 . ? O5 Eu1 C4 74.68(10) . . ? O1W Eu1 C4 73.80(12) . . ? O1 Eu1 C4 25.02(9) . . ? O3 Eu1 C4 102.67(10) . . ? O2 Eu1 C4 26.11(9) . . ? O4 Eu1 C4 89.16(9) . . ? O6 Eu1 C5 84.29(10) 2_545 . ? O2 Eu1 C5 93.92(9) 2_545 . ? O3 Eu1 C5 165.40(10) 2 . ? O5 Eu1 C5 92.77(11) . . ? O1W Eu1 C5 116.44(12) . . ? O1 Eu1 C5 67.55(9) . . ? O3 Eu1 C5 26.31(10) . . ? O2 Eu1 C5 118.67(9) . . ? O4 Eu1 C5 24.94(10) . . ? C4 Eu1 C5 92.56(11) . . ? O6 Eu1 Eu1 129.37(7) 2_545 2 ? O2 Eu1 Eu1 99.66(6) 2_545 2 ? O3 Eu1 Eu1 37.17(6) 2 2 ? O5 Eu1 Eu1 63.53(6) . 2 ? O1W Eu1 Eu1 75.94(8) . 2 ? O1 Eu1 Eu1 82.76(6) . 2 ? O3 Eu1 Eu1 135.34(6) . 2 ? O2 Eu1 Eu1 35.17(6) . 2 ? O4 Eu1 Eu1 148.04(6) . 2 ? C4 Eu1 Eu1 59.22(8) . 2 ? C5 Eu1 Eu1 146.12(8) . 2 ? C6 O5 Eu1 140.3(3) . . ? C4 O2 Eu1 147.0(3) . 2 ? C4 O2 Eu1 90.8(2) . . ? Eu1 O2 Eu1 106.02(10) 2 . ? O1 C4 O2 120.5(3) . . ? O1 C4 C1 119.8(3) . . ? O2 C4 C1 119.7(3) . . ? O1 C4 Eu1 57.4(2) . . ? O2 C4 Eu1 63.10(19) . . ? C1 C4 Eu1 175.2(3) . . ? C5 O3 Eu1 125.3(2) . 2_545 ? C5 O3 Eu1 94.3(2) . . ? Eu1 O3 Eu1 107.68(10) 2_545 . ? C5 O4 Eu1 91.5(2) . . ? O6 C6 O5 123.2(4) . . ? O6 C6 C7 118.3(4) . . ? O5 C6 C7 118.5(4) . . ? C3 C2 C1 119.3(3) . 1_545 ? C3 C2 C5 114.3(3) . . ? C1 C2 C5 126.4(3) 1_545 . ? C4 O1 Eu1 97.6(2) . . ? O4 C5 O3 120.9(4) . . ? O4 C5 C2 119.5(4) . . ? O3 C5 C2 119.1(4) . . ? O4 C5 Eu1 63.6(2) . . ? O3 C5 Eu1 59.42(18) . . ? C2 C5 Eu1 157.8(3) . . ? C3 C1 C2 119.2(3) 3_665 1_565 ? C3 C1 C4 117.5(3) 3_665 . ? C2 C1 C4 123.3(3) 1_565 . ? C2 C3 C1 121.6(4) . 3_665 ? C8 C8 C7 112.9(5) 3_565 . ? C6 O6 Eu1 133.3(3) . 2 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.535 _refine_diff_density_min -0.787 _refine_diff_density_rms 0.146 # Attachment '- 2.cif' data_2a _database_code_depnum_ccdc_archive 'CCDC 773491' #TrackingRef '- 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H10 O16 Tb2' _chemical_formula_weight 728.04 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.2191(12) _cell_length_b 8.5786(17) _cell_length_c 8.9113(18) _cell_angle_alpha 110.89(3) _cell_angle_beta 110.11(3) _cell_angle_gamma 91.64(3) _cell_volume 410.85(14) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3926 _cell_measurement_theta_min 3.525 _cell_measurement_theta_max 27.505 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.943 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 340 _exptl_absorpt_coefficient_mu 8.632 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2514 _exptl_absorpt_correction_T_max 0.4975 _exptl_absorpt_process_details 'Higashi, T. (1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID IP' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 4041 _diffrn_reflns_av_R_equivalents 0.0158 _diffrn_reflns_av_sigmaI/netI 0.0193 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.53 _diffrn_reflns_theta_max 27.48 _reflns_number_total 1864 _reflns_number_gt 1819 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Rgaku R-AXIS RAPID' _computing_cell_refinement 'Rgaku R-AXIS RAPID' _computing_data_reduction 'Rgaku R-AXIS RAPID' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXP-97 _computing_publication_material SHELXP-97 _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^)+(0.0241P)^2^+0.6199P] 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 1864 _refine_ls_number_parameters 152 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0158 _refine_ls_R_factor_gt 0.0152 _refine_ls_wR_factor_ref 0.0507 _refine_ls_wR_factor_gt 0.0505 _refine_ls_goodness_of_fit_ref 1.332 _refine_ls_restrained_S_all 1.330 _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 H2WB