# Electronic Supplementary Material for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Ji-Qing Xu' _publ_contact_author_email XJQ@MAIL.JLU.EDU.CN _publ_section_title ; Two- and Three-Dimensional Networks of Lanthanide with Mixed Dicarboxylate Ligands: Syntheses, Crystal Structures and Photoluminescent Properties ; loop_ _publ_author_name 'Ji-Qing Xu.' 'Tianyou Song.' 'Tie-Gang Wang.' 'Qing-Feng Yang.' 'Yang Yu.' ; Jie-Hui Yu ; 'Xiao Zhang.' # Attachment 'cif.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 715640' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C18 H18 Ce2 O17' _chemical_formula_sum 'C18 H18 Ce2 O17' _chemical_formula_weight 786.56 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' Ce Ce -0.2486 2.6331 '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 20.090(2) _cell_length_b 6.0758(7) _cell_length_c 20.626(2) _cell_angle_alpha 90.00 _cell_angle_beta 111.267(2) _cell_angle_gamma 90.00 _cell_volume 2346.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2907 _cell_measurement_theta_min 2.12 _cell_measurement_theta_max 28.30 _exptl_crystal_description rod _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 2.227 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1512 _exptl_absorpt_coefficient_mu 3.916 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7558 _exptl_absorpt_correction_T_max 0.8998 _exptl_absorpt_process_details SADABS _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 'Siemens Smart CCD' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 9.00cm _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 8119 _diffrn_reflns_av_R_equivalents 0.0582 _diffrn_reflns_av_sigmaI/netI 0.0445 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 28.30 _reflns_number_total 2907 _reflns_number_gt 2711 _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 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0674P)^2^+7.7665P] 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 2907 _refine_ls_number_parameters 188 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0392 _refine_ls_R_factor_gt 0.0360 _refine_ls_wR_factor_ref 0.0976 _refine_ls_wR_factor_gt 0.0959 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.041 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.24612(9) -0.0221(3) 0.60175(9) 0.0149(4) Uani 1 1 d . . . C2 C 0.29639(9) 0.0273(3) 0.67407(9) 0.0157(4) Uani 1 1 d . . . C3 C 0.29584(12) -0.1220(4) 0.72523(10) 0.0245(5) Uani 1 1 d . . . H3 H 0.2665 -0.2454 0.7130 0.029 Uiso 1 1 calc R . . C4 C 0.33895(11) -0.0873(4) 0.79443(10) 0.0242(5) Uani 1 1 d . . . H4 H 0.3389 -0.1887 0.8282 0.029 Uiso 1 1 calc R . . C5 C 0.38178(12) 0.0967(4) 0.81311(11) 0.0276(5) Uani 1 1 d . . . H5 H 0.4099 0.1206 0.8596 0.033 Uiso 1 1 calc R . . C6 C 0.38313(11) 0.2462(4) 0.76280(10) 0.0241(5) Uani 1 1 d . . . H6 H 0.4124 0.3696 0.7758 0.029 Uiso 1 1 calc R . . C7 C 0.34081(10) 0.2136(3) 0.69247(9) 0.0172(4) Uani 1 1 d . . . C8 C 0.34655(10) 0.3714(3) 0.63894(9) 0.0159(4) Uani 1 1 d . . . C9 C 0.50068(9) -0.3880(3) 0.48230(9) 0.0153(4) Uani 1 1 d . . . Ce1 Ce 0.362865(5) -0.330688(16) 0.533921(5) 0.01289(3) Uani 1 1 d . . . H1 H 0.368(2) 0.074(7) 0.471(2) 0.078(12) Uiso 1 1 d . . . H2 H 0.3051(16) 0.066(5) 0.4550(15) 0.040(8) Uiso 1 1 d . . . H7 H 0.4559(13) 0.057(4) 0.5947(13) 0.024(6) Uiso 1 1 d . . . H8 H 0.4693(12) -0.067(4) 0.6549(12) 0.016(5) Uiso 1 1 d . . . H9 H 0.4622(4) 0.7098(17) 0.7342(19) 0.062(11) Uiso 1 1 d D . . O1 O 0.26755(7) -0.1423(2) 0.56235(7) 0.0193(3) Uani 1 1 d . . . O2 O 0.18230(7) 0.0403(2) 0.58196(7) 0.0218(3) Uani 1 1 d . . . O3 O 0.30488(8) 0.3510(2) 0.57615(7) 0.0203(4) Uani 1 1 d . . . O4 O 0.39255(8) 0.5228(3) 0.65694(7) 0.0273(4) Uani 1 1 d . . . O5 O 0.45667(7) -0.2477(3) 0.48428(8) 0.0240(3) Uani 1 1 d . . . O6 O 0.54751(7) -0.3660(2) 0.45461(8) 0.0238(3) Uani 1 1 d . . . O7 O 0.33664(8) 0.0109(3) 0.46355(9) 0.0287(4) Uani 1 1 d . . . O8 O 0.44272(9) -0.0480(3) 0.61296(8) 0.0299(4) Uani 1 1 d . . . O9 O 0.5000 0.7879(4) 0.7500 0.0382(7) Uani 1 2 d SD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0163(7) 0.0147(7) 0.0134(6) 0.0000(6) 0.0050(5) -0.0032(6) C2 0.0152(7) 0.0196(8) 0.0121(6) 0.0007(6) 0.0046(5) 0.0029(6) C3 0.0310(9) 0.0265(9) 0.0161(8) 0.0052(7) 0.0084(7) -0.0037(8) C4 0.0278(8) 0.0330(10) 0.0129(7) 0.0082(7) 0.0086(6) 0.0021(8) C5 0.0280(9) 0.0378(11) 0.0143(8) 0.0041(8) 0.0042(7) -0.0015(9) C6 0.0245(8) 0.0286(10) 0.0154(8) -0.0028(8) 0.0028(6) -0.0083(8) C7 0.0237(7) 0.0168(7) 0.0159(7) 0.0049(6) 0.0128(5) 0.0027(6) C8 0.0180(7) 0.0154(7) 0.0155(7) 0.0026(6) 0.0075(5) 0.0018(6) C9 0.0132(6) 0.0178(8) 0.0168(7) 0.0045(6) 0.0077(5) 0.0016(6) Ce1 0.01112(4) 0.01581(5) 0.01266(5) 0.00035(3) 0.00541(3) 0.00076(3) O1 0.0178(5) 0.0259(6) 0.0163(5) -0.0053(5) 0.0086(4) 0.0006(5) O2 0.0174(5) 0.0263(7) 0.0219(6) -0.0058(5) 0.0073(4) 0.0049(5) O3 0.0204(6) 0.0229(6) 0.0152(6) 0.0035(5) 0.0036(5) -0.0029(5) O4 0.0301(7) 0.0310(7) 0.0162(6) -0.0005(5) 0.0028(5) -0.0131(6) O5 0.0232(5) 0.0220(6) 0.0337(6) 0.0069(6) 0.0185(5) 0.0066(5) O6 0.0207(5) 0.0248(6) 0.0333(6) 0.0106(5) 0.0188(5) 0.0076(5) O7 0.0237(6) 0.0244(7) 0.0391(7) 0.0109(6) 0.0129(5) 0.0056(6) O8 0.0340(7) 0.0302(8) 0.0220(6) -0.0006(6) 0.0060(6) -0.0135(6) O9 0.0352(13) 0.0434(13) 0.0249(11) 0.000 -0.0026(10) 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 C1 O2 1.255(2) . ? C1 O1 1.278(2) . ? C1 C2 1.497(2) . ? C1 Ce1 2.9967(16) 7_546 ? C2 C3 1.395(3) . ? C2 C7 1.406(3) . ? C3 C4 1.391(3) . ? C4 C5 1.378(3) . ? C5 C6 1.387(3) . ? C6 C7 1.404(2) . ? C7 C8 1.498(3) . ? C8 O4 1.260(2) . ? C8 O3 1.268(2) . ? C8 Ce1 2.931(2) 1_565 ? C9 O5 1.240(2) . ? C9 O6 1.272(3) . ? C9 C9 1.549(4) 5_646 ? Ce1 O1 2.4770(16) . ? Ce1 O7 2.4772(16) . ? Ce1 O5 2.5009(16) . ? Ce1 O8 2.5070(15) . ? Ce1 O6 2.5268(15) 5_646 ? Ce1 O4 2.5474(15) 1_545 ? Ce1 O2 2.5660(14) 7_546 ? Ce1 O3 2.5677(15) 1_545 ? Ce1 O1 2.6573(13) 7_546 ? Ce1 C8 2.931(2) 1_545 ? Ce1 C1 2.9967(16) 7_546 ? O1 Ce1 2.6573(13) 7_546 ? O2 Ce1 2.5660(14) 7_546 ? O3 Ce1 2.5677(15) 1_565 ? O4 Ce1 2.5474(15) 1_565 ? O6 Ce1 2.5268(15) 5_646 ? 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 C1 O1 120.40(15) . . ? O2 C1 C2 120.25(17) . . ? O1 C1 C2 119.14(15) . . ? O2 C1 Ce1 58.14(9) . 7_546 ? O1 C1 Ce1 62.37(8) . 7_546 ? C2 C1 Ce1 172.05(13) . 7_546 ? C3 C2 C7 119.86(16) . . ? C3 C2 C1 115.84(16) . . ? C7 C2 C1 124.26(16) . . ? C4 C3 C2 120.3(2) . . ? C5 C4 C3 120.2(2) . . ? C4 C5 C6 120.14(18) . . ? C5 C6 C7 120.8(2) . . ? C6 C7 C2 118.67(18) . . ? C6 C7 C8 119.44(17) . . ? C2 C7 C8 121.83(15) . . ? O4 C8 O3 120.97(18) . . ? O4 C8 C7 119.60(15) . . ? O3 C8 C7 119.43(16) . . ? O4 C8 Ce1 60.04(10) . 1_565 ? O3 C8 Ce1 60.99(10) . 1_565 ? C7 C8 Ce1 177.59(14) . 1_565 ? O5 C9 O6 126.51(18) . . ? O5 C9 C9 117.0(2) . 5_646 ? O6 C9 C9 116.5(2) . 5_646 ? O1 Ce1 O7 74.52(5) . . ? O1 Ce1 O5 139.98(5) . . ? O7 Ce1 O5 67.85(5) . . ? O1 Ce1 O8 84.07(5) . . ? O7 Ce1 O8 75.93(5) . . ? O5 Ce1 O8 74.25(6) . . ? O1 Ce1 O6 154.25(5) . 5_646 ? O7 Ce1 O6 131.20(6) . 5_646 ? O5 Ce1 O6 64.41(5) . 5_646 ? O8 Ce1 O6 99.94(5) . 5_646 ? O1 Ce1 O4 81.23(5) . 1_545 ? O7 Ce1 O4 143.10(5) . 1_545 ? O5 Ce1 O4 122.64(5) . 1_545 ? O8 Ce1 O4 74.24(5) . 1_545 ? O6 Ce1 O4 75.55(5) 5_646 1_545 ? O1 Ce1 O2 114.04(4) . 7_546 ? O7 Ce1 O2 86.66(5) . 7_546 ? O5 Ce1 O2 77.47(5) . 7_546 ? O8 Ce1 O2 150.74(6) . 7_546 ? O6 Ce1 O2 74.01(4) 5_646 7_546 ? O4 Ce1 O2 129.07(5) 1_545 7_546 ? O1 Ce1 O3 77.47(5) . 1_545 ? O7 Ce1 O3 143.47(5) . 1_545 ? O5 Ce1 O3 142.44(5) . 1_545 ? O8 Ce1 O3 123.89(5) . 1_545 ? O6 Ce1 O3 79.31(5) 5_646 1_545 ? O4 Ce1 O3 50.94(4) 1_545 1_545 ? O2 Ce1 O3 83.77(5) 7_546 1_545 ? O1 Ce1 O1 64.41(5) . 7_546 ? O7 Ce1 O1 70.82(5) . 7_546 ? O5 Ce1 O1 113.06(5) . 7_546 ? O8 Ce1 O1 138.87(5) . 7_546 ? O6 Ce1 O1 120.06(4) 5_646 7_546 ? O4 Ce1 O1 122.27(5) 1_545 7_546 ? O2 Ce1 O1 49.73(5) 7_546 7_546 ? O3 Ce1 O1 76.19(4) 1_545 7_546 ? O1 Ce1 C8 78.88(5) . 1_545 ? O7 Ce1 C8 153.29(6) . 1_545 ? O5 Ce1 C8 136.89(5) . 1_545 ? O8 Ce1 C8 99.17(5) . 1_545 ? O6 Ce1 C8 75.37(5) 5_646 1_545 ? O4 Ce1 C8 25.38(5) 1_545 1_545 ? O2 Ce1 C8 106.58(5) 7_546 1_545 ? O3 Ce1 C8 25.58(4) 1_545 1_545 ? O1 Ce1 C8 99.78(5) 7_546 1_545 ? O1 Ce1 C1 89.61(5) . 7_546 ? O7 Ce1 C1 76.99(5) . 7_546 ? O5 Ce1 C1 94.69(5) . 7_546 ? O8 Ce1 C1 152.90(5) . 7_546 ? O6 Ce1 C1 97.14(5) 5_646 7_546 ? O4 Ce1 C1 130.81(5) 1_545 7_546 ? O2 Ce1 C1 24.54(5) 7_546 7_546 ? O3 Ce1 C1 79.88(5) 1_545 7_546 ? O1 Ce1 C1 25.21(5) 7_546 7_546 ? C8 Ce1 C1 105.43(5) 1_545 7_546 ? C1 O1 Ce1 151.93(11) . . ? C1 O1 Ce1 92.42(10) . 7_546 ? Ce1 O1 Ce1 115.59(5) . 7_546 ? C1 O2 Ce1 97.32(11) . 7_546 ? C8 O3 Ce1 93.44(12) . 1_565 ? C8 O4 Ce1 94.58(11) . 1_565 ? C9 O5 Ce1 121.83(13) . . ? C9 O6 Ce1 119.95(12) . 5_646 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.047 _refine_diff_density_min -3.454 _refine_diff_density_rms 0.273 data_2 _database_code_depnum_ccdc_archive 'CCDC 715641' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C18 H18 O17 Pr2' _chemical_formula_sum 'C18 H18 O17 Pr2' _chemical_formula_weight 788.14 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pr Pr -0.2180 2.8214 '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 19.9212(19) _cell_length_b 6.0431(5) _cell_length_c 20.5250(18) _cell_angle_alpha 90.00 _cell_angle_beta 111.164(3) _cell_angle_gamma 90.00 _cell_volume 2304.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2870 _cell_measurement_theta_min 2.13 _cell_measurement_theta_max 28.36 _exptl_crystal_description rod _exptl_crystal_colour green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 2.272 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1520 _exptl_absorpt_coefficient_mu 4.265 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7350 _exptl_absorpt_correction_T_max 0.8504 _exptl_absorpt_process_details SADABS _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 'Siemens Smart CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 9.00cm _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 8050 _diffrn_reflns_av_R_equivalents 0.0861 _diffrn_reflns_av_sigmaI/netI 0.0617 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 28.36 _reflns_number_total 2870 _reflns_number_gt 2557 _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 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0357P)^2^+1.3034P] 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 2870 _refine_ls_number_parameters 172 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0361 _refine_ls_R_factor_gt 0.0307 _refine_ls_wR_factor_ref 0.0748 _refine_ls_wR_factor_gt 0.0731 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.089 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.15326(19) 0.6277(5) 0.36181(18) 0.0176(6) Uani 1 1 d . . . C2 C 0.15865(19) 0.7855(5) 0.30775(18) 0.0172(6) Uani 1 1 d . . . C3 C 0.20321(17) 0.9712(5) 0.32619(16) 0.0154(6) Uani 1 1 d . . . C4 C 0.25397(17) 1.0232(5) 0.39886(16) 0.0147(6) Uani 1 1 d . . . C5 C 0.2038(2) 1.1208(6) 0.27496(19) 0.0231(7) Uani 1 1 d . . . H5 H 0.2333 1.2448 0.2872 0.028 Uiso 1 1 calc R . . C6 C 0.1605(2) 1.0865(7) 0.20557(19) 0.0269(8) Uani 1 1 d . . . H6 H 0.1601 1.1896 0.1718 0.032 Uiso 1 1 calc R . . C7 C 0.1180(2) 0.8996(7) 0.18664(19) 0.0274(8) Uani 1 1 d . . . H7 H 0.0905 0.8730 0.1399 0.033 Uiso 1 1 calc R . . C8 C 0.1165(2) 0.7515(7) 0.23791(19) 0.0234(7) Uani 1 1 d . . . H8 H 0.0869 0.6277 0.2253 0.028 Uiso 1 1 calc R . . C9 C 0.00079(18) 0.6135(6) 0.48234(17) 0.0166(6) Uani 1 1 d . . . H9 H 0.033(4) 0.306(10) 0.268(4) 0.07(2) Uiso 1 1 d . . . O1 O 0.10700(15) 0.4742(4) 0.34414(13) 0.0258(6) Uani 1 1 d . . . O2 O 0.19489(14) 0.6496(4) 0.42478(13) 0.0189(5) Uani 1 1 d . . . O3 O 0.31834(13) 0.9612(4) 0.41812(13) 0.0207(5) Uani 1 1 d . . . O4 O 0.23264(14) 1.1439(4) 0.43763(13) 0.0183(5) Uani 1 1 d . . . O5 O 0.04769(14) 0.6334(4) 0.45483(15) 0.0228(5) Uani 1 1 d . . . O6 O -0.04352(14) 0.7537(4) 0.48389(14) 0.0230(5) Uani 1 1 d . . . O7 O 0.05729(16) 0.0491(4) 0.38743(14) 0.0300(6) Uani 1 1 d . . . O8 O 0.16363(14) -0.0120(4) 0.53641(14) 0.0248(5) Uani 1 1 d . . . O9 O 0.0000 0.2093(8) 0.2500 0.0379(11) Uani 1 2 d S . . Pr1 Pr 0.137233(9) 0.33049(3) 0.466475(8) 0.01254(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0191(17) 0.0137(15) 0.0203(16) 0.0009(12) 0.0073(13) 0.0005(13) C2 0.0191(17) 0.0138(14) 0.0184(15) 0.0014(12) 0.0066(13) 0.0019(13) C3 0.0142(14) 0.0164(15) 0.0157(14) -0.0018(12) 0.0057(11) 0.0002(12) C4 0.0173(15) 0.0106(13) 0.0169(14) 0.0002(11) 0.0071(12) -0.0023(12) C5 0.028(2) 0.0195(16) 0.0222(17) 0.0012(14) 0.0103(14) -0.0044(15) C6 0.032(2) 0.0298(19) 