# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Wei Shi' _publ_contact_author_email SHIWEI@NANKAI.EDU.CN _publ_section_title ; Systematic investigation of the lanthanide coordination polymers with ?-pyrone-2,6-dicarboxylic acid ; loop_ _publ_author_name 'Wei Shi' 'Peng Cheng' 'Yi Li' 'Zheng Niu' 'Zhen-Jie Zhang' ; Shi-Yuan Zhang ; # Attachment 'Nd-1.cif' data_Nd-1 _database_code_depnum_ccdc_archive 'CCDC 716750' #TrackingRef 'Nd-1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H38 Nd2 O34' _chemical_formula_weight 1122.99 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' Nd Nd -0.1943 3.0179 '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' _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 7.641(2) _cell_length_b 13.150(4) _cell_length_c 18.236(5) _cell_angle_alpha 77.837(14) _cell_angle_beta 80.450(14) _cell_angle_gamma 80.031(15) _cell_volume 1748.1(8) _cell_formula_units_Z 2 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 8235 _cell_measurement_theta_min 1.6005 _cell_measurement_theta_max 27.8884 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.133 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1112 _exptl_absorpt_coefficient_mu 3.063 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7493 _exptl_absorpt_correction_T_max 0.9137 _exptl_absorpt_process_details Crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13579 _diffrn_reflns_av_R_equivalents 0.0337 _diffrn_reflns_av_sigmaI/netI 0.0607 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.15 _diffrn_reflns_theta_max 27.88 _reflns_number_total 8235 _reflns_number_gt 5686 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0580P)^2^+1.3536P] 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 8235 _refine_ls_number_parameters 514 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0691 _refine_ls_R_factor_gt 0.0459 _refine_ls_wR_factor_ref 0.1274 _refine_ls_wR_factor_gt 0.1073 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.083 _refine_ls_shift/su_max 0.006 _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 Nd1 Nd 0.30945(4) 0.23538(2) 0.291235(16) 0.00753(9) Uani 1 1 d . . . Nd2 Nd 0.29866(4) -0.26270(2) 0.289617(17) 0.00765(9) Uani 1 1 d . . . O1 O 0.2804(6) 0.0059(3) 0.5020(2) 0.0093(8) Uani 1 1 d . . . O2 O 0.3471(6) 0.0528(3) 0.3582(2) 0.0120(9) Uani 1 1 d . . . O3 O 0.2679(6) -0.0947(3) 0.3392(2) 0.0108(9) Uani 1 1 d . . . O4 O -0.0397(6) -0.2100(3) 0.6130(2) 0.0109(9) Uani 1 1 d . . . O5 O 0.3785(6) 0.1438(3) 0.5632(2) 0.0122(9) Uani 1 1 d . . . O6 O 0.2768(6) 0.0651(3) 0.6803(2) 0.0101(8) Uani 1 1 d . . . O7 O 0.2671(6) 0.5005(3) 0.5010(2) 0.0090(8) Uani 1 1 d . . . O8 O 0.2993(6) 0.5538(3) 0.3535(2) 0.0124(9) Uani 1 1 d . . . O9 O 0.2386(6) 0.3986(3) 0.3405(2) 0.0124(9) Uani 1 1 d . . . O10 O -0.0268(6) 0.2720(3) 0.6147(2) 0.0128(9) Uani 1 1 d . . . O11 O 0.2680(6) 0.5543(3) 0.6811(2) 0.0125(9) Uani 1 1 d . . . O12 O 0.3709(6) 0.6346(3) 0.5653(2) 0.0148(10) Uani 1 1 d . . . O13 O 0.2849(6) 0.4149(3) 0.0144(2) 0.0134(9) Uani 1 1 d . . . O14 O 0.2426(7) 0.6209(3) -0.0016(3) 0.0191(10) Uani 1 1 d . . . O15 O 0.1319(8) 0.6429(3) -0.1107(3) 0.0259(12) Uani 1 1 d . . . O16 O 0.1402(7) 0.2656(3) -0.1357(2) 0.0183(10) Uani 1 1 d . . . O17 O 0.4873(7) 0.1671(3) 0.0914(2) 0.0177(10) Uani 1 1 d . . . O18 O 0.3599(6) 0.3015(3) 0.1494(2) 0.0130(9) Uani 1 1 d . . . O19 O 0.4664(6) 0.2110(3) 0.4040(2) 0.0113(9) Uani 1 1 d . . . O20 O 0.5718(6) 0.3334(3) 0.2504(2) 0.0177(10) Uani 1 1 d . . . O21 O 0.0383(6) 0.3435(3) 0.2393(2) 0.0188(10) Uani 1 1 d . . . O22 O 0.1886(6) 0.1123(3) 0.2299(2) 0.0158(10) Uani 1 1 d . . . O23 O 0.5876(6) 0.1227(3) 0.2305(2) 0.0143(9) Uani 1 1 d . . . O24 O 0.5980(7) -0.2065(4) 0.2618(3) 0.0219(11) Uani 1 1 d . . . H24A H 0.6196 -0.1556 0.2793 0.033 Uiso 1 1 d R . . H24B H 0.6980 -0.2393 0.2455 0.033 Uiso 1 1 d R . . O25 O 0.0432(6) -0.1353(3) 0.2426(2) 0.0175(10) Uani 1 1 d . . . H25A H -0.0244 -0.0950 0.2697 0.026 Uiso 1 1 d R . . H25B H 0.0966 -0.0968 0.2052 0.026 Uiso 1 1 d R . . O26 O 0.3663(6) -0.1808(4) 0.1543(2) 0.0179(10) Uani 1 1 d . . . H26A H 0.4010 -0.2261 0.1259 0.027 Uiso 1 1 d R . . H26B H 0.4566 -0.1527 0.1569 0.027 Uiso 1 1 d R . . O27 O 0.5350(6) -0.3873(3) 0.2239(2) 0.0172(10) Uani 1 1 d . . . H27A H 0.5805 -0.4394 0.2545 0.026 Uiso 1 1 d R . . H27B H 0.5290 -0.4086 0.1836 0.026 Uiso 1 1 d R . . O28 O 0.1340(6) -0.3494(3) 0.2197(2) 0.0167(10) Uani 1 1 d . . . H28A H 0.0571 -0.3181 0.1906 0.025 Uiso 1 1 d R . . H28B H 0.1754 -0.4084 0.2070 0.025 Uiso 1 1 d R . . O29 O 0.4415(6) -0.2989(3) 0.4074(2) 0.0133(9) Uani 1 1 d . . . H29A H 0.5070 -0.2530 0.4076 0.020 Uiso 1 1 d R . . H29B H 0.4050 -0.3241 0.4532 0.020 Uiso 1 1 d R . . C1 C 0.2873(8) -0.0330(4) 0.3802(3) 0.0097(12) Uani 1 1 d . . . C2 C 0.2284(8) -0.0618(4) 0.4650(3) 0.0088(11) Uani 1 1 d . . . C3 C 0.1303(8) -0.1362(4) 0.4998(3) 0.0094(12) Uani 1 1 d . . . H3 H 0.1020 -0.1819 0.4724 0.011 Uiso 1 1 calc R . . C4 C 0.0671(8) -0.1472(4) 0.5797(3) 0.0087(11) Uani 1 1 d . . . C5 C 0.1323(8) -0.0774(4) 0.6176(3) 0.0076(11) Uani 1 1 d . . . H5 H 0.1049 -0.0826 0.6691 0.009 Uiso 1 1 calc R . . C6 C 0.2322(8) -0.0052(4) 0.5771(3) 0.0091(11) Uani 1 1 d . . . C7 C 0.3041(8) 0.0749(4) 0.6086(3) 0.0072(11) Uani 1 1 d . . . C8 C 0.2575(8) 0.4648(4) 0.3781(3) 0.0103(12) Uani 1 1 d . . . C9 C 0.2169(8) 0.4339(4) 0.4637(3) 0.0091(11) Uani 1 1 d . . . C10 C 0.1245(8) 0.3541(4) 0.5001(3) 0.0096(11) Uani 1 1 d . . . H10 H 0.0966 0.3080 0.4729 0.011 Uiso 1 1 calc R . . C11 C 0.0697(8) 0.3409(4) 0.5803(3) 0.0102(12) Uani 1 1 d . . . C12 C 0.1318(9) 0.4113(4) 0.6179(3) 0.0123(12) Uani 1 1 d . . . H12 H 0.1058 0.4050 0.6701 0.015 Uiso 1 1 calc R . . C13 C 0.2274(8) 0.4861(4) 0.5772(3) 0.0077(11) Uani 1 1 d . . . C14 C 0.2938(8) 0.5665(4) 0.6098(3) 0.0099(12) Uani 1 1 d . . . C15 C 0.1946(9) 0.5886(5) -0.0532(4) 0.0157(13) Uani 1 1 d . . . C16 C 0.2102(9) 0.4704(5) -0.0472(3) 0.0137(12) Uani 1 1 d . . . C17 C 0.1557(9) 0.4257(5) -0.0972(3) 0.0141(12) Uani 1 1 d . . . H17 H 0.0983 0.4677 -0.1365 0.017 Uiso 1 1 calc R . . C18 C 0.1856(9) 0.3113(5) -0.0906(4) 0.0160(13) Uani 1 1 d . . . C19 C 0.2730(9) 0.2567(5) -0.0263(3) 0.0134(12) Uani 1 1 d . . . H19 H 0.3008 0.1838 -0.0185 0.016 Uiso 1 1 calc R . . C20 C 0.3155(9) 0.3099(4) 0.0231(4) 0.0140(13) Uani 1 1 d . . . C21 C 0.3952(9) 0.2545(4) 0.0941(4) 0.0136(13) Uani 1 1 d . . . O30 O -0.0432(7) 0.9570(3) 0.0979(3) 0.0227(11) Uani 1 1 d . . . H30A H 0.0198 0.9026 0.0842 0.034 Uiso 1 1 d R . . H30B H 0.0262 1.0023 0.0945 0.034 Uiso 1 1 d R . . O31 O 0.9317(7) 0.1469(3) 0.1421(3) 0.0224(11) Uani 1 1 d . . . H31A H 0.8362 0.1579 0.1725 0.034 Uiso 1 1 d R . . H31B H 1.0167 0.1636 0.1598 0.034 Uiso 1 1 d R . . O32 O 0.2188(7) 0.8220(3) 0.0263(3) 0.0202(10) Uani 1 1 d . . . H32A H 0.3087 0.8495 0.0014 0.030 Uiso 1 1 d R . . H32B H 0.2110 0.7691 0.0078 0.030 Uiso 1 1 d R . . O33 O 0.3633(7) 0.5224(3) 0.1340(3) 0.0218(11) Uani 1 1 d . . . H33A H 0.3476 0.5513 0.0888 0.033 Uiso 1 1 d R . . H33B H 0.3707 0.4564 0.1375 0.033 Uiso 1 1 d R . . O34 O 0.5979(8) 0.9537(4) 0.0867(3) 0.0358(14) Uani 1 1 d . . . H34A H 0.5718 1.0128 0.1008 0.054 Uiso 1 1 d R . . H34B H 0.7104 0.9353 0.0856 0.054 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd1 0.00875(18) 0.00692(14) 0.00707(16) -0.00195(11) 0.00023(12) -0.00196(12) Nd2 0.00845(18) 0.00712(14) 0.00753(16) -0.00248(11) 0.00047(12) -0.00169(12) O1 0.009(2) 0.0106(18) 0.008(2) -0.0027(15) 0.0035(17) -0.0043(17) O2 0.018(2) 0.0067(18) 0.009(2) 0.0000(15) -0.0008(18) 0.0003(17) O3 0.018(2) 0.0087(18) 0.0065(19) -0.0049(15) 0.0026(17) -0.0029(18) O4 0.014(2) 0.0107(18) 0.008(2) -0.0046(16) 0.0056(17) -0.0037(17) O5 0.012(2) 0.014(2) 0.010(2) -0.0005(16) 0.0004(18) -0.0056(18) O6 0.011(2) 0.0108(18) 0.009(2) -0.0035(15) -0.0001(17) -0.0026(17) O7 0.009(2) 0.0078(17) 0.010(2) -0.0016(15) -0.0020(17) -0.0025(16) O8 0.015(2) 0.0116(19) 0.012(2) -0.0027(16) 0.0003(18) -0.0064(18) O9 0.016(2) 0.0129(19) 0.009(2) -0.0028(16) -0.0025(18) -0.0005(18) O10 0.011(2) 0.014(2) 0.015(2) -0.0046(17) 0.0021(18) -0.0085(18) O11 0.015(2) 0.015(2) 0.010(2) -0.0065(17) -0.0048(18) -0.0003(18) O12 0.021(3) 0.013(2) 0.011(2) -0.0031(17) 0.0005(19) -0.0067(19) O13 0.011(2) 0.0118(19) 0.016(2) -0.0008(17) -0.0065(18) 0.0040(18) O14 0.028(3) 0.013(2) 0.017(2) -0.0009(18) -0.008(2) -0.002(2) O15 0.043(4) 0.013(2) 0.023(3) -0.0056(19) -0.011(2) 0.000(2) O16 0.023(3) 0.018(2) 0.016(2) -0.0052(18) -0.004(2) -0.005(2) O17 0.023(3) 0.017(2) 0.012(2) -0.0058(17) -0.0036(19) 0.004(2) O18 0.017(2) 0.0137(19) 0.009(2) 0.0013(16) -0.0047(18) -0.0036(18) O19 0.011(2) 0.0126(19) 0.013(2) -0.0042(16) -0.0042(18) -0.0034(17) O20 0.016(3) 0.025(2) 0.017(2) -0.0112(19) 0.0030(19) -0.012(2) O21 0.017(3) 0.025(2) 0.014(2) -0.0045(19) -0.0046(19) 0.001(2) O22 0.020(3) 0.015(2) 0.015(2) -0.0027(17) -0.0038(19) -0.0061(19) O23 0.014(2) 0.0140(19) 0.011(2) -0.0011(16) 0.0043(18) 0.0015(18) O24 0.018(3) 0.029(2) 0.026(3) -0.018(2) 0.004(2) -0.013(2) O25 0.011(2) 0.022(2) 0.014(2) 0.0000(18) -0.0003(19) 0.0053(19) O26 0.014(2) 0.027(2) 0.011(2) 0.0004(18) 0.0015(19) -0.006(2) O27 0.018(3) 0.018(2) 0.015(2) -0.0035(18) -0.0013(19) -0.002(2) O28 0.020(3) 0.019(2) 0.013(2) -0.0063(18) -0.0063(19) -0.002(2) O29 0.016(2) 0.0118(19) 0.011(2) 0.0000(16) 0.0002(18) -0.0049(18) C1 0.013(3) 0.005(2) 0.009(3) 0.000(2) -0.001(2) 0.002(2) C2 0.009(3) 0.009(2) 0.009(3) -0.005(2) -0.002(2) 0.002(2) C3 0.015(3) 0.004(2) 0.009(3) -0.003(2) -0.002(2) 0.000(2) C4 0.009(3) 