H 1.246(8) 0.346(7) 0.945(3) 0.027(14) Uiso 1 1 d D . . H2WA H 1.294(7) 0.271(6) 0.800(5) 0.022(13) Uiso 1 1 d D . . H1WA H 0.980(9) 0.323(8) 0.412(4) 0.038(17) Uiso 1 1 d D . . H1WB H 1.128(8) 0.253(7) 0.513(7) 0.039(17) Uiso 1 1 d D . . Tb1 Tb 0.80981(3) 0.353595(19) 0.685510(19) 0.00887(7) Uani 1 1 d . . . O1 O 0.5964(5) 0.5691(3) 0.7981(4) 0.0157(5) Uani 1 1 d . . . O5 O 0.7969(5) 0.0576(4) 0.5638(4) 0.0216(6) Uani 1 1 d . . . O2W O 1.1919(5) 0.3106(4) 0.8364(4) 0.0225(6) Uani 1 1 d D . . O6 O 0.4325(5) 0.1938(3) 0.6052(4) 0.0194(6) Uani 1 1 d . . . C1 C 0.4923(6) 0.8427(5) 0.8742(4) 0.0093(6) Uani 1 1 d . . . O1W O 1.0288(6) 0.3175(5) 0.5090(4) 0.0250(7) Uani 1 1 d D . . C4 C 0.5026(6) 0.6757(5) 0.7414(5) 0.0108(7) Uani 1 1 d . . . C2 C 0.6471(6) 1.1436(5) 1.0292(4) 0.0099(6) Uani 1 1 d . . . C3 C 0.6368(6) 0.9867(5) 0.9045(5) 0.0097(6) Uani 1 1 d . . . H3 H 0.7289 0.9776 0.8397 0.012 Uiso 1 1 calc R . . C6 C 0.6069(6) -0.0381(5) 0.4883(5) 0.0135(7) Uani 1 1 d . . . O2 O 0.4303(5) 0.6580(4) 0.5858(4) 0.0213(6) Uani 1 1 d . . . C5 C 0.8145(6) 1.2931(5) 1.0615(5) 0.0105(7) Uani 1 1 d . . . O3 O 0.9481(5) 1.3780(4) 1.2175(4) 0.0176(6) Uani 1 1 d . . . O4 O 0.8167(5) 1.3244(4) 0.9369(4) 0.0209(6) 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 Tb1 0.01030(10) 0.00741(10) 0.00826(10) 0.00233(7) 0.00366(7) 0.00013(6) O1 0.0207(13) 0.0109(13) 0.0137(13) 0.0034(10) 0.0056(11) 0.0062(10) O5 0.0129(12) 0.0135(14) 0.0334(17) 0.0033(12) 0.0090(12) 0.0008(11) O2W 0.0177(14) 0.0360(18) 0.0137(14) 0.0085(13) 0.0063(12) 0.0116(13) O6 0.0142(12) 0.0092(13) 0.0293(16) -0.0007(11) 0.0105(12) 0.0014(10) C1 0.0113(15) 0.0084(16) 0.0079(15) 0.0031(13) 0.0033(13) 0.0014(12) O1W 0.0246(15) 0.039(2) 0.0227(16) 0.0189(15) 0.0145(13) 0.0177(14) C4 0.0073(14) 0.0099(16) 0.0121(17) 0.0004(13) 0.0042(13) 0.0007(12) C2 0.0124(15) 0.0106(16) 0.0084(16) 0.0061(13) 0.0036(13) -0.0001(13) C3 0.0143(15) 0.0107(17) 0.0081(16) 0.0061(13) 0.0066(13) 0.0007(13) C6 0.0129(17) 0.0090(17) 0.0168(18) 0.0029(14) 0.0057(14) 0.0019(13) O2 0.0274(15) 0.0224(15) 0.0107(13) 0.0041(11) 0.0051(12) 0.0115(12) C5 0.0115(15) 0.0106(16) 0.0121(17) 0.0048(14) 0.0071(13) 0.0018(13) O3 0.0200(13) 0.0144(14) 0.0135(13) 0.0038(11) 0.0031(11) -0.0063(11) O4 0.0329(16) 0.0191(15) 0.0150(14) 0.0091(12) 0.0121(12) -0.0019(12) _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 2.328(3) 1_545 ? Tb1 O2 2.329(3) 2_666 ? Tb1 O1W 2.361(3) . ? Tb1 O5 2.365(3) . ? Tb1 O2W 2.408(3) . ? Tb1 O3 2.409(3) 2_777 ? Tb1 O6 2.421(3) . ? Tb1 O1 2.433(3) . ? O1 C4 1.261(5) . ? O5 C6 1.235(5) . ? O6 C6 1.259(5) 2_656 ? C1 C3 1.392(5) . ? C1 C2 1.398(5) 2_677 ? C1 C4 1.519(5) . ? C4 O2 1.251(5) . ? C2 C3 1.390(5) . ? C2 C1 1.398(5) 2_677 ? C2 C5 1.506(5) . ? C6 O6 1.259(5) 2_656 ? C6 C6 1.544(7) 2_656 ? O2 Tb1 2.329(3) 2_666 ? C5 O4 1.235(4) . ? C5 O3 1.266(5) . ? O3 Tb1 2.409(3) 2_777 ? O4 Tb1 2.328(3) 1_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 Tb1 O2 144.58(11) 1_545 2_666 ? O4 Tb1 O1W 141.42(11) 1_545 . ? O2 Tb1 O1W 70.97(11) 2_666 . ? O4 Tb1 O5 87.78(12) 1_545 . ? O2 Tb1 O5 89.62(12) 2_666 . ? O1W Tb1 O5 75.46(12) . . ? O4 Tb1 O2W 71.38(11) 1_545 . ? O2 Tb1 O2W 141.30(11) 2_666 . ? O1W Tb1 O2W 70.82(11) . . ? O5 Tb1 O2W 75.19(11) . . ? O4 Tb1 O3 105.53(10) 1_545 2_777 ? O2 Tb1 O3 97.72(11) 2_666 2_777 ? O1W Tb1 O3 72.64(12) . 2_777 ? O5 Tb1 O3 142.70(10) . 2_777 ? O2W Tb1 O3 76.47(11) . 