0.0181(16) 0.0072(15) 0.0080(15) -0.0011(17) C7 0.0255(19) 0.037(2) 0.0155(16) 0.0013(16) 0.0028(14) -0.0032(17) C8 0.0221(18) 0.0252(18) 0.0206(17) -0.0008(14) 0.0048(14) -0.0078(15) C9 0.0128(15) 0.0165(15) 0.0202(16) 0.0029(12) 0.0054(12) -0.0007(13) O1 0.0271(14) 0.0252(13) 0.0200(12) 0.0025(10) 0.0025(10) -0.0105(11) O2 0.0187(12) 0.0167(12) 0.0179(11) 0.0020(9) 0.0024(9) -0.0029(9) O3 0.0161(11) 0.0216(13) 0.0236(12) -0.0055(10) 0.0063(9) 0.0028(10) O4 0.0159(12) 0.0196(12) 0.0197(11) -0.0051(9) 0.0066(9) 0.0023(9) O5 0.0194(13) 0.0207(12) 0.0355(14) 0.0115(11) 0.0184(11) 0.0071(10) O6 0.0207(13) 0.0169(12) 0.0372(15) 0.0063(11) 0.0174(11) 0.0054(11) O7 0.0334(15) 0.0260(14) 0.0271(13) -0.0022(11) 0.0066(11) -0.0135(12) O8 0.0227(13) 0.0182(12) 0.0336(13) 0.0077(11) 0.0102(10) 0.0029(10) O9 0.032(3) 0.038(2) 0.030(2) 0.000 -0.0045(19) 0.000 Pr1 0.01022(11) 0.01192(11) 0.01540(11) 0.00027(6) 0.00452(7) 0.00066(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.265(4) . ? C1 O2 1.266(4) . ? C1 C2 1.496(5) . ? C2 C8 1.390(5) . ? C2 C3 1.396(5) . ? C3 C5 1.390(5) . ? C3 C4 1.502(4) . ? C4 O3 1.255(4) . ? C4 O4 1.261(4) . ? C4 Pr1 2.965(3) 7_566 ? C5 C6 1.388(5) . ? C6 C7 1.381(6) . ? C7 C8 1.390(6) . ? C9 O6 1.232(4) . ? C9 O5 1.260(4) . ? C9 C9 1.557(7) 5_566 ? O1 Pr1 2.516(2) . ? O2 Pr1 2.546(2) . ? O3 Pr1 2.543(2) 7_566 ? O4 Pr1 2.459(2) 1_565 ? O4 Pr1 2.633(3) 7_566 ? O5 Pr1 2.506(2) . ? O6 Pr1 2.481(3) 5_566 ? O7 Pr1 2.489(3) . ? O8 Pr1 2.465(2) . ? Pr1 O4 2.459(2) 1_545 ? Pr1 O6 2.481(3) 5_566 ? Pr1 O3 2.543(2) 7_566 ? Pr1 O4 2.633(3) 7_566 ? Pr1 C4 2.965(3) 7_566 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 O2 120.7(3) . . ? O1 C1 C2 119.7(3) . . ? O2 C1 C2 119.7(3) . . ? C8 C2 C3 119.1(3) . . ? C8 C2 C1 119.5(3) . . ? C3 C2 C1 121.4(3) . . ? C5 C3 C2 119.7(3) . . ? C5 C3 C4 115.4(3) . . ? C2 C3 C4 124.9(3) . . ? O3 C4 O4 120.8(3) . . ? O3 C4 C3 119.7(3) . . ? O4 C4 C3 119.2(3) . . ? O3 C4 Pr1 58.37(16) . 7_566 ? O4 C4 Pr1 62.53(17) . 7_566 ? C3 C4 Pr1 172.4(2) . 7_566 ? C6 C5 C3 120.5(3) . . ? C7 C6 C5 120.1(3) . . ? C6 C7 C8 119.5(3) . . ? C2 C8 C7 121.0(4) . . ? O6 C9 O5 126.9(3) . . ? O6 C9 C9 117.3(4) . 5_566 ? O5 C9 C9 115.8(4) . 5_566 ? C1 O1 Pr1 94.6(2) . . ? C1 O2 Pr1 93.2(2) . . ? C4 O3 Pr1 96.78(19) . 7_566 ? C4 O4 Pr1 152.0(2) . 1_565 ? C4 O4 Pr1 92.3(2) . 7_566 ? Pr1 O4 Pr1 115.53(9) 1_565 7_566 ? C9 O5 Pr1 120.4(2) . . ? C9 O6 Pr1 121.5(2) . 5_566 ? O4 Pr1 O8 74.59(9) 1_545 . ? O4 Pr1 O6 140.04(8) 1_545 5_566 ? O8 Pr1 O6 67.84(9) . 5_566 ? O4 Pr1 O7 84.15(9) 1_545 . ? O8 Pr1 O7 75.98(9) . . ? O6 Pr1 O7 74.24(10) 5_566 . ? O4 Pr1 O5 153.80(8) 1_545 . ? O8 Pr1 O5 131.57(8) . . ? O6 Pr1 O5 64.76(8) 5_566 . ? O7 Pr1 O5 99.84(10) . . ? O4 Pr1 O1 81.10(9) 1_545 . ? O8 Pr1 O1 142.65(9) . . ? O6 Pr1 O1 122.42(9) 5_566 . ? O7 Pr1 O1 73.69(9) . . ? O5 Pr1 O1 75.35(9) . . ? O4 Pr1 O3 114.33(8) 1_545 7_566 ? O8 Pr1 O3 86.78(9) . 7_566 ? O6 Pr1 O3 77.26(9) 5_566 7_566 ? O7 Pr1 O3 150.59(9) . 7_566 ? O5 Pr1 O3 73.96(9) . 7_566 ? O1 Pr1 O3 129.51(9) . 7_566 ? O4 Pr1 O2 77.56(8) 1_545 . ? O8 Pr1 O2 143.57(9) . . ? O6 Pr1 O2 142.28(9) 5_566 . ? O7 Pr1 O2 123.96(8) . . ? O5 Pr1 O2 78.85(8) . . ? O1 Pr1 O2 51.50(8) . . ? O3 Pr1 O2 83.71(8) 7_566 . ? O4 Pr1 O4 64.47(9) 1_545 7_566 ? O8 Pr1 O4 70.64(8) . 7_566 ? O6 Pr1 O4 112.88(8) 5_566 7_566 ? O7 Pr1 O4 138.84(9) . 7_566 ? O5 Pr1 O4 120.21(8) . 7_566 ? O1 Pr1 O4 122.82(9) . 7_566 ? O3 Pr1 O4 49.98(7) 7_566 7_566 ? O2 Pr1 O4 76.40(8) . 7_566 ? O4 Pr1 C4 89.59(9) 1_545 7_566 ? O8 Pr1 C4 77.12(9) . 7_566 ? O6 Pr1 C4 94.79(9) 5_566 7_566 ? O7 Pr1 C4 153.08(9) . 7_566 ? O5 Pr1 C4 97.27(9) . 7_566 ? O1 Pr1 C4 131.17(8) . 7_566 ? O3 Pr1 C4 24.85(8) 7_566 7_566 ? O2 Pr1 C4 79.68(8) . 7_566 ? O4 Pr1 C4 25.15(8) 7_566 7_566 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.36 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.302 _refine_diff_density_min -1.585 _refine_diff_density_rms 0.228 data_3 _database_code_depnum_ccdc_archive 'CCDC 715642' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C18 H18 Nd2 O17' _chemical_formula_sum 'C18 H18 Nd2 O17' _chemical_formula_weight 794.80 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' Nd Nd -0.1943 3.0179 '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 19.8310(18) _cell_length_b 6.0329(5) _cell_length_c 20.4964(19) _cell_angle_alpha 90.00 _cell_angle_beta 111.096(2) _cell_angle_gamma 90.00 _cell_volume 2287.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2840 _cell_measurement_theta_min 2.13 _cell_measurement_theta_max 28.34 _exptl_crystal_description rod _exptl_crystal_colour pink _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 2.308 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1528 _exptl_absorpt_coefficient_mu 4.576 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4140 _exptl_absorpt_correction_T_max 0.6358 _exptl_absorpt_process_details SADABS _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 'Siemens Smart CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 9.00cm _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 7989 _diffrn_reflns_av_R_equivalents 0.0534 _diffrn_reflns_av_sigmaI/netI 0.0417 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 28.34 _reflns_number_total 2840 _reflns_number_gt 2499 _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 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0253P)^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 2840 _refine_ls_number_parameters 188 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0291 _refine_ls_R_factor_gt 0.0236 _refine_ls_wR_factor_ref 0.0509 _refine_ls_wR_factor_gt 0.0495 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.016 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.15353(15) 0.8744(4) 0.86240(15) 0.0165(5) Uani 1 1 d . . . C2 C 0.15868(16) 0.7170(4) 0.80834(15) 0.0171(6) Uani 1 1 d . . . C3 C 0.11628(17) 0.7506(5) 0.73837(16) 0.0225(6) Uani 1 1 d . . . H3 H 0.0865 0.8745 0.7257 0.027 Uiso 1 1 calc R . . C4 C 0.11784(17) 0.6021(6) 0.68734(16) 0.0263(7) Uani 1 1 d . . . H4 H 0.0899 0.6281 0.6407 0.032 Uiso 1 1 calc R . . C5 C 0.16061(18) 0.4167(6) 0.70561(15) 0.0260(7) Uani 1 1 d . . . H5 H 0.1608 0.3153 0.6715 0.031 Uiso 1 1 calc R . . C6 C 0.20355(17) 0.3804(5) 0.77501(16) 0.0222(6) Uani 1 1 d . . . H6 H 0.2326 0.2548 0.7871 0.027 Uiso 1 1 calc R . . C7 C 0.20359(14) 0.5297(4) 0.82657(13) 0.0157(5) Uani 1 1 d . . . C8 C 0.25401(14) 0.4768(4) 0.89930(13) 0.0139(5) Uani 1 1 d . . . C9 C -0.00083(14) 1.1128(4) 1.01762(14) 0.0151(5) Uani 1 1 d . . . H1 H 0.199(2) 1.558(7) 1.041(2) 0.031(11) Uiso 1 1 d . . . H2 H 0.139(3) 1.580(10) 1.036(3) 0.08(2) Uiso 1 1 d . . . H7 H 0.044(2) 1.577(8) 0.906(2) 0.059(14) Uiso 1 1 d . . . H8 H 0.034(2) 1.432(7) 0.854(2) 0.040(13) Uiso 1 1 d . . . H9 H 0.036(3) 0.791(7) 0.267(3) 0.061(15) Uiso 1 1 d . . . Nd1 Nd 0.137328(7) 1.16956(2) 0.966874(7) 0.01264(5) Uani 1 1 d . . . O1 O 0.19462(11) 0.8516(3) 0.92564(10) 0.0188(4) Uani 1 1 d . . . O2 O 0.10733(12) 1.0288(4) 0.84477(10) 0.0252(5) Uani 1 1 d . . . O3 O 0.31860(10) 0.5396(3) 0.91877(10) 0.0203(4) Uani 1 1 d . . . O4 O 0.23263(11) 0.3560(3) 0.93846(10) 0.0184(4) Uani 1 1 d . . . O5 O 0.04383(11) 1.2534(3) 1.01632(12) 0.0225(5) Uani 1 1 d . . . O6 O -0.04827(11) 1.1338(3) 1.04522(12) 0.0228(5) Uani 1 1 d . . . O7 O 0.16341(15) 1.5088(4) 1.03623(13) 0.0262(5) Uani 1 1 d . . . O8 O 0.05788(14) 1.4487(4) 0.88850(13) 0.0296(6) Uani 1 1 d . . . O9 O 0.0000 0.7068(7) 0.2500 0.0365(9) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0172(13) 0.0142(13) 0.0184(13) 0.0011(10) 0.0067(11) 0.0003(10) C2 0.0215(14) 0.0149(13) 0.0162(13) -0.0008(10) 0.0083(11) -0.0009(11) C3 0.0235(15) 0.0246(15) 0.0174(14) 0.0015(12) 0.0049(12) 0.0057(12) C4 0.0260(16) 0.0366(17) 0.0127(13) -0.0024(13) 0.0028(12) 0.0028(14) C5 0.0321(17) 0.0306(16) 0.0159(14) -0.0078(12) 0.0094(13) -0.0009(14) C6 0.0277(16) 0.0187(14) 0.0205(14) -0.0016(11) 0.0089(13) 0.0040(12) C7 0.0175(13) 0.0170(13) 0.0136(12) 0.0014(10) 0.0069(11) -0.0009(10) C8 0.0194(13) 0.0093(12) 0.0139(12) -0.0008(10) 0.0068(10) 0.0003(10) C9 0.0116(12) 0.0159(13) 0.0171(13) -0.0021(10) 0.0041(11) 0.0000(10) Nd1 0.01210(8) 0.01247(8) 0.01357(8) -0.00039(5) 0.00487(6) -0.00065(5) O1 0.0199(10) 0.0184(10) 0.0161(9) -0.0015(8) 0.0043(8) 0.0023(8) O2 0.0282(11) 0.0261(11) 0.0191(10) -0.0001(9) 0.0056(9) 0.0110(9) O3 0.0180(10) 0.0200(11) 0.0223(10) 0.0060(8) 0.0066(8) -0.0026(8) O4 0.0174(10) 0.0213(10) 0.0170(10) 0.0043(8) 0.0068(8) -0.0016(8) O5 0.0213(11) 0.0155(9) 0.0360(13) -0.0065(9) 0.0168(10) -0.0047(8) O6 0.0212(10) 0.0209(11) 0.0327(12) -0.0113(9) 0.0175(10) -0.0070(8) O7 0.0202(12) 0.0207(11) 0.0395(13) -0.0101(10) 0.0128(11) -0.0045(11) O8 0.0338(13) 0.0285(14) 0.0193(12) -0.0001(10) 0.0007(11) 0.0135(11) O9 0.033(2) 0.037(2) 0.0284(19) 0.000 -0.0032(16) 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 C1 O2 1.265(3) . ? C1 O1 1.266(3) . ? C1 C2 1.490(4) . ? C2 C3 1.392(4) . ? C2 C7 1.404(4) . ? C3 C4 1.386(4) . ? C4 C5 1.372(5) . ? C5 C6 1.387(4) . ? C6 C7 1.388(4) . ? C7 C8 1.500(4) . ? C8 O3 1.255(3) . ? C8 O4 1.265(3) . ? C8 Nd1 2.948(3) 7_567 ? C9 O5 1.234(3) . ? C9 O6 1.267(3) . ? C9 C9 1.547(5) 5_577 ? Nd1 O7 2.439(2) . ? Nd1 O4 2.443(2) 1_565 ? Nd1 O5 2.464(2) . ? Nd1 O8 2.465(2) . ? Nd1 O6 2.493(2) 5_577 ? Nd1 O2 2.503(2) . ? Nd1 O3 2.5249(19) 7_567 ? Nd1 O1 2.5252(19) . ? Nd1 O4 2.615(2) 7_567 ? Nd1 C8 2.948(3) 7_567 ? O3 Nd1 2.5249(19) 7_567 ? O4 Nd1 2.4430(19) 1_545 ? O4 Nd1 2.615(2) 7_567 ? O6 Nd1 2.493(2) 5_577 ? 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 C1 O1 120.4(3) . . ? O2 C1 C2 119.6(2) . . ? O1 C1 C2 120.1(2) . . ? C3 C2 C7 118.8(3) . . ? C3 C2 C1 119.7(3) . . ? C7 C2 C1 121.4(2) . . ? C4 C3 C2 120.9(3) . . ? C5 C4 C3 120.0(3) . . ? C4 C5 C6 120.0(3) . . ? C5 C6 C7 120.7(3) . . ? C6 C7 C2 119.5(3) . . ? C6 C7 C8 115.9(2) . . ? C2 C7 C8 124.6(2) . . ? O3 C8 O4 120.6(2) . . ? O3 C8 C7 119.4(2) . . ? O4 C8 C7 119.8(2) . . ? O3 C8 Nd1 58.27(13) . 7_567 ? O4 C8 Nd1 62.41(14) . 7_567 ? C7 C8 Nd1 172.17(18) . 7_567 ? O5 C9 O6 126.5(3) . . ? O5 C9 C9 117.3(3) . 5_577 ? O6 C9 C9 116.2(3) . 5_577 ? O7 Nd1 O4 74.49(8) . 1_565 ? O7 Nd1 O5 67.74(8) . . ? O4 Nd1 O5 139.87(6) 1_565 . ? O7 Nd1 O8 76.01(9) . . ? O4 Nd1 O8 84.14(8) 1_565 . ? O5 Nd1 O8 74.26(8) . . ? O7 Nd1 O6 131.92(8) . 5_577 ? O4 Nd1 O6 153.56(7) 1_565 5_577 ? O5 Nd1 O6 65.21(7) . 5_577 ? O8 Nd1 O6 99.96(8) . 5_577 ? O7 Nd1 O2 142.34(8) . . ? O4 Nd1 O2 81.01(7) 1_565 . ? O5 Nd1 O2 122.51(7) . . ? O8 Nd1 O2 73.39(8) . . ? O6 Nd1 O2 75.32(7) 5_577 . ? O7 Nd1 O3 87.04(8) . 7_567 ? O4 Nd1 O3 114.36(6) 1_565 7_567 ? O5 Nd1 O3 77.36(7) . 7_567 ? O8 Nd1 O3 150.79(8) . 7_567 ? O6 Nd1 O3 73.83(7) 5_577 7_567 ? O2 Nd1 O3 129.56(7) . 7_567 ? O7 Nd1 O1 143.71(8) . . ? O4 Nd1 O1 77.88(6) 1_565 . ? O5 Nd1 O1 142.13(7) . . ? O8 Nd1 O1 124.05(8) . . ? O6 Nd1 O1 78.28(7) 5_577 . ? O2 Nd1 O1 51.78(6) . . ? O3 Nd1 O1 83.34(7) 7_567 . ? O7 Nd1 O4 70.81(8) . 7_567 ? O4 Nd1 O4 64.09(7) 1_565 7_567 ? O5 Nd1 O4 113.21(7) . 7_567 ? O8 Nd1 O4 138.78(8) . 7_567 ? O6 Nd1 O4 120.31(7) 5_577 7_567 ? O2 Nd1 O4 122.54(7) . 7_567 ? O3 Nd1 O4 50.38(6) 7_567 7_567 ? O1 Nd1 O4 76.18(6) . 7_567 ? O7 Nd1 C8 77.20(8) . 7_567 ? O4 Nd1 C8 89.46(7) 1_565 7_567 ? O5 Nd1 C8 94.88(7) . 7_567 ? O8 Nd1 C8 153.20(8) . 7_567 ? O6 Nd1 C8 97.29(7) 5_577 7_567 ? O2 Nd1 C8 131.27(7) . 7_567 ? O3 Nd1 C8 25.01(7) 7_567 7_567 ? O1 Nd1 C8 79.49(7) . 7_567 ? O4 Nd1 C8 25.39(6) 7_567 7_567 ? C1 O1 Nd1 93.37(16) . . ? C1 O2 Nd1 94.43(16) . . ? C8 O3 Nd1 96.72(16) . 7_567 ? C8 O4 Nd1 151.80(18) . 1_545 ? C8 O4 Nd1 92.20(16) . 7_567 ? Nd1 O4 Nd1 115.91(7) 1_545 7_567 ? C9 O5 Nd1 121.32(18) . . ? C9 O6 Nd1 119.69(17) . 