0.008(2) 0.007(3) -0.002(2) -0.001(2) 0.006(2) C5 0.004(3) 0.008(2) 0.009(3) -0.002(2) 0.002(2) 0.003(2) C6 0.006(3) 0.011(3) 0.009(3) -0.003(2) -0.001(2) 0.002(2) C7 0.002(3) 0.006(2) 0.012(3) -0.002(2) 0.000(2) 0.002(2) C8 0.012(3) 0.010(3) 0.008(3) -0.001(2) -0.004(2) 0.000(2) C9 0.007(3) 0.012(3) 0.010(3) -0.007(2) -0.001(2) -0.001(2) C10 0.007(3) 0.013(3) 0.012(3) -0.008(2) -0.003(2) 0.000(2) C11 0.008(3) 0.009(2) 0.015(3) -0.005(2) 0.002(2) -0.003(2) C12 0.013(3) 0.012(3) 0.016(3) -0.005(2) -0.005(3) -0.006(2) C13 0.009(3) 0.007(2) 0.008(3) -0.003(2) -0.005(2) -0.001(2) C14 0.006(3) 0.013(3) 0.014(3) -0.009(2) -0.001(2) -0.002(2) C15 0.019(4) 0.012(3) 0.015(3) -0.002(2) -0.004(3) 0.002(3) C16 0.010(3) 0.016(3) 0.014(3) -0.001(2) -0.001(2) -0.001(3) C17 0.010(3) 0.018(3) 0.014(3) -0.005(2) -0.003(2) 0.003(3) C18 0.008(3) 0.019(3) 0.022(3) -0.010(3) 0.003(3) -0.001(3) C19 0.013(3) 0.015(3) 0.011(3) -0.003(2) 0.004(2) -0.002(3) C20 0.017(3) 0.011(3) 0.013(3) -0.006(2) 0.004(3) -0.002(3) C21 0.014(3) 0.010(3) 0.016(3) -0.001(2) 0.000(3) -0.003(2) O30 0.025(3) 0.018(2) 0.025(3) -0.006(2) -0.004(2) 0.000(2) O31 0.020(3) 0.019(2) 0.031(3) -0.010(2) -0.013(2) 0.004(2) O32 0.020(3) 0.019(2) 0.022(2) -0.0072(19) 0.001(2) -0.003(2) O33 0.032(3) 0.017(2) 0.020(2) -0.0050(19) -0.010(2) -0.005(2) O34 0.026(3) 0.018(2) 0.060(4) -0.011(2) 0.009(3) -0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd1 O9 2.440(4) . ? Nd1 O2 2.445(4) . ? Nd1 O19 2.485(4) . ? Nd1 O4 2.491(4) 2_556 ? Nd1 O20 2.496(4) . ? Nd1 O21 2.505(5) . ? Nd1 O22 2.519(4) . ? Nd1 O18 2.537(4) . ? Nd1 O23 2.600(4) . ? Nd2 O8 2.447(4) 1_545 ? Nd2 O24 2.465(4) . ? Nd2 O28 2.480(4) . ? Nd2 O10 2.484(4) 2_556 ? Nd2 O26 2.483(4) . ? Nd2 O25 2.484(5) . ? Nd2 O29 2.490(4) . ? Nd2 O3 2.519(4) . ? Nd2 O27 2.543(5) . ? O1 C6 1.341(7) . ? O1 C2 1.368(6) . ? O2 C1 1.253(6) . ? O3 C1 1.254(7) . ? O4 C4 1.255(7) . ? O4 Nd1 2.491(4) 2_556 ? O5 C7 1.240(6) . ? O6 C7 1.271(7) . ? O7 C13 1.351(7) . ? O7 C9 1.354(6) . ? O8 C8 1.239(6) . ? O8 Nd2 2.447(4) 1_565 ? O9 C8 1.257(7) . ? O10 C11 1.264(6) . ? O10 Nd2 2.484(4) 2_556 ? O11 C14 1.263(7) . ? O12 C14 1.235(7) . ? O13 C20 1.340(7) . ? O13 C16 1.357(7) . ? O14 C15 1.240(7) . ? O15 C15 1.253(8) . ? O16 C18 1.237(7) . ? O17 C21 1.245(7) . ? O18 C21 1.259(7) . ? O24 H24A 0.8500 . ? O24 H24B 0.8500 . ? O25 H25A 0.8501 . ? O25 H25B 0.8500 . ? O26 H26A 0.8501 . ? O26 H26B 0.8499 . ? O27 H27A 0.8499 . ? O27 H27B 0.8500 . ? O28 H28A 0.8499 . ? O28 H28B 0.8499 . ? O29 H29A 0.8499 . ? O29 H29B 0.8500 . ? C1 C2 1.523(8) . ? C2 C3 1.326(7) . ? C3 C4 1.441(8) . ? C3 H3 0.9300 . ? C4 C5 1.446(7) . ? C5 C6 1.335(7) . ? C5 H5 0.9300 . ? C6 C7 1.518(7) . ? C8 C9 1.520(8) . ? C9 C10 1.359(8) . ? C10 C11 1.436(8) . ? C10 H10 0.9300 . ? C11 C12 1.441(7) . ? C12 C13 1.346(7) . ? C12 H12 0.9300 . ? C13 C14 1.510(7) . ? C15 C16 1.521(8) . ? C16 C17 1.336(8) . ? C17 C18 1.465(8) . ? C17 H17 0.9300 . ? C18 C19 1.441(9) . ? C19 C20 1.360(8) . ? C19 H19 0.9300 . ? C20 C21 1.513(9) . ? O30 H30A 0.8500 . ? O30 H30B 0.8500 . ? O31 H31A 0.8499 . ? O31 H31B 0.8500 . ? O32 H32A 0.8499 . ? O32 H32B 0.8503 . ? O33 H33A 0.8499 . ? O33 H33B 0.8499 . ? O34 H34A 0.8499 . ? O34 H34B 0.8500 . ? 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 O9 Nd1 O2 130.16(14) . . ? O9 Nd1 O19 72.25(14) . . ? O2 Nd1 O19 67.46(13) . . ? O9 Nd1 O4 75.76(13) . 2_556 ? O2 Nd1 O4 72.05(14) . 2_556 ? O19 Nd1 O4 83.95(14) . 2_556 ? O9 Nd1 O20 71.74(14) . . ? O2 Nd1 O20 120.71(16) . . ? O19 Nd1 O20 73.51(14) . . ? O4 Nd1 O20 144.72(13) 2_556 . ? O9 Nd1 O21 70.52(14) . . ? O2 Nd1 O21 129.00(14) . . ? O19 Nd1 O21 138.90(14) . . ? O4 Nd1 O21 70.65(14) 2_556 . ? O20 Nd1 O21 109.85(15) . . ? O9 Nd1 O22 144.72(16) . . ? O2 Nd1 O22 66.41(14) . . ? O19 Nd1 O22 133.84(13) . . ? O4 Nd1 O22 83.41(14) 2_556 . ? O20 Nd1 O22 131.67(14) . . ? O21 Nd1 O22 75.87(15) . . ? O9 Nd1 O18 102.31(13) . . ? O2 Nd1 O18 127.39(13) . . ? O19 Nd1 O18 139.71(14) . . ? O4 Nd1 O18 134.58(15) 2_556 . ? O20 Nd1 O18 67.13(14) . . ? O21 Nd1 O18 66.33(15) . . ? O22 Nd1 O18 72.85(13) . . ? O9 Nd1 O23 138.65(14) . . ? O2 Nd1 O23 67.67(13) . . ? O19 Nd1 O23 87.71(14) . . ? O4 Nd1 O23 138.97(13) 2_556 . ? O20 Nd1 O23 67.95(14) . . ? O21 Nd1 O23 132.47(14) . . ? O22 Nd1 O23 73.89(15) . . ? O18 Nd1 O23 70.16(14) . . ? O8 Nd2 O24 113.81(16) 1_545 . ? O8 Nd2 O28 71.69(14) 1_545 . ? O24 Nd2 O28 132.61(15) . . ? O8 Nd2 O10 72.12(14) 1_545 2_556 ? O24 Nd2 O10 143.48(14) . 2_556 ? O28 Nd2 O10 83.90(14) . 2_556 ? O8 Nd2 O26 132.01(14) 1_545 . ? O24 Nd2 O26 68.49(15) . . ? O28 Nd2 O26 74.54(14) . . ? O10 Nd2 O26 136.16(15) 2_556 . ? O8 Nd2 O25 128.28(14) 1_545 . ? O24 Nd2 O25 117.73(16) . . ? O28 Nd2 O25 70.99(15) . . ? O10 Nd2 O25 69.49(15) 2_556 . ? O26 Nd2 O25 67.54(15) . . ? O8 Nd2 O29 68.79(13) 1_545 . ? O24 Nd2 O29 69.88(15) . . ? O28 Nd2 O29 140.26(13) . . ? O10 Nd2 O29 80.39(14) 2_556 . ? O26 Nd2 O29 138.31(14) . . ? O25 Nd2 O29 134.02(14) . . ? O8 Nd2 O3 132.18(13) 1_545 . ? O24 Nd2 O3 73.66(15) . . ? O28 Nd2 O3 139.64(15) . . ? O10 Nd2 O3 76.92(13) 2_556 . ? O26 Nd2 O3 95.41(14) . . ? O25 Nd2 O3 69.10(14) . . ? O29 Nd2 O3 70.83(13) . . ? O8 Nd2 O27 67.64(14) 1_545 . ? O24 Nd2 O27 66.58(14) . . ? O28 Nd2 O27 74.17(15) . . ? O10 Nd2 O27 138.43(13) 2_556 . ? O26 Nd2 O27 71.03(15) . . ? O25 Nd2 O27 131.22(15) . . ? O29 Nd2 O27 94.31(15) . . ? O3 Nd2 O27 140.23(14) . . ? C6 O1 C2 118.2(4) . . ? C1 O2 Nd1 149.3(4) . . ? C1 O3 Nd2 159.2(4) . . ? C4 O4 Nd1 145.3(4) . 2_556 ? C13 O7 C9 119.0(4) . . ? C8 O8 Nd2 163.1(4) . 1_565 ? C8 O9 Nd1 156.6(4) . . ? C11 O10 Nd2 137.1(4) . 2_556 ? C20 O13 C16 118.2(5) . . ? C21 O18 Nd1 132.2(4) . . ? Nd2 O24 H24A 121.0 . . ? Nd2 O24 H24B 129.4 . . ? H24A O24 H24B 107.7 . . ? Nd2 O25 H25A 122.6 . . ? Nd2 O25 H25B 101.4 . . ? H25A O25 H25B 107.7 . . ? Nd2 O26 H26A 112.6 . . ? Nd2 O26 H26B 99.3 . . ? H26A O26 H26B 107.7 . . ? Nd2 O27 H27A 113.1 . . ? Nd2 O27 H27B 126.8 . . ? H27A O27 H27B 107.7 . . ? Nd2 O28 H28A 125.4 . . ? Nd2 O28 H28B 122.5 . . ? H28A O28 H28B 107.7 . . ? Nd2 O29 H29A 112.0 . . ? Nd2 O29 H29B 132.3 . . ? H29A O29 H29B 107.7 . . ? O3 C1 O2 126.5(5) . . ? O3 C1 C2 118.0(5) . . ? O2 C1 C2 115.5(5) . . ? C3 C2 O1 122.9(5) . . ? C3 C2 C1 126.7(5) . . ? O1 C2 C1 110.3(4) . . ? C2 C3 C4 120.8(5) . . ? C2 C3 H3 119.6 . . ? C4 C3 H3 119.6 . . ? O4 C4 C3 122.4(5) . . ? O4 C4 C5 123.4(5) . . ? C3 C4 C5 114.2(5) . . ? C6 C5 C4 120.6(5) . . ? C6 C5 H5 119.7 . . ? C4 C5 H5 119.7 . . ? O1 C6 C5 123.2(5) . . ? O1 C6 C7 110.9(4) . . ? C5 C6 C7 125.9(5) . . ? O5 C7 O6 126.7(5) . . ? O5 C7 C6 118.0(5) . . ? O6 C7 C6 115.3(4) . . ? O8 C8 O9 127.5(5) . . ? O8 C8 C9 116.2(5) . . ? O9 C8 C9 116.3(5) . . ? O7 C9 C10 122.2(5) . . ? O7 C9 C8 113.1(4) . . ? C10 C9 C8 124.4(5) . . ? C9 C10 C11 120.2(5) . . ? C9 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? O10 C11 C10 121.5(5) . . ? O10 C11 C12 123.1(5) . . ? C10 C11 C12 115.4(5) . . ? C13 C12 C11 120.0(6) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C12 C13 O7 123.0(5) . . ? C12 C13 C14 124.7(5) . . ? O7 C13 C14 112.2(4) . . ? O12 C14 O11 126.8(5) . . ? O12 C14 C13 117.9(5) . . ? O11 C14 C13 115.3(5) . . ? O14 C15 O15 127.2(6) . . ? O14 C15 C16 117.7(5) . . ? O15 C15 C16 115.1(5) . . ? C17 C16 O13 123.5(5) . . ? C17 C16 C15 123.5(6) . . ? O13 C16 C15 112.9(5) . . ? C16 C17 C18 120.6(6) . . ? C16 C17 H17 119.7 . . ? C18 C17 H17 119.7 . . ? O16 C18 C19 123.1(6) . . ? O16 C18 C17 123.5(6) . . ? C19 C18 C17 113.4(5) . . ? C20 C19 C18 121.1(6) . . ? C20 C19 H19 119.5 . . ? C18 C19 H19 119.5 . . ? O13 C20 C19 123.0(6) . . ? O13 C20 C21 114.6(5) . . ? C19 C20 C21 122.3(5) . . ? O17 C21 O18 127.3(6) . . ? O17 C21 C20 116.2(6) . . ? O18 C21 C20 116.4(6) . . ? H30A O30 H30B 107.7 . . ? H31A O31 H31B 107.7 . . ? H32A O32 H32B 107.7 . . ? H33A O33 H33B 107.7 . . ? H34A O34 H34B 107.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O9 Nd1 O2 C1 105.6(7) . . . . ? O19 Nd1 O2 C1 144.2(8) . . . . ? O4 Nd1 O2 C1 53.4(7) 2_556 . . . ? O20 Nd1 O2 C1 -163.0(7) . . . . ? O21 Nd1 O2 C1 8.6(8) . . . . ? O22 Nd1 O2 C1 -37.2(7) . . . . ? O18 Nd1 O2 C1 -79.6(8) . . . . ? O23 Nd1 O2 C1 -118.7(8) . . . . ? O8 Nd2 O3 C1 39.2(12) 1_545 . . . ? O24 Nd2 O3 C1 -68.4(11) . . . . ? O28 Nd2 O3 C1 153.5(11) . . . . ? O10 Nd2 O3 C1 89.7(11) 2_556 . . . ? O26 Nd2 O3 C1 -134.1(11) . . . . ? O25 Nd2 O3 C1 162.4(11) . . . . ? O29 Nd2 O3 C1 5.5(11) . . . . ? O27 Nd2 O3 C1 -67.5(12) . . . . ? O2 Nd1 O9 C8 55.3(10) . . . . ? O19 Nd1 O9 C8 18.1(10) . . . . ? O4 Nd1 O9 C8 106.2(10) 2_556 . . . ? O20 Nd1 O9 C8 -59.9(10) . . . . ? O21 Nd1 O9 C8 -179.6(10) . . . . ? O22 Nd1 O9 C8 161.9(9) . . . . ? O18 Nd1 O9 C8 -120.5(10) . . . . ? O23 Nd1 O9 C8 -46.6(10) . . . . ? O9 Nd1 O18 C21 -177.5(5) . . . . ? O2 Nd1 O18 C21 6.5(6) . . . . ? O19 Nd1 O18 C21 105.5(6) . . . . ? O4 Nd1 O18 C21 -95.5(6) 2_556 . . . ? O20 Nd1 O18 C21 118.6(6) . . . . ? O21 Nd1 O18 C21 -115.5(6) . . . . ? O22 Nd1 O18 C21 -33.7(5) . . . . ? O23 Nd1 O18 C21 44.9(5) . . . . ? Nd2 O3 C1 O2 124.6(9) . . . . ? Nd2 O3 C1 C2 -57.4(14) . . . . ? Nd1 O2 C1 O3 69.0(11) . . . . ? Nd1 O2 C1 C2 -109.0(7) . . . . ? C6 O1 C2 C3 1.2(9) . . . . ? C6 O1 C2 C1 177.1(5) . . . . ? O3 C1 C2 C3 -12.3(10) . . . . ? O2 C1 C2 C3 165.9(6) . . . . ? O3 C1 C2 O1 172.0(5) . . . . ? O2 C1 C2 O1 -9.8(8) . . . . ? O1 C2 C3 C4 2.3(10) . . . . ? C1 C2 C3 C4 -172.9(6) . . . . ? Nd1 O4 C4 C3 -138.3(6) 2_556 . . . ? Nd1 O4 C4 C5 39.5(10) 2_556 . . . ? C2 C3 C4 O4 173.1(6) . . . . ? C2 C3 C4 C5 -4.9(9) . . . . ? O4 C4 C5 C6 -173.6(6) . . . . ? C3 C4 C5 C6 4.4(8) . . . . ? C2 O1 C6 C5 -1.7(9) . . . . ? C2 O1 C6 C7 179.0(5) . . . . ? C4 C5 C6 O1 -1.3(9) . . . . ? C4 C5 C6 C7 177.9(5) . . . . ? O1 C6 C7 O5 6.8(8) . . . . ? C5 C6 C7 O5 -172.4(6) . . . . ? O1 C6 C7 O6 -174.8(5) . . . . ? C5 C6 C7 O6 5.9(9) . . . . ? Nd2 O8 C8 O9 62.9(17) 1_565 . . . ? Nd2 O8 C8 C9 -114.4(13) 1_565 . . . ? Nd1 O9 C8 O8 112.4(9) . . . . ? Nd1 O9 C8 C9 -70.3(12) . . . . ? C13 O7 C9 C10 1.4(9) . . . . ? C13 O7 C9 C8 175.5(5) . . . . ? O8 C8 C9 O7 -12.4(8) . . . . ? O9 C8 C9 O7 170.0(5) . . . . ? O8 C8 C9 C10 161.5(6) . . . . ? O9 C8 C9 C10 -16.0(9) . . . . ? O7 C9 C10 C11 2.8(9) . . . . ? C8 C9 C10 C11 -170.7(6) . . . . ? Nd2 O10 C11 C10 -133.4(5) 2_556 . . . ? Nd2 O10 C11 C12 46.3(9) 2_556 . . . ? C9 C10 C11 O10 175.1(6) . . . . ? C9 C10 C11 C12 -4.7(9) . . . . ? O10 C11 C12 C13 -176.9(6) . . . . ? C10 C11 C12 C13 2.9(9) . . . . ? C11 C12 C13 O7 1.1(10) . . . . ? C11 C12 C13 C14 177.7(6) . . . . ? C9 O7 C13 C12 -3.4(9) . . . . ? C9 O7 C13 C14 179.6(5) . . . . ? C12 C13 C14 O12 -175.8(6) . . . . ? O7 C13 C14 O12 1.1(8) . . . . ? C12 C13 C14 O11 6.2(9) . . . . ? O7 C13 C14 O11 -176.9(5) . . . . ? C20 O13 C16 C17 4.1(9) . . . . ? C20 O13 C16 C15 -176.0(5) . . . . ? O14 C15 C16 C17 176.9(7) . . . . ? O15 C15 C16 C17 -2.4(10) . . . . ? O14 C15 C16 O13 -3.0(9) . . . . ? O15 C15 C16 O13 177.6(6) . . . . ? O13 C16 C17 C18 -4.2(10) . . . . ? C15 C16 C17 C18 175.9(6) . . . . ? C16 C17 C18 O16 -179.1(6) . . . . ? C16 C17 C18 C19 1.0(9) . . . . ? O16 C18 C19 C20 -177.9(6) . . . . ? C17 C18 C19 C20 2.0(9) . . . . ? C16 O13 C20 C19 -0.8(9) . . . . ? C16 O13 C20 C21 -178.7(5) . . . . ? C18 C19 C20 O13 -2.2(10) . . . . ? C18 C19 C20 C21 175.6(6) . . . . ? Nd1 O18 C21 O17 -33.8(10) . . . . ? Nd1 O18 C21 C20 145.7(4) . . . . ? O13 C20 C21 O17 -153.1(6) . . . . ? C19 C20 C21 O17 29.0(9) . . . . ? O13 C20 C21 O18 27.3(8) . . . . ? C19 C20 C21 O18 -150.6(6) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.708 _refine_diff_density_min -1.410 _refine_diff_density_rms 0.212 # Attachment 'Eu-2.cif' data_Eu-2 _database_code_depnum_ccdc_archive 'CCDC 716751' #TrackingRef 'Eu-2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H30 Eu2 O30' _chemical_formula_weight 1066.37 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.4966(19) _cell_length_b 9.6020(19) _cell_length_c 10.144(2) _cell_angle_alpha 69.48(3) _cell_angle_beta 68.52(3) _cell_angle_gamma 83.79(3) _cell_volume 805.9(3) _cell_formula_units_Z 1 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 2794 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 25.01 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.197 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 522 _exptl_absorpt_coefficient_mu 3.975 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5036 _exptl_absorpt_correction_T_max 0.8260 _exptl_absorpt_process_details Crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8214 _diffrn_reflns_av_R_equivalents 0.0636 _diffrn_reflns_av_sigmaI/netI 0.0738 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 25.01 _reflns_number_total 2794 _reflns_number_gt 2607 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. A few of restraints containing 'isor' and 'simu' have been used to restrict the disordered ligand and water molecules. ; _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^)+(0.1019P)^2^+4.6364P] 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 2794 _refine_ls_number_parameters 316 _refine_ls_number_restraints 138 _refine_ls_R_factor_all 0.0694 _refine_ls_R_factor_gt 0.0653 _refine_ls_wR_factor_ref 0.1707 _refine_ls_wR_factor_gt 0.1668 _refine_ls_goodness_of_fit_ref 1.112 _refine_ls_restrained_S_all 1.090 _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 Eu1 Eu 0.82651(5) 0.30986(5) 0.21007(5) 0.0191(2) Uani 1 1 d . . . C1 C 0.6183(10) 0.3623(10) 0.5489(10) 0.0152(19) Uani 1 1 d . . . C2 C 0.4776(10) 0.2596(10) 0.6366(10) 0.0146(18) Uani 1 1 d U . . C3 C 0.4613(10) 0.1336(10) 0.6178(10) 0.0135(18) Uani 1 1 d U . . H3A H 0.5348 0.1067 0.5410 0.016 Uiso 1 1 calc R . . C4 C 0.3296(11) 0.0369(11) 0.7161(11) 0.018(2) Uani 1 1 d . . . C5 C 0.2185(11) 0.0967(10) 0.8220(10) 0.0160(19) Uani 1 1 d U . . H5A H 0.1282 0.0441 0.8852 0.019 Uiso 1 1 calc R . . C6 C 0.2437(10) 0.2266(10) 0.8305(10) 0.0147(18) Uani 1 1 d U . . C7 C 0.1364(10) 0.2981(10) 0.9367(10) 0.0124(18) Uani 1 1 d U . . C8 C 0.808(2) 0.290(2) -0.108(2) 0.013(4) Uani 0.50 1 d PU . . C9 C 0.6785(18) 0.1727(18) -0.0656(18) 0.006(3) Uani 0.50 1 d PU . . C10 C 0.694(2) 0.077(2) -0.134(2) 0.015(4) Uani 0.50 1 d P . . H10A H 0.7795 0.0814 -0.2231 0.018 Uiso 0.50 1 d PR . . C11 C 0.578(2) -0.043(2) -0.076(2) 0.009(3) Uani 0.50 1 d PU . . C12 C 0.454(2) -0.032(2) 0.055(2) 0.014(4) Uani 0.50 1 d PU . . H12A H 0.3725 -0.1043 0.0995 0.017 Uiso 0.50 1 d PR . . C13 C 0.443(2) 0.077(2) 0.115(2) 0.009(3) Uani 0.50 1 d PU . . C14 C 0.322(2) 0.089(2) 0.255(2) 0.015(4) Uani 0.50 1 d P . . O1 O 0.7158(7) 0.3235(7) 0.4490(7) 0.0133(13) Uani 1 1 d U . . O2 O 0.6235(7) 0.4700(7) 0.5858(7) 0.0191(15) Uani 1 1 d . . . O3 O 0.3733(7) 0.3091(7) 0.7415(7) 0.0122(13) Uani 1 1 d U . . O4 O 0.1540(7) 0.4329(7) 0.9088(7) 0.0158(14) Uani 1 1 d U . . O5 O 0.0317(7) 0.2162(7) 1.0441(8) 0.0185(14) Uani 1 1 d U . . O6 O 0.3165(7) -0.0869(7) 0.7085(7) 0.0180(14) Uani 1 1 d . . . O7 O 0.794(2) 0.344(2) -0.0128(19) 0.0083(19) Uani 0.50 1 d PU . . O8 O 0.9057(15) 0.3020(16) -0.2319(15) 0.020(3) Uani 0.50 1 d PU . . O9 O 0.5565(13) 0.1792(13) 0.0546(13) 0.010(2) Uani 0.50 1 d PU . . O10 O 0.3400(15) 0.1786(15) 0.3074(15) 0.018(3) Uani 0.50 1 d PU . . O11 O 0.2089(14) -0.0006(15) 0.3035(15) 0.017(3) Uani 0.50 1 d P . . O12 O 0.5925(16) -0.1415(17) -0.1289(15) 0.018(3) Uani 0.50 1 d PU . . O13 O 0.9285(8) 0.1091(7) 0.3631(8) 0.0232(15) Uani 1 1 d . . . H13A H 0.8929 0.0436 0.4483 0.035 Uiso 1 1 d R . . H13B H 1.0187 0.0901 0.3575 0.035 Uiso 1 1 d R . . O14 O 1.0373(8) 0.3972(7) 0.2355(7) 0.0187(14) Uani 1 1 d . . . H14B H 1.0563 0.3908 0.3127 0.028 Uiso 1 1 d R . . H14A H 1.1021 0.4640 0.1706 0.028 Uiso 1 1 d R . . O15 O 0.5662(7) 0.3817(7) 0.2400(7) 0.0181(14) Uani 1 1 d U . . H15A H 0.5174 0.4397 0.2874 0.027 Uiso 1 1 d R . . H15B H 0.4907 0.3323 0.2547 0.027 Uiso 1 1 d R . . O16 O 0.8689(8) 0.6465(9) 0.5199(7) 0.0247(16) Uani 1 1 d . . . H16A H 0.9545 0.6615 0.4510 0.030 Uiso 1 1 d R . . H16B H 0.8021 0.6846 0.4835 0.030 Uiso 1 1 d R . . O17 O 0.5086(15) 0.5761(14) 0.0047(15) 0.016(3) Uani 0.50 1 d P . . O18 O 0.9029(16) 0.2167(17) -0.2380(16) 0.024(3) Uani 0.50 1 d PU . . O19 O 0.2053(15) 0.1187(15) 0.4083(15) 0.020(3) Uani 0.50 1 d P . . O20 O 0.779(2) 0.355(2) -0.0341(19) 0.0082(19) Uani 0.50 1 d PU . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Eu1 0.0200(3) 0.0169(3) 0.0156(3) -0.0099(2) 0.0042(2) -0.0027(2) C1 0.014(4) 0.010(4) 0.014(4) -0.004(4) 0.004(4) 0.000(3) C2 0.014(2) 0.015(2) 0.015(2) -0.0055(11) -0.0048(11) 0.0005(10) C3 0.014(2) 0.013(2) 0.014(2) -0.0051(11) -0.0039(11) 0.0001(10) C4 0.016(5) 0.017(5) 0.022(5) -0.013(4) -0.004(4) 0.005(4) C5 0.016(2) 0.016(2) 0.016(2) -0.0060(11) -0.0047(11) 0.0003(10) C6 0.014(2) 0.015(2) 0.015(2) -0.0052(11) -0.0045(11) 0.0008(10) C7 0.012(2) 0.013(2) 0.012(2) -0.0050(11) -0.0038(11) 0.0007(10) C8 0.013(4) 0.013(4) 0.013(4) -0.0043(15) -0.0045(16) 0.0004(10) C9 0.006(3) 0.007(3) 0.006(3) -0.0022(14) -0.0022(15) 0.0002(10) C10 0.013(9) 0.017(9) 0.019(9) -0.011(8) -0.006(8) 0.000(7) C11 0.009(4) 0.009(4) 0.009(4) -0.0031(15) -0.0029(15) 0.0003(10) C12 0.014(4) 0.014(4) 0.014(4) -0.0049(15) -0.0048(16) 0.0002(10) C13 0.009(4) 0.009(4) 0.009(4) -0.0029(15) -0.0034(16) 0.0003(10) C14 0.011(8) 0.012(9) 0.019(10) -0.008(7) 0.003(8) 0.000(7) O1 0.0138(16) 0.0130(16) 0.0126(15) -0.0059(10) -0.0026(10) 0.0006(9) O2 0.014(3) 0.015(3) 0.020(3) -0.013(3) 0.012(3) -0.008(3) O3 0.0127(15) 0.0118(15) 0.0121(15) -0.0053(10) -0.0030(10) 0.0002(9) O4 0.0160(16) 0.0150(16) 0.0155(16) -0.0062(10) -0.0039(10) 0.0016(9) O5 0.0185(17) 0.0173(17) 0.0189(16) -0.0082(10) -0.0038(10) 0.0003(10) O6 0.016(3) 0.016(3) 0.020(3) -0.015(3) 0.004(3) -0.003(3) O7 0.008(2) 0.0084(19) 0.008(2) -0.0029(10) -0.0028(9) 0.0006(8) O8 0.020(3) 0.020(3) 0.020(3) -0.0069(14) -0.0063(14) 0.0004(10) O9 0.010(3) 0.010(3) 0.010(3) -0.0035(12) -0.0031(13) 0.0005(10) O10 0.018(3) 0.018(3) 0.018(3) -0.0064(13) -0.0058(14) 0.0002(10) O11 0.010(6) 0.021(7) 0.019(7) -0.007(6) -0.004(5) 0.000(5) O12 0.018(3) 0.018(3) 0.018(3) -0.0063(14) -0.0062(14) 0.0003(10) O13 0.025(4) 0.015(3) 0.026(4) -0.003(3) -0.011(3) 0.005(3) O14 0.020(3) 0.021(4) 0.010(3) -0.002(3) -0.001(3) -0.009(3) O15 0.0178(17) 0.0179(17) 0.0185(16) -0.0076(10) -0.0049(10) 0.0005(10) O16 0.014(3) 0.046(5) 0.007(3) -0.008(3) 0.004(3) -0.008(3) O17 0.022(7) 0.012(7) 0.018(7) 0.003(5) -0.017(6) 0.000(5) O18 0.024(3) 0.024(3) 0.024(3) -0.0085(14) -0.0079(15) 0.0004(10) O19 0.020(7) 0.017(7) 0.016(7) -0.004(6) 0.001(6) -0.002(5) O20 0.008(2) 0.0083(19) 0.008(2) -0.0029(10) -0.0028(9) 0.0005(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 Eu1 O7 2.299(16) . ? Eu1 O1 2.307(6) . ? Eu1 O4 2.332(6) 2_666 ? Eu1 O13 2.380(7) . ? Eu1 O14 2.382(7) . ? Eu1 O6 2.383(6) 2_656 ? Eu1 O5 2.392(7) 1_654 ? Eu1 O15 2.431(7) . ? Eu1 O20 2.559(16) . ? Eu1 C7 3.245(9) 1_654 ? C1 O2 1.228(11) . ? C1 O1 1.236(11) . ? C1 C2 1.533(12) . ? C2 C3 1.322(13) . ? C2 O3 1.349(11) . ? C3 C4 1.453(13) . ? C3 H3A 0.9300 . ? C4 O6 1.240(11) . ? C4 C5 1.439(13) . ? C5 C6 1.333(13) . ? C5 H5A 0.9300 . ? C6 O3 1.361(11) . ? C6 C7 1.495(12) . ? C7 O4 1.241(11) . ? C7 O5 1.252(11) . ? C7 Eu1 3.245(9) 1_456 ? C8 O20 1.09(2) . ? C8 O7 1.22(3) . ? C8 O8 1.23(2) . ? C8 C9 1.59(2) . ? C8 O18 1.63(2) . ? C9 C10 1.30(2) . ? C9 O9 1.36(2) . ? C10 C12 1.36(3) 2_655 ? C10 H10A 0.9599 . ? C11 C13 0.67(2) 2_655 ? C11 C12 0.82(2) 2_655 ? C11 O12 1.21(3) . ? C11 C12 1.45(3) . ? C11 O9 1.83(2) 2_655 ? C12 C11 0.82(2) 2_655 ? C12 C12 1.15(4) 2_655 ? C12 C10 1.36(3) 2_655 ? C12 H12A 0.9563 . ? C13 C11 0.67(2) 2_655 ? C13 O12 0.708(19) 2_655 ? C13 O9 1.35(2) . ? C13 C14 1.50(3) . ? C14 O12 1.19(2) 2_655 ? C14 O10 1.22(2) . ? C14 O11 1.28(2) . ? C14 O19 1.65(2) . ? O4 Eu1 2.332(6) 2_666 ? O5 Eu1 2.392(7) 1_456 ? O6 Eu1 2.383(6) 2_656 ? O8 O18 0.847(17) . ? O9 O12 1.357(18) 2_655 ? O9 C11 1.83(2) 2_655 ? O10 O19 1.343(18) . ? O11 O19 1.806(19) . ? O12 C13 0.708(19) 2_655 ? O12 C14 1.19(2) 2_655 ? O12 O9 1.357(18) 2_655 ? O13 H13A 0.8411 . ? O13 H13B 0.8419 . ? O14 H14B 0.8459 . ? O14 H14A 0.8465 . ? O15 H15A 0.8508 . ? O15 H15B 0.8410 . ? O16 H16A 0.8422 . ? O16 H16B 0.8364 . ? O17 O17 1.53(3) 2_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 O7 Eu1 O1 145.7(5) . . ? O7 Eu1 O4 76.1(5) . 