2_777 ? O4 Tb1 O6 74.84(11) 1_545 . ? O2 Tb1 O6 71.60(12) 2_666 . ? O1W Tb1 O6 126.44(12) . . ? O5 Tb1 O6 67.41(10) . . ? O2W Tb1 O6 129.80(11) . . ? O3 Tb1 O6 149.35(10) 2_777 . ? O4 Tb1 O1 76.34(10) 1_545 . ? O2 Tb1 O1 85.07(10) 2_666 . ? O1W Tb1 O1 135.29(11) . . ? O5 Tb1 O1 143.26(10) . . ? O2W Tb1 O1 127.75(11) . . ? O3 Tb1 O1 74.01(10) 2_777 . ? O6 Tb1 O1 76.45(10) . . ? C4 O1 Tb1 130.7(2) . . ? C6 O5 Tb1 119.5(2) . . ? C6 O6 Tb1 117.8(2) 2_656 . ? C3 C1 C2 119.2(3) . 2_677 ? C3 C1 C4 117.6(3) . . ? C2 C1 C4 123.1(3) 2_677 . ? O2 C4 O1 124.9(3) . . ? O2 C4 C1 117.8(3) . . ? O1 C4 C1 117.1(3) . . ? C3 C2 C1 119.1(3) . 2_677 ? C3 C2 C5 119.2(3) . . ? C1 C2 C5 121.7(3) 2_677 . ? C2 C3 C1 121.7(3) . . ? O5 C6 O6 127.0(4) . 2_656 ? O5 C6 C6 117.4(4) . 2_656 ? O6 C6 C6 115.5(4) 2_656 2_656 ? C4 O2 Tb1 161.7(3) . 2_666 ? O4 C5 O3 124.1(3) . . ? O4 C5 C2 119.2(3) . . ? O3 C5 C2 116.7(3) . . ? C5 O3 Tb1 124.1(2) . 2_777 ? C5 O4 Tb1 174.1(3) . 1_565 ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.706 _refine_diff_density_min -0.762 _refine_diff_density_rms 0.153 # Attachment '- 6.cif' data_xc _database_code_depnum_ccdc_archive 'CCDC 773492' #TrackingRef '- 6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H18 Eu2 O17' _chemical_formula_weight 774.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 18.886(4) _cell_length_b 7.8133(16) _cell_length_c 14.793(3) _cell_angle_alpha 90.00 _cell_angle_beta 113.604(2) _cell_angle_gamma 90.00 _cell_volume 2000.3(7) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3364 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 28.72 _exptl_crystal_description prismatic _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.571 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1480 _exptl_absorpt_coefficient_mu 6.306 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3402 _exptl_absorpt_correction_T_max 0.5798 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 'Bruker SMART APEX' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 5484 _diffrn_reflns_av_R_equivalents 0.0219 _diffrn_reflns_av_sigmaI/netI 0.0271 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 26.75 _reflns_number_total 2109 _reflns_number_gt 1950 _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^)+(0.0200P)^2^+3.1200P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2109 _refine_ls_number_parameters 156 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0224 _refine_ls_R_factor_gt 0.0198 _refine_ls_wR_factor_ref 0.0456 _refine_ls_wR_factor_gt 0.0444 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _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 0.253987(8) 0.36653(2) 0.383820(10) 0.01290(6) Uani 1 1 d . . . O1 O 0.11486(13) 0.4501(4) 0.35243(17) 0.0267(6) Uani 1 1 d . . . O2 O 0.19188(13) 0.3799(3) 0.50359(16) 0.0189(5) Uani 1 1 d . . . O1W O 0.34900(13) 0.5430(3) 0.35081(17) 0.0233(6) Uani 1 1 d . . . H1A H 0.3493 0.5325 0.2958 0.035 Uiso 1 1 d R . . H1B H 0.3907 0.4988 0.3843 0.035 Uiso 1 1 d R . . O2W O 0.23745(16) 0.6880(4) 0.4017(2) 0.0337(7) Uani 1 1 d . . . H2A H 0.2301 0.7262 0.4488 0.051 Uiso 0.50 1 d PR A 1 H2B H 0.2165 0.7472 0.3523 0.051 Uiso 0.50 1 d PR A 1 H2C H 0.2716 0.7189 0.3843 0.051 Uiso 0.50 1 d PR A 2 H2D H 0.2014 0.6656 0.3493 0.051 Uiso 0.50 1 d PR A 2 O3W O 0.5000 0.5000 0.5000 0.127(3) Uani 1 2 d S . . O3 O 0.17747(13) 0.3090(3) 0.68295(17) 0.0206(5) Uani 1 1 d . . . O4 O 0.18483(13) 0.5909(3) 0.70782(16) 0.0208(5) Uani 1 1 d . . . O5 O 0.17058(13) 0.1145(3) 0.33521(17) 0.0217(5) Uani 1 1 d . . . O6 O 0.14712(14) 0.0360(4) 0.46572(17) 0.0267(6) Uani 1 1 d . . . C1 C 0.06186(18) 0.4637(5) 0.4741(2) 0.0154(7) Uani 1 1 d . . . C2 C 0.07482(18) 0.4822(4) 0.5739(2) 0.0143(6) Uani 1 1 d . . . C3 C 0.01269(18) 0.5190(5) 0.5981(2) 0.0182(7) Uani 