5_577 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.34 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.641 _refine_diff_density_min -1.701 _refine_diff_density_rms 0.189 data_4 _database_code_depnum_ccdc_archive 'CCDC 715643' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C18 H18 O17 Sm2' _chemical_formula_sum 'C18 H18 O17 Sm2' _chemical_formula_weight 807.02 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' Sm Sm -0.1638 3.4418 '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 19.697(4) _cell_length_b 6.0193(12) _cell_length_c 20.472(4) _cell_angle_alpha 90.00 _cell_angle_beta 110.89(3) _cell_angle_gamma 90.00 _cell_volume 2267.5(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2585 _cell_measurement_theta_min 3.56 _cell_measurement_theta_max 27.42 _exptl_crystal_description rod _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 2.364 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1544 _exptl_absorpt_coefficient_mu 5.216 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4383 _exptl_absorpt_correction_T_max 0.5000 _exptl_absorpt_process_details Process-auto _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' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 9.00cm _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 10452 _diffrn_reflns_av_R_equivalents 0.0330 _diffrn_reflns_av_sigmaI/netI 0.0287 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.56 _diffrn_reflns_theta_max 27.42 _reflns_number_total 2585 _reflns_number_gt 2338 _reflns_threshold_expression >2sigma(I) _computing_data_collection Process-auto _computing_cell_refinement Process-auto _computing_data_reduction Process-auto _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^+22.1488P] 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 2585 _refine_ls_number_parameters 188 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0315 _refine_ls_R_factor_gt 0.0280 _refine_ls_wR_factor_ref 0.0619 _refine_ls_wR_factor_gt 0.0606 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2972(2) -0.0312(7) 0.6728(2) 0.0133(8) Uani 1 1 d . . . C2 C 0.3414(2) -0.2186(7) 0.6903(2) 0.0144(8) Uani 1 1 d . . . C3 C 0.3841(3) -0.2563(9) 0.7611(2) 0.0223(10) Uani 1 1 d . . . H3 H 0.4135 -0.3817 0.7737 0.027 Uiso 1 1 calc R . . C4 C 0.3823(3) -0.1066(9) 0.8118(2) 0.0229(10) Uani 1 1 d . . . H4 H 0.4102 -0.1333 0.8584 0.028 Uiso 1 1 calc R . . C5 C 0.3397(3) 0.0812(9) 0.7940(2) 0.0247(10) Uani 1 1 d . . . H5 H 0.3399 0.1827 0.8283 0.030 Uiso 1 1 calc R . . C6 C 0.2963(3) 0.1186(8) 0.7245(2) 0.0200(9) Uani 1 1 d . . . H6 H 0.2667 0.2437 0.7125 0.024 Uiso 1 1 calc R . . C7 C 0.2461(2) 0.0239(7) 0.6002(2) 0.0121(8) Uani 1 1 d . . . C8 C 0.3470(2) -0.3773(7) 0.6363(2) 0.0133(8) Uani 1 1 d . . . C9 C -0.0008(2) 0.1125(7) 0.5178(2) 0.0136(8) Uani 1 1 d . . . H1 H 0.198(3) 0.568(10) 0.545(3) 0.017(14) Uiso 1 1 d . . . H2 H 0.134(5) 0.588(16) 0.530(5) 0.08(3) Uiso 1 1 d . . . H7 H 0.044(4) 0.543(15) 0.407(4) 0.06(3) Uiso 1 1 d . . . H8 H 0.037(4) 0.423(11) 0.354(4) 0.04(2) Uiso 1 1 d . . . H9 H 0.035(4) 0.218(12) 0.270(4) 0.06(2) Uiso 1 1 d . . . O1 O 0.18105(16) -0.0390(5) 0.57999(16) 0.0182(6) Uani 1 1 d . . . O2 O 0.26818(16) 0.1447(5) 0.56137(15) 0.0164(6) Uani 1 1 d . . . O3 O 0.30592(16) -0.3532(5) 0.57283(15) 0.0155(6) Uani 1 1 d . . . O4 O 0.39285(17) -0.5337(6) 0.65384(16) 0.0228(7) Uani 1 1 d . . . O5 O 0.04436(17) 0.2539(5) 0.51702(17) 0.0202(7) Uani 1 1 d . . . O6 O -0.04850(17) 0.1319(5) 0.54564(17) 0.0208(7) Uani 1 1 d . . . O7 O 0.1637(2) 0.5055(6) 0.5366(2) 0.0228(7) Uani 1 1 d . . . O8 O 0.0581(2) 0.4460(7) 0.3900(2) 0.0286(9) Uani 1 1 d . . . O9 O 0.0000 0.2970(10) 0.2500 0.0359(14) Uani 1 2 d S . . Sm1 Sm 0.137333(10) 0.17003(3) 0.467527(10) 0.00999(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 C1 0.0137(19) 0.013(2) 0.0135(19) 0.0009(16) 0.0058(16) -0.0022(15) C2 0.020(2) 0.012(2) 0.016(2) -0.0042(16) 0.0115(17) -0.0031(16) C3 0.025(2) 0.025(2) 0.014(2) 0.0040(18) 0.0042(19) 0.0074(19) C4 0.022(2) 0.033(3) 0.011(2) -0.0017(18) 0.0033(18) 0.000(2) C5 0.026(2) 0.033(3) 0.016(2) -0.0088(19) 0.009(2) -0.002(2) C6 0.026(2) 0.015(2) 0.022(2) -0.0014(17) 0.012(2) 0.0036(17) C7 0.0159(19) 0.0073(19) 0.0144(19) -0.0004(15) 0.0070(16) 0.0015(15) C8 0.0144(19) 0.008(2) 0.017(2) -0.0001(15) 0.0057(17) -0.0011(15) C9 0.0127(19) 0.013(2) 0.017(2) -0.0015(16) 0.0083(17) -0.0006(15) O1 0.0167(15) 0.0193(17) 0.0189(15) 0.0063(12) 0.0067(13) -0.0003(12) O2 0.0160(15) 0.0183(16) 0.0173(14) 0.0038(12) 0.0087(13) 0.0001(12) O3 0.0168(15) 0.0139(15) 0.0137(14) -0.0020(11) 0.0030(12) 0.0027(11) O4 0.0255(17) 0.0217(18) 0.0172(15) 0.0007(13) 0.0026(14) 0.0112(13) O5 0.0209(16) 0.0143(15) 0.0319(18) -0.0069(13) 0.0174(14) -0.0064(12) O6 0.0182(15) 0.0179(17) 0.0323(18) -0.0121(13) 0.0163(14) -0.0057(12) O7 0.0177(18) 0.0163(17) 0.036(2) -0.0113(15) 0.0111(16) -0.0060(15) O8 0.035(2) 0.026(2) 0.0206(19) -0.0001(16) 0.0046(18) 0.0144(16) O9 0.030(3) 0.039(4) 0.025(3) 0.000 -0.006(2) 0.000 Sm1 0.00918(11) 0.00974(11) 0.01167(11) -0.00029(8) 0.00450(8) -0.00055(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.393(6) . ? C1 C6 1.396(6) . ? C1 C7 1.504(5) . ? C2 C3 1.411(6) . ? C2 C8 1.494(6) . ? C3 C4 1.385(7) . ? C4 C5 1.378(7) . ? C5 C6 1.393(6) . ? C7 O1 1.255(5) . ? C7 O2 1.264(5) . ? C8 O4 1.265(5) . ? C8 O3 1.270(5) . ? C8 Sm1 2.861(4) 7_546 ? C9 O5 1.235(5) . ? C9 O6 1.267(5) . ? C9 C9 1.543(8) 5_556 ? O1 Sm1 2.492(3) . ? O2 Sm1 2.417(3) 7_556 ? O2 Sm1 2.612(3) . ? O3 Sm1 2.496(3) 7_546 ? O4 Sm1 2.479(3) 7_546 ? O5 Sm1 2.441(3) . ? O6 Sm1 2.470(3) 5_556 ? O7 Sm1 2.413(3) . ? O8 Sm1 2.439(4) . ? Sm1 O2 2.417(3) 7_556 ? Sm1 O6 2.470(3) 5_556 ? Sm1 O4 2.479(3) 7_546 ? Sm1 O3 2.496(3) 7_546 ? Sm1 C8 2.861(4) 7_546 ? 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 C2 C1 C6 120.3(4) . . ? C2 C1 C7 124.7(4) . . ? C6 C1 C7 115.0(4) . . ? C1 C2 C3 118.9(4) . . ? C1 C2 C8 122.2(4) . . ? C3 C2 C8 118.9(4) . . ? C4 C3 C2 120.1(4) . . ? C5 C4 C3 120.8(4) . . ? C4 C5 C6 119.8(4) . . ? C5 C6 C1 120.1(4) . . ? O1 C7 O2 120.4(4) . . ? O1 C7 C1 120.2(4) . . ? O2 C7 C1 119.2(4) . . ? O4 C8 O3 120.4(4) . . ? O4 C8 C2 119.9(4) . . ? O3 C8 C2 119.7(4) . . ? O4 C8 Sm1 59.8(2) . 7_546 ? O3 C8 Sm1 60.6(2) . 7_546 ? C2 C8 Sm1 177.5(3) . 7_546 ? O5 C9 O6 126.5(4) . . ? O5 C9 C9 117.7(4) . 5_556 ? O6 C9 C9 115.8(4) . 5_556 ? C7 O1 Sm1 97.4(2) . . ? C7 O2 Sm1 152.6(3) . 7_556 ? C7 O2 Sm1 91.4(2) . . ? Sm1 O2 Sm1 115.90(11) 7_556 . ? C8 O3 Sm1 93.1(2) . 7_546 ? C8 O4 Sm1 94.0(2) . 7_546 ? C9 O5 Sm1 120.8(3) . . ? C9 O6 Sm1 119.6(3) . 5_556 ? O7 Sm1 O2 74.53(12) . 7_556 ? O7 Sm1 O8 76.44(14) . . ? O2 Sm1 O8 84.07(12) 7_556 . ? O7 Sm1 O5 67.70(12) . . ? O2 Sm1 O5 139.74(11) 7_556 . ? O8 Sm1 O5 74.22(13) . . ? O7 Sm1 O6 132.54(12) . 5_556 ? O2 Sm1 O6 152.89(10) 7_556 5_556 ? O8 Sm1 O6 99.55(13) . 5_556 ? O5 Sm1 O6 65.82(10) . 5_556 ? O7 Sm1 O4 142.07(12) . 7_546 ? O2 Sm1 O4 80.67(11) 7_556 7_546 ? O8 Sm1 O4 72.81(13) . 7_546 ? O5 Sm1 O4 122.49(11) . 7_546 ? O6 Sm1 O4 74.91(11) 5_556 7_546 ? O7 Sm1 O1 87.13(12) . . ? O2 Sm1 O1 114.62(10) 7_556 . ? O8 Sm1 O1 151.04(12) . . ? O5 Sm1 O1 77.54(11) . . ? O6 Sm1 O1 74.17(11) 5_556 . ? O4 Sm1 O1 129.72(11) 7_546 . ? O7 Sm1 O3 143.61(12) . 7_546 ? O2 Sm1 O3 78.28(10) 7_556 7_546 ? O8 Sm1 O3 124.31(12) . 7_546 ? O5 Sm1 O3 141.85(10) . 7_546 ? O6 Sm1 O3 77.59(10) 5_556 7_546 ? O4 Sm1 O3 52.47(10) 7_546 7_546 ? O1 Sm1 O3 82.65(10) . 7_546 ? O7 Sm1 O2 70.61(12) . . ? O2 Sm1 O2 64.10(11) 7_556 . ? O8 Sm1 O2 138.86(12) . . ? O5 Sm1 O2 113.35(10) . . ? O6 Sm1 O2 120.79(10) 5_556 . ? O4 Sm1 O2 122.59(10) 7_546 . ? O1 Sm1 O2 50.65(10) . . ? O3 Sm1 O2 75.99(9) 7_546 . ? O7 Sm1 C8 153.23(12) . 7_546 ? O2 Sm1 C8 78.81(11) 7_556 7_546 ? O8 Sm1 C8 98.62(13) . 7_546 ? O5 Sm1 C8 137.01(11) . 7_546 ? O6 Sm1 C8 74.08(11) 5_556 7_546 ? O4 Sm1 C8 26.17(11) 7_546 7_546 ? O1 Sm1 C8 106.38(11) . 7_546 ? O3 Sm1 C8 26.32(11) 7_546 7_546 ? O2 Sm1 C8 99.83(11) . 7_546 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.42 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.726 _refine_diff_density_min -2.663 _refine_diff_density_rms 0.149 data_5 _database_code_depnum_ccdc_archive 'CCDC 715644' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C18 H18 Eu2 O17' _chemical_formula_sum 'C18 H18 Eu2 O17' _chemical_formula_weight 810.24 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 19.6326(12) _cell_length_b 6.0048(4) _cell_length_c 20.4684(17) _cell_angle_alpha 90.00 _cell_angle_beta 110.895(4) _cell_angle_gamma 90.00 _cell_volume 2254.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2176 _cell_measurement_theta_min 2.13 _cell_measurement_theta_max 25.82 _exptl_crystal_description rod _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 2.387 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1552 _exptl_absorpt_coefficient_mu 5.602 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3760 _exptl_absorpt_correction_T_max 0.5710 _exptl_absorpt_process_details SADABS _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 'Siemens Smart CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 9.00cm _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 6436 _diffrn_reflns_av_R_equivalents 0.0728 _diffrn_reflns_av_sigmaI/netI 0.0547 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 25.82 _reflns_number_total 2176 _reflns_number_gt 1941 _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 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0567P)^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 2176 _refine_ls_number_parameters 188 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0377 _refine_ls_R_factor_gt 0.0336 _refine_ls_wR_factor_ref 0.0884 _refine_ls_wR_factor_gt 0.0862 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2463(3) 0.4774(8) 0.5999(2) 0.0130(10) Uani 1 1 d . . . C2 C 0.2969(3) 0.5312(8) 0.6724(3) 0.0152(10) Uani 1 1 d . . . C3 C 0.2970(3) 0.3821(9) 0.7247(3) 0.0221(12) Uani 1 1 d . . . H3 H 0.2681 0.2551 0.7129 0.027 Uiso 1 1 calc R . . C4 C 0.3397(3) 0.4205(10) 0.7940(3) 0.0236(12) Uani 1 1 d . . . H4 H 0.3396 0.3195 0.8284 0.028 Uiso 1 1 calc R . . C5 C 0.3824(3) 0.6096(11) 0.8117(3) 0.0259(13) Uani 1 1 d . . . H5 H 0.4104 0.6379 0.8582 0.031 Uiso 1 1 calc R . . C6 C 0.3836(3) 0.7563(10) 0.7602(3) 0.0212(12) Uani 1 1 d . . . H6 H 0.4131 0.8818 0.7727 0.025 Uiso 1 1 calc R . . C7 C 0.3417(3) 0.7217(9) 0.6902(3) 0.0173(11) Uani 1 1 d . . . C8 C 0.3467(3) 0.8779(8) 0.6357(3) 0.0152(10) Uani 1 1 d . . . C9 C -0.0007(3) 0.3867(9) 0.5177(3) 0.0162(11) Uani 1 1 d . . . Eu1 Eu 0.137337(12) 0.32964(4) 0.467693(12) 0.01198(13) Uani 1 1 d . . . H1 H 0.136(4) -0.097(10) 0.545(4) 0.04(2) Uiso 1 1 d D . . H2 H 0.193(5) -0.060(18) 0.575(3) 0.09(3) Uiso 1 1 d D . . H7 H 0.045(5) -0.062(9) 0.405(5) 0.07(3) Uiso 1 1 d D . . H8 H 0.037(4) 0.083(13) 0.345(4) 0.04(2) Uiso 1 1 d . . . H9 H 0.033(4) 0.256(13) 0.268(4) 0.03(2) Uiso 1 1 d . . . O1 O 0.18095(19) 0.5384(6) 0.5800(2) 0.0198(8) Uani 1 1 d . . . O2 O 0.2680(2) 0.3546(6) 0.5610(2) 0.0162(8) Uani 1 1 d . . . O3 O 0.3063(2) 0.8537(5) 0.5722(2) 0.0165(8) Uani 1 1 d . . . O4 O 0.3930(2) 1.0361(6) 0.6531(2) 0.0255(9) Uani 1 1 d . . . O5 O 0.0444(2) 0.2464(6) 0.5170(2) 0.0215(8) Uani 1 1 d . . . O6 O -0.0488(2) 0.3689(6) 0.5455(2) 0.0217(9) Uani 1 1 d . . . O7 O 0.1641(2) -0.0049(7) 0.5364(2) 0.0233(8) Uani 1 1 d D . . O8 O 0.0574(2) 0.0562(7) 0.3898(2) 0.0279(10) Uani 1 1 d D . . O9 O 0.0000 0.1989(12) 0.2500 0.0364(18) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.018(2) 0.007(2) 0.015(2) 0.0011(19) 0.006(2) -0.0007(19) C2 0.015(2) 0.014(2) 0.016(2) -0.001(2) 0.004(2) 0.0035(19) C3 0.028(3) 0.016(3) 0.023(3) 0.002(2) 0.009(2) -0.004(2) C4 0.028(3) 0.025(3) 0.019(3) 0.008(2) 0.009(2) 0.001(2) C5 0.023(3) 0.033(3) 0.015(3) 0.000(3) -0.001(2) -0.003(2) C6 0.021(3) 0.017(3) 0.022(3) -0.006(2) 0.004(2) -0.007(2) C7 0.017(3) 0.012(2) 0.021(3) 0.003(2) 0.004(2) 0.003(2) C8 0.014(2) 0.013(2) 0.017(3) -0.001(2) 0.004(2) -0.001(2) C9 0.013(2) 0.015(2) 0.021(3) 0.002(2) 0.006(2) 0.000(2) Eu1 0.01021(17) 0.00943(18) 0.01583(18) 0.00037(9) 0.00407(12) 0.00057(8) O1 0.0139(17) 0.018(2) 0.0253(19) -0.0050(16) 0.0047(16) 0.0025(14) O2 0.0147(18) 0.0157(18) 0.0186(19) -0.0032(15) 0.0064(15) 0.0021(14) O3 0.0148(18) 0.0135(18) 0.0180(19) 0.0004(14) 0.0022(16) -0.0020(13) O4 0.028(2) 0.019(2) 0.025(2) -0.0005(16) 0.0042(18) -0.0105(16) O5 0.020(2) 0.0124(18) 0.038(2) 0.0061(18) 0.0172(18) 0.0067(16) O6 0.020(2) 0.0166(19) 0.034(2) 0.0100(17) 0.0154(18) 0.0067(15) O7 0.0195(19) 0.0152(19) 0.035(2) 0.0106(19) 0.0092(17) 0.0012(16) O8 0.033(2) 0.020(2) 0.023(2) -0.0010(18) 0.0018(19) -0.0149(18) O9 0.024(4) 0.038(4) 0.032(4) 0.000 -0.008(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 C1 O1 1.254(6) . ? C1 O2 1.265(6) . ? C1 C2 1.498(7) . ? C2 C3 1.394(8) . ? C2 C7 1.410(7) . ? C3 C4 1.385(8) . ? C4 C5 1.381(9) . ? C5 C6 1.379(9) . ? C6 C7 1.390(8) . ? C7 C8 1.489(8) . ? C8 O3 1.267(6) . ? C8 O4 1.274(6) . ? C8 Eu1 2.851(5) 7_566 ? C9 O5 1.226(7) . ? C9 O6 1.268(7) . ? C9 C9 1.548(10) 5_566 ? Eu1 O7 2.401(4) . ? Eu1 O2 2.409(4) 7_556 ? Eu1 O8 2.432(4) . ? Eu1 O5 2.432(4) . ? Eu1 O6 2.457(4) 5_566 ? Eu1 O4 2.463(4) 7_566 ? Eu1 O3 2.480(4) 7_566 ? Eu1 O1 2.487(4) . ? Eu1 O2 2.599(4) . ? Eu1 C8 2.851(5) 7_566 ? Eu1 Eu1 4.2497(5) 7_556 ? O2 Eu1 2.409(4) 7_556 ? O3 Eu1 2.480(4) 7_566 ? O4 Eu1 2.463(4) 7_566 ? O6 Eu1 2.457(4) 5_566 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 O2 120.1(4) . . ? O1 C1 C2 119.9(5) . . ? O2 C1 C2 119.8(4) . . ? C3 C2 C7 119.5(5) . . ? C3 C2 C1 116.2(5) . . ? C7 C2 C1 124.3(5) . . ? C4 C3 C2 120.9(5) . . ? C3 C4 C5 119.6(5) . . ? C6 C5 C4 119.9(5) . . ? C5 C6 C7 121.8(5) . . ? C6 C7 C2 118.2(5) . . ? C6 C7 C8 120.4(5) . . ? C2 C7 C8 121.3(5) . . ? O3 C8 O4 119.7(5) . . ? O3 C8 C7 120.8(5) . . ? O4 C8 C7 119.4(5) . . ? O3 C8 Eu1 60.2(3) . 