2_666 ? O1 Eu1 O4 94.3(2) . 2_666 ? O7 Eu1 O13 131.4(5) . . ? O1 Eu1 O13 75.0(2) . . ? O4 Eu1 O13 142.4(2) 2_666 . ? O7 Eu1 O14 125.8(5) . . ? O1 Eu1 O14 79.9(2) . . ? O4 Eu1 O14 72.3(2) 2_666 . ? O13 Eu1 O14 70.4(2) . . ? O7 Eu1 O6 82.7(5) . 2_656 ? O1 Eu1 O6 89.3(2) . 2_656 ? O4 Eu1 O6 147.1(2) 2_666 2_656 ? O13 Eu1 O6 69.9(2) . 2_656 ? O14 Eu1 O6 140.2(2) . 2_656 ? O7 Eu1 O5 67.5(5) . 1_654 ? O1 Eu1 O5 146.1(2) . 1_654 ? O4 Eu1 O5 104.3(2) 2_666 1_654 ? O13 Eu1 O5 73.0(2) . 1_654 ? O14 Eu1 O5 79.2(2) . 1_654 ? O6 Eu1 O5 90.0(2) 2_656 1_654 ? O7 Eu1 O15 72.3(5) . . ? O1 Eu1 O15 73.4(2) . . ? O4 Eu1 O15 76.6(2) 2_666 . ? O13 Eu1 O15 131.0(2) . . ? O14 Eu1 O15 136.9(2) . . ? O6 Eu1 O15 73.2(2) 2_656 . ? O5 Eu1 O15 138.1(2) 1_654 . ? O7 Eu1 O20 2.7(8) . . ? O1 Eu1 O20 143.1(4) . . ? O4 Eu1 O20 74.8(4) 2_666 . ? O13 Eu1 O20 133.7(4) . . ? O14 Eu1 O20 127.1(4) . . ? O6 Eu1 O20 82.8(4) 2_656 . ? O5 Eu1 O20 70.2(4) 1_654 . ? O15 Eu1 O20 69.7(4) . . ? O7 Eu1 C7 65.6(5) . 1_654 ? O1 Eu1 C7 147.6(2) . 1_654 ? O4 Eu1 C7 85.8(2) 2_666 1_654 ? O13 Eu1 C7 85.3(2) . 1_654 ? O14 Eu1 C7 69.2(2) . 1_654 ? O6 Eu1 C7 108.0(2) 2_656 1_654 ? O5 Eu1 C7 18.9(2) 1_654 1_654 ? O15 Eu1 C7 137.2(2) . 1_654 ? O20 Eu1 C7 68.1(4) . 1_654 ? O2 C1 O1 127.6(9) . . ? O2 C1 C2 118.0(8) . . ? O1 C1 C2 114.5(8) . . ? C3 C2 O3 123.2(8) . . ? C3 C2 C1 124.7(9) . . ? O3 C2 C1 112.0(7) . . ? C2 C3 C4 120.6(9) . . ? C2 C3 H3A 119.7 . . ? C4 C3 H3A 119.7 . . ? O6 C4 C5 123.6(9) . . ? O6 C4 C3 122.1(9) . . ? C5 C4 C3 114.3(8) . . ? C6 C5 C4 120.6(9) . . ? C6 C5 H5A 119.7 . . ? C4 C5 H5A 119.7 . . ? C5 C6 O3 122.8(9) . . ? C5 C6 C7 124.9(9) . . ? O3 C6 C7 112.4(7) . . ? O4 C7 O5 125.6(9) . . ? O4 C7 C6 118.1(8) . . ? O5 C7 C6 116.2(8) . . ? O4 C7 Eu1 87.4(5) . 1_456 ? O5 C7 Eu1 38.3(4) . 1_456 ? C6 C7 Eu1 153.7(6) . 1_456 ? O20 C8 O7 12.7(16) . . ? O20 C8 O8 134(2) . . ? O7 C8 O8 132.9(19) . . ? O20 C8 C9 113.1(17) . . ? O7 C8 C9 115.1(16) . . ? O8 C8 C9 111.9(15) . . ? O20 C8 O18 161.7(19) . . ? O7 C8 O18 154.2(17) . . ? O8 C8 O18 30.4(8) . . ? C9 C8 O18 84.9(12) . . ? C10 C9 O9 124.8(16) . . ? C10 C9 C8 122.9(16) . . ? O9 C9 C8 112.1(13) . . ? C10 C9 C12 46.1(11) . 2_655 ? O9 C9 C12 79.2(11) . 2_655 ? C8 C9 C12 168.1(14) . 2_655 ? C9 C10 C12 90.3(16) . 2_655 ? C9 C10 C11 120.7(17) . . ? C12 C10 C11 33.2(10) 2_655 . ? C9 C10 C13 133.4(16) . 2_655 ? C12 C10 C13 43.2(12) 2_655 2_655 ? C11 C10 C13 15.2(9) . 2_655 ? C9 C10 H10A 121.4 . . ? C12 C10 H10A 145.4 2_655 . ? C11 C10 H10A 117.9 . . ? C13 C10 H10A 104.5 2_655 . ? C13 C11 C12 131(4) 2_655 2_655 ? C13 C11 O12 30(2) 2_655 . ? C12 C11 O12 160(3) 2_655 . ? C13 C11 C12 112(3) 2_655 . ? C12 C11 C12 52(2) 2_655 . ? O12 C11 C12 125.3(18) . . ? C13 C11 C10 129(3) 2_655 . ? C12 C11 C10 65(2) 2_655 . ? O12 C11 C10 123.2(17) . . ? C12 C11 C10 111.4(19) . . ? C13 C11 O9 37(2) 2_655 2_655 ? C12 C11 O9 120(2) 2_655 2_655 ? O12 C11 O9 48.0(11) . 2_655 ? C12 C11 O9 79.2(12) . 2_655 ? C10 C11 O9 166.0(15) . 2_655 ? C13 C11 C14 46(2) 2_655 2_655 ? C12 C11 C14 136(2) 2_655 2_655 ? O12 C11 C14 37.8(10) . 2_655 ? C12 C11 C14 157.9(17) . 2_655 ? C10 C11 C14 88.1(12) . 2_655 ? O9 C11 C14 80.0(11) 2_655 2_655 ? C11 C12 C12 93(3) 2_655 2_655 ? C11 C12 C10 82(2) 2_655 2_655 ? C12 C12 C10 150(3) 2_655 2_655 ? C11 C12 C13 22.1(17) 2_655 . ? C12 C12 C13 92(2) 2_655 . ? C10 C12 C13 93.6(17) 2_655 . ? C11 C12 C11 128(2) 2_655 . ? C12 C12 C11 34.5(14) 2_655 . ? C10 C12 C11 140(2) 2_655 . ? C13 C12 C11 123.8(18) . . ? C11 C12 C13 137(2) 2_655 2_655 ? C12 C12 C13 48.5(17) 2_655 2_655 ? C10 C12 C13 120.1(16) 2_655 2_655 ? C13 C12 C13 140.7(15) . 2_655 ? C11 C12 C13 20.1(9) . 2_655 ? C11 C12 C9 122(2) 2_655 2_655 ? C12 C12 C9 123(2) 2_655 2_655 ? C10 C12 C9 43.6(11) 2_655 2_655 ? C13 C12 C9 137.1(16) . 2_655 ? C11 C12 C9 97.4(15) . 2_655 ? C13 C12 C9 78.1(11) 2_655 2_655 ? C11 C12 H12A 109.3 2_655 . ? C12 C12 H12A 144.7 2_655 . ? C10 C12 H12A 27.5 2_655 . ? C13 C12 H12A 118.7 . . ? C11 C12 H12A 117.4 . . ? C13 C12 H12A 99.1 2_655 . ? C9 C12 H12A 22.0 2_655 . ? C11 C13 O12 122(4) 2_655 2_655 ? C11 C13 O9 126(3) 2_655 . ? O12 C13 O9 75(2) 2_655 . ? C11 C13 C12 27(2) 2_655 . ? O12 C13 C12 150(3) 2_655 . ? O9 C13 C12 119.8(18) . . ? C11 C13 C14 116(3) 2_655 . ? O12 C13 C14 51.4(19) 2_655 . ? O9 C13 C14 114.0(18) . . ? C12 C13 C14 125.9(17) . . ? C11 C13 C12 48(2) 2_655 2_655 ? O12 C13 C12 134(2) 2_655 2_655 ? O9 C13 C12 82.0(12) . 2_655 ? C12 C13 C12 39.3(15) . 2_655 ? C14 C13 C12 163.2(17) . 2_655 ? C11 C13 C10 35(2) 2_655 2_655 ? O12 C13 C10 115(2) 2_655 2_655 ? O9 C13 C10 160.8(17) . 2_655 ? C12 C13 C10 43.2(12) . 2_655 ? C14 C13 C10 84.4(12) . 2_655 ? C12 C13 C10 79.2(12) 2_655 2_655 ? O12 C14 O10 99.2(16) 2_655 . ? O12 C14 O11 128.5(18) 2_655 . ? O10 C14 O11 128.2(17) . . ? O12 C14 C13 27.6(9) 2_655 . ? O10 C14 C13 118.4(17) . . ? O11 C14 C13 113.3(17) . . ? O12 C14 O19 147.0(17) 2_655 . ? O10 C14 O19 53.3(10) . . ? O11 C14 O19 74.9(12) . . ? C13 C14 O19 171.7(16) . . ? O12 C14 C11 38.5(11) 2_655 2_655 ? O10 C14 C11 136.0(15) . 2_655 ? O11 C14 C11 95.4(13) . 2_655 ? C13 C14 C11 18.8(8) . 2_655 ? O19 C14 C11 169.1(14) . 2_655 ? C1 O1 Eu1 154.6(6) . . ? C2 O3 C6 118.4(7) . . ? C7 O4 Eu1 162.3(6) . 2_666 ? C7 O5 Eu1 122.8(6) . 1_456 ? C4 O6 Eu1 150.3(6) . 2_656 ? C8 O7 Eu1 145.7(15) . . ? O18 O8 C8 102.2(18) . . ? C13 O9 C9 119.4(15) . . ? C13 O9 O12 30.3(8) . 2_655 ? C9 O9 O12 143.7(13) . 2_655 ? C13 O9 C11 17.5(10) . 2_655 ? C9 O9 C11 104.1(11) . 2_655 ? O12 O9 C11 41.5(10) 2_655 2_655 ? C14 O10 O19 80.0(13) . . ? C14 O11 O19 61.8(11) . . ? C13 O12 C14 101(2) 2_655 2_655 ? C13 O12 C11 28.1(19) 2_655 . ? C14 O12 C11 103.7(16) 2_655 . ? C13 O12 O9 74(2) 2_655 2_655 ? C14 O12 O9 139.1(15) 2_655 2_655 ? C11 O12 O9 90.6(15) . 2_655 ? Eu1 O13 H13A 135.2 . . ? Eu1 O13 H13B 130.5 . . ? H13A O13 H13B 93.3 . . ? Eu1 O14 H14B 131.3 . . ? Eu1 O14 H14A 127.7 . . ? H14B O14 H14A 99.0 . . ? Eu1 O15 H15A 124.8 . . ? Eu1 O15 H15B 130.8 . . ? H15A O15 H15B 96.5 . . ? H16A O16 H16B 109.7 . . ? O8 O18 C8 47.4(14) . . ? O10 O19 C14 46.7(10) . . ? O10 O19 O11 90.0(10) . . ? C14 O19 O11 43.3(8) . . ? C8 O20 Eu1 131.0(15) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 C1 C2 C3 -174.3(9) . . . . ? O1 C1 C2 C3 4.5(14) . . . . ? O2 C1 C2 O3 2.8(12) . . . . ? O1 C1 C2 O3 -178.4(8) . . . . ? O3 C2 C3 C4 -2.7(14) . . . . ? C1 C2 C3 C4 174.2(8) . . . . ? C2 C3 C4 O6 -174.6(9) . . . . ? C2 C3 C4 C5 4.9(13) . . . . ? O6 C4 C5 C6 175.9(9) . . . . ? C3 C4 C5 C6 -3.6(13) . . . . ? C4 C5 C6 O3 0.0(14) . . . . ? C4 C5 C6 C7 -179.7(8) . . . . ? C5 C6 C7 O4 -161.8(9) . . . . ? O3 C6 C7 O4 18.5(11) . . . . ? C5 C6 C7 O5 15.3(14) . . . . ? O3 C6 C7 O5 -164.4(8) . . . . ? C5 C6 C7 Eu1 3(2) . . . 1_456 ? O3 C6 C7 Eu1 -176.3(9) . . . 1_456 ? O20 C8 C9 C10 -175.3(19) . . . . ? O7 C8 C9 C10 -161.6(18) . . . . ? O8 C8 C9 C10 16(2) . . . . ? O18 C8 C9 C10 1.5(18) . . . . ? O20 C8 C9 O9 1(2) . . . . ? O7 C8 C9 O9 15(2) . . . . ? O8 C8 C9 O9 -168.1(14) . . . . ? O18 C8 C9 O9 177.7(13) . . . . ? O20 C8 C9 C12 163(6) . . . 2_655 ? O7 C8 C9 C12 177(6) . . . 2_655 ? O8 C8 C9 C12 -6(7) . . . 2_655 ? O18 C8 C9 C12 -20(7) . . . 2_655 ? O9 C9 C10 C12 10(2) . . . 2_655 ? C8 C9 C10 C12 -174.0(16) . . . 2_655 ? O9 C9 C10 C11 -4(3) . . . . ? C8 C9 C10 C11 171.8(15) . . . . ? C12 C9 C10 C11 -14.2(13) 2_655 . . . ? O9 C9 C10 C13 7(3) . . . 2_655 ? C8 C9 C10 C13 -177.6(15) . . . 2_655 ? C12 C9 C10 C13 -3.6(15) 2_655 . . 2_655 ? C9 C10 C11 C13 149(4) . . . 2_655 ? C12 C10 C11 C13 123(5) 2_655 . . 2_655 ? C9 C10 C11 C12 27(2) . . . 2_655 ? C13 C10 C11 C12 -123(5) 2_655 . . 2_655 ? C9 C10 C11 O12 -174.2(18) . . . . ? C12 C10 C11 O12 159(3) 2_655 . . . ? C13 C10 C11 O12 36(3) 2_655 . . . ? C9 C10 C11 C12 1(2) . . . . ? C12 C10 C11 C12 -25(2) 2_655 . . . ? C13 C10 C11 C12 -148(5) 2_655 . . . ? C9 C10 C11 O9 139(6) . . . 2_655 ? C12 C10 C11 O9 112(7) 2_655 . . 2_655 ? C13 C10 C11 O9 -11(4) 2_655 . . 2_655 ? C9 C10 C11 C14 170.8(17) . . . 2_655 ? C12 C10 C11 C14 144(2) 2_655 . . 2_655 ? C13 C10 C11 C14 21(4) 2_655 . . 2_655 ? C13 C11 C12 C11 -125(4) 2_655 . . 2_655 ? C12 C11 C12 C11 -0.003(2) 2_655 . . 2_655 ? O12 C11 C12 C11 -156(3) . . . 2_655 ? C10 C11 C12 C11 29(3) . . . 2_655 ? O9 C11 C12 C11 -141(3) 2_655 . . 2_655 ? C14 C11 C12 C11 -122(5) 2_655 . . 