1 1 d . . . H3 H 0.0210 0.5324 0.6641 0.022 Uiso 1 1 calc R . . C4 C 0.12574(18) 0.4291(5) 0.4402(2) 0.0163(7) Uani 1 1 d . . . C5 C 0.15264(17) 0.4597(5) 0.6597(2) 0.0146(7) Uani 1 1 d . . . C6 C 0.13427(18) 0.0292(5) 0.3755(2) 0.0180(7) Uani 1 1 d . . . C7 C 0.06959(19) -0.0860(5) 0.3103(2) 0.0209(7) Uani 1 1 d . . . H7A H 0.0556 -0.1660 0.3505 0.025 Uiso 1 1 calc R . . H7B H 0.0863 -0.1510 0.2665 0.025 Uiso 1 1 calc R . . C8 C 0.0000 0.0250(7) 0.2500 0.0211(11) Uani 1 2 d S . . H8A H -0.0130 0.0984 0.2943 0.025 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 Eu1 0.01152(9) 0.01742(11) 0.00959(9) 0.00041(6) 0.00405(6) 0.00121(6) O1 0.0163(12) 0.0482(19) 0.0151(12) 0.0035(11) 0.0058(10) 0.0106(12) O2 0.0129(11) 0.0285(15) 0.0143(11) 0.0025(10) 0.0046(9) 0.0042(10) O1W 0.0207(12) 0.0325(16) 0.0172(12) 0.0026(11) 0.0081(10) -0.0007(11) O2W 0.0419(16) 0.0299(17) 0.0331(15) -0.0011(13) 0.0190(13) 0.0057(13) O3W 0.032(3) 0.243(11) 0.098(5) 0.039(6) 0.019(3) -0.005(5) O3 0.0199(12) 0.0240(15) 0.0183(12) 0.0041(10) 0.0080(10) 0.0080(11) O4 0.0166(12) 0.0271(15) 0.0155(11) -0.0054(10) 0.0029(9) -0.0023(11) O5 0.0186(12) 0.0302(16) 0.0160(12) -0.0027(10) 0.0067(10) -0.0053(11) O6 0.0248(13) 0.0397(17) 0.0139(11) -0.0019(11) 0.0060(10) -0.0078(12) C1 0.0125(15) 0.0178(18) 0.0156(15) -0.0004(13) 0.0053(13) 0.0004(13) C2 0.0117(15) 0.0139(17) 0.0163(15) -0.0016(13) 0.0045(12) 0.0021(13) C3 0.0171(16) 0.024(2) 0.0124(15) -0.0022(14) 0.0050(13) 0.0020(14) C4 0.0137(15) 0.0186(18) 0.0146(15) 0.0001(13) 0.0037(13) 0.0009(13) C5 0.0111(15) 0.024(2) 0.0110(14) 0.0005(13) 0.0069(12) 0.0039(13) C6 0.0128(15) 0.022(2) 0.0175(16) 0.0006(14) 0.0042(13) 0.0042(14) C7 0.0179(17) 0.0208(19) 0.0183(17) -0.0011(14) 0.0013(14) -0.0011(15) C8 0.016(2) 0.024(3) 0.020(2) 0.000 0.0041(19) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu1 O3 2.357(2) 7_556 ? Eu1 O6 2.386(2) 7_556 ? Eu1 O4 2.423(2) 6_565 ? Eu1 O5 2.443(2) . ? Eu1 O1W 2.462(2) . ? Eu1 O2 2.482(2) 7_556 ? Eu1 O2 2.488(2) . ? Eu1 O2W 2.558(3) . ? Eu1 O1 2.563(2) . ? Eu1 C4 2.902(3) . ? Eu1 Eu1 3.9456(7) 7_556 ? Eu1 H1B 2.7781 . ? Eu1 H2C 2.7731 . ? Eu1 H2D 2.5106 . ? O1 C4 1.242(4) . ? O2 C4 1.284(4) . ? O2 Eu1 2.482(2) 7_556 ? O1W H1A 0.8200 . ? O1W H1B 0.8201 . ? O2W H2A 0.8199 . ? O2W H2B 0.8200 . ? O2W H2C 0.8200 . ? O2W H2D 0.8200 . ? O3 C5 1.263(4) . ? O3 Eu1 2.357(2) 7_556 ? O4 C5 1.257(4) . ? O4 Eu1 2.423(2) 6_566 ? O5 C6 1.264(4) . ? O6 C6 1.258(4) . ? O6 Eu1 2.386(2) 7_556 ? C1 C3 1.392(4) 5_566 ? C1 C2 1.404(4) . ? C1 C4 1.505(4) . ? C2 C3 1.387(4) . ? C2 C5 1.519(4) . ? C3 C1 1.392(4) 5_566 ? C3 H3 0.9300 . ? C6 C7 1.513(5) . ? C7 C8 1.529(4) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C7 1.529(4) 2 ? C8 H8A 0.9730 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Eu1 O6 102.74(9) 7_556 7_556 ? O3 Eu1 O4 77.29(8) 7_556 6_565 ? O6 Eu1 O4 147.37(9) 7_556 6_565 ? O3 Eu1 O5 78.77(9) 7_556 . ? O6 Eu1 O5 134.70(8) 7_556 . ? O4 Eu1 O5 77.76(8) 6_565 . ? O3 Eu1 O1W 71.13(9) 7_556 . ? O6 Eu1 O1W 69.26(8) 7_556 . ? O4 Eu1 O1W 80.33(8) 6_565 . ? O5 Eu1 O1W 145.92(8) . . ? O3 Eu1 O2 71.46(8) 7_556 7_556 ? O6 Eu1 O2 70.34(9) 7_556 7_556 ? O4 Eu1 O2 136.67(8) 6_565 7_556 ? O5 Eu1 O2 67.43(8) . 7_556 ? O1W Eu1 O2 115.49(8) . 