7_566 ? O4 C8 Eu1 59.5(3) . 7_566 ? C7 C8 Eu1 177.6(4) . 7_566 ? O5 C9 O6 127.1(5) . . ? O5 C9 C9 117.7(6) . 5_566 ? O6 C9 C9 115.2(6) . 5_566 ? O7 Eu1 O2 74.46(13) . 7_556 ? O7 Eu1 O8 76.93(14) . . ? O2 Eu1 O8 84.47(14) 7_556 . ? O7 Eu1 O5 67.94(13) . . ? O2 Eu1 O5 139.95(12) 7_556 . ? O8 Eu1 O5 74.27(15) . . ? O7 Eu1 O6 132.79(14) . 5_566 ? O2 Eu1 O6 152.71(13) 7_556 5_566 ? O8 Eu1 O6 99.20(15) . 5_566 ? O5 Eu1 O6 65.85(13) . 5_566 ? O7 Eu1 O4 141.81(14) . 7_566 ? O2 Eu1 O4 80.61(14) 7_556 7_566 ? O8 Eu1 O4 72.22(14) . 7_566 ? O5 Eu1 O4 122.37(14) . 7_566 ? O6 Eu1 O4 74.94(14) 5_566 7_566 ? O7 Eu1 O3 143.55(13) . 7_566 ? O2 Eu1 O3 78.35(12) 7_556 7_566 ? O8 Eu1 O3 124.16(14) . 7_566 ? O5 Eu1 O3 141.56(13) . 7_566 ? O6 Eu1 O3 77.30(12) 5_566 7_566 ? O4 Eu1 O3 52.80(12) 7_566 7_566 ? O7 Eu1 O1 87.08(13) . . ? O2 Eu1 O1 114.55(12) 7_556 . ? O8 Eu1 O1 151.05(15) . . ? O5 Eu1 O1 77.41(14) . . ? O6 Eu1 O1 74.16(13) 5_566 . ? O4 Eu1 O1 130.03(13) 7_566 . ? O3 Eu1 O1 82.57(13) 7_566 . ? O7 Eu1 O2 70.46(12) . . ? O2 Eu1 O2 63.93(14) 7_556 . ? O8 Eu1 O2 139.23(13) . . ? O5 Eu1 O2 113.38(13) . . ? O6 Eu1 O2 120.82(12) 5_566 . ? O4 Eu1 O2 122.73(13) 7_566 . ? O3 Eu1 O2 76.01(12) 7_566 . ? O1 Eu1 O2 50.76(12) . . ? O7 Eu1 C8 153.04(15) . 7_566 ? O2 Eu1 C8 78.68(14) 7_556 7_566 ? O8 Eu1 C8 98.37(15) . 7_566 ? O5 Eu1 C8 137.03(14) . 7_566 ? O6 Eu1 C8 74.04(14) 5_566 7_566 ? O4 Eu1 C8 26.47(13) 7_566 7_566 ? O3 Eu1 C8 26.33(13) 7_566 7_566 ? O1 Eu1 C8 106.42(14) . 7_566 ? O2 Eu1 C8 99.74(13) . 7_566 ? O7 Eu1 Eu1 69.12(9) . 7_556 ? O2 Eu1 Eu1 33.32(9) 7_556 7_556 ? O8 Eu1 Eu1 114.11(11) . 7_556 ? O5 Eu1 Eu1 132.58(9) . 7_556 ? O6 Eu1 Eu1 144.79(9) 5_566 7_556 ? O4 Eu1 Eu1 103.78(10) 7_566 7_556 ? O3 Eu1 Eu1 74.79(8) 7_566 7_556 ? O1 Eu1 Eu1 81.30(8) . 7_556 ? O2 Eu1 Eu1 30.61(8) . 7_556 ? C8 Eu1 Eu1 89.55(10) 7_566 7_556 ? C1 O1 Eu1 97.3(3) . . ? C1 O2 Eu1 152.0(3) . 7_556 ? C1 O2 Eu1 91.8(3) . . ? Eu1 O2 Eu1 116.07(14) 7_556 . ? C8 O3 Eu1 93.4(3) . 7_566 ? C8 O4 Eu1 94.0(3) . 7_566 ? C9 O5 Eu1 121.0(3) . . ? C9 O6 Eu1 119.9(3) . 5_566 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.82 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.527 _refine_diff_density_min -1.800 _refine_diff_density_rms 0.232 data_6 _database_code_depnum_ccdc_archive 'CCDC 715645' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C18 H18 Gd2 O17' _chemical_formula_sum 'C18 H18 Gd2 O17' _chemical_formula_weight 820.82 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 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 19.556(4) _cell_length_b 5.9957(12) _cell_length_c 20.412(4) _cell_angle_alpha 90.00 _cell_angle_beta 110.82(3) _cell_angle_gamma 90.00 _cell_volume 2237.0(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2559 _cell_measurement_theta_min 3.58 _cell_measurement_theta_max 27.46 _exptl_crystal_description rod _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 2.437 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1560 _exptl_absorpt_coefficient_mu 5.967 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3927 _exptl_absorpt_correction_T_max 0.5000 _exptl_absorpt_process_details Process-auto _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' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 9.00cm _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 10565 _diffrn_reflns_av_R_equivalents 0.0204 _diffrn_reflns_av_sigmaI/netI 0.0168 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.58 _diffrn_reflns_theta_max 27.46 _reflns_number_total 2559 _reflns_number_gt 2418 _reflns_threshold_expression >2sigma(I) _computing_data_collection Process-auto _computing_cell_refinement Process-auto _computing_data_reduction Process-auto _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0317P)^2^+22.8529P] 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 2559 _refine_ls_number_parameters 188 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0212 _refine_ls_R_factor_gt 0.0193 _refine_ls_wR_factor_ref 0.0599 _refine_ls_wR_factor_gt 0.0478 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7970(2) 0.4684(6) 0.17249(19) 0.0136(7) Uani 1 1 d . . . C2 C 0.8420(2) 0.2796(7) 0.1902(2) 0.0153(7) Uani 1 1 d . . . C3 C 0.8842(2) 0.2411(7) 0.2606(2) 0.0193(8) Uani 1 1 d . . . H3 H 0.9135 0.1147 0.2730 0.023 Uiso 1 1 calc R . . C4 C 0.8826(2) 0.3896(8) 0.3120(2) 0.0245(9) Uani 1 1 d . . . H4 H 0.9102 0.3612 0.3587 0.029 Uiso 1 1 calc R . . C5 C 0.8399(2) 0.5806(8) 0.2941(2) 0.0220(9) Uani 1 1 d . . . H5 H 0.8400 0.6826 0.3284 0.026 Uiso 1 1 calc R . . C6 C 0.7970(2) 0.6180(7) 0.2240(2) 0.0210(8) Uani 1 1 d . . . H6 H 0.7679 0.7451 0.2118 0.025 Uiso 1 1 calc R . . C7 C 0.7461(2) 0.5223(6) 0.09970(18) 0.0129(7) Uani 1 1 d . . . C8 C 0.8472(2) 0.1209(6) 0.1356(2) 0.0141(7) Uani 1 1 d . . . C9 C 0.49899(19) 0.6118(6) 0.01800(18) 0.0108(7) Uani 1 1 d . . . Gd1 Gd 0.637328(9) 0.67065(3) -0.032106(8) 0.01000(7) Uani 1 1 d . . . H1 H 0.636(5) 1.101(14) 0.037(4) 0.07(2) Uiso 1 1 d . . . H2 H 0.699(3) 1.068(10) 0.040(3) 0.032(16) Uiso 1 1 d . . . H7 H 0.535(3) 0.911(10) -0.146(3) 0.025(14) Uiso 1 1 d . . . H8 H 0.546(4) 1.069(7) -0.096(4) 0.08(3) Uiso 1 1 d D . . H9 H 0.038(3) 0.772(12) 0.269(4) 0.05(2) Uiso 1 1 d . . . O1 O 0.68058(15) 0.4626(5) 0.07966(15) 0.0178(6) Uani 1 1 d . . . O2 O 0.89310(16) -0.0373(5) 0.15292(15) 0.0222(6) Uani 1 1 d . . . O3 O 0.80621(15) 0.1454(4) 0.07186(14) 0.0150(5) Uani 1 1 d . . . O4 O 0.54435(15) 0.7551(5) 0.01714(16) 0.0191(6) Uani 1 1 d . . . O5 O 0.45085(16) 0.6323(5) 0.04569(16) 0.0200(6) Uani 1 1 d . . . O6 O 0.66404(18) 1.0031(5) 0.03649(17) 0.0219(6) Uani 1 1 d . . . O7 O 0.76824(15) 0.6467(4) 0.06073(14) 0.0155(5) Uani 1 1 d . . . O8 O 0.55844(19) 0.9445(5) -0.10854(17) 0.0253(7) Uani 1 1 d D . . O9 O 0.0000 0.7000(9) 0.2500 0.0336(11) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0149(16) 0.0151(18) 0.0109(16) 0.0021(14) 0.0048(13) 0.0007(14) C2 0.0177(17) 0.0139(17) 0.0165(18) 0.0026(15) 0.0089(15) 0.0003(15) C3 0.024(2) 0.0155(18) 0.0160(18) 0.0044(15) 0.0047(16) 0.0065(16) C4 0.023(2) 0.039(3) 0.0095(17) -0.0030(17) 0.0034(15) 0.0018(19) C5 0.028(2) 0.024(2) 0.0141(18) -0.0071(16) 0.0079(16) -0.0022(18) C6 0.024(2) 0.022(2) 0.0188(19) 0.0005(16) 0.0092(16) 0.0040(17) C7 0.0152(16) 0.0140(17) 0.0120(16) 0.0012(14) 0.0079(13) 0.0032(14) C8 0.0141(17) 0.0145(17) 0.0144(17) -0.0028(14) 0.0058(14) -0.0021(14) C9 0.0108(15) 0.0078(16) 0.0141(16) -0.0025(13) 0.0048(13) 0.0005(13) Gd1 0.00915(10) 0.01044(10) 0.01109(10) -0.00039(6) 0.00445(7) -0.00051(6) O1 0.0162(13) 0.0171(14) 0.0195(13) 0.0046(11) 0.0056(11) -0.0020(11) O2 0.0247(15) 0.0220(15) 0.0174(13) -0.0002(12) 0.0042(12) 0.0109(12) O3 0.0158(13) 0.0155(13) 0.0121(12) 0.0003(10) 0.0031(10) 0.0017(10) O4 0.0180(13) 0.0154(13) 0.0285(15) -0.0075(12) 0.0139(12) -0.0044(11) O5 0.0175(13) 0.0208(14) 0.0275(15) -0.0093(12) 0.0151(12) -0.0055(12) O6 0.0174(14) 0.0174(15) 0.0329(16) -0.0063(13) 0.0115(13) -0.0050(13) O7 0.0165(13) 0.0164(13) 0.0152(13) 0.0016(10) 0.0078(11) 0.0000(11) O8 0.0310(17) 0.0223(17) 0.0175(15) 0.0017(13) 0.0024(13) 0.0132(14) O9 0.025(2) 0.040(3) 0.026(2) 0.000 -0.002(2) 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 C1 C6 1.383(6) . ? C1 C2 1.400(5) . ? C1 C7 1.501(5) . ? C2 C3 1.399(5) . ? C2 C8 1.496(5) . ? C3 C4 1.384(6) . ? C4 C5 1.387(7) . ? C5 C6 1.395(6) . ? C7 O1 1.251(5) . ? C7 O7 1.273(4) . ? C8 O2 1.266(5) . ? C8 O3 1.271(5) . ? C8 Gd1 2.839(4) 7_655 ? C9 O4 1.239(5) . ? C9 O5 1.265(4) . ? C9 C9 1.536(7) 5_665 ? Gd1 O6 2.385(3) . ? Gd1 O7 2.391(3) 7_665 ? Gd1 O8 2.408(3) . ? Gd1 O4 2.423(3) . ? Gd1 O5 2.451(3) 5_665 ? Gd1 O2 2.456(3) 7_655 ? Gd1 O1 2.471(3) . ? Gd1 O3 2.471(3) 7_655 ? Gd1 O7 2.592(3) . ? Gd1 C8 2.839(4) 7_655 ? O2 Gd1 2.456(3) 7_655 ? O3 Gd1 2.471(3) 7_655 ? O5 Gd1 2.451(3) 5_665 ? O7 Gd1 2.391(3) 7_665 ? 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 C1 C2 119.9(4) . . ? C6 C1 C7 115.7(3) . . ? C2 C1 C7 124.4(3) . . ? C3 C2 C1 119.0(4) . . ? C3 C2 C8 119.3(4) . . ? C1 C2 C8 121.7(3) . . ? C4 C3 C2 120.5(4) . . ? C3 C4 C5 120.4(4) . . ? C4 C5 C6 119.3(4) . . ? C1 C6 C5 120.8(4) . . ? O1 C7 O7 120.0(3) . . ? O1 C7 C1 120.3(3) . . ? O7 C7 C1 119.4(3) . . ? O2 C8 O3 119.9(3) . . ? O2 C8 C2 119.8(3) . . ? O3 C8 C2 120.2(3) . . ? O2 C8 Gd1 59.6(2) . 7_655 ? O3 C8 Gd1 60.33(19) . 7_655 ? C2 C8 Gd1 177.5(3) . 7_655 ? O4 C9 O5 126.1(3) . . ? O4 C9 C9 117.2(4) . 5_665 ? O5 C9 C9 116.6(4) . 5_665 ? O6 Gd1 O7 74.55(10) . 7_665 ? O6 Gd1 O8 76.51(12) . . ? O7 Gd1 O8 84.38(11) 7_665 . ? O6 Gd1 O4 67.78(11) . . ? O7 Gd1 O4 139.84(9) 7_665 . ? O8 Gd1 O4 73.98(11) . . ? O6 Gd1 O5 133.17(10) . 5_665 ? O7 Gd1 O5 152.25(9) 7_665 5_665 ? O8 Gd1 O5 99.73(12) . 5_665 ? O4 Gd1 O5 66.44(9) . 5_665 ? O6 Gd1 O2 141.81(11) . 7_655 ? O7 Gd1 O2 80.58(10) 7_665 7_655 ? O8 Gd1 O2 72.58(11) . 7_655 ? O4 Gd1 O2 122.33(10) . 7_655 ? O5 Gd1 O2 74.67(10) 5_665 7_655 ? O6 Gd1 O1 87.03(11) . . ? O7 Gd1 O1 114.60(9) 7_665 . ? O8 Gd1 O1 150.77(10) . . ? O4 Gd1 O1 77.49(10) . . ? O5 Gd1 O1 74.13(10) 5_665 . ? O2 Gd1 O1 130.10(10) 7_655 . ? O6 Gd1 O3 143.48(10) . 7_655 ? O7 Gd1 O3 78.28(9) 7_665 7_655 ? O8 Gd1 O3 124.63(10) . 7_655 ? O4 Gd1 O3 141.74(9) . 7_655 ? O5 Gd1 O3 76.89(9) 5_665 7_655 ? O2 Gd1 O3 52.96(9) 7_655 7_655 ? O1 Gd1 O3 82.52(9) . 7_655 ? O6 Gd1 O7 70.35(10) . . ? O7 Gd1 O7 63.64(11) 7_665 . ? O8 Gd1 O7 138.62(11) . . ? O4 Gd1 O7 113.59(9) . . ? O5 Gd1 O7 120.93(10) 5_665 . ? O2 Gd1 O7 122.68(9) 7_655 . ? O1 Gd1 O7 51.09(9) . . ? O3 Gd1 O7 75.93(9) 7_655 . ? O6 Gd1 C8 153.17(11) . 7_655 ? O7 Gd1 C8 78.73(10) 7_665 7_655 ? O8 Gd1 C8 98.67(11) . 7_655 ? O4 Gd1 C8 136.98(10) . 7_655 ? O5 Gd1 C8 73.52(10) 5_665 7_655 ? O2 Gd1 C8 26.42(10) 7_655 7_655 ? O1 Gd1 C8 106.51(10) . 7_655 ? O3 Gd1 C8 26.55(10) 7_655 7_655 ? O7 Gd1 C8 99.86(10) . 7_655 ? C7 O1 Gd1 97.6(2) . . ? C8 O2 Gd1 93.9(2) . 7_655 ? C8 O3 Gd1 93.1(2) . 7_655 ? C9 O4 Gd1 120.5(2) . . ? C9 O5 Gd1 118.9(2) . 5_665 ? C7 O7 Gd1 152.2(2) . 7_665 ? C7 O7 Gd1 91.3(2) . . ? Gd1 O7 Gd1 116.36(11) 7_665 . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.804 _refine_diff_density_min -1.969 _refine_diff_density_rms 0.171 data_7 _database_code_depnum_ccdc_archive 'CCDC 715646' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C7 H3 K O9 Tb' _chemical_formula_sum 'C7 H3 K O9 Tb' _chemical_formula_weight 429.11 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' K K 0.2009 0.2494 '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 6.6743(4) _cell_length_b 7.6033(5) _cell_length_c 11.0030(6) _cell_angle_alpha 100.210(4) _cell_angle_beta 103.892(4) _cell_angle_gamma 106.921(4) _cell_volume 499.87(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1901 _cell_measurement_theta_min 1.98 _cell_measurement_theta_max 25.76 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 2.851 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 402 _exptl_absorpt_coefficient_mu 7.532 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4885 _exptl_absorpt_correction_T_max 0.5627 _exptl_absorpt_process_details SADABS _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 'Siemens Smart CCD' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 9.00cm _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 2997 _diffrn_reflns_av_R_equivalents 0.0424 _diffrn_reflns_av_sigmaI/netI 0.0401 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 25.76 _reflns_number_total 1901 _reflns_number_gt 1783 _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 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0362P)^2^+0.2181P] 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 1901 _refine_ls_number_parameters 171 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0261 _refine_ls_R_factor_gt 0.0240 _refine_ls_wR_factor_ref 0.0619 _refine_ls_wR_factor_gt 0.0609 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.8999(8) 0.4863(7) 0.3697(4) 0.0132(9) Uani 1 1 d . . . C2 C 0.9359(7) 0.3268(7) 0.4062(4) 0.0125(9) Uani 1 1 d . . . C3 C 1.0347(8) 0.3440(7) 0.5358(5) 0.0142(10) Uani 1 1 d . . . H3 H 1.0577 0.2386 0.5600 0.017 Uiso 1 1 calc R . . C4 C 0.7919(8) 0.4784(7) 0.2288(5) 0.0160(10) Uani 1 1 d . . . C5 C 0.8668(8) 0.1356(7) 0.3098(5) 0.0147(10) Uani 1 1 d . . . C6 C 0.5310(7) 0.4378(7) 0.5448(4) 0.0128(10) Uani 1 1 d . . . C7 C 0.0158(8) -0.0975(7) -0.0070(4) 0.0155(10) Uani 1 1 d . . . H1 H 0.150(11) -0.205(9) 0.291(6) 0.021(15) Uiso 1 1 d . . . H2 H 0.372(12) -0.157(9) 0.376(6) 0.031(18) Uiso 1 1 d . . . K1 K 0.3649(3) 0.6253(2) 0.10294(13) 0.0382(3) Uani 1 1 d . . . O1 O 0.8873(7) 0.6005(6) 0.1819(4) 0.0382(11) Uani 1 1 d . . . O2 O 0.6076(6) 0.3473(5) 0.1668(3) 0.0218(8) Uani 1 1 d . . . O3 O 0.6626(6) 0.0394(5) 0.2635(4) 0.0233(8) Uani 1 1 d . . . O4 O 1.0140(6) 0.0800(5) 0.2863(4) 0.0219(8) Uani 1 1 d . . . O5 O 0.5063(6) 0.2700(5) 0.4893(3) 0.0156(7) Uani 1 1 d . . . O6 O 0.3979(6) 0.4855(5) 0.3362(3) 0.0176(7) Uani 1 1 d . . . O7 O 0.1891(6) -0.1001(5) 0.0671(3) 0.0184(7) Uani 1 1 d . . . O8 O 0.1325(6) 0.2372(5) 0.0896(3) 0.0230(8) Uani 1 1 d . . . O9 O 0.2861(7) -0.1331(6) 0.3188(4) 0.0215(8) Uani 1 1 d . . . Tb1 Tb 0.36549(3) 0.15624(3) 0.256321(19) 0.01101(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.011(2) 0.017(2) 0.011(2) 0.0028(19) 0.0041(18) 0.0040(19) C2 0.004(2) 0.016(2) 0.015(2) 0.0007(18) 0.0049(18) 0.0006(18) C3 0.014(2) 0.013(2) 0.017(2) 0.0071(19) 0.0057(19) 0.0051(19) C4 0.018(3) 0.012(2) 0.016(2) 0.0037(19) 0.005(2) 0.003(2) C5 0.014(2) 0.017(2) 0.015(2) 0.007(2) 0.0035(19) 0.006(2) C6 0.008(2) 0.015(2) 0.012(2) 0.0005(19) 0.0018(18) 0.0032(19) C7 0.019(3) 0.018(3) 0.008(2) 0.0022(19) 0.0033(19) 0.008(2) K1 0.0648(10) 0.0335(8) 0.0269(7) 0.0092(6) 0.0139(7) 0.0319(7) O1 0.037(3) 0.034(2) 0.024(2) 0.0172(19) -0.0006(18) -0.013(2) O2 0.0160(18) 0.025(2) 0.0127(17) 0.0003(15) 0.0012(14) -0.0039(15) O3 0.0110(18) 0.0179(19) 0.031(2) -0.0035(16) 0.0008(15) 0.0018(15) O4 0.0153(18) 0.023(2) 0.029(2) 0.0013(16) 0.0082(16) 0.0094(16) O5 0.0210(18) 0.0106(17) 0.0100(16) -0.0015(13) 0.0001(14) 0.0042(14) O6 0.0223(19) 0.0166(18) 0.0098(16) 0.0007(14) 0.0003(14) 0.0065(15) O7 0.0180(18) 0.0195(19) 0.0112(17) -0.0037(14) -0.0036(14) 0.0084(15) O8 0.026(2) 0.0121(17) 0.0178(19) -0.0020(14) -0.0075(15) 0.0029(15) O9 0.016(2) 0.023(2) 0.025(2) 0.0133(17) 0.0025(16) 0.0040(17) Tb1 0.00964(14) 0.01079(14) 0.00930(14) -0.00020(9) 0.00046(9) 0.00252(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 C1 C3 1.384(7) 2_766 ? C1 C2 1.409(7) . ? C1 C4 1.527(6) . ? C2 C3 1.385(7) . ? C2 C5 1.510(7) . ? C3 C1 1.384(7) 2_766 ? C4 O1 1.232(6) . ? C4 O2 1.270(6) . ? C4 K1 3.421(5) 2_665 ? C5 O4 1.239(6) . ? C5 O3 1.267(6) . ? C6 O6 1.244(6) 2_666 ? C6 O5 1.257(6) . ? C6 C6 1.550(9) 2_666 ? C7 O8 1.244(6) 2 ? C7 O7 1.253(6) . ? C7 C7 1.544(10) 2 ? K1 O7 2.718(4) 1_565 ? K1 O8 2.865(4) . ? K1 O6 2.932(4) . ? K1 O9 2.985(4) 1_565 ? K1 O2 3.057(4) 2_665 ? K1 O1 3.079(4) 2_665 ? K1 O2 3.092(4) . ? K1 O3 3.112(4) 1_565 ? K1 C4 3.421(5) 2_665 ? K1 K1 3.801(3) 2_665 ? K1 Tb1 4.0886(14) 1_565 ? K1 K1 4.501(3) 2_565 ? O1 K1 3.079(4) 2_665 ? O2 Tb1 2.366(3) . ? O2 K1 3.057(4) 2_665 ? O3 Tb1 2.388(4) . ? O3 K1 3.112(4) 1_545 ? O4 Tb1 2.366(3) 1_655 ? O5 Tb1 2.406(3) . ? O6 C6 1.244(6) 2_666 ? O6 Tb1 2.429(3) . ? O7 Tb1 2.359(3) . ? O7 K1 2.718(4) 1_545 ? O8 C7 1.244(6) 2 ? O8 Tb1 2.397(4) . ? O9 Tb1 2.372(4) . ? O9 K1 2.985(4) 1_545 ? Tb1 O4 2.366(3) 1_455 ? Tb1 K1 4.0886(14) 1_545 ? 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 C1 C2 119.1(4) 2_766 . ? C3 C1 C4 118.8(4) 2_766 . ? C2 C1 C4 122.1(4) . . ? C3 C2 C1 119.1(4) . . ? C3 C2 C5 118.3(4) . . ? C1 C2 C5 122.6(4) . . ? C1 C3 C2 121.9(5) 2_766 . ? O1 C4 O2 123.6(5) . . ? O1 C4 C1 118.2(4) . . ? O2 C4 C1 118.2(4) . . ? O1 C4 K1 63.7(3) . 2_665 ? O2 C4 K1 62.8(3) . 2_665 ? C1 C4 K1 163.2(3) . 2_665 ? O4 C5 O3 124.6(5) . . ? O4 C5 C2 117.7(4) . . ? O3 C5 C2 117.6(4) . . ? O6 C6 O5 126.8(4) 2_666 . ? O6 C6 C6 116.9(5) 2_666 2_666 ? O5 C6 C6 116.3(5) . 2_666 ? O8 C7 O7 126.1(5) 2 . ? O8 C7 C7 117.4(5) 2 2 ? O7 C7 C7 116.5(5) . 2 ? O7 K1 O8 127.02(12) 1_565 . ? O7 K1 O6 122.37(11) 1_565 . ? O8 K1 O6 58.35(10) . . ? O7 K1 O9 57.72(10) 1_565 1_565 ? O8 K1 O9 106.43(11) . 1_565 ? O6 K1 O9 66.02(10) . 1_565 ? O7 K1 O2 78.59(11) 1_565 2_665 ? O8 K1 O2 109.05(11) . 2_665 ? O6 K1 O2 158.95(11) . 2_665 ? O9 K1 O2 134.81(11) 1_565 2_665 ? O7 K1 O1 89.59(12) 1_565 2_665 ? O8 K1 O1 70.08(11) . 2_665 ? O6 K1 O1 128.38(11) . 2_665 ? O9 K1 O1 137.43(14) 1_565 2_665 ? O2 K1 O1 42.13(10) 2_665 2_665 ? O7 K1 O2 173.77(11) 1_565 . ? O8 K1 O2 58.03(10) . . ? O6 K1 O2 55.74(10) . . ? O9 K1 O2 118.68(10) 1_565 . ? O2 K1 O2 103.65(9) 2_665 . ? O1 K1 O2 95.94(12) 2_665 . ? O7 K1 O3 64.32(10) 1_565 1_565 ? O8 K1 O3 150.64(11) . 1_565 ? O6 K1 O3 92.39(11) . 1_565 ? O9 K1 O3 53.36(10) 1_565 1_565 ? O2 K1 O3 99.58(11) 2_665 1_565 ? O1 K1 O3 139.23(12) 2_665 1_565 ? O2 K1 O3 109.48(10) . 1_565 ? O7 K1 C4 80.37(11) 1_565 2_665 ? O8 K1 C4 90.56(11) . 2_665 ? O6 K1 C4 148.19(12) . 2_665 ? O9 K1 C4 137.03(12) 1_565 2_665 ? O2 K1 C4 21.69(10) 2_665 2_665 ? O1 K1 C4 21.01(11) 2_665 2_665 ? O2 K1 C4 103.90(11) . 2_665 ? O3 K1 C4 118.78(12) 1_565 2_665 ? O7 K1 K1 130.51(10) 1_565 2_665 ? O8 K1 K1 80.31(9) . 2_665 ? O6 K1 K1 107.02(9) . 2_665 ? O9 K1 K1 163.20(11) 1_565 2_665 ? O2 K1 K1 52.24(8) 2_665 2_665 ? O1 K1 K1 59.18(10) 2_665 2_665 ? O2 K1 K1 51.41(7) . 2_665 ? O3 K1 K1 113.90(10) 1_565 2_665 ? C4 K1 K1 56.49(9) 2_665 2_665 ? O7 K1 Tb1 33.48(7) 1_565 1_565 ? O8 K1 Tb1 138.13(9) . 1_565 ? O6 K1 Tb1 98.77(7) . 1_565 ? O9 K1 Tb1 34.97(7) 1_565 1_565 ? O2 K1 Tb1 101.04(8) 2_665 1_565 ? O1 K1 Tb1 122.72(10) 2_665 1_565 ? O2 K1 Tb1 140.60(8) . 1_565 ? O3 K1 Tb1 35.58(7) 1_565 1_565 ? C4 K1 Tb1 110.25(9) 2_665 1_565 ? K1 K1 Tb1 141.51(7) 2_665 1_565 ? O7 K1 K1 68.19(8) 1_565 2_565 ? O8 K1 K1 61.18(8) . 2_565 ? O6 K1 K1 101.73(9) . 2_565 ? O9 K1 K1 89.89(9) 1_565 2_565 ? O2 K1 K1 83.57(8) 2_665 2_565 ? O1 K1 K1 50.18(9) 2_665 2_565 ? O2 K1 K1 117.67(8) . 2_565 ? O3 K1 K1 130.56(8) 1_565 2_565 ? C4 K1 K1 63.86(9) 2_665 2_565 ? K1 K1 K1 106.72(6) 2_665 2_565 ? Tb1 K1 K1 95.12(4) 1_565 2_565 ? C4 O1 K1 95.3(3) . 2_665 ? C4 O2 Tb1 126.8(3) . . ? C4 O2 K1 95.5(3) . 2_665 ? Tb1 O2 K1 137.61(14) . 2_665 ? C4 O2 K1 94.5(3) . . ? Tb1 O2 K1 100.04(13) . . ? K1 O2 K1 76.35(9) 2_665 . ? C5 O3 Tb1 127.1(3) . . ? C5 O3 K1 137.5(3) . 1_545 ? Tb1 O3 K1 95.14(11) . 1_545 ? C5 O4 Tb1 148.3(3) . 1_655 ? C6 O5 Tb1 120.2(3) . . ? C6 O6 Tb1 119.6(3) 2_666 . ? C6 O6 K1 134.8(3) 2_666 . ? Tb1 O6 K1 103.02(11) . . ? C7 O7 Tb1 115.9(3) . . ? C7 O7 K1 134.7(3) . 1_545 ? Tb1 O7 K1 107.05(12) . 1_545 ? C7 O8 Tb1 114.3(3) 2 . ? C7 O8 K1 136.7(3) 2 . ? Tb1 O8 K1 105.84(13) . . ? Tb1 O9 K1 98.85(12) . 1_545 ? O7 Tb1 O2 95.60(12) . . ? O7 Tb1 O4 84.90(12) . 1_455 ? O2 Tb1 O4 144.61(13) . 1_455 ? O7 Tb1 O9 71.46(13) . . ? O2 Tb1 O9 142.04(14) . . ? O4 Tb1 O9 71.48(13) 1_455 . ? O7 Tb1 O3 82.19(12) . . ? O2 Tb1 O3 72.71(13) . . ? O4 Tb1 O3 141.74(13) 1_455 . ? O9 Tb1 O3 70.28(13) . . ? O7 Tb1 O8 68.46(12) . . ? O2 Tb1 O8 74.89(13) . . ? O4 Tb1 O8 72.45(13) 1_455 . ? O9 Tb1 O8 127.46(13) . . ? O3 Tb1 O8 133.30(13) . . ? O7 Tb1 O5 149.70(12) . . ? O2 Tb1 O5 108.81(12) . . ? O4 Tb1 O5 85.25(12) 1_455 . ? O9 Tb1 O5 78.24(13) . . ? O3 Tb1 O5 88.07(12) . . ? O8 Tb1 O5 134.39(12) . . ? O7 Tb1 O6 140.13(12) . . ? O2 Tb1 O6 72.03(13) . . ? O4 Tb1 O6 85.01(12) 1_455 . ? O9 Tb1 O6 139.46(12) . . ? O3 Tb1 O6 126.30(12) . . ? O8 Tb1 O6 71.71(12) . . ? O5 Tb1 O6 67.04(11) . . ? O7 Tb1 K1 39.46(9) . 1_545 ? O2 Tb1 K1 101.48(10) . 1_545 ? O4 Tb1 K1 101.05(9) 1_455 1_545 ? O9 Tb1 K1 46.17(10) . 1_545 ? O3 Tb1 K1 49.29(9) . 1_545 ? O8 Tb1 K1 107.63(9) . 1_545 ? O5 Tb1 K1 115.54(8) . 1_545 ? O6 Tb1 K1 173.48(9) . 1_545 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.76 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.979 _refine_diff_density_min -1.494 _refine_diff_density_rms 0.165 data_8 _database_code_depnum_ccdc_archive 'CCDC 715647' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C7 H3 Dy K O9' _chemical_formula_sum 'C7 H3 Dy K O9' _chemical_formula_weight 432.69 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' K K 0.2009 0.2494 '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 6.6560(2) _cell_length_b 7.5778(3) _cell_length_c 10.9904(3) _cell_angle_alpha 100.325(2) _cell_angle_beta 103.827(2) _cell_angle_gamma 106.904(2) _cell_volume 496.21(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2446 _cell_measurement_theta_min 1.98 _cell_measurement_theta_max 28.29 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 2.896 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 404 _exptl_absorpt_coefficient_mu 7.990 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4453 _exptl_absorpt_correction_T_max 0.5754 _exptl_absorpt_process_details SADABS _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 'Siemens Smart CCD' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 9.00cm _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 3649 _diffrn_reflns_av_R_equivalents 0.0300 _diffrn_reflns_av_sigmaI/netI 0.0451 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 28.29 _reflns_number_total 2446 _reflns_number_gt 2218 _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 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0265P)^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 2446 _refine_ls_number_parameters 171 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0290 _refine_ls_R_factor_gt 0.0249 _refine_ls_wR_factor_ref 0.0568 _refine_ls_wR_factor_gt 0.0556 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.000 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1008(7) 0.5145(6) 0.6312(4) 0.0131(8) Uani 1 1 d . . . C2 C 0.0639(7) 0.6733(6) 0.5942(4) 0.0131(8) Uani 1 1 d . . . C3 C -0.0352(7) 0.6575(6) 0.4648(4) 0.0149(8) Uani 1 1 d . . . H3 H -0.0586 0.7634 0.4411 0.018 Uiso 1 1 calc R . . C4 C 0.2101(8) 0.5222(6) 0.7705(4) 0.0161(9) Uani 1 1 d . . . C5 C 0.1358(7) 0.8651(6) 0.6914(4) 0.0130(8) Uani 1 1 d . . . C6 C 0.4679(7) 0.5622(6) 0.4552(4) 0.0133(8) Uani 1 1 d . . . C7 C 0.9831(8) 1.0981(6) 1.0067(4) 0.0159(9) Uani 1 1 d . . . H1 H 0.839(10) 1.195(9) 0.696(6) 0.030(17) Uiso 1 1 d . . . H2 H 0.654(9) 1.168(7) 0.632(5) 0.012(14) Uiso 1 1 d . . . K1 K 0.6340(2) 0.37423(18) 0.89687(12) 0.0356(3) Uani 1 1 d . . . O1 O 0.1157(7) 0.3973(5) 0.8179(3) 0.0351(10) Uani 1 1 d . . . O2 O 0.3939(5) 0.6537(5) 0.8330(3) 0.0207(7) Uani 1 1 d . . . O3 O 0.3388(5) 0.9606(5) 0.7373(3) 0.0213(7) Uani 1 1 d . . . O4 O -0.0129(5) 0.9217(5) 0.7152(3) 0.0220(7) Uani 1 1 d . . . O5 O 0.4945(5) 0.7309(4) 0.5114(3) 0.0160(6) Uani 1 1 d . . . O6 O 0.6048(5) 0.5145(4) 0.6638(3) 0.0175(7) Uani 1 1 d . . . O7 O 0.8091(5) 1.0985(5) 0.9318(3) 0.0184(7) Uani 1 1 d . . . O8 O 0.8679(6) 0.7628(5) 0.9092(3) 0.0216(7) Uani 1 1 d . . . O9 O 0.7150(6) 1.1331(5) 0.6822(4) 0.0210(7) Uani 1 1 d . . . Dy1 Dy 0.63606(3) 0.84399(3) 0.743752(19) 0.01073(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 C1 0.0102(19) 0.016(2) 0.013(2) 0.0032(17) 0.0048(16) 0.0036(16) C2 0.011(2) 0.014(2) 0.018(2) 0.0052(17) 0.0093(17) 0.0044(16) C3 0.014(2) 0.015(2) 0.017(2) 0.0051(17) 0.0062(17) 0.0048(16) C4 0.017(2) 0.016(2) 0.016(2) 0.0059(18) 0.0058(18) 0.0061(17) C5 0.015(2) 0.015(2) 0.013(2) 0.0065(17) 0.0057(17) 0.0082(17) C6 0.012(2) 0.014(2) 0.014(2) 0.0036(17) 0.0064(17) 0.0034(16) C7 0.018(2) 0.016(2) 0.014(2) 0.0045(18) 0.0054(18) 0.0067(18) K1 0.0598(9) 0.0322(7) 0.0263(6) 0.0108(5) 0.0140(6) 0.0302(6) O1 0.040(2) 0.028(2) 0.0183(18) 0.0146(16) -0.0018(16) -0.0120(17) O2 0.0151(16) 0.0251(18) 0.0152(15) 0.0063(14) 0.0026(13) -0.0016(13) O3 0.0102(15) 0.0177(17) 0.0314(19) 0.0003(15) 0.0035(14) 0.0043(13) O4 0.0149(16) 0.0196(17) 0.0316(19) 0.0009(15) 0.0101(15) 0.0074(13) O5 0.0200(16) 0.0111(15) 0.0141(15) 0.0015(12) 0.0019(13) 0.0054(12) O6 0.0238(17) 0.0164(16) 0.0099(14) 0.0006(12) 0.0016(13) 0.0083(13) O7 0.0183(16) 0.0194(17) 0.0158(15) 0.0026(13) -0.0009(13) 0.0105(13) O8 0.0230(18) 0.0138(16) 0.0175(16) -0.0006(13) -0.0045(14) 0.0027(13) O9 0.0173(18) 0.0200(18) 0.0263(19) 0.0134(16) 0.0036(15) 0.0054(15) Dy1 0.01022(10) 0.01055(10) 0.01026(10) 0.00157(7) 0.00202(7) 0.00362(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C3 1.399(6) 2_566 ? C1 C2 1.405(6) . ? C1 C4 1.512(6) . ? C2 C3 1.384(6) . ? C2 C5 1.509(6) . ? C3 C1 1.399(6) 2_566 ? C4 O1 1.245(5) . ? C4 O2 1.267(5) . ? C4 K1 3.427(5) 2_667 ? C5 O4 1.250(5) . ? C5 O3 1.257(5) . ? C6 O6 1.242(5) 2_666 ? C6 O5 1.258(5) . ? C6 C6 1.552(8) 2_666 ? C7 O8 1.246(6) 2_777 ? C7 O7 1.252(5) . ? C7 C7 1.554(9) 2_777 ? K1 O7 2.713(3) 1_545 ? K1 O8 2.864(4) . ? K1 O6 2.930(3) . ? K1 O9 2.972(4) 1_545 ? K1 O2 3.059(3) 2_667 ? K1 O1 3.079(4) 2_667 ? K1 O2 3.082(4) . ? K1 O3 3.092(4) 1_545 ? K1 O1 3.415(5) . ? K1 C4 3.427(5) 2_667 ? K1 K1 3.784(2) 2_667 ? K1 Dy1 4.0738(12) 1_545 ? O1 K1 3.079(4) 2_667 ? O2 Dy1 2.356(3) . ? O2 K1 3.059(3) 2_667 ? O3 Dy1 2.382(3) . ? O3 K1 3.092(3) 1_565 ? O4 Dy1 2.350(3) 1_455 ? O5 Dy1 2.396(3) . ? O6 C6 1.242(5) 2_666 ? O6 Dy1 2.424(3) . ? O7 Dy1 2.336(3) . ? O7 K1 2.713(3) 1_565 ? O8 C7 1.246(6) 2_777 ? O8 Dy1 2.383(3) . ? O9 Dy1 2.359(3) . ? O9 K1 2.972(4) 1_565 ? Dy1 O4 2.350(3) 1_655 ? Dy1 K1 4.0738(12) 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 C3 C1 C2 118.7(4) 2_566 . ? C3 C1 C4 118.6(4) 2_566 . ? C2 C1 C4 122.7(4) . . ? C3 C2 C1 119.9(4) . . ? C3 C2 C5 118.3(4) . . ? C1 C2 C5 121.8(4) . . ? C2 C3 C1 121.4(4) . 