2_655 ? C13 C11 C12 C12 -125(4) 2_655 . . 2_655 ? O12 C11 C12 C12 -156(3) . . . 2_655 ? C10 C11 C12 C12 29(3) . . . 2_655 ? O9 C11 C12 C12 -141(3) 2_655 . . 2_655 ? C14 C11 C12 C12 -122(5) 2_655 . . 2_655 ? C13 C11 C12 C10 5(5) 2_655 . . 2_655 ? C12 C11 C12 C10 130(4) 2_655 . . 2_655 ? O12 C11 C12 C10 -26(4) . . . 2_655 ? C10 C11 C12 C10 159(2) . . . 2_655 ? O9 C11 C12 C10 -12(3) 2_655 . . 2_655 ? C14 C11 C12 C10 8(6) 2_655 . . 2_655 ? C13 C11 C12 C13 -152(2) 2_655 . . . ? C12 C11 C12 C13 -27(2) 2_655 . . . ? O12 C11 C12 C13 177.6(19) . . . . ? C10 C11 C12 C13 2(3) . . . . ? O9 C11 C12 C13 -168.3(19) 2_655 . . . ? C14 C11 C12 C13 -149(3) 2_655 . . . ? C12 C11 C12 C13 125(4) 2_655 . . 2_655 ? O12 C11 C12 C13 -31(2) . . . 2_655 ? C10 C11 C12 C13 154(4) . . . 2_655 ? O9 C11 C12 C13 -17(3) 2_655 . . 2_655 ? C14 C11 C12 C13 3(3) 2_655 . . 2_655 ? C13 C11 C12 C9 16(3) 2_655 . . 2_655 ? C12 C11 C12 C9 140(3) 2_655 . . 2_655 ? O12 C11 C12 C9 -15(2) . . . 2_655 ? C10 C11 C12 C9 169.4(13) . . . 2_655 ? O9 C11 C12 C9 -1.0(10) 2_655 . . 2_655 ? C14 C11 C12 C9 19(5) 2_655 . . 2_655 ? C12 C12 C13 C11 93(5) 2_655 . . 2_655 ? C10 C12 C13 C11 -58(4) 2_655 . . 2_655 ? C11 C12 C13 C11 107(5) . . . 2_655 ? C13 C12 C13 C11 93(5) 2_655 . . 2_655 ? C9 C12 C13 C11 -54(5) 2_655 . . 2_655 ? C11 C12 C13 O12 3(5) 2_655 . . 2_655 ? C12 C12 C13 O12 95(5) 2_655 . . 2_655 ? C10 C12 C13 O12 -55(5) 2_655 . . 2_655 ? C11 C12 C13 O12 110(5) . . . 2_655 ? C13 C12 C13 O12 95(5) 2_655 . . 2_655 ? C9 C12 C13 O12 -51(6) 2_655 . . 2_655 ? C11 C12 C13 O9 -111(5) 2_655 . . . ? C12 C12 C13 O9 -18(3) 2_655 . . . ? C10 C12 C13 O9 -168.6(17) 2_655 . . . ? C11 C12 C13 O9 -3(3) . . . . ? C13 C12 C13 O9 -18(3) 2_655 . . . ? C9 C12 C13 O9 -164.7(16) 2_655 . . . ? C11 C12 C13 C14 76(5) 2_655 . . . ? C12 C12 C13 C14 169(2) 2_655 . . . ? C10 C12 C13 C14 18(2) 2_655 . . . ? C11 C12 C13 C14 -176.5(17) . . . . ? C13 C12 C13 C14 169(2) 2_655 . . . ? C9 C12 C13 C14 22(3) 2_655 . . . ? C11 C12 C13 C12 -93(5) 2_655 . . 2_655 ? C10 C12 C13 C12 -150(3) 2_655 . . 2_655 ? C11 C12 C13 C12 14.9(12) . . . 2_655 ? C13 C12 C13 C12 -0.001(2) 2_655 . . 2_655 ? C9 C12 C13 C12 -147(4) 2_655 . . 2_655 ? C11 C12 C13 C10 58(4) 2_655 . . 2_655 ? C12 C12 C13 C10 150(3) 2_655 . . 2_655 ? C11 C12 C13 C10 165(3) . . . 2_655 ? C13 C12 C13 C10 150(3) 2_655 . . 2_655 ? C9 C12 C13 C10 3.9(16) 2_655 . . 2_655 ? C11 C13 C14 O12 -112(4) 2_655 . . 2_655 ? O9 C13 C14 O12 45(2) . . . 2_655 ? C12 C13 C14 O12 -142(4) . . . 2_655 ? C12 C13 C14 O12 -116(6) 2_655 . . 2_655 ? C10 C13 C14 O12 -129(3) 2_655 . . 2_655 ? C11 C13 C14 O10 -162(3) 2_655 . . . ? O12 C13 C14 O10 -50(3) 2_655 . . . ? O9 C13 C14 O10 -5(3) . . . . ? C12 C13 C14 O10 168.4(19) . . . . ? C12 C13 C14 O10 -166(5) 2_655 . . . ? C10 C13 C14 O10 -179.2(17) 2_655 . . . ? C11 C13 C14 O11 18(4) 2_655 . . . ? O12 C13 C14 O11 130(3) 2_655 . . . ? O9 C13 C14 O11 174.5(15) . . . . ? C12 C13 C14 O11 -12(3) . . . . ? C12 C13 C14 O11 13(6) 2_655 . . . ? C10 C13 C14 O11 0.4(17) 2_655 . . . ? C11 C13 C14 O19 -167(10) 2_655 . . . ? O12 C13 C14 O19 -55(12) 2_655 . . . ? O9 C13 C14 O19 -10(12) . . . . ? C12 C13 C14 O19 163(10) . . . . ? C12 C13 C14 O19 -171(8) 2_655 . . . ? C10 C13 C14 O19 176(11) 2_655 . . . ? O12 C13 C14 C11 112(4) 2_655 . . 2_655 ? O9 C13 C14 C11 157(4) . . . 2_655 ? C12 C13 C14 C11 -30(2) . . . 2_655 ? C12 C13 C14 C11 -4(4) 2_655 . . 2_655 ? C10 C13 C14 C11 -17(3) 2_655 . . 2_655 ? O2 C1 O1 Eu1 -96.4(16) . . . . ? C2 C1 O1 Eu1 84.9(15) . . . . ? O7 Eu1 O1 C1 -14.8(17) . . . . ? O4 Eu1 O1 C1 56.6(14) 2_666 . . . ? O13 Eu1 O1 C1 -160.0(14) . . . . ? O14 Eu1 O1 C1 127.8(14) . . . . ? O6 Eu1 O1 C1 -90.7(14) 2_656 . . . ? O5 Eu1 O1 C1 -179.6(13) 1_654 . . . ? O15 Eu1 O1 C1 -18.0(14) . . . . ? O20 Eu1 O1 C1 -13.6(16) . . . . ? C7 Eu1 O1 C1 145.5(13) 1_654 . . . ? C3 C2 O3 C6 -1.3(13) . . . . ? C1 C2 O3 C6 -178.5(7) . . . . ? C5 C6 O3 C2 2.7(13) . . . . ? C7 C6 O3 C2 -177.7(7) . . . . ? O5 C7 O4 Eu1 -115.7(19) . . . 2_666 ? C6 C7 O4 Eu1 61(2) . . . 2_666 ? Eu1 C7 O4 Eu1 -112.4(19) 1_456 . . 2_666 ? O4 C7 O5 Eu1 5.4(12) . . . 1_456 ? C6 C7 O5 Eu1 -171.5(5) . . . 1_456 ? C5 C4 O6 Eu1 3(2) . . . 2_656 ? C3 C4 O6 Eu1 -177.1(8) . . . 2_656 ? O20 C8 O7 Eu1 163(10) . . . . ? O8 C8 O7 Eu1 -97(3) . . . . ? C9 C8 O7 Eu1 79(3) . . . . ? O18 C8 O7 Eu1 -59(5) . . . . ? O1 Eu1 O7 C8 -131(2) . . . . ? O4 Eu1 O7 C8 153(3) 2_666 . . . ? O13 Eu1 O7 C8 2(3) . . . . ? O14 Eu1 O7 C8 97(3) . . . . ? O6 Eu1 O7 C8 -53(3) 2_656 . . . ? O5 Eu1 O7 C8 40(3) 1_654 . . . ? O15 Eu1 O7 C8 -127(3) . . . . ? O20 Eu1 O7 C8 -146(19) . . . . ? C7 Eu1 O7 C8 61(3) 1_654 . . . ? O20 C8 O8 O18 165(2) . . . . ? O7 C8 O8 O18 148(2) . . . . ? C9 C8 O8 O18 -29(2) . . . . ? C11 C13 O9 C9 -31(4) 2_655 . . . ? O12 C13 O9 C9 -150(2) 2_655 . . . ? C12 C13 O9 C9 1(2) . . . . ? C14 C13 O9 C9 174.9(14) . . . . ? C12 C13 O9 C9 -10.5(15) 2_655 . . . ? C10 C13 O9 C9 -23(5) 2_655 . . . ? C11 C13 O9 O12 119(5) 2_655 . . 2_655 ? C12 C13 O9 O12 151(3) . . . 2_655 ? C14 C13 O9 O12 -34.8(18) . . . 2_655 ? C12 C13 O9 O12 140(2) 2_655 . . 2_655 ? C10 C13 O9 O12 127(6) 2_655 . . 2_655 ? O12 C13 O9 C11 -119(5) 2_655 . . 2_655 ? C12 C13 O9 C11 32(3) . . . 2_655 ? C14 C13 O9 C11 -154(5) . . . 2_655 ? C12 C13 O9 C11 20(4) 2_655 . . 2_655 ? C10 C13 O9 C11 8(3) 2_655 . . 2_655 ? C10 C9 O9 C13 3(2) . . . . ? C8 C9 O9 C13 -173.4(14) . . . . ? C12 C9 O9 C13 10.2(15) 2_655 . . . ? C10 C9 O9 O12 -22(3) . . . 2_655 ? C8 C9 O9 O12 161.6(19) . . . 2_655 ? C12 C9 O9 O12 -15(2) 2_655 . . 2_655 ? C10 C9 O9 C11 -6(2) . . . 2_655 ? C8 C9 O9 C11 177.4(12) . . . 2_655 ? C12 C9 O9 C11 1.1(10) 2_655 . . 2_655 ? O12 C14 O10 O19 159.8(15) 2_655 . . . ? O11 C14 O10 O19 1(2) . . . . ? C13 C14 O10 O19 -179.1(18) . . . . ? C11 C14 O10 O19 173(2) 2_655 . . . ? O12 C14 O11 O19 -153(2) 2_655 . . . ? O10 C14 O11 O19 -1.2(18) . . . . ? C13 C14 O11 O19 179.3(19) . . . . ? C11 C14 O11 O19 -175.1(13) 2_655 . . . ? C12 C11 O12 C13 -4(7) 2_655 . . 2_655 ? C12 C11 O12 C13 72(4) . . . 2_655 ? C10 C11 O12 C13 -112(4) . . . 2_655 ? O9 C11 O12 C13 54(4) 2_655 . . 2_655 ? C14 C11 O12 C13 -88(4) 2_655 . . 2_655 ? C13 C11 O12 C14 88(4) 2_655 . . 2_655 ? C12 C11 O12 C14 84(8) 2_655 . . 2_655 ? C12 C11 O12 C14 160.1(18) . . . 2_655 ? C10 C11 O12 C14 -25(3) . . . 2_655 ? O9 C11 O12 C14 141.3(18) 2_655 . . 2_655 ? C13 C11 O12 O9 -54(4) 2_655 . . 2_655 ? C12 C11 O12 O9 -57(8) 2_655 . . 2_655 ? C12 C11 O12 O9 19(2) . . . 2_655 ? C10 C11 O12 O9 -166.2(17) . . . 2_655 ? C14 C11 O12 O9 -141.3(18) 2_655 . . 2_655 ? O20 C8 O18 O8 -36(6) . . . . ? O7 C8 O18 O8 -64(4) . . . . ? C9 C8 O18 O8 153(2) . . . . ? C14 O10 O19 O11 -0.8(12) . . . . ? O12 C14 O19 O10 -39(3) 2_655 . . . ? O11 C14 O19 O10 -178.9(17) . . . . ? C13 C14 O19 O10 5(11) . . . . ? C11 C14 O19 O10 -152(8) 2_655 . . . ? O12 C14 O19 O11 140(4) 2_655 . . . ? O10 C14 O19 O11 178.9(17) . . . . ? C13 C14 O19 O11 -176(12) . . . . ? C11 C14 O19 O11 27(7) 2_655 . . . ? C14 O11 O19 O10 0.8(13) . . . . ? O7 C8 O20 Eu1 -11(6) . . . . ? O8 C8 O20 Eu1 -104(3) . . . . ? C9 C8 O20 Eu1 90(2) . . . . ? O18 C8 O20 Eu1 -79(6) . . . . ? O7 Eu1 O20 C8 28(16) . . . . ? O1 Eu1 O20 C8 -137.7(18) . . . . ? O4 Eu1 O20 C8 146(2) 2_666 . . . ? O13 Eu1 O20 C8 -5(2) . . . . ? O14 Eu1 O20 C8 93(2) . . . . ? O6 Eu1 O20 C8 -59(2) 2_656 . . . ? O5 Eu1 O20 C8 34(2) 1_654 . . . ? O15 Eu1 O20 C8 -133(2) . . . . ? C7 Eu1 O20 C8 54(2) 1_654 . . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.520 _refine_diff_density_min -3.514 _refine_diff_density_rms 0.296 # Attachment 'Gd-3.cif' data_Gd-3 _database_code_depnum_ccdc_archive 'CCDC 716752' #TrackingRef 'Gd-3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H30 Gd2 O30' _chemical_formula_weight 1076.95 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.507(2) _cell_length_b 9.649(2) _cell_length_c 10.1681(18) _cell_angle_alpha 69.731(11) _cell_angle_beta 68.642(9) _cell_angle_gamma 84.062(12) _cell_volume 814.6(3) _cell_formula_units_Z 1 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 3872 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 27.88 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.195 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 524 _exptl_absorpt_coefficient_mu 4.153 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6815 _exptl_absorpt_correction_T_max 0.7887 _exptl_absorpt_process_details Crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10270 _diffrn_reflns_av_R_equivalents 0.0397 _diffrn_reflns_av_sigmaI/netI 0.0485 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 27.88 _reflns_number_total 3872 _reflns_number_gt 3435 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. A few of restraints containing 'isor' and 'simu' have been used to restrict the disordered ligand and water molecules. ; _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^)+(0.0247P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3872 _refine_ls_number_parameters 316 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0265 _refine_ls_R_factor_gt 0.0231 _refine_ls_wR_factor_ref 0.0564 _refine_ls_wR_factor_gt 0.0553 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.026 _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 Gd1 Gd 0.826191(15) 0.309867(15) 0.210242(16) 0.00741(5) Uani 1 1 d . . . C1 C 0.6160(3) 0.3621(3) 0.5496(3) 0.0096(6) Uani 1 1 d . . . C2 C 0.4773(3) 0.2594(3) 0.6376(3) 0.0104(6) Uani 1 1 d . . . C3 C 0.4596(3) 0.1317(3) 0.6193(4) 0.0116(6) Uani 1 1 d . . . H3A H 0.5323 0.1040 0.5431 0.014 