7_556 ? O3 Eu1 O2 144.82(8) 7_556 . ? O6 Eu1 O2 74.84(8) 7_556 . ? O4 Eu1 O2 123.66(8) 6_565 . ? O5 Eu1 O2 79.11(8) . . ? O1W Eu1 O2 134.96(8) . . ? O2 Eu1 O2 74.91(9) 7_556 . ? O3 Eu1 O2W 136.47(9) 7_556 . ? O6 Eu1 O2W 70.88(9) 7_556 . ? O4 Eu1 O2W 86.59(9) 6_565 . ? O5 Eu1 O2W 136.96(9) . . ? O1W Eu1 O2W 66.38(9) . . ? O2 Eu1 O2W 136.62(8) 7_556 . ? O2 Eu1 O2W 76.90(8) . . ? O3 Eu1 O1 140.13(8) 7_556 . ? O6 Eu1 O1 116.77(8) 7_556 . ? O4 Eu1 O1 72.42(7) 6_565 . ? O5 Eu1 O1 70.04(9) . . ? O1W Eu1 O1 126.67(9) . . ? O2 Eu1 O1 115.85(8) 7_556 . ? O2 Eu1 O1 51.45(7) . . ? O2W Eu1 O1 67.03(9) . . ? O3 Eu1 C4 151.65(9) 7_556 . ? O6 Eu1 C4 96.30(9) 7_556 . ? O4 Eu1 C4 97.63(8) 6_565 . ? O5 Eu1 C4 72.92(9) . . ? O1W Eu1 C4 136.16(9) . . ? O2 Eu1 C4 96.01(9) 7_556 . ? O2 Eu1 C4 26.15(8) . . ? O2W Eu1 C4 69.78(10) . . ? O1 Eu1 C4 25.30(8) . . ? O3 Eu1 Eu1 108.38(6) 7_556 7_556 ? O6 Eu1 Eu1 67.87(6) 7_556 7_556 ? O4 Eu1 Eu1 143.83(6) 6_565 7_556 ? O5 Eu1 Eu1 68.86(5) . 7_556 ? O1W Eu1 Eu1 135.75(5) . 7_556 ? O2 Eu1 Eu1 37.51(5) 7_556 7_556 ? O2 Eu1 Eu1 37.41(5) . 7_556 ? O2W Eu1 Eu1 108.32(6) . 7_556 ? O1 Eu1 Eu1 83.19(6) . 7_556 ? C4 Eu1 Eu1 59.99(7) . 7_556 ? O3 Eu1 H1B 63.4 7_556 . ? O6 Eu1 H1B 60.0 7_556 . ? O4 Eu1 H1B 93.0 6_565 . ? O5 Eu1 H1B 142.1 . . ? O1W Eu1 H1B 16.6 . . ? O2 Eu1 H1B 98.9 7_556 . ? O2 Eu1 H1B 133.2 . . ? O2W Eu1 H1B 77.7 . . ? O1 Eu1 H1B 142.2 . . ? C4 Eu1 H1B 144.9 . . ? Eu1 Eu1 H1B 121.9 7_556 . ? O3 Eu1 H2C 119.6 7_556 . ? O6 Eu1 H2C 68.4 7_556 . ? O4 Eu1 H2C 83.0 6_565 . ? O5 Eu1 H2C 149.7 . . ? O1W Eu1 H2C 49.3 . . ? O2 Eu1 H2C 138.7 7_556 . ? O2 Eu1 H2C 92.7 . . ? O2W Eu1 H2C 17.1 . . ? O1 Eu1 H2C 82.0 . . ? C4 Eu1 H2C 86.8 . . ? Eu1 Eu1 H2C 120.2 7_556 . ? H1B Eu1 H2C 61.3 . . ? O3 Eu1 H2D 134.0 7_556 . ? O6 Eu1 H2D 89.5 7_556 . ? O4 Eu1 H2D 69.8 6_565 . ? O5 Eu1 H2D 122.3 . . ? O1W Eu1 H2D 72.5 . . ? O2 Eu1 H2D 151.8 7_556 . ? O2 Eu1 H2D 81.1 . . ? O2W Eu1 H2D 18.6 . . ? O1 Eu1 H2D 55.4 . . ? C4 Eu1 H2D 66.1 . . ? Eu1 Eu1 H2D 117.2 7_556 . ? H1B Eu1 H2D 86.9 . . ? H2C Eu1 H2D 27.5 . . ? C4 O1 Eu1 92.78(19) . . ? C4 O2 Eu1 137.8(2) . 7_556 ? C4 O2 Eu1 95.20(18) . . ? Eu1 O2 Eu1 105.09(9) 7_556 . ? Eu1 O1W H1A 115.8 . . ? Eu1 O1W H1B 104.1 . . ? H1A O1W H1B 99.9 . . ? Eu1 O2W H2A 121.0 . . ? Eu1 O2W H2B 119.8 . . ? H2A O2W H2B 111.5 . . ? Eu1 O2W H2C 96.5 . . ? H2A O2W H2C 125.6 . . ? H2B O2W H2C 73.4 . . ? Eu1 O2W H2D 77.4 . . ? H2A O2W H2D 121.5 . . ? H2B O2W H2D 49.9 . . ? H2C O2W H2D 103.0 . . ? C5 O3 Eu1 129.38(19) . 7_556 ? C5 O4 Eu1 130.6(2) . 6_566 ? C6 O5 Eu1 134.0(2) . . ? C6 O6 Eu1 138.5(2) . 7_556 ? C3 C1 C2 119.6(3) 5_566 . ? C3 C1 C4 117.5(3) 5_566 . ? C2 C1 C4 122.9(3) . . ? C3 C2 C1 118.9(3) . . ? C3 C2 C5 116.4(3) . . ? C1 C2 C5 124.7(3) . . ? C2 C3 C1 121.5(3) . 5_566 ? C2 C3 H3 119.2 . . ? C1 C3 H3 119.2 5_566 . ? O1 C4 O2 120.6(3) . . ? O1 C4 C1 120.4(3) . . ? O2 C4 C1 119.1(3) . . ? O1 C4 Eu1 61.92(17) . . ? O2 C4 Eu1 58.65(16) . . ? C1 C4 Eu1 177.4(2) . . ? O4 C5 O3 124.2(3) . . ? O4 C5 C2 117.7(3) . . ? O3 C5 C2 117.7(3) . . ? O6 C6 O5 124.6(3) . . ? O6 C6 C7 117.7(3) . . ? O5 C6 C7 117.7(3) . . ? C6 C7 C8 108.7(3) . . ? C6 C7 H7A 110.0 . . ? C8 C7 H7A 110.0 . . ? C6 C7 H7B 110.0 . . ? C8 C7 H7B 110.0 . . ? H7A C7 H7B 108.3 . . ? C7 C8 C7 110.8(4) . 2 ? C7 C8 H8A 109.3 . . ? C7 C8 H8A 109.8 2 . ? 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 O3 Eu1 O1 C4 132.8(2) 7_556 . . . ? O6 Eu1 O1 C4 -38.8(2) 7_556 . . . ? O4 Eu1 O1 C4 175.1(2) 6_565 . . . ? O5 Eu1 O1 C4 92.1(2) . . . . ? O1W Eu1 O1 C4 -122.0(2) . . . . ? O2 Eu1 O1 C4 41.2(2) 7_556 . . . ? O2 Eu1 O1 C4 0.3(2) . . . . ? O2W Eu1 O1 C4 -91.0(2) . . . . ? Eu1 Eu1 O1 C4 22.2(2) 7_556 . . . ? O3 Eu1 O2 C4 -125.2(2) 7_556 . . . ? O6 Eu1 O2 C4 144.1(2) 7_556 . . . ? O4 Eu1 O2 C4 -6.1(2) 6_565 . . . ? O5 Eu1 O2 C4 -73.3(2) . . . . ? O1W Eu1 O2 C4 106.2(2) . . . . ? O2 Eu1 O2 C4 -142.7(2) 7_556 . . . ? O2W Eu1 O2 C4 70.7(2) . . . . ? O1 Eu1 O2 C4 -0.3(2) . . . . ? Eu1 Eu1 O2 C4 -142.7(2) 7_556 . . . ? O3 Eu1 O2 Eu1 17.44(17) 7_556 . . 