2_566 ? O1 C4 O2 123.1(4) . . ? O1 C4 C1 118.2(4) . . ? O2 C4 C1 118.7(4) . . ? O1 C4 K1 63.5(2) . 2_667 ? O2 C4 K1 62.6(2) . 2_667 ? C1 C4 K1 162.6(3) . 2_667 ? O4 C5 O3 124.6(4) . . ? O4 C5 C2 117.1(4) . . ? O3 C5 C2 118.1(4) . . ? O6 C6 O5 126.8(4) 2_666 . ? O6 C6 C6 117.1(5) 2_666 2_666 ? O5 C6 C6 116.0(5) . 2_666 ? O8 C7 O7 127.4(4) 2_777 . ? O8 C7 C7 116.4(5) 2_777 2_777 ? O7 C7 C7 116.3(5) . 2_777 ? O7 K1 O8 126.95(11) 1_545 . ? O7 K1 O6 121.97(10) 1_545 . ? O8 K1 O6 57.98(9) . . ? O7 K1 O9 57.47(10) 1_545 1_545 ? O8 K1 O9 106.00(10) . 1_545 ? O6 K1 O9 65.88(10) . 1_545 ? O7 K1 O2 78.59(10) 1_545 2_667 ? O8 K1 O2 109.43(10) . 2_667 ? O6 K1 O2 159.32(10) . 2_667 ? O9 K1 O2 134.64(10) 1_545 2_667 ? O7 K1 O1 90.13(11) 1_545 2_667 ? O8 K1 O1 70.18(10) . 2_667 ? O6 K1 O1 128.10(10) . 2_667 ? O9 K1 O1 137.58(13) 1_545 2_667 ? O2 K1 O1 42.17(9) 2_667 2_667 ? O7 K1 O2 173.79(11) 1_545 . ? O8 K1 O2 57.87(9) . . ? O6 K1 O2 55.87(9) . . ? O9 K1 O2 118.72(10) 1_545 . ? O2 K1 O2 103.94(8) 2_667 . ? O1 K1 O2 95.52(11) 2_667 . ? O7 K1 O3 63.97(10) 1_545 1_545 ? O8 K1 O3 150.49(10) . 1_545 ? O6 K1 O3 92.63(10) . 1_545 ? O9 K1 O3 53.46(9) 1_545 1_545 ? O2 K1 O3 99.43(10) 2_667 1_545 ? O1 K1 O3 139.26(10) 2_667 1_545 ? O2 K1 O3 109.88(9) . 1_545 ? O7 K1 O1 135.90(11) 1_545 . ? O8 K1 O1 97.11(10) . . ? O6 K1 O1 77.01(9) . . ? O9 K1 O1 113.43(11) 1_545 . ? O2 K1 O1 89.42(9) 2_667 . ? O1 K1 O1 108.93(9) 2_667 . ? O2 K1 O1 39.32(8) . . ? O3 K1 O1 76.73(9) 1_545 . ? O7 K1 C4 80.47(10) 1_545 2_667 ? O8 K1 C4 90.96(11) . 2_667 ? O6 K1 C4 148.26(11) . 2_667 ? O9 K1 C4 136.85(11) 1_545 2_667 ? O2 K1 C4 21.58(9) 2_667 2_667 ? O1 K1 C4 21.21(10) 2_667 2_667 ? O2 K1 C4 104.00(10) . 2_667 ? O3 K1 C4 118.54(11) 1_545 2_667 ? O1 K1 C4 103.06(10) . 2_667 ? O7 K1 K1 130.53(9) 1_545 2_667 ? O8 K1 K1 80.55(8) . 2_667 ? O6 K1 K1 107.42(8) . 2_667 ? O9 K1 K1 163.64(10) 1_545 2_667 ? O2 K1 K1 52.24(7) 2_667 2_667 ? O1 K1 K1 58.60(9) 2_667 2_667 ? O2 K1 K1 51.70(6) . 2_667 ? O3 K1 K1 114.17(8) 1_545 2_667 ? O1 K1 K1 50.33(7) . 2_667 ? C4 K1 K1 56.31(8) 2_667 2_667 ? O7 K1 Dy1 33.19(7) 1_545 1_545 ? O8 K1 Dy1 137.63(8) . 1_545 ? O6 K1 Dy1 98.61(7) . 1_545 ? O9 K1 Dy1 34.89(7) 1_545 1_545 ? O2 K1 Dy1 100.98(7) 2_667 1_545 ? O1 K1 Dy1 122.99(9) 2_667 1_545 ? O2 K1 Dy1 140.83(7) . 1_545 ? O3 K1 Dy1 35.61(6) 1_545 1_545 ? O1 K1 Dy1 112.29(8) . 1_545 ? C4 K1 Dy1 110.14(8) 2_667 1_545 ? K1 K1 Dy1 141.76(6) 2_667 1_545 ? C4 O1 K1 95.3(3) . 2_667 ? C4 O1 K1 79.6(3) . . ? K1 O1 K1 71.07(9) 2_667 . ? C4 O2 Dy1 126.5(3) . . ? C4 O2 K1 95.8(3) . 2_667 ? Dy1 O2 K1 137.70(13) . 2_667 ? C4 O2 K1 94.2(3) . . ? Dy1 O2 K1 100.24(11) . . ? K1 O2 K1 76.06(8) 2_667 . ? C5 O3 Dy1 127.2(3) . . ? C5 O3 K1 137.2(3) . 1_565 ? Dy1 O3 K1 95.30(10) . 1_565 ? C5 O4 Dy1 147.9(3) . 1_455 ? C6 O5 Dy1 120.3(3) . . ? C6 O6 Dy1 119.2(3) 2_666 . ? C6 O6 K1 134.9(3) 2_666 . ? Dy1 O6 K1 102.90(10) . . ? C7 O7 Dy1 116.4(3) . . ? C7 O7 K1 133.8(3) . 1_565 ? Dy1 O7 K1 107.34(12) . 1_565 ? C7 O8 Dy1 115.0(3) 2_777 . ? C7 O8 K1 135.8(3) 2_777 . ? Dy1 O8 K1 105.96(12) . . ? Dy1 O9 K1 99.02(12) . 1_565 ? O7 Dy1 O4 84.85(11) . 1_655 ? O7 Dy1 O2 95.23(11) . . ? O4 Dy1 O2 144.76(12) 1_655 . ? O7 Dy1 O9 71.46(12) . . ? O4 Dy1 O9 71.45(13) 1_655 . ? O2 Dy1 O9 141.77(13) . . ? O7 Dy1 O3 81.86(11) . . ? O4 Dy1 O3 141.72(12) 1_655 . ? O2 Dy1 O3 72.43(12) . . ? O9 Dy1 O3 70.30(12) . . ? O7 Dy1 O8 68.67(11) . . ? O4 Dy1 O8 72.33(12) 1_655 . ? O2 Dy1 O8 74.94(12) . . ? O9 Dy1 O8 127.53(13) . . ? O3 Dy1 O8 133.21(12) . . ? O7 Dy1 O5 149.67(11) . . ? O4 Dy1 O5 85.78(11) 1_655 . ? O2 Dy1 O5 108.80(11) . . ? O9 Dy1 O5 78.21(12) . . ? O3 Dy1 O5 87.91(11) . . ? O8 Dy1 O5 134.57(11) . . ? O7 Dy1 O6 140.12(11) . . ? O4 Dy1 O6 85.18(11) 1_655 . ? O2 Dy1 O6 72.29(11) . . ? O9 Dy1 O6 139.56(12) . . ? O3 Dy1 O6 126.43(11) . . ? O8 Dy1 O6 71.51(11) . . ? O5 Dy1 O6 67.30(10) . . ? O7 Dy1 K1 39.47(8) . 1_565 ? O4 Dy1 K1 100.92(8) 1_655 1_565 ? O2 Dy1 K1 101.19(9) . 1_565 ? O9 Dy1 K1 46.10(9) . 1_565 ? O3 Dy1 K1 49.09(8) . 1_565 ? O8 Dy1 K1 107.86(8) . 1_565 ? O5 Dy1 K1 115.24(7) . 1_565 ? O6 Dy1 K1 173.44(8) . 1_565 ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.200 _refine_diff_density_min -1.294 _refine_diff_density_rms 0.181 data_9 _database_code_depnum_ccdc_archive 'CCDC 715648' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C25 H18 Ce2 K O17' _chemical_formula_sum 'C25 H18 Ce2 K O17' _chemical_formula_weight 909.73 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' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 '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 10.4541(7) _cell_length_b 11.7756(8) _cell_length_c 12.3649(9) _cell_angle_alpha 93.8060(10) _cell_angle_beta 112.6500(10) _cell_angle_gamma 98.5580(10) _cell_volume 1376.30(17) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6809 _cell_measurement_theta_min 1.77 _cell_measurement_theta_max 28.32 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 2.195 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 878 _exptl_absorpt_coefficient_mu 3.502 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3610 _exptl_absorpt_correction_T_max 0.5910 _exptl_absorpt_process_details SADABS _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 'Siemens Smart CCD' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 9.00cm _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 10149 _diffrn_reflns_av_R_equivalents 0.0680 _diffrn_reflns_av_sigmaI/netI 0.0469 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 28.32 _reflns_number_total 6809 _reflns_number_gt 6081 _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 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0698P)^2^+0.9064P] 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 6809 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0400 _refine_ls_R_factor_gt 0.0348 _refine_ls_wR_factor_ref 0.1072 _refine_ls_wR_factor_gt 0.0970 _refine_ls_goodness_of_fit_ref 1.108 _refine_ls_restrained_S_all 1.108 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.4637(4) 0.6879(3) 0.4085(3) 0.0172(7) Uani 1 1 d . . . C2 C 0.5361(4) 0.8063(3) 0.4086(3) 0.0203(7) Uani 1 1 d . . . C3 C 0.5367(4) 0.8410(3) 0.3028(3) 0.0207(8) Uani 1 1 d . . . H3 H 0.4945 0.7889 0.2335 0.025 Uiso 1 1 calc R . . C4 C 0.5994(5) 0.9518(3) 0.3006(4) 0.0224(8) Uani 1 1 d . . . C5 C 0.6683(6) 1.0280(4) 0.4059(4) 0.0367(12) Uani 1 1 d . . . H5 H 0.7113 1.1027 0.4049 0.044 Uiso 1 1 calc R . . C6 C 0.6729(7) 0.9931(5) 0.5112(4) 0.0456(15) Uani 1 1 d . . . H6 H 0.7217 1.0433 0.5814 0.055 Uiso 1 1 calc R . . C7 C 0.6052(6) 0.8835(4) 0.5126(4) 0.0340(11) Uani 1 1 d . . . H7 H 0.6058 0.8612 0.5835 0.041 Uiso 1 1 calc R . . C8 C 0.5918(4) 0.9903(3) 0.1852(3) 0.0181(7) Uani 1 1 d . . . C9 C 0.8860(4) 0.7766(3) 1.0988(3) 0.0180(7) Uani 1 1 d . . . C10 C 0.9628(4) 0.8974(3) 1.1570(3) 0.0186(7) Uani 1 1 d . . . C11 C 1.0760(4) 0.9508(3) 1.1331(3) 0.0186(7) Uani 1 1 d . . . H11 H 1.1090 0.9094 1.0859 0.022 Uiso 1 1 calc R . . C12 C 1.1398(4) 1.0663(3) 1.1799(3) 0.0193(7) Uani 1 1 d . . . C13 C 1.0917(5) 1.1261(4) 1.2532(4) 0.0282(9) Uani 1 1 d . . . H13 H 1.1330 1.2031 1.2841 0.034 Uiso 1 1 calc R . . C14 C 0.9827(5) 1.0719(4) 1.2803(5) 0.0349(11) Uani 1 1 d . . . H14 H 0.9526 1.1121 1.3306 0.042 Uiso 1 1 calc R . . C15 C 0.9189(5) 0.9585(4) 1.2328(4) 0.0282(9) Uani 1 1 d . . . H15 H 0.8460 0.9225 1.2514 0.034 Uiso 1 1 calc R . . C16 C 1.2598(4) 1.1222(3) 1.1508(3) 0.0176(7) Uani 1 1 d . . . C17 C 0.2793(4) 0.6668(3) 0.7110(3) 0.0155(7) Uani 1 1 d . . . C18 C 0.1525(4) 0.6598(3) 0.5998(3) 0.0154(7) Uani 1 1 d . . . C19 C 0.0180(4) 0.6332(3) 0.6006(3) 0.0154(7) Uani 1 1 d . . . H19 H 0.0087 0.6205 0.6709 0.018 Uiso 1 1 calc R . . C20 C -0.1016(4) 0.6257(3) 0.4974(3) 0.0174(7) Uani 1 1 d . . . C21 C -0.0873(4) 0.6482(4) 0.3924(4) 0.0235(8) Uani 1 1 d . . . H21 H -0.1673 0.6431 0.3230 0.028 Uiso 1 1 calc R . . C22 C 0.0449(4) 0.6778(4) 0.3915(4) 0.0259(9) Uani 1 1 d . . . H22 H 0.0541 0.6955 0.3224 0.031 Uiso 1 1 calc R . . C23 C 0.1643(4) 0.6810(4) 0.4941(4) 0.0208(8) Uani 1 1 d . . . H23 H 0.2532 0.6976 0.4922 0.025 Uiso 1 1 calc R . . C24 C -0.2434(4) 0.5866(3) 0.5000(3) 0.0159(7) Uani 1 1 d . . . C25 C 0.5252(4) 0.4808(3) 0.9507(3) 0.0134(6) Uani 1 1 d . . . Ce1 Ce 0.578686(19) 0.575448(16) 0.688348(16) 0.01174(8) Uani 1 1 d . . . Ce2 Ce 0.52108(2) 0.771246(16) 0.939807(16) 0.01344(8) Uani 1 1 d . . . K1 K 0.79029(10) 0.33869(9) 0.90276(9) 0.0297(2) Uani 1 1 d . . . O1 O 0.4816(3) 0.6515(3) 0.5051(3) 0.0251(6) Uani 1 1 d . . . O2 O 0.3859(3) 0.6274(2) 0.3089(3) 0.0214(6) Uani 1 1 d . . . O3 O 0.5619(4) 0.9124(3) 0.1002(3) 0.0261(6) Uani 1 1 d . . . O4 O 0.6158(3) 1.0964(2) 0.1800(3) 0.0247(6) Uani 1 1 d . . . O5 O 0.7574(3) 0.7493(3) 1.0794(3) 0.0248(6) Uani 1 1 d . . . O6 O 0.9555(3) 0.7077(3) 1.0723(3) 0.0301(7) Uani 1 1 d . . . O7 O 1.3134(3) 1.2298(2) 1.1893(3) 0.0239(6) Uani 1 1 d . . . O8 O 1.3026(3) 1.0665(3) 1.0873(3) 0.0264(6) Uani 1 1 d . . . O9 O 0.2668(3) 0.6574(3) 0.8073(2) 0.0210(6) Uani 1 1 d . . . O10 O 0.4020(3) 0.6872(2) 0.7087(2) 0.0181(5) Uani 1 1 d . . . O11 O -0.2512(3) 0.5897(3) 0.5987(3) 0.0224(6) Uani 1 1 d . . . O12 O -0.3460(3) 0.5498(2) 0.4013(3) 0.0203(6) Uani 1 1 d . . . O13 O 0.5444(3) 0.5572(2) 0.8889(2) 0.0171(5) Uani 1 1 d . . . O14 O 0.4572(3) 0.6213(2) 1.0581(2) 0.0190(5) Uani 1 1 d . . . O1W O 0.8191(3) 0.5682(3) 0.8539(3) 0.0241(6) Uani 1 1 d . . . O2W O 0.9174(4) 0.4749(3) 1.1205(3) 0.0334(7) Uani 1 1 d . . . O3W O 0.7331(5) 0.1723(3) 1.0186(3) 0.0427(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0157(16) 0.0199(18) 0.0180(17) 0.0026(14) 0.0088(14) 0.0038(14) C2 0.025(2) 0.0183(18) 0.0141(17) -0.0004(14) 0.0063(15) 0.0003(15) C3 0.026(2) 0.0174(18) 0.0134(16) -0.0024(13) 0.0055(15) -0.0018(15) C4 0.029(2) 0.0185(18) 0.0201(18) -0.0009(15) 0.0119(16) 0.0011(15) C5 0.055(3) 0.020(2) 0.023(2) -0.0045(17) 0.010(2) -0.012(2) C6 0.070(4) 0.032(3) 0.019(2) -0.0063(18) 0.012(2) -0.018(3) C7 0.053(3) 0.027(2) 0.0148(19) -0.0011(16) 0.0102(19) -0.003(2) C8 0.0194(17) 0.0171(17) 0.0185(17) 0.0008(14) 0.0081(14) 0.0043(14) C9 0.0148(16) 0.0182(17) 0.0175(17) 0.0021(13) 0.0043(14) -0.0012(13) C10 0.0130(16) 0.0177(17) 0.0226(18) 0.0003(14) 0.0062(14) -0.0010(13) C11 0.0171(17) 0.0174(18) 0.0179(17) -0.0021(13) 0.0067(14) -0.0039(14) C12 0.0152(17) 0.0188(18) 0.0195(17) -0.0026(14) 0.0064(14) -0.0056(14) C13 0.025(2) 0.0193(19) 0.037(2) -0.0089(17) 0.0144(18) -0.0062(16) C14 0.032(2) 0.030(2) 0.046(3) -0.015(2) 0.026(2) -0.0057(19) C15 0.022(2) 0.028(2) 0.037(2) -0.0058(18) 0.0194(19) -0.0046(16) C16 0.0123(16) 0.0174(17) 0.0173(17) 0.0011(13) 0.0025(13) -0.0042(13) C17 0.0111(15) 0.0130(16) 0.0186(17) -0.0035(13) 0.0033(13) 0.0005(12) C18 0.0117(16) 0.0158(16) 0.0152(16) -0.0034(13) 0.0037(13) -0.0009(13) C19 0.0108(15) 0.0185(17) 0.0155(16) -0.0018(13) 0.0062(13) -0.0022(13) C20 0.0116(16) 0.0206(18) 0.0168(17) -0.0006(14) 0.0053(14) -0.0038(13) C21 0.0134(17) 0.035(2) 0.0157(17) 0.0018(15) 0.0018(14) -0.0026(15) C22 0.0203(19) 0.040(2) 0.0172(18) 0.0040(16) 0.0095(16) -0.0005(17) C23 0.0144(17) 0.027(2) 0.0209(18) -0.0007(15) 0.0095(15) -0.0015(14) C24 0.0113(16) 0.0172(17) 0.0181(17) -0.0027(13) 0.0062(13) 0.0007(13) C25 0.0114(15) 0.0147(16) 0.0124(15) -0.0001(12) 0.0045(12) -0.0016(12) Ce1 0.00940(11) 0.01318(12) 0.01065(11) -0.00133(7) 0.00369(8) -0.00157(7) Ce2 0.01429(12) 0.01108(11) 0.01282(12) -0.00076(7) 0.00508(8) -0.00200(8) K1 0.0240(4) 0.0331(5) 0.0301(5) 0.0069(4) 0.0082(4) 0.0058(4) O1 0.0250(15) 0.0346(17) 0.0204(14) 0.0122(12) 0.0119(12) 0.0085(12) O2 0.0249(14) 0.0163(13) 0.0195(13) -0.0007(10) 0.0071(11) -0.0002(11) O3 0.0389(18) 0.0218(14) 0.0182(14) -0.0016(11) 0.0130(13) 0.0046(13) O4 0.0323(16) 0.0164(13) 0.0248(15) 0.0042(11) 0.0106(13) 0.0046(12) O5 0.0126(13) 0.0245(15) 0.0281(15) -0.0006(12) 0.0026(11) -0.0068(11) O6 0.0225(15) 0.0237(15) 0.0409(19) -0.0081(13) 0.0125(14) 0.0002(12) O7 