Uiso 1 1 calc R . . C4 C 0.3293(3) 0.0380(4) 0.7165(4) 0.0114(6) Uani 1 1 d . . . C5 C 0.2190(3) 0.0959(4) 0.8229(4) 0.0139(7) Uani 1 1 d . . . H5A H 0.1296 0.0427 0.8866 0.017 Uiso 1 1 calc R . . C6 C 0.2441(3) 0.2269(3) 0.8311(3) 0.0098(6) Uani 1 1 d . . . C7 C 0.1345(3) 0.2988(4) 0.9373(3) 0.0105(6) Uani 1 1 d . . . C8 C 0.8040(7) 0.2871(7) -0.1093(7) 0.0096(12) Uani 0.50 1 d P . . C9 C 0.6786(7) 0.1755(7) -0.0688(7) 0.0101(13) Uani 0.50 1 d PU . . C10 C 0.6899(7) 0.0771(7) -0.1381(7) 0.0127(13) Uani 0.50 1 d P . . H10A H 0.7755 0.0817 -0.2272 0.015 Uiso 0.50 1 d PR . . C11 C 0.5763(12) -0.0391(11) -0.0783(10) 0.014(2) Uani 0.50 1 d P . . C12 C 0.4491(8) -0.0278(9) 0.0498(8) 0.0127(15) Uani 0.50 1 d P . . H12A H 0.3681 -0.0996 0.0941 0.015 Uiso 0.50 1 d PR . . C13 C 0.4442(11) 0.0758(12) 0.1125(10) 0.011(2) Uani 0.50 1 d P . . C14 C 0.3199(7) 0.0895(7) 0.2524(7) 0.0088(12) Uani 0.50 1 d P . . O1 O 0.7155(2) 0.3237(2) 0.4477(2) 0.0124(5) Uani 1 1 d . . . O2 O 0.6232(2) 0.4703(2) 0.5860(2) 0.0143(5) Uani 1 1 d . . . O3 O 0.3720(2) 0.3091(2) 0.7418(2) 0.0092(4) Uani 1 1 d . . . O4 O 0.1547(3) 0.4326(2) 0.9099(2) 0.0141(5) Uani 1 1 d . . . O5 O 0.0321(2) 0.2162(3) 1.0442(3) 0.0197(6) Uani 1 1 d . . . O6 O 0.3156(2) -0.0873(2) 0.7094(2) 0.0138(5) Uani 1 1 d . . . O7 O 0.7930(13) 0.3452(15) -0.0174(13) 0.0102(10) Uani 0.50 1 d PU . . O8 O 0.9059(6) 0.2983(6) -0.2313(6) 0.0197(12) Uani 0.50 1 d P . . O9 O 0.5563(5) 0.1787(5) 0.0538(5) 0.0125(9) Uani 0.50 1 d P . . O10 O 0.3388(5) 0.1776(5) 0.3058(5) 0.0148(10) Uani 0.50 1 d PU . . O11 O 0.2099(5) -0.0007(5) 0.3041(5) 0.0131(9) Uani 0.50 1 d P . . O12 O 0.5884(7) -0.1374(7) -0.1345(7) 0.0213(16) Uani 0.50 1 d P . . O13 O 0.9279(3) 0.1099(3) 0.3638(3) 0.0219(6) Uani 1 1 d . . . H13A H 0.8923 0.0444 0.4490 0.033 Uiso 1 1 d R . . H13B H 1.0181 0.0910 0.3582 0.033 Uiso 1 1 d R . . O14 O 1.0382(2) 0.3988(3) 0.2350(2) 0.0178(5) Uani 1 1 d . . . H14B H 1.0571 0.3924 0.3121 0.027 Uiso 1 1 d R . . H14A H 1.1030 0.4656 0.1701 0.027 Uiso 1 1 d R . . O15 O 0.5674(2) 0.3808(3) 0.2404(2) 0.0155(5) Uani 1 1 d . . . H15A H 0.5186 0.4388 0.2877 0.023 Uiso 1 1 d R . . H15B H 0.4919 0.3314 0.2551 0.023 Uiso 1 1 d R . . O16 O 0.8701(3) 0.6468(3) 0.5209(3) 0.0262(6) Uani 1 1 d . . . H16A H 0.9557 0.6618 0.4519 0.031 Uiso 1 1 d R . . H16B H 0.8033 0.6848 0.4844 0.031 Uiso 1 1 d R . . O17 O 0.5078(6) 0.5760(5) 0.0030(5) 0.0188(11) Uani 0.50 1 d P . . O18 O 0.9021(6) 0.2170(6) -0.2385(6) 0.0228(13) Uani 0.50 1 d P . . O19 O 0.2032(5) 0.1201(5) 0.4077(5) 0.0149(10) Uani 0.50 1 d P . . O20 O 0.7787(13) 0.3546(15) -0.0301(13) 0.0106(11) Uani 0.50 1 d PU . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.00655(8) 0.00712(8) 0.00735(8) -0.00384(6) 0.00085(6) -0.00204(6) C1 0.0064(15) 0.0123(16) 0.0102(15) -0.0049(13) -0.0022(12) 0.0009(12) C2 0.0071(15) 0.0128(16) 0.0090(14) -0.0046(12) 0.0012(12) -0.0018(12) C3 0.0079(15) 0.0131(16) 0.0129(15) -0.0079(13) 0.0012(12) -0.0017(13) C4 0.0094(15) 0.0130(16) 0.0136(15) -0.0067(13) -0.0033(12) -0.0015(12) C5 0.0052(15) 0.0178(17) 0.0178(17) -0.0100(14) 0.0023(13) -0.0053(13) C6 0.0048(14) 0.0113(15) 0.0117(15) -0.0058(12) 0.0009(12) -0.0004(12) C7 0.0039(14) 0.0155(16) 0.0139(15) -0.0083(13) -0.0024(12) 0.0014(12) C8 0.008(3) 0.007(3) 0.011(3) -0.002(2) -0.001(2) -0.002(2) C9 0.006(3) 0.014(3) 0.009(3) -0.002(2) 0.000(2) -0.005(2) C10 0.008(3) 0.017(3) 0.010(3) -0.005(3) 0.001(2) -0.002(3) C11 0.017(5) 0.015(5) 0.006(4) -0.005(4) 0.000(3) 0.002(4) C12 0.007(3) 0.020(4) 0.012(3) -0.005(3) -0.003(3) -0.004(3) C13 0.006(4) 0.019(6) 0.004(4) -0.003(4) 0.001(3) -0.001(4) C14 0.007(3) 0.006(3) 0.010(3) 0.001(2) -0.001(2) -0.003(2) O1 0.0107(11) 0.0153(12) 0.0093(11) -0.0070(9) 0.0019(9) -0.0015(9) O2 0.0095(11) 0.0136(12) 0.0184(12) -0.0103(10) 0.0022(9) -0.0023(9) O3 0.0067(10) 0.0085(11) 0.0105(10) -0.0059(9) 0.0023(9) -0.0024(8) O4 0.0195(12) 0.0099(11) 0.0142(11) -0.0066(10) -0.0056(10) 0.0022(10) O5 0.0089(12) 0.0214(13) 0.0253(13) -0.0153(11) 0.0072(10) -0.0075(10) O6 0.0126(12) 0.0129(12) 0.0160(12) -0.0086(10) -0.0006(9) -0.0036(9) O7 0.0102(13) 0.0103(12) 0.0100(13) -0.0033(9) -0.0036(8) 0.0005(9) O8 0.015(3) 0.023(3) 0.014(3) -0.006(2) 0.006(2) -0.014(2) O9 0.008(2) 0.016(2) 0.012(2) -0.0074(19) 0.0012(18) -0.0001(19) O10 0.0149(13) 0.0147(13) 0.0153(13) -0.0065(9) -0.0043(9) -0.0006(9) O11 0.009(2) 0.016(2) 0.012(2) -0.0050(19) -0.0004(18) -0.0046(18) O12 0.022(3) 0.020(4) 0.020(3) -0.012(3) 0.002(3) -0.003(3) O13 0.0171(13) 0.0145(12) 0.0296(14) 0.0006(11) -0.0109(11) 0.0015(10) O14 0.0152(12) 0.0225(13) 0.0129(11) 0.0007(10) -0.0046(10) -0.0127(10) O15 0.0082(11) 0.0215(13) 0.0198(12) -0.0131(11) -0.0025(10) 0.0007(10) O16 0.0132(12) 0.0480(18) 0.0116(12) -0.0042(12) 0.0004(10) -0.0133(12) O17 0.025(3) 0.015(2) 0.019(2) 0.001(2) -0.017(2) 0.000(2) O18 0.022(3) 0.024(3) 0.022(3) -0.017(3) 0.004(2) -0.009(3) O19 0.014(2) 0.013(2) 0.014(2) -0.0029(19) -0.0015(19) -0.0036(19) O20 0.0105(16) 0.0104(13) 0.0102(15) -0.0032(13) -0.0031(12) 0.0005(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 O1 2.302(2) . ? Gd1 O4 2.351(2) 2_666 ? Gd1 O7 2.353(12) . ? Gd1 O6 2.383(2) 2_656 ? Gd1 O13 2.392(2) . ? Gd1 O14 2.396(2) . ? Gd1 O5 2.405(2) 1_654 ? Gd1 O15 2.421(2) . ? Gd1 O20 2.529(12) . ? C1 O2 1.238(4) . ? C1 O1 1.259(3) . ? C1 C2 1.522(4) . ? C2 C3 1.344(4) . ? C2 O3 1.355(3) . ? C3 C4 1.432(4) . ? C3 H3A 0.9300 . ? C4 O6 1.259(4) . ? C4 C5 1.433(4) . ? C5 C6 1.346(4) . ? C5 H5A 0.9300 . ? C6 O3 1.352(3) . ? C6 C7 1.511(4) . ? C7 O4 1.243(4) . ? C7 O5 1.246(4) . ? C8 O20 1.149(15) . ? C8 O7 1.216(15) . ? C8 O8 1.241(8) . ? C8 C9 1.533(8) . ? C8 O18 1.626(8) . ? C9 C10 1.340(9) . ? C9 O9 1.368(7) . ? C10 C12 1.322(9) 2_655 ? C10 C11 1.446(11) . ? C10 H10A 0.9631 . ? C11 C13 0.658(10) 2_655 ? C11 C12 0.777(11) 2_655 ? C11 O12 1.243(11) . ? C11 C12 1.448(13) . ? C11 O9 1.832(11) 2_655 ? C12 C11 0.777(11) 2_655 ? C12 C12 1.126(14) 2_655 ? C12 C10 1.322(9) 2_655 ? C12 C13 1.347(12) . ? C12 H12A 0.9584 . ? C13 C11 0.658(10) 2_655 ? C13 O12 0.709(10) 2_655 ? C13 O9 1.350(10) . ? C14 O12 1.162(8) 2_655 ? C14 O10 1.214(7) . ? C14 O11 1.264(7) . ? C14 O19 1.671(8) . ? O4 Gd1 2.351(2) 2_666 ? O5 Gd1 2.405(2) 1_456 ? O6 Gd1 2.383(2) 2_656 ? O8 O18 0.819(6) . ? O9 O12 1.337(7) 2_655 ? O9 C11 1.832(11) 2_655 ? O10 O19 1.349(6) . ? O10 O12 1.789(8) 2_655 ? O11 O19 1.805(6) . ? O12 C13 0.709(10) 2_655 ? O12 C14 1.162(8) 2_655 ? O12 O9 1.337(7) 2_655 ? O12 O10 1.789(8) 2_655 ? O13 H13A 0.8459 . ? O13 H13B 0.8439 . ? O14 H14B 0.8477 . ? O14 H14A 0.8498 . ? O15 H15A 0.8544 . ? O15 H15B 0.8416 . ? O16 H16A 0.8447 . ? O16 H16B 0.8393 . ? O17 O17 1.512(9) 2_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 O1 Gd1 O4 94.53(8) . 2_666 ? O1 Gd1 O7 145.5(3) . . ? O4 Gd1 O7 75.4(3) 2_666 . ? O1 Gd1 O6 89.34(7) . 2_656 ? O4 Gd1 O6 147.03(8) 2_666 2_656 ? O7 Gd1 O6 83.0(3) . 2_656 ? O1 Gd1 O13 74.95(8) . . ? O4 Gd1 O13 142.80(8) 2_666 . ? O7 Gd1 O13 131.7(3) . . ? O6 Gd1 O13 69.64(8) 2_656 . ? O1 Gd1 O14 80.17(8) . . ? O4 Gd1 O14 72.45(8) 2_666 . ? O7 Gd1 O14 125.5(3) . . ? O6 Gd1 O14 140.27(8) 2_656 . ? O13 Gd1 O14 70.63(8) . . ? O1 Gd1 O5 146.15(9) . 1_654 ? O4 Gd1 O5 104.28(8) 2_666 1_654 ? O7 Gd1 O5 67.7(3) . 1_654 ? O6 Gd1 O5 89.75(7) 2_656 1_654 ? O13 Gd1 O5 73.06(9) . 1_654 ? O14 Gd1 O5 79.09(8) . 1_654 ? O1 Gd1 O15 73.14(8) . . ? O4 Gd1 O15 76.30(8) 2_666 . ? O7 Gd1 O15 72.4(3) . . ? O6 Gd1 O15 73.57(8) 2_656 . ? O13 Gd1 O15 130.83(8) . . ? O14 Gd1 O15 136.68(8) . . ? O5 Gd1 O15 138.31(8) 1_654 . ? O1 Gd1 O20 142.8(3) . . ? O4 Gd1 O20 74.2(3) 2_666 . ? O7 Gd1 O20 2.8(6) . . ? O6 Gd1 O20 83.0(3) 2_656 . ? O13 Gd1 O20 134.0(3) . . ? O14 Gd1 O20 126.8(3) . . ? O5 Gd1 O20 70.5(3) 1_654 . ? O15 Gd1 O20 69.7(3) . . ? O2 C1 O1 126.5(3) . . ? O2 C1 C2 118.6(3) . . ? O1 C1 C2 114.9(3) . . ? C3 C2 O3 122.6(3) . . ? C3 C2 C1 125.2(3) . . ? O3 C2 C1 112.2(3) . . ? C2 C3 C4 120.3(3) . . ? C2 C3 H3A 119.8 . . ? C4 C3 H3A 119.8 . . ? O6 C4 C3 121.6(3) . . ? O6 C4 C5 123.1(3) . . ? C3 C4 C5 115.3(3) . . ? C6 C5 C4 120.4(3) . . ? C6 C5 H5A 119.8 . . ? C4 C5 H5A 119.8 . . ? C5 C6 O3 122.5(3) . . ? C5 C6 C7 124.6(3) . . ? O3 C6 C7 112.9(3) . . ? O4 C7 O5 126.7(3) . . ? O4 C7 C6 117.5(3) . . ? O5 C7 C6 115.8(3) . . ? O20 C8 O7 9.8(11) . . ? O20 C8 O8 132.0(8) . . ? O7 C8 O8 130.1(8) . . ? O20 C8 C9 114.4(7) . . ? O7 C8 C9 116.8(7) . . ? O8 C8 C9 113.0(5) . . ? O20 C8 O18 158.5(8) . . ? O7 C8 O18 152.2(7) . . ? O8 C8 O18 29.5(3) . . ? C9 C8 O18 86.4(4) . . ? C10 C9 O9 122.6(5) . . ? C10 C9 C8 124.3(5) . . ? O9 C9 C8 112.9(5) . . ? C10 C9 C12 44.7(4) . 2_655 ? O9 C9 C12 78.1(4) . 2_655 ? C8 C9 C12 168.9(5) . 2_655 ? C12 C10 C9 89.9(6) 2_655 . ? C12 C10 C11 32.2(5) 2_655 . ? C9 C10 C11 120.6(7) . . ? C12 C10 C13 44.0(5) 2_655 2_655 ? C9 C10 C13 133.9(6) . 2_655 ? C11 C10 C13 15.1(4) . 2_655 ? C12 C10 H10A 148.9 2_655 . ? C9 C10 H10A 120.1 . . ? C11 C10 H10A 119.3 . . ? C13 C10 H10A 105.7 2_655 . ? C13 C11 C12 140(2) 2_655 2_655 ? C13 C11 O12 25.6(14) 2_655 . ? C12 C11 O12 165.2(14) 2_655 . ? C13 C11 C10 130.1(15) 2_655 . ? C12 C11 C10 65.1(9) 2_655 . ? O12 C11 C10 122.2(9) . . ? C13 C11 C12 110.0(16) 2_655 . ? C12 C11 C12 50.4(10) 2_655 . ? O12 C11 C12 124.1(10) . . ? C10 C11 C12 113.7(10) . . ? C13 C11 O9 35.4(11) 2_655 2_655 ? C12 C11 O9 123.0(12) 2_655 2_655 ? O12 C11 O9 46.9(5) . 2_655 ? C10 C11 O9 165.2(7) . 2_655 ? C12 C11 O9 78.0(6) . 2_655 ? C13 C11 C14 47.2(12) 2_655 2_655 ? C12 C11 C14 142.9(11) 2_655 2_655 ? O12 C11 C14 36.7(5) . 