7_556 ? O6 Eu1 O2 Eu1 -73.26(10) 7_556 . . 7_556 ? O4 Eu1 O2 Eu1 136.52(9) 6_565 . . 7_556 ? O5 Eu1 O2 Eu1 69.33(9) . . . 7_556 ? O1W Eu1 O2 Eu1 -111.14(11) . . . 7_556 ? O2 Eu1 O2 Eu1 0.0 7_556 . . 7_556 ? O2W Eu1 O2 Eu1 -146.68(10) . . . 7_556 ? O1 Eu1 O2 Eu1 142.40(14) . . . 7_556 ? C4 Eu1 O2 Eu1 142.7(2) . . . 7_556 ? O3 Eu1 O5 C6 137.3(3) 7_556 . . . ? O6 Eu1 O5 C6 40.4(3) 7_556 . . . ? O4 Eu1 O5 C6 -143.5(3) 6_565 . . . ? O1W Eu1 O5 C6 165.4(3) . . . . ? O2 Eu1 O5 C6 62.8(3) 7_556 . . . ? O2 Eu1 O5 C6 -15.2(3) . . . . ? O2W Eu1 O5 C6 -72.3(3) . . . . ? O1 Eu1 O5 C6 -68.0(3) . . . . ? C4 Eu1 O5 C6 -41.4(3) . . . . ? Eu1 Eu1 O5 C6 22.3(3) 7_556 . . . ? C3 C1 C2 C3 -0.6(6) 5_566 . . . ? C4 C1 C2 C3 178.1(3) . . . . ? C3 C1 C2 C5 177.5(3) 5_566 . . . ? C4 C1 C2 C5 -3.8(5) . . . . ? C1 C2 C3 C1 0.6(6) . . . 5_566 ? C5 C2 C3 C1 -177.7(3) . . . 5_566 ? Eu1 O1 C4 O2 -0.5(4) . . . . ? Eu1 O1 C4 C1 178.5(3) . . . . ? Eu1 O2 C4 O1 -118.8(3) 7_556 . . . ? Eu1 O2 C4 O1 0.5(4) . . . . ? Eu1 O2 C4 C1 62.2(5) 7_556 . . . ? Eu1 O2 C4 C1 -178.5(3) . . . . ? Eu1 O2 C4 Eu1 -119.3(3) 7_556 . . . ? C3 C1 C4 O1 14.3(5) 5_566 . . . ? C2 C1 C4 O1 -164.4(3) . . . . ? C3 C1 C4 O2 -166.7(3) 5_566 . . . ? C2 C1 C4 O2 14.6(5) . . . . ? C3 C1 C4 Eu1 164(5) 5_566 . . . ? C2 C1 C4 Eu1 -14(6) . . . . ? O3 Eu1 C4 O1 -82.0(3) 7_556 . . . ? O6 Eu1 C4 O1 145.8(2) 7_556 . . . ? O4 Eu1 C4 O1 -4.7(2) 6_565 . . . ? O5 Eu1 C4 O1 -79.3(2) . . . . ? O1W Eu1 C4 O1 79.3(2) . . . . ? O2 Eu1 C4 O1 -143.4(2) 7_556 . . . ? O2 Eu1 C4 O1 -179.5(4) . . . . ? O2W Eu1 C4 O1 78.8(2) . . . . ? Eu1 Eu1 C4 O1 -154.3(2) 7_556 . . . ? O3 Eu1 C4 O2 97.5(2) 7_556 . . . ? O6 Eu1 C4 O2 -34.7(2) 7_556 . . . ? O4 Eu1 C4 O2 174.9(2) 6_565 . . . ? O5 Eu1 C4 O2 100.2(2) . . . . ? O1W Eu1 C4 O2 -101.2(2) . . . . ? O2 Eu1 C4 O2 36.1(2) 7_556 . . . ? O2W Eu1 C4 O2 -101.7(2) . . . . ? O1 Eu1 C4 O2 179.5(4) . . . . ? Eu1 Eu1 C4 O2 25.19(17) 7_556 . . . ? O3 Eu1 C4 C1 127(5) 7_556 . . . ? O6 Eu1 C4 C1 -5(5) 7_556 . . . ? O4 Eu1 C4 C1 -155(5) 6_565 . . . ? O5 Eu1 C4 C1 130(5) . . . . ? O1W Eu1 C4 C1 -72(5) . . . . ? O2 Eu1 C4 C1 66(5) 7_556 . . . ? O2 Eu1 C4 C1 30(5) . . . . ? O2W Eu1 C4 C1 -72(5) . . . . ? O1 Eu1 C4 C1 -151(6) . . . . ? Eu1 Eu1 C4 C1 55(5) 7_556 . . . ? Eu1 O4 C5 O3 -35.2(4) 6_566 . . . ? Eu1 O4 C5 C2 138.5(2) 6_566 . . . ? Eu1 O3 C5 O4 -102.0(3) 7_556 . . . ? Eu1 O3 C5 C2 84.3(3) 7_556 . . . ? C3 C2 C5 O4 -71.3(4) . . . . ? C1 C2 C5 O4 110.6(4) . . . . ? C3 C2 C5 O3 102.8(4) . . . . ? C1 C2 C5 O3 -75.3(4) . . . . ? Eu1 O6 C6 O5 -16.3(6) 7_556 . . . ? Eu1 O6 C6 C7 165.2(3) 7_556 . . . ? Eu1 O5 C6 O6 -16.8(5) . . . . ? Eu1 O5 C6 C7 161.7(2) . . . . ? O6 C6 C7 C8 103.9(3) . . . . ? O5 C6 C7 C8 -74.7(4) . . . . ? C6 C7 C8 C7 -174.8(3) . . . 2 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.75 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.625 _refine_diff_density_min -0.728 _refine_diff_density_rms 0.119 # Attachment '- 11.cif' data_1f _database_code_depnum_ccdc_archive 'CCDC 773493' #TrackingRef '- 11.