0.0205(14) 0.0170(14) 0.0268(15) -0.0029(11) 0.0066(12) -0.0084(11) O8 0.0270(16) 0.0209(14) 0.0350(17) -0.0020(12) 0.0204(14) -0.0044(12) O9 0.0153(13) 0.0288(15) 0.0161(13) 0.0006(11) 0.0055(10) -0.0013(11) O10 0.0122(12) 0.0213(13) 0.0189(13) -0.0009(10) 0.0062(10) -0.0009(10) O11 0.0145(13) 0.0329(16) 0.0198(14) -0.0004(12) 0.0094(11) -0.0006(11) O12 0.0134(13) 0.0217(14) 0.0203(13) -0.0054(11) 0.0048(10) -0.0042(10) O13 0.0211(13) 0.0153(12) 0.0164(12) 0.0020(10) 0.0103(11) 0.0001(10) O14 0.0248(14) 0.0138(12) 0.0222(13) 0.0015(10) 0.0142(11) 0.0024(10) O1W 0.0177(14) 0.0289(15) 0.0197(14) -0.0041(11) 0.0028(11) 0.0028(11) O2W 0.0266(17) 0.0389(19) 0.0361(18) 0.0053(15) 0.0146(14) 0.0042(14) O3W 0.061(3) 0.0313(19) 0.040(2) 0.0025(15) 0.0294(19) -0.0045(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.251(5) . ? C1 O2 1.275(5) . ? C1 C2 1.484(5) . ? C2 C7 1.391(6) . ? C2 C3 1.398(5) . ? C3 C4 1.378(5) . ? C4 C5 1.396(6) . ? C4 C8 1.503(5) . ? C5 C6 1.376(7) . ? C6 C7 1.381(7) . ? C8 O4 1.249(5) . ? C8 O3 1.256(5) . ? C9 O5 1.257(5) . ? C9 O6 1.272(5) . ? C9 C10 1.506(5) . ? C10 C15 1.395(6) . ? C10 C11 1.398(5) . ? C11 C12 1.398(5) . ? C12 C13 1.394(6) . ? C12 C16 1.507(5) . ? C13 C14 1.388(6) . ? C14 C15 1.379(6) . ? C16 O8 1.239(5) . ? C16 O7 1.284(5) . ? C16 Ce2 3.064(4) 2_777 ? C17 O9 1.257(5) . ? C17 O10 1.282(4) . ? C17 C18 1.484(5) . ? C18 C23 1.395(5) . ? C18 C19 1.398(5) . ? C19 C20 1.387(5) . ? C20 C21 1.401(5) . ? C20 C24 1.498(5) . ? C21 C22 1.378(6) . ? C22 C23 1.388(6) . ? C24 O11 1.252(5) . ? C24 O12 1.269(4) . ? C25 O14 1.247(4) 2_667 ? C25 O13 1.262(4) . ? C25 C25 1.569(7) 2_667 ? Ce1 O1 2.395(3) . ? Ce1 O11 2.424(3) 1_655 ? Ce1 O12 2.441(3) 2_566 ? Ce1 O2 2.472(3) 2_666 ? Ce1 O10 2.499(3) . ? Ce1 O7 2.505(3) 2_777 ? Ce1 O1W 2.577(3) . ? Ce1 O13 2.656(3) . ? Ce2 O3 2.362(3) 1_556 ? Ce2 O4 2.451(3) 2_676 ? Ce2 O5 2.472(3) . ? Ce2 O14 2.540(3) . ? Ce2 O8 2.583(3) 2_777 ? Ce2 O9 2.616(3) . ? Ce2 O13 2.626(3) . ? Ce2 O10 2.686(3) . ? Ce2 O7 2.771(3) 2_777 ? Ce2 C16 3.064(4) 2_777 ? Ce2 K1 4.4746(11) 2_667 ? K1 O3W 2.632(4) . ? K1 O2 2.655(3) 2_666 ? K1 O6 2.698(3) 2_767 ? K1 O2W 2.761(4) . ? K1 O1W 2.806(3) . ? K1 O14 2.906(3) 2_667 ? K1 Ce2 4.4746(10) 2_667 ? K1 K1 5.015(2) 2_767 ? O2 Ce1 2.472(3) 2_666 ? O2 K1 2.655(3) 2_666 ? O3 Ce2 2.362(3) 1_554 ? O4 Ce2 2.451(3) 2_676 ? O6 K1 2.698(3) 2_767 ? O7 Ce1 2.505(3) 2_777 ? O7 Ce2 2.771(3) 2_777 ? O8 Ce2 2.583(3) 2_777 ? O11 Ce1 2.424(3) 1_455 ? O12 Ce1 2.441(3) 2_566 ? O14 C25 1.247(4) 2_667 ? O14 K1 2.906(3) 2_667 ? 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 C1 O2 122.8(4) . . ? O1 C1 C2 119.1(4) . . ? O2 C1 C2 118.0(3) . . ? C7 C2 C3 119.1(4) . . ? C7 C2 C1 121.2(4) . . ? C3 C2 C1 119.7(3) . . ? C4 C3 C2 120.4(4) . . ? C3 C4 C5 119.5(4) . . ? C3 C4 C8 119.9(3) . . ? C5 C4 C8 120.5(4) . . ? C6 C5 C4 120.4(4) . . ? C5 C6 C7 120.0(4) . . ? C6 C7 C2 120.4(4) . . ? O4 C8 O3 124.4(4) . . ? O4 C8 C4 118.4(3) . . ? O3 C8 C4 117.1(3) . . ? O5 C9 O6 123.7(4) . . ? O5 C9 C10 118.5(4) . . ? O6 C9 C10 117.8(3) . . ? C15 C10 C11 119.3(4) . . ? C15 C10 C9 120.1(3) . . ? C11 C10 C9 120.5(3) . . ? C10 C11 C12 120.3(4) . . ? C13 C12 C11 119.1(4) . . ? C13 C12 C16 121.7(3) . . ? C11 C12 C16 119.1(3) . . ? C14 C13 C12 120.6(4) . . ? C15 C14 C13 120.1(4) . . ? C14 C15 C10 120.5(4) . . ? O8 C16 O7 120.6(4) . . ? O8 C16 C12 120.6(3) . . ? O7 C16 C12 118.8(3) . . ? O8 C16 Ce2 56.0(2) . 2_777 ? O7 C16 Ce2 64.7(2) . 2_777 ? C12 C16 Ce2 173.1(3) . 2_777 ? O9 C17 O10 120.2(3) . . ? O9 C17 C18 120.4(3) . . ? O10 C17 C18 119.3(3) . . ? C23 C18 C19 118.9(3) . . ? C23 C18 C17 121.4(3) . . ? C19 C18 C17 119.7(3) . . ? C20 C19 C18 120.5(3) . . ? C19 C20 C21 119.6(3) . . ? C19 C20 C24 118.7(3) . . ? C21 C20 C24 121.6(3) . . ? C22 C21 C20 120.3(4) . . ? C21 C22 C23 119.9(4) . . ? C22 C23 C18 120.8(4) . . ? O11 C24 O12 125.1(3) . . ? O11 C24 C20 118.0(3) . . ? O12 C24 C20 116.9(3) . . ? O14 C25 O13 126.8(3) 2_667 . ? O14 C25 C25 117.1(4) 2_667 2_667 ? O13 C25 C25 116.1(4) . 2_667 ? O1 Ce1 O11 71.35(10) . 1_655 ? O1 Ce1 O12 79.67(10) . 2_566 ? O11 Ce1 O12 123.55(10) 1_655 2_566 ? O1 Ce1 O2 120.75(10) . 2_666 ? O11 Ce1 O2 82.31(10) 1_655 2_666 ? O12 Ce1 O2 72.46(10) 2_566 2_666 ? O1 Ce1 O10 74.51(10) . . ? O11 Ce1 O10 138.15(10) 1_655 . ? O12 Ce1 O10 71.72(9) 2_566 . ? O2 Ce1 O10 137.09(9) 2_666 . ? O1 Ce1 O7 94.71(11) . 2_777 ? O11 Ce1 O7 93.05(11) 1_655 2_777 ? O12 Ce1 O7 137.52(10) 2_566 2_777 ? O2 Ce1 O7 139.82(10) 2_666 2_777 ? O10 Ce1 O7 66.26(9) . 2_777 ? O1 Ce1 O1W 140.41(10) . . ? O11 Ce1 O1W 73.37(10) 1_655 . ? O12 Ce1 O1W 136.34(10) 2_566 . ? O2 Ce1 O1W 70.72(10) 2_666 . ? O10 Ce1 O1W 125.30(9) . . ? O7 Ce1 O1W 69.73(10) 2_777 . ? O1 Ce1 O13 141.17(9) . . ? O11 Ce1 O13 144.66(9) 1_655 . ? O12 Ce1 O13 83.97(9) 2_566 . ? O2 Ce1 O13 86.57(9) 2_666 . ? O10 Ce1 O13 66.94(9) . . ? O7 Ce1 O13 74.41(9) 2_777 . ? O1W Ce1 O13 71.29(9) . . ? O3 Ce2 O4 84.13(10) 1_556 2_676 ? O3 Ce2 O5 78.87(11) 1_556 . ? O4 Ce2 O5 145.02(10) 2_676 . ? O3 Ce2 O14 87.14(10) 1_556 . ? O4 Ce2 O14 130.99(10) 2_676 . ? O5 Ce2 O14 78.67(10) . . ? O3 Ce2 O8 79.11(10) 1_556 2_777 ? O4 Ce2 O8 72.50(11) 2_676 2_777 ? O5 Ce2 O8 74.38(10) . 2_777 ? O14 Ce2 O8 151.60(10) . 2_777 ? O3 Ce2 O9 121.34(10) 1_556 . ? O4 Ce2 O9 70.97(10) 2_676 . ? O5 Ce2 O9 143.62(10) . . ? O14 Ce2 O9 73.12(9) . . ? O8 Ce2 O9 135.16(10) 2_777 . ? O3 Ce2 O13 142.43(10) 1_556 . ? O4 Ce2 O13 132.24(9) 2_676 . ? O5 Ce2 O13 73.75(9) . . ? O14 Ce2 O13 62.79(8) . . ? O8 Ce2 O13 116.51(9) 2_777 . ? O9 Ce2 O13 73.14(9) . . ? O3 Ce2 O10 152.13(10) 1_556 . ? O4 Ce2 O10 68.03(9) 2_676 . ? O5 Ce2 O10 125.17(9) . . ? O14 Ce2 O10 109.71(9) . . ? O8 Ce2 O10 93.24(9) 2_777 . ? O9 Ce2 O10 49.05(8) . . ? O13 Ce2 O10 64.77(8) . . ? O3 Ce2 O7 125.04(10) 1_556 2_777 ? O4 Ce2 O7 92.23(10) 2_676 2_777 ? O5 Ce2 O7 73.58(10) . 2_777 ? O14 Ce2 O7 130.70(9) . 2_777 ? O8 Ce2 O7 48.18(9) 2_777 2_777 ? O9 Ce2 O7 108.62(9) . 2_777 ? O13 Ce2 O7 70.65(8) . 2_777 ? O10 Ce2 O7 60.13(8) . 2_777 ? O3 Ce2 C16 101.25(11) 1_556 2_777 ? O4 Ce2 C16 82.34(10) 2_676 2_777 ? O5 Ce2 C16 71.46(10) . 2_777 ? O14 Ce2 C16 146.54(10) . 2_777 ? O8 Ce2 C16 23.43(10) 2_777 2_777 ? O9 Ce2 C16 125.45(9) . 2_777 ? O13 Ce2 C16 93.97(9) . 2_777 ? O10 Ce2 C16 77.17(9) . 2_777 ? O7 Ce2 C16 24.78(9) 2_777 2_777 ? O3 Ce2 K1 71.65(8) 1_556 2_667 ? O4 Ce2 K1 94.58(8) 2_676 2_667 ? O5 Ce2 K1 108.46(8) . 2_667 ? O14 Ce2 K1 37.51(6) . 2_667 ? O8 Ce2 K1 149.16(7) 2_777 2_667 ? O9 Ce2 K1 59.10(6) . 2_667 ? O13 Ce2 K1 93.09(6) . 2_667 ? O10 Ce2 K1 108.02(6) . 2_667 ? O7 Ce2 K1 162.63(6) 2_777 2_667 ? C16 Ce2 K1 172.58(7) 2_777 2_667 ? O3W K1 O2 123.89(12) . 2_666 ? O3W K1 O6 95.27(13) . 2_767 ? O2 K1 O6 118.64(11) 2_666 2_767 ? O3W K1 O2W 85.80(12) . . ? O2 K1 O2W 133.40(10) 2_666 . ? O6 K1 O2W 89.15(10) 2_767 . ? O3W K1 O1W 154.25(11) . . ? O2 K1 O1W 64.65(9) 2_666 . ? O6 K1 O1W 100.65(10) 2_767 . ? O2W K1 O1W 74.42(10) . . ? O3W K1 O14 73.61(11) . 2_667 ? O2 K1 O14 76.70(9) 2_666 2_667 ? O6 K1 O14 164.63(10) 2_767 2_667 ? O2W K1 O14 79.63(9) . 2_667 ? O1W K1 O14 86.52(9) . 2_667 ? O3W K1 Ce2 41.49(10) . 2_667 ? O2 K1 Ce2 99.47(7) 2_666 2_667 ? O6 K1 Ce2 135.46(8) 2_767 2_667 ? O2W K1 Ce2 79.39(7) . 2_667 ? O1W K1 Ce2 116.86(7) . 2_667 ? O14 K1 Ce2 32.16(5) 2_667 2_667 ? O3W K1 K1 121.60(10) . 2_767 ? O2 K1 K1 113.70(7) 2_666 2_767 ? O6 K1 K1 62.72(7) 2_767 2_767 ? O2W K1 K1 44.45(7) . 2_767 ? O1W K1 K1 52.00(6) . 2_767 ? O14 K1 K1 113.68(7) 2_667 2_767 ? Ce2 K1 K1 123.49(3) 2_667 2_767 ? C1 O1 Ce1 163.7(3) . . ? C1 O2 Ce1 110.5(2) . 2_666 ? C1 O2 K1 137.7(2) . 2_666 ? Ce1 O2 K1 111.64(10) 2_666 2_666 ? C8 O3 Ce2 176.0(3) . 1_554 ? C8 O4 Ce2 134.1(3) . 2_676 ? C9 O5 Ce2 141.5(3) . . ? C9 O6 K1 147.9(3) . 2_767 ? C16 O7 Ce1 166.0(3) . 2_777 ? C16 O7 Ce2 90.5(2) . 2_777 ? Ce1 O7 Ce2 99.53(9) 2_777 2_777 ? C16 O8 Ce2 100.6(2) . 2_777 ? C17 O9 Ce2 95.1(2) . . ? C17 O10 Ce1 138.3(2) . . ? C17 O10 Ce2 91.3(2) . . ? Ce1 O10 Ce2 102.01(9) . . ? C24 O11 Ce1 141.6(2) . 1_455 ? C24 O12 Ce1 142.4(3) . 2_566 ? C25 O13 Ce2 120.2(2) . . ? C25 O13 Ce1 139.9(2) . . ? Ce2 O13 Ce1 99.49(9) . . ? C25 O14 Ce2 123.3(2) 2_667 . ? C25 O14 K1 117.5(2) 2_667 2_667 ? Ce2 O14 K1 110.33(10) . 2_667 ? Ce1 O1W K1 103.94(10) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 2.080 _refine_diff_density_min -2.218 _refine_diff_density_rms 0.245 data_10 _database_code_depnum_ccdc_archive 'CCDC 715649' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C25 H18 K O17 Pr2' _chemical_formula_sum 'C25 H18 K O17 Pr2' _chemical_formula_weight 911.31 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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pr Pr -0.2180 2.8214 '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 10.3647(7) _cell_length_b 11.5338(8) _cell_length_c 12.2664(8) _cell_angle_alpha 82.0820(10) _cell_angle_beta 65.0190(10) _cell_angle_gamma 84.3190(10) _cell_volume 1315.16(15) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6512 _cell_measurement_theta_min 1.78 _cell_measurement_theta_max 28.29 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 2.301 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 882 _exptl_absorpt_coefficient_mu 3.908 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4130 _exptl_absorpt_correction_T_max 0.6770 _exptl_absorpt_process_details SADABS _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 'Siemens Smart CCD' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 9.00cm _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 9690 _diffrn_reflns_av_R_equivalents 0.0367 _diffrn_reflns_av_sigmaI/netI 0.0300 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 28.29 _reflns_number_total 6512 _reflns_number_gt 5876 _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 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0416P)^2^+7.4554P] 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 6512 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0344 _refine_ls_R_factor_gt 0.0302 _refine_ls_wR_factor_ref 0.0907 _refine_ls_wR_factor_gt 0.0878 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.090 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3975(5) 0.6265(4) 0.3449(4) 0.0167(8) Uani 1 1 d . . . C2 C 0.5405(5) 0.5670(4) 0.3177(4) 0.0174(8) Uani 1 1 d . . . C3 C 0.6651(5) 0.6254(4) 0.2484(5) 0.0248(10) Uani 1 1 d . . . H3 H 0.6606 0.7038 0.2192 0.030 Uiso 1 1 calc R . . C4 C 0.7975(6) 0.5658(5) 0.2226(5) 0.0310(11) Uani 1 1 d . . . H4 H 0.8810 0.6036 0.1732 0.037 Uiso 1 1 calc R . . C5 C 0.8043(5) 0.4504(4) 0.2705(5) 0.0244(10) Uani 1 1 d . . . H5 H 0.8925 0.4116 0.2538 0.029 Uiso 1 1 calc R . . C6 C 0.6803(5) 0.3921(4) 0.3436(4) 0.0180(8) Uani 1 1 d . . . C7 C 0.6869(5) 0.2697(4) 0.4029(4) 0.0188(8) Uani 1 1 d . . . C8 C 0.5483(5) 0.4500(4) 0.3647(4) 0.0186(8) Uani 1 1 d . . . H8 H 0.4650 0.4105 0.4104 0.022 Uiso 1 1 calc R . . C9 C 0.0829(5) 0.4887(4) 0.3169(4) 0.0171(8) Uani 1 1 d . . . C10 C 0.1952(5) 0.4504(4) 0.2026(4) 0.0196(8) Uani 1 1 d . . . C11 C 0.2348(6) 0.5229(4) 0.0938(5) 0.0294(11) Uani 1 1 d . . . H11 H 0.1909 0.5971 0.0924 0.035 Uiso 1 1 calc R . . C12 C 0.3379(7) 0.4858(5) -0.0110(5) 0.0339(12) Uani 1 1 d . . . H12 H 0.3601 0.5335 -0.0835 0.041 Uiso 1 1 calc R . . C13 C 0.4097(6) 0.3771(4) -0.0099(4) 0.0282(11) Uani 1 1 d . . . H13 H 0.4813 0.3531 -0.0808 0.034 Uiso 1 1 calc R . . C14 C 0.3729(5) 0.3048(4) 0.0987(4) 0.0182(8) Uani 1 1 d . . . C15 C 0.2642(5) 0.3407(4) 0.2045(4) 0.0189(8) Uani 1 1 d . . . H15 H 0.2377 0.2913 0.2763 0.023 Uiso 1 1 calc R . . C16 C 0.4449(4) 0.1875(4) 0.1042(4) 0.0156(8) Uani 1 1 d . . . C17 C 0.0782(4) 0.8288(3) 0.2091(4) 0.0140(7) Uani 1 1 d . . . C18 C 0.0567(4) 0.8366(4) 0.0951(4) 0.0154(8) Uani 1 1 d . . . C19 C 0.1710(5) 0.8180(4) -0.0143(4) 0.0183(8) Uani 1 1 d . . . H19 H 0.2618 0.8009 -0.0170 0.022 Uiso 1 1 calc R . . C20 C 0.1498(5) 0.8249(5) -0.1194(4) 0.0242(9) Uani 1 1 d . . . H20 H 0.2260 0.8096 -0.1917 0.029 Uiso 1 1 calc R . . C21 C 0.0160(5) 0.8545(4) -0.1174(4) 0.0212(9) Uani 1 1 d . . . H21 H 0.0027 0.8616 -0.1885 0.025 Uiso 1 1 calc R . . C22 C -0.0996(4) 0.8738(4) -0.0071(4) 0.0150(8) Uani 1 1 d . . . C23 C -0.2428(4) 0.9156(4) -0.0041(4) 0.0155(8) Uani 1 1 d . . . C24 C -0.0789(4) 0.8636(4) 0.0976(4) 0.0150(8) Uani 1 1 d . . . H24 H -0.1559 0.8748 0.1707 0.018 Uiso 1 1 calc R . . C25 C -0.0726(4) 0.9777(4) 0.5503(4) 0.0136(7) Uani 1 1 d . . . K1 K 0.3734(2) 1.15344(19) 0.41305(19) 0.0687(5) Uani 1 1 d . . . O1 O 0.2875(4) 0.5708(3) 0.4051(3) 0.0245(7) Uani 1 1 d . . . O2 O 0.3882(4) 0.7352(3) 0.3077(3) 0.0220(7) Uani 1 1 d . . . O3 O 0.7964(4) 0.2376(3) 0.4217(3) 