2_655 ? C10 C11 C14 86.7(6) . 2_655 ? C12 C11 C14 157.1(8) . 2_655 ? O9 C11 C14 80.3(5) 2_655 2_655 ? C11 C12 C12 97.4(13) 2_655 2_655 ? C11 C12 C10 82.7(11) 2_655 2_655 ? C12 C12 C10 163.4(11) 2_655 2_655 ? C11 C12 C13 18.5(11) 2_655 . ? C12 C12 C13 91.9(10) 2_655 . ? C10 C12 C13 93.0(7) 2_655 . ? C11 C12 C11 129.6(10) 2_655 . ? C12 C12 C11 32.2(6) 2_655 . ? C10 C12 C11 144.4(10) 2_655 . ? C13 C12 C11 122.3(9) . . ? C11 C12 C13 142.9(11) 2_655 2_655 ? C12 C12 C13 49.0(7) 2_655 2_655 ? C10 C12 C13 124.4(8) 2_655 2_655 ? C13 C12 C13 140.9(6) . 2_655 ? C11 C12 C13 20.3(5) . 2_655 ? C11 C12 C9 126.0(11) 2_655 2_655 ? C12 C12 C9 127.6(10) 2_655 2_655 ? C10 C12 C9 45.4(4) 2_655 2_655 ? C13 C12 C9 138.4(7) . 2_655 ? C11 C12 C9 99.1(8) . 2_655 ? C13 C12 C9 79.6(5) 2_655 2_655 ? C11 C12 H12A 110.0 2_655 . ? C12 C12 H12A 148.0 2_655 . ? C10 C12 H12A 27.3 2_655 . ? C13 C12 H12A 119.2 . . ? C11 C12 H12A 118.4 . . ? C13 C12 H12A 99.6 2_655 . ? C9 C12 H12A 20.5 2_655 . ? C11 C13 O12 131(3) 2_655 2_655 ? C11 C13 C12 22.0(14) 2_655 . ? O12 C13 C12 152.7(16) 2_655 . ? C11 C13 O9 128.3(15) 2_655 . ? O12 C13 O9 73.7(11) 2_655 . ? C12 C13 O9 121.0(8) . . ? C11 C13 C14 114.3(15) 2_655 . ? O12 C13 C14 47.2(8) 2_655 . ? C12 C13 C14 125.7(8) . . ? O9 C13 C14 113.3(8) . . ? C11 C13 C12 49.7(13) 2_655 2_655 ? O12 C13 C12 141.4(12) 2_655 2_655 ? C12 C13 C12 39.1(6) . 2_655 ? O9 C13 C12 82.2(5) . 2_655 ? C14 C13 C12 164.0(8) . 2_655 ? C11 C13 C10 34.9(11) 2_655 2_655 ? O12 C13 C10 118.2(12) 2_655 2_655 ? C12 C13 C10 43.0(5) . 2_655 ? O9 C13 C10 163.0(8) . 2_655 ? C14 C13 C10 83.1(5) . 2_655 ? C12 C13 C10 81.2(6) 2_655 2_655 ? O12 C14 O10 97.7(6) 2_655 . ? O12 C14 O11 133.2(7) 2_655 . ? O10 C14 O11 127.3(6) . . ? O12 C14 C13 26.6(4) 2_655 . ? O10 C14 C13 118.3(6) . . ? O11 C14 C13 114.2(6) . . ? O12 C14 O19 147.4(6) 2_655 . ? O10 C14 O19 52.9(3) . . ? O11 C14 O19 74.5(4) . . ? C13 C14 O19 171.0(6) . . ? O12 C14 C11 39.8(4) 2_655 2_655 ? O10 C14 C11 136.2(6) . 2_655 ? O11 C14 C11 96.5(5) . 2_655 ? C13 C14 C11 18.5(4) . 2_655 ? O19 C14 C11 170.5(5) . 2_655 ? C1 O1 Gd1 154.8(2) . . ? C6 O3 C2 118.7(2) . . ? C7 O4 Gd1 161.3(2) . 2_666 ? C7 O5 Gd1 122.1(2) . 1_456 ? C4 O6 Gd1 150.8(2) . 2_656 ? C8 O7 Gd1 144.1(9) . . ? O18 O8 C8 102.3(7) . . ? O12 O9 C13 30.6(4) 2_655 . ? O12 O9 C9 146.1(5) 2_655 . ? C13 O9 C9 119.5(6) . . ? O12 O9 C11 42.7(4) 2_655 2_655 ? C13 O9 C11 16.4(5) . 2_655 ? C9 O9 C11 104.7(5) . 2_655 ? C14 O10 O19 81.2(4) . . ? C14 O10 O12 40.1(4) . 2_655 ? O19 O10 O12 119.7(4) . 2_655 ? C14 O11 O19 63.1(4) . . ? C13 O12 C14 106.1(11) 2_655 2_655 ? C13 O12 C11 23.6(12) 2_655 . ? C14 O12 C11 103.5(7) 2_655 . ? C13 O12 O9 75.7(10) 2_655 2_655 ? C14 O12 O9 147.5(7) 2_655 2_655 ? C11 O12 O9 90.4(7) . 2_655 ? C13 O12 O10 136.2(12) 2_655 2_655 ? C14 O12 O10 42.3(4) 2_655 2_655 ? C11 O12 O10 144.2(7) . 2_655 ? O9 O12 O10 114.5(5) 2_655 2_655 ? Gd1 O13 H13A 135.4 . . ? Gd1 O13 H13B 130.5 . . ? H13A O13 H13B 93.1 . . ? Gd1 O14 H14B 130.9 . . ? Gd1 O14 H14A 127.9 . . ? H14B O14 H14A 99.3 . . ? Gd1 O15 H15A 125.0 . . ? Gd1 O15 H15B 130.6 . . ? H15A O15 H15B 96.5 . . ? H16A O16 H16B 109.6 . . ? O8 O18 C8 48.2(5) . . ? O10 O19 C14 45.9(3) . . ? O10 O19 O11 88.3(3) . . ? C14 O19 O11 42.4(3) . . ? C8 O20 Gd1 132.6(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 C1 C2 C3 -174.1(3) . . . . ? O1 C1 C2 C3 3.8(5) . . . . ? O2 C1 C2 O3 4.4(4) . . . . ? O1 C1 C2 O3 -177.8(3) . . . . ? O3 C2 C3 C4 -3.3(5) . . . . ? C1 C2 C3 C4 175.0(3) . . . . ? C2 C3 C4 O6 -174.3(3) . . . . ? C2 C3 C4 C5 4.4(5) . . . . ? O6 C4 C5 C6 175.9(3) . . . . ? C3 C4 C5 C6 -2.8(5) . . . . ? C4 C5 C6 O3 -0.2(5) . . . . ? C4 C5 C6 C7 179.0(3) . . . . ? C5 C6 C7 O4 -163.3(3) . . . . ? O3 C6 C7 O4 16.0(4) . . . . ? C5 C6 C7 O5 16.5(5) . . . . ? O3 C6 C7 O5 -164.2(3) . . . . ? O20 C8 C9 C10 -174.1(9) . . . . ? O7 C8 C9 C10 -163.5(9) . . . . ? O8 C8 C9 C10 13.5(9) . . . . ? O18 C8 C9 C10 0.5(7) . . . . ? O20 C8 C9 O9 1.4(10) . . . . ? O7 C8 C9 O9 11.9(10) . . . . ? O8 C8 C9 O9 -171.0(6) . . . . ? O18 C8 C9 O9 176.0(5) . . . . ? O20 C8 C9 C12 -176(3) . . . 2_655 ? O7 C8 C9 C12 -165(3) . . . 2_655 ? O8 C8 C9 C12 12(3) . . . 2_655 ? O18 C8 C9 C12 -1(3) . . . 2_655 ? O9 C9 C10 C12 5.4(8) . . . 2_655 ? C8 C9 C10 C12 -179.5(6) . . . 2_655 ? O9 C9 C10 C11 -4.7(11) . . . . ? C8 C9 C10 C11 170.3(7) . . . . ? C12 C9 C10 C11 -10.2(7) 2_655 . . . ? O9 C9 C10 C13 4.3(11) . . . 2_655 ? C8 C9 C10 C13 179.3(6) . . . 2_655 ? C12 C9 C10 C13 -1.2(6) 2_655 . . 2_655 ? C12 C10 C11 C13 135(3) 2_655 . . 2_655 ? C9 C10 C11 C13 154(2) . . . 2_655 ? C9 C10 C11 C12 19.4(12) . . . 2_655 ? C13 C10 C11 C12 -135(3) 2_655 . . 2_655 ? C12 C10 C11 O12 165.3(16) 2_655 . . . ? C9 C10 C11 O12 -175.4(8) . . . . ? C13 C10 C11 O12 30(2) 2_655 . . . ? C12 C10 C11 C12 -14.0(9) 2_655 . . . ? C9 C10 C11 C12 5.3(11) . . . . ? C13 C10 C11 C12 -149(3) 2_655 . . . ? C12 C10 C11 O9 127(4) 2_655 . . 2_655 ? C9 C10 C11 O9 146(3) . . . 2_655 ? C13 C10 C11 O9 -8.4(17) 2_655 . . 2_655 ? C12 C10 C11 C14 155.2(12) 2_655 . . 2_655 ? C9 C10 C11 C14 174.6(6) . . . 2_655 ? C13 C10 C11 C14 20(2) 2_655 . . 2_655 ? C13 C11 C12 C11 -139(3) 2_655 . . 2_655 ? C12 C11 C12 C11 -0.001(2) 2_655 . . 2_655 ? O12 C11 C12 C11 -162.7(18) . . . 2_655 ? C10 C11 C12 C11 16.6(11) . . . 2_655 ? O9 C11 C12 C11 -153.9(14) 2_655 . . 2_655 ? C14 C11 C12 C11 -135(3) 2_655 . . 2_655 ? C13 C11 C12 C12 -139(3) 2_655 . . 2_655 ? O12 C11 C12 C12 -162.7(18) . . . 2_655 ? C10 C11 C12 C12 16.6(11) . . . 2_655 ? O9 C11 C12 C12 -153.9(14) 2_655 . . 2_655 ? C14 C11 C12 C12 -135(3) 2_655 . . 2_655 ? C13 C11 C12 C10 12(2) 2_655 . . 2_655 ? C12 C11 C12 C10 151(2) 2_655 . . 2_655 ? O12 C11 C12 C10 -12.1(18) . . . 2_655 ? C10 C11 C12 C10 167.2(10) . . . 2_655 ? O9 C11 C12 C10 -3.3(13) 2_655 . . 2_655 ? C14 C11 C12 C10 16(3) 2_655 . . 2_655 ? C13 C11 C12 C13 -159.6(13) 2_655 . . . ? C12 C11 C12 C13 -21.1(13) 2_655 . . . ? O12 C11 C12 C13 176.2(9) . . . . ? C10 C11 C12 C13 -4.5(13) . . . . ? O9 C11 C12 C13 -174.9(8) 2_655 . . . ? C14 C11 C12 C13 -155.8(15) 2_655 . . . ? C12 C11 C12 C13 139(3) 2_655 . . 2_655 ? O12 C11 C12 C13 -24.2(13) . . . 2_655 ? C10 C11 C12 C13 155(2) . . . 2_655 ? O9 C11 C12 C13 -15.3(15) 2_655 . . 2_655 ? C14 C11 C12 C13 3.8(13) 2_655 . . 2_655 ? C13 C11 C12 C9 16.3(18) 2_655 . . 2_655 ? C12 C11 C12 C9 154.8(14) 2_655 . . 2_655 ? O12 C11 C12 C9 -7.9(10) . . . 2_655 ? C10 C11 C12 C9 171.4(7) . . . 2_655 ? O9 C11 C12 C9 0.9(4) 2_655 . . 2_655 ? C14 C11 C12 C9 20(2) 2_655 . . 2_655 ? C12 C12 C13 C11 108(3) 2_655 . . 2_655 ? C10 C12 C13 C11 -56(3) 2_655 . . 2_655 ? C11 C12 C13 C11 119(3) . . . 2_655 ? C13 C12 C13 C11 108(3) 2_655 . . 2_655 ? C9 C12 C13 C11 -55(3) 2_655 . . 2_655 ? C11 C12 C13 O12 1(3) 2_655 . . 2_655 ? C12 C12 C13 O12 109(3) 2_655 . . 2_655 ? C10 C12 C13 O12 -56(3) 2_655 . . 2_655 ? C11 C12 C13 O12 120(3) . . . 2_655 ? C13 C12 C13 O12 109(3) 2_655 . . 2_655 ? C9 C12 C13 O12 -54(3) 2_655 . . 2_655 ? C11 C12 C13 O9 -116(3) 2_655 . . . ? C12 C12 C13 O9 -8.2(12) 2_655 . . . ? C10 C12 C13 O9 -172.3(9) 2_655 . . . ? C11 C12 C13 O9 2.8(15) . . . . ? C13 C12 C13 O9 -8.2(12) 2_655 . . . ? C9 C12 C13 O9 -171.0(7) 2_655 . . . ? C11 C12 C13 C14 65(3) 2_655 . . . ? C12 C12 C13 C14 173.0(10) 2_655 . . . ? C10 C12 C13 C14 8.9(10) 2_655 . . . ? C11 C12 C13 C14 -176.0(6) . . . . ? C13 C12 C13 C14 173.0(10) 2_655 . . . ? C9 C12 C13 C14 10.2(16) 2_655 . . . ? C11 C12 C13 C12 -108(3) 2_655 . . 2_655 ? C10 C12 C13 C12 -164.1(11) 2_655 . . 2_655 ? C11 C12 C13 C12 11.0(7) . . . 2_655 ? C13 C12 C13 C12 0.002(1) 2_655 . . 2_655 ? C9 C12 C13 C12 -162.8(15) 2_655 . . 2_655 ? C11 C12 C13 C10 56(3) 2_655 . . 2_655 ? C12 C12 C13 C10 164.1(11) 2_655 . . 2_655 ? C11 C12 C13 C10 175.1(11) . . . 2_655 ? C13 C12 C13 C10 164.1(11) 2_655 . . 2_655 ? C9 C12 C13 C10 1.3(7) 2_655 . . 2_655 ? C11 C13 C14 O12 -124(3) 2_655 . . 2_655 ? C12 C13 C14 O12 -146(2) . . . 2_655 ? O9 C13 C14 O12 35.4(10) . . . 2_655 ? C12 C13 C14 O12 -129(4) 2_655 . . 2_655 ? C10 C13 C14 O12 -139.6(15) 2_655 . . 2_655 ? C11 C13 C14 O10 -166.4(17) 2_655 . . . ? O12 C13 C14 O10 -42.6(15) 2_655 . . . ? C12 C13 C14 O10 171.7(8) . . . . ? O9 C13 C14 O10 -7.2(11) . . . . ? C12 C13 C14 O10 -172(3) 2_655 . . . ? C10 C13 C14 O10 177.8(6) 2_655 . . . ? C11 C13 C14 O11 17(2) 2_655 . . . ? O12 C13 C14 O11 140.9(14) 2_655 . . . ? C12 C13 C14 O11 -4.8(12) . . . . ? O9 C13 C14 O11 176.3(6) . . . . ? C12 C13 C14 O11 11(3) 2_655 . . . ? C10 C13 C14 O11 1.3(7) 2_655 . . . ? C11 C13 C14 O19 -178(3) 2_655 . . . ? O12 C13 C14 O19 -54(4) 2_655 . . . ? C12 C13 C14 O19 160(3) . . . . ? O9 C13 C14 O19 -19(4) . . . . ? C12 C13 C14 O19 176(2) 2_655 . . . ? C10 C13 C14 O19 166(4) 2_655 . . . ? O12 C13 C14 C11 124(3) 2_655 . . 2_655 ? C12 C13 C14 C11 -21.9(13) . . . 2_655 ? O9 C13 C14 C11 159(2) . . . 2_655 ? C12 C13 C14 C11 -5.6(18) 2_655 . . 2_655 ? C10 C13 C14 C11 -15.8(16) 2_655 . . 2_655 ? O2 C1 O1 Gd1 -97.4(5) . . . . ? C2 C1 O1 Gd1 85.0(5) . . . . ? O4 Gd1 O1 C1 57.1(5) 2_666 . . . ? O7 Gd1 O1 C1 -13.6(8) . . . . ? O6 Gd1 O1 C1 -90.1(5) 2_656 . . . ? O13 Gd1 O1 C1 -159.2(5) . . . . ? O14 Gd1 O1 C1 128.4(5) . . . . ? O5 Gd1 O1 C1 -178.7(4) 1_654 . . . ? O15 Gd1 O1 C1 -17.1(5) . . . . ? O20 Gd1 O1 C1 -12.6(7) . . . . ? C5 C6 O3 C2 1.6(5) . . . . ? C7 C6 O3 C2 -177.7(3) . . . . ? C3 C2 O3 C6 0.2(5) . . . . ? C1 C2 O3 C6 -178.3(3) . . . . ? O5 C7 O4 Gd1 -114.4(6) . . . 2_666 ? C6 C7 O4 Gd1 65.4(8) . . . 2_666 ? O4 C7 O5 Gd1 7.7(5) . . . 1_456 ? C6 C7 O5 Gd1 -172.08(19) . . . 1_456 ? C3 C4 O6 Gd1 -177.1(3) . . . 