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H14 Dy2 O14' _chemical_formula_weight 755.27 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.7659(7) _cell_length_b 7.2009(6) _cell_length_c 17.3199(15) _cell_angle_alpha 90.00 _cell_angle_beta 91.4520(10) _cell_angle_gamma 90.00 _cell_volume 968.24(15) _cell_formula_units_Z 2 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 2633 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 28.90 _exptl_crystal_description Spicule _exptl_crystal_colour yellow _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.591 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 708 _exptl_absorpt_coefficient_mu 7.735 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4149 _exptl_absorpt_correction_T_max 0.6498 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 'Bruker SMART APEX' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 4641 _diffrn_reflns_av_R_equivalents 0.0229 _diffrn_reflns_av_sigmaI/netI 0.0273 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 24.99 _reflns_number_total 1710 _reflns_number_gt 1526 _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^)+(0.0239P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1710 _refine_ls_number_parameters 153 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0225 _refine_ls_R_factor_gt 0.0190 _refine_ls_wR_factor_ref 0.0491 _refine_ls_wR_factor_gt 0.0472 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.084 _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 H1WB H 0.442(8) 0.734(9) 0.205(4) 0.07(3) Uiso 1 1 d . . . H1WA H 0.318(9) 0.833(11) 0.202(4) 0.11(3) Uiso 1 1 d . . . O6 O 0.9929(4) 0.6777(4) 0.34066(15) 0.0243(7) Uani 1 1 d . . . Dy1 Dy 0.65051(2) 1.01178(2) 0.255224(10) 0.01206(9) Uani 1 1 d . . . C1 C 0.5492(5) 0.6144(5) 0.4388(2) 0.0147(8) Uani 1 1 d . . . C2 C 0.5302(5) 1.4227(5) 0.4270(2) 0.0150(8) Uani 1 1 d . . . C3 C 0.5196(5) 0.6880(6) 0.5116(2) 0.0167(9) Uani 1 1 d . . . H3 H 0.5335 0.8149 0.5194 0.020 Uiso 1 1 calc R . . C4 C 0.5937(5) 0.7457(5) 0.3757(2) 0.0142(8) Uani 1 1 d . . . C5 C 0.5575(5) 1.3189(5) 0.3530(2) 0.0156(9) Uani 1 1 d . . . C6 C 1.0086(5) 0.8477(5) 0.3545(2) 0.0159(8) Uani 1 1 d . . . C7 C 1.1381(5) 0.9085(6) 0.4150(2) 0.0258(10) Uani 1 1 d . . . H7A H 1.2340 0.9674 0.3899 0.031 Uiso 1 1 calc R . . H7B H 1.1821 0.7997 0.4420 0.031 Uiso 1 1 calc R . . C8 C 1.0647(7) 1.0441(7) 0.4743(3) 0.0351(12) Uani 1 1 d . . . H8A H 1.1587 1.0936 0.5060 0.042 Uiso 1 1 calc R . . H8B H 1.0105 1.1472 0.4470 0.042 Uiso 1 1 calc R . . O1 O 0.6417(3) 0.6824(3) 0.31069(14) 0.0161(6) Uani 1 1 d . . . O1W O 0.4150(5) 0.8239(6) 0.2118(2) 0.0367(9) Uani 1 1 d . . . O2 O 0.5778(4) 0.9155(4) 0.38510(14) 0.0213(6) Uani 1 1 d . . . O3 O 0.4354(3) 1.2349(4) 0.32171(14) 0.0205(6) Uani 1 1 d . . . O4 O 0.7124(3) 1.3007(3) 0.32808(14) 0.0141(6) Uani 1 1 d . . . O5 O 0.9220(4) 0.9728(3) 0.31855(17) 0.0204(7) 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 O6 0.0355(18) 0.0178(15) 0.0193(15) -0.0038(12) -0.0059(13) 0.0009(13) Dy1 0.01742(14) 0.00897(12) 0.00996(13) 0.00059(7) 0.00345(8) 0.00005(7) C1 0.020(2) 0.013(2) 0.0112(19) 0.0020(16) 0.0020(16) 0.0006(16) C2 0.018(2) 0.0124(19) 0.0141(19) -0.0023(16) 0.0015(16) 0.0019(16) C3 0.023(2) 0.012(2) 0.015(2) 0.0000(15) 0.0045(18) 0.0008(15) C4 0.013(2) 0.016(2) 0.014(2) 0.0016(16) -0.0005(16) 0.0016(16) C5 0.027(2) 0.0103(19) 0.0097(19) 0.0066(15) 0.0042(17) 0.0039(16) C6 0.016(2) 0.021(2) 0.0106(19) -0.0021(16) 0.0040(16) 0.0007(17) C7 0.025(2) 0.029(2) 0.023(2) -0.005(2) -0.0062(19) 0.002(2) C8 0.048(3) 0.037(3) 0.019(2) -0.004(2) -0.005(2) -0.010(2) O1 0.0232(16) 0.0168(14) 0.0087(13) 0.0017(11) 0.0072(11) 0.0027(12) O1W 0.026(2) 0.025(2) 0.059(2) 0.0051(18) -0.0123(19) -0.0028(16) O2 0.0365(18) 0.0105(14) 0.0175(15) 0.0021(12) 0.0103(13) 0.0014(12) O3 0.0218(16) 0.0218(15) 0.0178(15) -0.0070(12) 0.0012(13) -0.0034(12) O4 0.0174(15) 0.0125(13) 0.0126(14) 0.0024(11) 0.0051(12) 0.0005(11) O5 0.0212(17) 0.0183(15) 0.0216(16) 0.0013(12) -0.0022(13) 0.0006(12) _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 O6 C6 1.253(4) . ? O6 