0.0250(7) Uani 1 1 d . . . O4 O 0.5854(4) 0.2055(3) 0.4307(4) 0.0297(8) Uani 1 1 d . . . O5 O 0.0514(4) 0.5959(3) 0.3237(3) 0.0211(6) Uani 1 1 d . . . O6 O 0.0240(4) 0.4100(3) 0.4012(3) 0.0258(7) Uani 1 1 d . . . O7 O 0.2017(3) 0.8070(3) 0.2057(3) 0.0163(6) Uani 1 1 d . . . O8 O -0.0276(3) 0.8391(3) 0.3080(3) 0.0194(6) Uani 1 1 d . . . O9 O 0.4232(4) 0.1325(3) 0.2072(3) 0.0199(6) Uani 1 1 d . . . O10 O 0.5220(3) 0.1429(3) 0.0077(3) 0.0222(7) Uani 1 1 d . . . O11 O -0.2483(3) 0.9536(3) -0.1028(3) 0.0186(6) Uani 1 1 d . . . O12 O -0.3467(3) 0.9109(3) 0.0989(3) 0.0222(7) Uani 1 1 d . . . O13 O -0.0911(4) 0.8710(3) 0.5648(3) 0.0219(7) Uani 1 1 d . . . O14 O -0.1617(3) 1.0552(3) 0.6073(3) 0.0164(6) Uani 1 1 d . . . O15 O 0.4732(4) 0.9469(3) 0.3587(3) 0.0220(7) Uani 1 1 d . . . O16 O 0.2786(4) 1.0352(3) 0.6058(3) 0.0308(8) Uani 1 1 d . . . O17 O 0.2262(5) 1.3166(4) 0.5066(4) 0.0356(9) Uani 1 1 d . . . Pr1 Pr 0.39826(2) 0.927130(18) 0.186756(19) 0.01171(7) Uani 1 1 d . . . Pr2 Pr 0.09399(2) 0.730313(18) 0.440322(19) 0.01398(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 C1 0.022(2) 0.0140(18) 0.0154(19) -0.0029(15) -0.0102(16) 0.0045(16) C2 0.021(2) 0.0147(19) 0.0168(19) -0.0012(15) -0.0087(16) 0.0020(16) C3 0.029(2) 0.015(2) 0.030(2) 0.0052(18) -0.015(2) -0.0013(18) C4 0.023(2) 0.025(2) 0.042(3) 0.010(2) -0.013(2) -0.0052(19) C5 0.019(2) 0.022(2) 0.031(2) 0.0015(19) -0.0121(19) 0.0038(17) C6 0.024(2) 0.0131(19) 0.0178(19) -0.0012(15) -0.0105(17) 0.0013(16) C7 0.026(2) 0.0142(19) 0.017(2) -0.0040(15) -0.0103(17) 0.0051(16) C8 0.021(2) 0.0143(19) 0.018(2) 0.0009(15) -0.0076(17) 0.0012(16) C9 0.0184(19) 0.0136(18) 0.020(2) -0.0014(15) -0.0090(17) 0.0002(15) C10 0.024(2) 0.0148(19) 0.016(2) -0.0031(16) -0.0044(17) 0.0005(16) C11 0.042(3) 0.016(2) 0.024(2) 0.0020(18) -0.011(2) 0.006(2) C12 0.052(3) 0.023(2) 0.015(2) 0.0033(18) -0.007(2) 0.004(2) C13 0.039(3) 0.022(2) 0.014(2) 0.0000(17) -0.004(2) 0.001(2) C14 0.024(2) 0.0137(19) 0.0145(19) -0.0027(15) -0.0059(17) 0.0001(16) C15 0.023(2) 0.0146(19) 0.0152(19) -0.0006(15) -0.0046(17) 0.0000(16) C16 0.0147(18) 0.0135(18) 0.0175(19) -0.0039(15) -0.0048(15) -0.0010(14) C17 0.0175(19) 0.0105(17) 0.0145(18) 0.0006(14) -0.0077(15) -0.0012(14) C18 0.0167(19) 0.0145(18) 0.0150(19) -0.0004(15) -0.0072(16) 0.0006(15) C19 0.0147(19) 0.020(2) 0.020(2) -0.0031(16) -0.0072(16) 0.0032(16) C20 0.019(2) 0.035(3) 0.015(2) -0.0061(18) -0.0030(17) 0.0046(18) C21 0.021(2) 0.028(2) 0.0140(19) -0.0033(17) -0.0077(17) 0.0029(18) C22 0.0140(18) 0.0140(18) 0.0176(19) -0.0004(15) -0.0082(16) 0.0023(14) C23 0.0150(18) 0.0118(18) 0.019(2) -0.0003(15) -0.0072(16) -0.0001(14) C24 0.0145(18) 0.0146(18) 0.0143(18) 0.0003(15) -0.0052(15) 0.0004(14) C25 0.0149(18) 0.0132(18) 0.0118(18) -0.0027(14) -0.0044(15) -0.0001(14) K1 0.0799(13) 0.0642(12) 0.0619(11) -0.0078(9) -0.0300(10) 0.0013(10) O1 0.0198(16) 0.0184(16) 0.0308(18) -0.0004(13) -0.0079(14) 0.0040(12) O2 0.0299(17) 0.0131(14) 0.0237(16) 0.0010(12) -0.0139(14) 0.0055(12) O3 0.0317(18) 0.0222(16) 0.0243(17) -0.0029(13) -0.0167(15) 0.0088(14) O4 0.038(2) 0.0195(16) 0.036(2) 0.0055(15) -0.0207(17) -0.0054(15) O5 0.0279(17) 0.0130(14) 0.0220(16) -0.0055(12) -0.0092(13) 0.0014(12) O6 0.0319(18) 0.0172(15) 0.0181(16) 0.0021(12) -0.0012(14) -0.0034(13) O7 0.0162(14) 0.0178(14) 0.0162(14) 0.0002(11) -0.0085(12) -0.0015(11) O8 0.0174(14) 0.0231(16) 0.0157(14) -0.0006(12) -0.0062(12) 0.0036(12) O9 0.0271(16) 0.0139(14) 0.0183(15) -0.0014(12) -0.0097(13) 0.0017(12) O10 0.0181(15) 0.0269(17) 0.0206(16) -0.0120(13) -0.0051(13) 0.0031(13) O11 0.0182(14) 0.0198(15) 0.0187(15) 0.0033(12) -0.0100(12) -0.0010(12) O12 0.0153(14) 0.0300(18) 0.0196(16) -0.0016(13) -0.0066(12) 0.0017(13) O13 0.0236(16) 0.0119(14) 0.0215(16) -0.0020(12) -0.0008(13) -0.0020(12) O14 0.0178(14) 0.0128(13) 0.0159(14) -0.0042(11) -0.0042(12) 0.0029(11) O15 0.0245(16) 0.0241(16) 0.0181(15) -0.0005(13) -0.0103(13) 0.0002(13) O16 0.0296(19) 0.0304(19) 0.0279(19) -0.0043(15) -0.0092(15) 0.0076(15) O17 0.041(2) 0.028(2) 0.030(2) -0.0058(16) -0.0076(17) 0.0032(17) Pr1 0.01254(11) 0.01090(11) 0.01081(11) -0.00048(7) -0.00454(8) 0.00117(7) Pr2 0.01862(12) 0.00864(11) 0.01229(11) -0.00099(8) -0.00478(9) 0.00237(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.249(6) . ? C1 O2 1.282(5) . ? C1 C2 1.492(6) . ? C2 C3 1.390(7) . ? C2 C8 1.402(6) . ? C3 C4 1.401(7) . ? C4 C5 1.387(7) . ? C5 C6 1.392(7) . ? C6 C8 1.397(6) . ? C6 C7 1.505(6) . ? C7 O4 1.247(6) . ? C7 O3 1.262(6) . ? C9 O5 1.252(5) . ? C9 O6 1.259(5) . ? C9 C10 1.485(6) . ? C10 C15 1.392(6) . ? C10 C11 1.395(6) . ? C11 C12 1.371(7) . ? C12 C13 1.395(7) . ? C13 C14 1.393(6) . ? C14 C15 1.395(6) . ? C14 C16 1.486(6) . ? C16 O10 1.262(5) . ? C16 O9 1.272(5) . ? C16 Pr1 3.052(4) 1_545 ? C16 K1 3.512(5) 1_545 ? C17 O8 1.257(5) . ? C17 O7 1.264(5) . ? C17 C18 1.496(6) . ? C18 C19 1.392(6) . ? C18 C24 1.398(6) . ? C19 C20 1.386(6) . ? C20 C21 1.387(7) . ? C21 C22 1.406(6) . ? C22 C24 1.376(6) . ? C22 C23 1.502(6) . ? C23 O11 1.251(5) . ? C23 O12 1.266(5) . ? C25 O13 1.240(5) . ? C25 O14 1.267(5) . ? C25 C25 1.569(8) 2_576 ? C25 K1 3.431(5) 2_576 ? K1 O17 2.395(4) . ? K1 O9 2.397(4) 1_565 ? K1 O16 2.414(4) . ? K1 O4 2.436(4) 1_565 ? K1 O15 2.561(4) . ? K1 O13 2.861(4) 2_576 ? K1 C25 3.431(5) 2_576 ? K1 C16 3.512(5) 1_565 ? K1 Pr2 4.530(2) 2_576 ? K1 K1 4.978(4) 2_676 ? O1 Pr2 2.520(3) . ? O2 Pr1 2.474(3) . ? O2 Pr2 2.787(4) . ? O3 Pr2 2.484(3) 2_666 ? O4 K1 2.436(4) 1_545 ? O5 Pr2 2.434(3) . ? O6 Pr2 2.326(3) 2_566 ? O7 Pr1 2.489(3) . ? O7 Pr2 2.663(3) . ? O8 Pr2 2.579(3) . ? O9 K1 2.397(4) 1_545 ? O9 Pr1 2.465(3) 1_545 ? O10 Pr1 2.400(3) 2_665 ? O11 Pr1 2.431(3) 2_575 ? O12 Pr1 2.395(3) 1_455 ? O13 Pr2 2.498(3) . ? O13 K1 2.861(4) 2_576 ? O14 Pr2 2.560(3) 2_576 ? O14 Pr1 2.692(3) 2_576 ? O15 Pr1 2.580(3) . ? Pr1 O12 2.395(3) 1_655 ? Pr1 O10 2.400(3) 2_665 ? Pr1 O11 2.431(3) 2_575 ? Pr1 O9 2.465(3) 1_565 ? Pr1 O14 2.692(3) 2_576 ? Pr1 C16 3.052(4) 1_565 ? Pr2 O6 2.326(3) 2_566 ? Pr2 O3 2.484(4) 2_666 ? Pr2 O14 2.560(3) 2_576 ? Pr2 K1 4.530(2) 2_576 ? 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 C1 O2 120.4(4) . . ? O1 C1 C2 119.9(4) . . ? O2 C1 C2 119.7(4) . . ? C3 C2 C8 119.7(4) . . ? C3 C2 C1 121.5(4) . . ? C8 C2 C1 118.8(4) . . ? C2 C3 C4 119.8(4) . . ? C5 C4 C3 120.0(5) . . ? C4 C5 C6 120.7(4) . . ? C5 C6 C8 119.1(4) . . ? C5 C6 C7 120.9(4) . . ? C8 C6 C7 119.9(4) . . ? O4 C7 O3 123.4(4) . . ? O4 C7 C6 119.0(4) . . ? O3 C7 C6 117.6(4) . . ? C6 C8 C2 120.5(4) . . ? O5 C9 O6 124.0(4) . . ? O5 C9 C10 118.8(4) . . ? O6 C9 C10 117.2(4) . . ? C15 C10 C11 119.3(4) . . ? C15 C10 C9 119.3(4) . . ? C11 C10 C9 121.3(4) . . ? C12 C11 C10 120.6(5) . . ? C11 C12 C13 120.6(5) . . ? C14 C13 C12 119.3(5) . . ? C13 C14 C15 120.1(4) . . ? C13 C14 C16 121.2(4) . . ? C15 C14 C16 118.6(4) . . ? C10 C15 C14 120.1(4) . . ? O10 C16 O9 121.3(4) . . ? O10 C16 C14 119.9(4) . . ? O9 C16 C14 118.8(4) . . ? O10 C16 Pr1 78.8(3) . 1_545 ? O9 C16 Pr1 51.3(2) . 1_545 ? C14 C16 Pr1 144.7(3) . 1_545 ? O10 C16 K1 140.6(3) . 1_545 ? O9 C16 K1 23.27(19) . 1_545 ? C14 C16 K1 98.4(3) . 1_545 ? Pr1 C16 K1 74.28(10) 1_545 1_545 ? O8 C17 O7 120.6(4) . . ? O8 C17 C18 119.6(4) . . ? O7 C17 C18 119.7(4) . . ? C19 C18 C24 119.3(4) . . ? C19 C18 C17 120.6(4) . . ? C24 C18 C17 120.0(4) . . ? C20 C19 C18 120.2(4) . . ? C19 C20 C21 120.5(4) . . ? C20 C21 C22 119.4(4) . . ? C24 C22 C21 119.9(4) . . ? C24 C22 C23 119.5(4) . . ? C21 C22 C23 120.4(4) . . ? O11 C23 O12 126.1(4) . . ? O11 C23 C22 117.4(4) . . ? O12 C23 C22 116.5(4) . . ? C22 C24 C18 120.6(4) . . ? O13 C25 O14 126.1(4) . . ? O13 C25 C25 117.6(4) . 2_576 ? O14 C25 C25 116.3(4) . 2_576 ? O13 C25 K1 53.0(2) . 2_576 ? O14 C25 K1 83.2(2) . 2_576 ? C25 C25 K1 141.5(3) 2_576 2_576 ? O17 K1 O9 119.49(16) . 1_565 ? O17 K1 O16 89.34(15) . . ? O9 K1 O16 137.05(16) 1_565 . ? O17 K1 O4 95.68(16) . 1_565 ? O9 K1 O4 110.98(15) 1_565 1_565 ? O16 K1 O4 95.47(15) . 1_565 ? O17 K1 O15 163.95(16) . . ? O9 K1 O15 68.51(12) 1_565 . ? O16 K1 O15 76.84(13) . . ? O4 K1 O15 93.75(14) 1_565 . ? O17 K1 O13 71.51(14) . 2_576 ? O9 K1 O13 79.96(12) 1_565 2_576 ? O16 K1 O13 80.45(13) . 2_576 ? O4 K1 O13 166.49(15) 1_565 2_576 ? O15 K1 O13 97.81(12) . 2_576 ? O17 K1 C25 88.96(14) . 2_576 ? O9 K1 C25 79.13(12) 1_565 2_576 ? O16 K1 C25 69.67(13) . 2_576 ? O4 K1 C25 164.44(14) 1_565 2_576 ? O15 K1 C25 78.70(12) . 2_576 ? O13 K1 C25 20.25(10) 2_576 2_576 ? O17 K1 C16 109.31(14) . 1_565 ? O9 K1 C16 12.10(10) 1_565 1_565 ? O16 K1 C16 148.24(15) . 1_565 ? O4 K1 C16 107.51(14) 1_565 1_565 ? O15 K1 C16 80.00(11) . 1_565 ? O13 K1 C16 81.50(11) 2_576 1_565 ? C25 K1 C16 84.76(11) 2_576 1_565 ? O17 K1 Pr2 42.14(11) . 2_576 ? O9 K1 Pr2 101.43(10) 1_565 2_576 ? O16 K1 Pr2 78.28(10) . 2_576 ? O4 K1 Pr2 136.71(12) 1_565 2_576 ? O15 K1 Pr2 125.22(11) . 2_576 ? O13 K1 Pr2 29.92(7) 2_576 2_576 ? C25 K1 Pr2 46.91(7) 2_576 2_576 ? C16 K1 Pr2 98.16(8) 1_565 2_576 ? O17 K1 K1 127.78(14) . 2_676 ? O9 K1 K1 112.64(11) 1_565 2_676 ? O16 K1 K1 51.60(10) . 2_676 ? O4 K1 K1 61.54(10) 1_565 2_676 ? O15 K1 K1 47.78(8) . 2_676 ? O13 K1 K1 122.72(11) 2_576 2_676 ? C25 K1 K1 104.05(10) 2_576 2_676 ? C16 K1 K1 121.97(10) 1_565 2_676 ? Pr2 K1 K1 129.79(7) 2_576 2_676 ? C1 O1 Pr2 102.1(3) . . ? C1 O2 Pr1 166.0(3) . . ? C1 O2 Pr2 88.5(3) . . ? Pr1 O2 Pr2 98.65(11) . . ? C7 O3 Pr2 139.7(3) . 2_666 ? C7 O4 K1 152.0(3) . 1_545 ? C9 O5 Pr2 130.4(3) . . ? C9 O6 Pr2 177.5(3) . 2_566 ? C17 O7 Pr1 135.2(3) . . ? C17 O7 Pr2 91.2(2) . . ? Pr1 O7 Pr2 101.64(10) . . ? C17 O8 Pr2 95.3(2) . . ? C16 O9 K1 144.6(3) . 1_545 ? C16 O9 Pr1 105.0(3) . 1_545 ? K1 O9 Pr1 109.90(13) 1_545 1_545 ? C16 O10 Pr1 161.8(3) . 2_665 ? C23 O11 Pr1 141.8(3) . 2_575 ? C23 O12 Pr1 139.8(3) . 1_455 ? C25 O13 Pr2 122.0(3) . . ? C25 O13 K1 106.7(3) . 2_576 ? Pr2 O13 K1 115.24(13) . 2_576 ? C25 O14 Pr2 119.4(3) . 2_576 ? C25 O14 Pr1 139.6(3) . 2_576 ? Pr2 O14 Pr1 99.01(10) 2_576 2_576 ? K1 O15 Pr1 101.46(12) . . ? O12 Pr1 O10 71.51(11) 1_655 2_665 ? O12 Pr1 O11 126.80(11) 1_655 2_575 ? O10 Pr1 O11 78.46(11) 2_665 2_575 ? O12 Pr1 O9 86.23(12) 1_655 1_565 ? O10 Pr1 O9 121.64(11) 2_665 1_565 ? O11 Pr1 O9 73.48(11) 2_575 1_565 ? O12 Pr1 O2 90.42(12) 1_655 . ? O10 Pr1 O2 97.99(12) 2_665 . ? O11 Pr1 O2 137.28(11) 2_575 . ? O9 Pr1 O2 136.43(11) 1_565 . ? O12 Pr1 O7 136.36(11) 1_655 . ? O10 Pr1 O7 75.51(11) 2_665 . ? O11 Pr1 O7 71.40(10) 2_575 . ? O9 Pr1 O7 136.16(11) 1_565 . ? O2 Pr1 O7 66.60(11) . . ? O12 Pr1 O15 74.08(11) 1_655 . ? O10 Pr1 O15 143.44(11) 2_665 . ? O11 Pr1 O15 133.94(11) 2_575 . ? O9 Pr1 O15 67.20(11) 1_565 . ? O2 Pr1 O15 70.13(11) . . ? O7 Pr1 O15 125.12(10) . . ? O12 Pr1 O14 145.33(10) 1_655 2_576 ? O10 Pr1 O14 140.72(10) 2_665 2_576 ? O11 Pr1 O14 81.38(10) 2_575 2_576 ? O9 Pr1 O14 83.42(10) 1_565 2_576 ? O2 Pr1 O14 75.10(10) . 2_576 ? O7 Pr1 O14 66.20(10) . 2_576 ? O15 Pr1 O14 71.40(10) . 2_576 ? O12 Pr1 C16 83.62(12) 1_655 1_565 ? O10 Pr1 C16 98.78(12) 2_665 1_565 ? O11 Pr1 C16 58.60(11) 2_575 1_565 ? O9 Pr1 C16 23.74(11) 1_565 1_565 ? O2 Pr1 C16 159.38(11) . 1_565 ? O7 Pr1 C16 129.64(11) . 1_565 ? O15 Pr1 C16 89.25(11) . 1_565 ? O14 Pr1 C16 98.90(10) 2_576 1_565 ? O6 Pr2 O5 81.80(12) 2_566 . ? O6 Pr2 O3 81.50(13) 2_566 2_666 ? O5 Pr2 O3 147.92(11) . 2_666 ? O6 Pr2 O13 84.78(11) 2_566 . ? O5 Pr2 O13 124.02(12) . . ? O3 Pr2 O13 81.32(12) 2_666 . ? O6 Pr2 O1 79.60(12) 2_566 . ? O5 Pr2 O1 74.12(12) . . ? O3 Pr2 O1 76.05(12) 2_666 . ? O13 Pr2 O1 154.09(12) . . ? O6 Pr2 O14 142.73(11) 2_566 2_576 ? O5 Pr2 O14 132.43(11) . 2_576 ? O3 Pr2 O14 73.58(11) 2_666 2_576 ? O13 Pr2 O14 64.66(10) . 2_576 ? O1 Pr2 O14 119.22(11) . 2_576 ? O6 Pr2 O8 121.03(12) 2_566 . ? O5 Pr2 O8 69.13(11) . . ? O3 Pr2 O8 142.60(11) 2_666 . ? O13 Pr2 O8 72.49(11) . . ? O1 Pr2 O8 133.40(11) . . ? O14 Pr2 O8 71.26(10) 2_576 . ? O6 Pr2 O7 150.57(11) 2_566 . ? O5 Pr2 O7 68.79(10) . . ? O3 Pr2 O7 123.58(11) 2_666 . ? O13 Pr2 O7 112.04(10) . . ? O1 Pr2 O7 91.17(11) . . ? O14 Pr2 O7 65.70(10) 2_576 . ? O8 Pr2 O7 49.36(9) . . ? O6 Pr2 O2 125.43(11) 2_566 . ? O5 Pr2 O2 96.61(11) . . ? O3 Pr2 O2 71.66(11) 2_666 . ? O13 Pr2 O2 133.93(10) . . ? O1 Pr2 O2 48.59(10) . . ? O14 Pr2 O2 72.14(9) 2_576 . ? O8 Pr2 O2 108.48(10) . . ? O7 Pr2 O2 59.95(9) . . ? O6 Pr2 K1 73.92(10) 2_566 2_576 ? O5 Pr2 K1 89.39(9) . 2_576 ? O3 Pr2 K1 111.82(9) 2_666 2_576 ? O13 Pr2 K1 34.85(9) . 2_576 ? O1 Pr2 K1 150.55(8) . 2_576 ? O14 Pr2 K1 89.97(7) 2_576 2_576 ? O8 Pr2 K1 56.35(7) . 2_576 ? O7 Pr2 K1 105.64(7) . 2_576 ? O2 Pr2 K1 160.31(7) . 2_576 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.049 _refine_diff_density_min -2.474 _refine_diff_density_rms 0.194