Dy1 2.309(3) 2_645 ? Dy1 O6 2.309(3) 2_655 ? Dy1 O1 2.347(2) 2_655 ? Dy1 O4 2.367(2) 2_645 ? Dy1 O5 2.368(3) . ? Dy1 O1W 2.381(4) . ? Dy1 O2 2.434(2) . ? Dy1 O4 2.474(2) . ? Dy1 O1 2.561(2) . ? Dy1 O3 2.607(3) . ? Dy1 C4 2.875(4) . ? Dy1 C5 2.889(4) . ? Dy1 Dy1 3.9240(3) 2_645 ? C1 C3 1.392(5) . ? C1 C2 1.403(6) 1_545 ? C1 C4 1.491(5) . ? C2 C3 1.391(5) 3_676 ? C2 C1 1.403(6) 1_565 ? C2 C5 1.503(5) . ? C3 C2 1.391(5) 3_676 ? C4 O2 1.240(4) . ? C4 O1 1.279(4) . ? C5 O3 1.238(5) . ? C5 O4 1.295(5) . ? C6 O5 1.277(5) . ? C6 C7 1.499(5) . ? C7 C8 1.537(6) . ? C8 C8 1.501(10) 3_776 ? O1 Dy1 2.347(2) 2_645 ? O4 Dy1 2.367(2) 2_655 ? 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 C6 O6 Dy1 133.3(3) . 2_645 ? O6 Dy1 O1 72.80(10) 2_655 2_655 ? O6 Dy1 O4 96.31(9) 2_655 2_645 ? O1 Dy1 O4 73.40(9) 2_655 2_645 ? O6 Dy1 O5 143.29(10) 2_655 . ? O1 Dy1 O5 70.87(9) 2_655 . ? O4 Dy1 O5 78.32(9) 2_645 . ? O6 Dy1 O1W 73.42(12) 2_655 . ? O1 Dy1 O1W 132.53(12) 2_655 . ? O4 Dy1 O1W 78.25(13) 2_645 . ? O5 Dy1 O1W 138.27(12) . . ? O6 Dy1 O2 133.88(10) 2_655 . ? O1 Dy1 O2 140.99(9) 2_655 . ? O4 Dy1 O2 119.93(8) 2_645 . ? O5 Dy1 O2 76.29(10) . . ? O1W Dy1 O2 86.29(12) . . ? O6 Dy1 O4 90.89(9) 2_655 . ? O1 Dy1 O4 71.38(8) 2_655 . ? O4 Dy1 O4 140.02(4) 2_645 . ? O5 Dy1 O4 72.79(9) . . ? O1W Dy1 O4 140.95(13) . . ? O2 Dy1 O4 79.34(8) . . ? O6 Dy1 O1 137.07(9) 2_655 . ? O1 Dy1 O1 133.83(6) 2_655 . ? O4 Dy1 O1 69.55(8) 2_645 . ? O5 Dy1 O1 75.44(9) . . ? O1W Dy1 O1 64.17(11) . . ? O2 Dy1 O1 51.71(8) . . ? O4 Dy1 O1 126.47(8) . . ? O6 Dy1 O3 72.30(9) 2_655 . ? O1 Dy1 O3 110.39(9) 2_655 . ? O4 Dy1 O3 165.49(8) 2_645 . ? O5 Dy1 O3 116.19(9) . . ? O1W Dy1 O3 89.65(12) . . ? O2 Dy1 O3 66.49(8) . . ? O4 Dy1 O3 51.31(8) . . ? O1 Dy1 O3 112.44(8) . . ? O6 Dy1 C4 141.88(11) 2_655 . ? O1 Dy1 C4 145.26(10) 2_655 . ? O4 Dy1 C4 95.41(9) 2_645 . ? O5 Dy1 C4 74.70(10) . . ? O1W Dy1 C4 73.71(12) . . ? O2 Dy1 C4 25.30(9) . . ? O4 Dy1 C4 102.81(9) . . ? O1 Dy1 C4 26.42(9) . . ? O3 Dy1 C4 88.76(9) . . ? O6 Dy1 C5 84.40(10) 2_655 . ? O1 Dy1 C5 94.00(9) 2_655 . ? O4 Dy1 C5 166.43(10) 2_645 . ? O5 Dy1 C5 92.98(10) . . ? O1W Dy1 C5 114.74(14) . . ? O2 Dy1 C5 66.97(9) . . ? O4 Dy1 C5 26.54(10) . . ? O1 Dy1 C5 118.67(9) . . ? O3 Dy1 C5 25.38(9) . . ? C4 Dy1 C5 92.25(10) . . ? O6 Dy1 Dy1 128.68(7) 2_655 2_645 ? O1 Dy1 Dy1 100.45(6) 2_655 2_645 ? O4 Dy1 Dy1 36.78(6) 2_645 2_645 ? O5 Dy1 Dy1 64.26(6) . 2_645 ? O1W Dy1 Dy1 76.37(11) . 2_645 ? O2 Dy1 Dy1 83.23(6) . 2_645 ? O4 Dy1 Dy1 136.34(6) . 2_645 ? O1 Dy1 Dy1 35.09(5) . 2_645 ? O3 Dy1 Dy1 147.50(6) . 2_645 ? C4 Dy1 Dy1 59.33(7) . 2_645 ? C5 Dy1 Dy1 146.53(7) . 2_645 ? C3 C1 C2 119.1(3) . 1_545 ? C3 C1 C4 118.0(3) . . ? C2 C1 C4 122.9(3) 1_545 . ? C3 C2 C1 118.9(3) 3_676 1_565 ? C3 C2 C5 114.5(3) 3_676 . ? C1 C2 C5 126.6(3) 1_565 . ? C2 C3 C1 122.0(4) 3_676 . ? O2 C4 O1 119.9(3) . . ? O2 C4 C1 120.2(3) . . ? O1 C4 C1 119.8(3) . . ? O2 C4 Dy1 57.02(18) . . ? O1 C4 Dy1 62.93(18) . . ? C1 C4 Dy1 175.1(3) . . ? O3 C5 O4 120.8(3) . . ? O3 C5 C2 119.5(3) . . ? O4 C5 C2 119.1(3) . . ? O3 C5 Dy1 64.5(2) . . ? O4 C5 Dy1 58.59(18) . . ? C2 C5 Dy1 157.4(2) . . ? O6 C6 O5 123.2(4) . . ? O6 C6 C7 118.6(4) . . ? O5 C6 C7 118.1(4) . . ? C6 C7 C8 113.5(4) . . ? C8 C8 C7 113.1(5) 3_776 . ? C4 O1 Dy1 146.5(2) . 2_645 ? C4 O1 Dy1 90.7(2) . . ? Dy1 O1 Dy1 106.08(9) 2_645 . ? C4 O2 Dy1 97.7(2) . . ? C5 O3 Dy1 90.1(2) . . ? C5 O4 Dy1 125.1(2) . 2_655 ? C5 O4 Dy1 94.9(2) . . ? Dy1 O4 Dy1 108.28(9) 2_655 . ? C6 O5 Dy1 139.6(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.476 _refine_diff_density_min -0.725 _refine_diff_density_rms 0.138