2_656 ? C5 C4 O6 Gd1 4.3(7) . . . 2_656 ? O20 C8 O7 Gd1 156(7) . . . . ? O8 C8 O7 Gd1 -98.7(15) . . . . ? C9 C8 O7 Gd1 77.7(15) . . . . ? O18 C8 O7 Gd1 -66(2) . . . . ? O1 Gd1 O7 C8 -128.0(12) . . . . ? O4 Gd1 O7 C8 155.6(14) 2_666 . . . ? O6 Gd1 O7 C8 -49.5(14) 2_656 . . . ? O13 Gd1 O7 C8 5.1(16) . . . . ? O14 Gd1 O7 C8 100.2(14) . . . . ? O5 Gd1 O7 C8 43.1(13) 1_654 . . . ? O15 Gd1 O7 C8 -124.4(14) . . . . ? O20 Gd1 O7 C8 -140(13) . . . . ? O20 C8 O8 O18 162.2(11) . . . . ? O7 C8 O8 O18 149.4(11) . . . . ? C9 C8 O8 O18 -27.2(9) . . . . ? C11 C13 O9 O12 129(3) 2_655 . . 2_655 ? C12 C13 O9 O12 154.7(17) . . . 2_655 ? C14 C13 O9 O12 -26.3(8) . . . 2_655 ? C12 C13 O9 O12 149.5(13) 2_655 . . 2_655 ? C10 C13 O9 O12 137(3) 2_655 . . 2_655 ? C11 C13 O9 C9 -27(3) 2_655 . . . ? O12 C13 O9 C9 -156.4(10) 2_655 . . . ? C12 C13 O9 C9 -1.7(12) . . . . ? C14 C13 O9 C9 177.3(6) . . . . ? C12 C13 O9 C9 -6.9(7) 2_655 . . . ? C10 C13 O9 C9 -20(3) 2_655 . . . ? O12 C13 O9 C11 -129(3) 2_655 . . 2_655 ? C12 C13 O9 C11 25.3(19) . . . 2_655 ? C14 C13 O9 C11 -156(3) . . . 2_655 ? C12 C13 O9 C11 20(2) 2_655 . . 2_655 ? C10 C13 O9 C11 7.2(14) 2_655 . . 2_655 ? C10 C9 O9 O12 -18.7(13) . . . 2_655 ? C8 C9 O9 O12 165.8(8) . . . 2_655 ? C12 C9 O9 O12 -14.8(10) 2_655 . . 2_655 ? C10 C9 O9 C13 2.7(10) . . . . ? C8 C9 O9 C13 -172.8(6) . . . . ? C12 C9 O9 C13 6.6(7) 2_655 . . . ? C10 C9 O9 C11 -4.9(8) . . . 2_655 ? C8 C9 O9 C11 179.5(5) . . . 2_655 ? C12 C9 O9 C11 -1.0(4) 2_655 . . 2_655 ? O12 C14 O10 O19 164.4(6) 2_655 . . . ? O11 C14 O10 O19 -1.8(7) . . . . ? C13 C14 O10 O19 -177.8(7) . . . . ? C11 C14 O10 O19 176.1(8) 2_655 . . . ? O11 C14 O10 O12 -166.2(10) . . . 2_655 ? C13 C14 O10 O12 17.8(6) . . . 2_655 ? O19 C14 O10 O12 -164.4(6) . . . 2_655 ? C11 C14 O10 O12 11.7(6) 2_655 . . 2_655 ? O12 C14 O11 O19 -159.6(10) 2_655 . . . ? O10 C14 O11 O19 1.5(6) . . . . ? C13 C14 O11 O19 177.6(7) . . . . ? C11 C14 O11 O19 -177.0(5) 2_655 . . . ? C12 C11 O12 C13 -1(5) 2_655 . . 2_655 ? C10 C11 O12 C13 -116(3) . . . 2_655 ? C12 C11 O12 C13 63(2) . . . 2_655 ? O9 C11 O12 C13 51(2) 2_655 . . 2_655 ? C14 C11 O12 C13 -99(2) 2_655 . . 2_655 ? C13 C11 O12 C14 99(2) 2_655 . . 2_655 ? C12 C11 O12 C14 99(5) 2_655 . . 2_655 ? C10 C11 O12 C14 -17.0(11) . . . 2_655 ? C12 C11 O12 C14 162.2(8) . . . 2_655 ? O9 C11 O12 C14 150.4(8) 2_655 . . 2_655 ? C13 C11 O12 O9 -51(2) 2_655 . . 2_655 ? C12 C11 O12 O9 -52(5) 2_655 . . 2_655 ? C10 C11 O12 O9 -167.4(9) . . . 2_655 ? C12 C11 O12 O9 11.9(9) . . . 2_655 ? C14 C11 O12 O9 -150.4(8) 2_655 . . 2_655 ? C13 C11 O12 O10 85(2) 2_655 . . 2_655 ? C12 C11 O12 O10 84(5) 2_655 . . 2_655 ? C10 C11 O12 O10 -31.5(16) . . . 2_655 ? C12 C11 O12 O10 147.7(9) . . . 2_655 ? O9 C11 O12 O10 135.8(12) 2_655 . . 2_655 ? C14 C11 O12 O10 -14.5(8) 2_655 . . 2_655 ? O20 C8 O18 O8 -38(2) . . . . ? O7 C8 O18 O8 -56.7(18) . . . . ? C9 C8 O18 O8 155.1(8) . . . . ? O12 O10 O19 C14 11.5(4) 2_655 . . . ? C14 O10 O19 O11 1.0(4) . . . . ? O12 O10 O19 O11 12.5(5) 2_655 . . . ? O12 C14 O19 O10 -29.6(11) 2_655 . . . ? O11 C14 O19 O10 178.6(6) . . . . ? C13 C14 O19 O10 13(4) . . . . ? C11 C14 O19 O10 -163(3) 2_655 . . . ? O12 C14 O19 O11 151.9(13) 2_655 . . . ? O10 C14 O19 O11 -178.6(6) . . . . ? C13 C14 O19 O11 -166(4) . . . . ? C11 C14 O19 O11 18(3) 2_655 . . . ? C14 O11 O19 O10 -1.0(4) . . . . ? O7 C8 O20 Gd1 -18(6) . . . . ? O8 C8 O20 Gd1 -100.7(12) . . . . ? C9 C8 O20 Gd1 88.8(11) . . . . ? O18 C8 O20 Gd1 -76(2) . . . . ? O1 Gd1 O20 C8 -135.9(9) . . . . ? O4 Gd1 O20 C8 147.8(11) 2_666 . . . ? O7 Gd1 O20 C8 33(11) . . . . ? O6 Gd1 O20 C8 -56.3(11) 2_656 . . . ? O13 Gd1 O20 C8 -3.5(13) . . . . ? O14 Gd1 O20 C8 94.9(11) . . . . ? O5 Gd1 O20 C8 35.9(10) 1_654 . . . ? O15 Gd1 O20 C8 -131.3(11) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.024 _refine_diff_density_min -1.213 _refine_diff_density_rms 0.138 # Attachment 'Tb-4.cif' data_Tb-4 _database_code_depnum_ccdc_archive 'CCDC 716753' #TrackingRef 'Tb-4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H30 O30 Tb2' _chemical_formula_weight 1080.29 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 9.508(4) _cell_length_b 9.648(4) _cell_length_c 10.153(3) _cell_angle_alpha 69.650(11) _cell_angle_beta 68.520(12) _cell_angle_gamma 83.930(13) _cell_volume 812.3(5) _cell_formula_units_Z 1 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 2898 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 25.1 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.208 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 526 _exptl_absorpt_coefficient_mu 4.436 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6653 _exptl_absorpt_correction_T_max 0.7767 _exptl_absorpt_process_details Crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8397 _diffrn_reflns_av_R_equivalents 0.0672 _diffrn_reflns_av_sigmaI/netI 0.0885 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 25.10 _reflns_number_total 2898 _reflns_number_gt 2458 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. A few of restraints containing 'isor' and 'simu' have been used to restrict the disordered ligand and water molecules. ; _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^)+(0.0388P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2898 _refine_ls_number_parameters 316 _refine_ls_number_restraints 84 _refine_ls_R_factor_all 0.0452 _refine_ls_R_factor_gt 0.0403 _refine_ls_wR_factor_ref 0.0948 _refine_ls_wR_factor_gt 0.0925 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tb1 Tb 0.82591(3) 0.30944(3) 0.21043(4) 0.01035(14) Uani 1 1 d . . . C1 C 0.6179(8) 0.3619(8) 0.5482(8) 0.0125(16) Uani 1 1 d . . . C2 C 0.4768(7) 0.2594(7) 0.6372(7) 0.0102(15) Uani 1 1 d U . . C3 C 0.4609(7) 0.1319(7) 0.6198(7) 0.0107(15) Uani 1 1 d U . . H3A H 0.5356 0.1038 0.5448 0.013 Uiso 1 1 calc R . . C4 C 0.3294(8) 0.0367(7) 0.7160(8) 0.0131(16) Uani 1 1 d . . . C5 C 0.2200(7) 0.0951(8) 0.8231(8) 0.0150(17) Uani 1 1 d . . . H5A H 0.1313 0.0412 0.8886 0.018 Uiso 1 1 calc R . . C6 C 0.2440(7) 0.2270(7) 0.8299(7) 0.0097(15) Uani 1 1 d . . . C7 C 0.1349(7) 0.2989(8) 0.9377(8) 0.0119(16) Uani 1 1 d U . . C8 C 0.8059(15) 0.2851(15) -0.1100(15) 0.011(3) Uani 0.50 1 d PU . . C9 C 0.6795(15) 0.1736(15) -0.0664(15) 0.011(3) Uani 0.50 1 d PU . . C10 C 0.6894(16) 0.0780(16) -0.1376(16) 0.018(3) Uani 0.50 1 d P . . H10A H 0.7750 0.0827 -0.2268 0.021 Uiso 0.50 1 d PR . . C11 C 0.5773(19) -0.036(2) -0.0773(18) 0.009(4) Uani 0.50 1 d PU . . C12 C 0.4504(16) -0.0310(18) 0.0515(17) 0.015(4) Uani 0.50 1 d P . . H12A H 0.3693 -0.1029 0.0957 0.018 Uiso 0.50 1 d PR . . C13 C 0.443(2) 0.076(2) 0.111(2) 0.010(4) Uani 0.50 1 d PU . . C14 C 0.3193(15) 0.0900(15) 0.2566(16) 0.010(3) Uani 0.50 1 d PU . . O1 O 0.7168(5) 0.3237(5) 0.4469(5) 0.0110(11) Uani 1 1 d . . . O2 O 0.6238(5) 0.4701(5) 0.5860(5) 0.0146(11) Uani 1 1 d . . . O3 O 0.3733(5) 0.3095(5) 0.7417(5) 0.0114(11) Uani 1 1 d . . . O4 O 0.1547(5) 0.4337(5) 0.9100(5) 0.0150(11) Uani 1 1 d . . . O5 O 0.0321(5) 0.2182(6) 1.0433(6) 0.0211(13) Uani 1 1 d . . . O6 O 0.3144(5) -0.0887(5) 0.7103(5) 0.0159(12) Uani 1 1 d . . . O7 O 0.788(3) 0.343(3) -0.007(2) 0.0307(18) Uani 0.50 1 d PU . . O8 O 0.9088(13) 0.3029(13) -0.2315(13) 0.022(3) Uani 0.50 1 d P . . O9 O 0.5558(10) 0.1797(10) 0.0545(10) 0.011(2) Uani 0.50 1 d P . . O10 O 0.3382(10) 0.1772(11) 0.3078(11) 0.016(2) Uani 0.50 1 d P . . O11 O 0.2109(10) -0.0003(10) 0.3049(10) 0.015(2) Uani 0.50 1 d P . . O12 O 0.5894(12) -0.1369(13) -0.1329(12) 0.021(3) Uani 0.50 1 d P . . O13 O 0.9274(6) 0.1095(5) 0.3631(6) 0.0238(13) Uani 1 1 d . . . H13A H 0.8918 0.0440 0.4482 0.036 Uiso 1 1 d R . . H13B H 1.0177 0.0905 0.3575 0.036 Uiso 1 1 d R . . O14 O 1.0359(5) 0.3978(5) 0.2348(5) 0.0183(12) Uani 1 1 d . . . H14B H 1.0548 0.3915 0.3119 0.027 Uiso 1 1 d R . . H14A H 1.1007 0.4647 0.1698 0.027 Uiso 1 1 d R . . O15 O 0.5692(5) 0.3806(5) 0.2394(5) 0.0168(12) Uani 1 1 d U . . H15A H 0.5204 0.4385 0.2868 0.025 Uiso 1 1 d R . . H15B H 0.4936 0.3312 0.2541 0.025 Uiso 1 1 d R . . O16 O 0.8696(6) 0.6457(6) 0.5220(6) 0.0279(14) Uani 1 1 d . . . H16A H 0.9530 0.6605 0.4553 0.033 Uiso 1 1 d R . . H16B H 0.8006 0.6836 0.4879 0.033 Uiso 1 1 d R . . O17 O 0.5100(11) 0.5730(10) 0.0028(12) 0.019(2) Uani 0.50 1 d P . . O18 O 0.9021(13) 0.2197(13) -0.2371(13) 0.021(3) Uani 0.50 1 d P . . O19 O 0.2022(10) 0.1204(11) 0.4064(11) 0.017(2) Uani 0.50 1 d P . . O20 O 0.7850(18) 0.3538(17) -0.0329(15) 0.0306(18) Uani 0.75 1 d PU . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tb1 0.0080(2) 0.0090(2) 0.0126(2) -0.00644(15) 0.00001(15) 0.00254(15) C1 0.011(4) 0.012(4) 0.013(4) -0.003(3) -0.004(3) 0.001(3) C2 0.0096(17) 0.0103(17) 0.0104(17) -0.0037(10) -0.0031(10) 0.0008(10) C3 0.0101(18) 0.0107(18) 0.0109(17) -0.0040(10) -0.0030(11) 0.0001(10) C4 0.010(4) 0.008(4) 0.019(4) -0.004(3) -0.003(3) 0.001(3) C5 0.004(3) 0.014(4) 0.023(4) -0.008(3) 0.003(3) -0.003(3) C6 0.004(3) 0.013(4) 0.011(4) -0.004(3) -0.001(3) 0.000(3) C7 0.004(3) 0.021(4) 0.014(4) -0.010(3) -0.004(3) 0.006(3) C8 0.012(3) 0.011(3) 0.011(3) -0.0040(14) -0.0040(14) 0.0003(10) C9 0.009(6) 0.016(6) 0.005(6) -0.002(5) 0.001(5) 0.000(5) C10 0.020(9) 0.021(9) 0.013(8) -0.011(7) -0.006(7) 0.014(7) C11 0.009(4) 0.009(4) 0.009(4) -0.0034(15) -0.0033(16) 0.0003(10) C12 0.010(8) 0.011(9) 0.030(10) -0.015(8) -0.006(7) 0.003(7) C13 0.010(4) 0.010(4) 0.010(4) -0.0033(16) -0.0036(17) 0.0002(10) C14 0.007(6) 0.006(6) 0.011(6) 0.004(5) -0.003(5) 0.000(5) O1 0.009(2) 0.010(3) 0.012(3) -0.007(2) 0.003(2) 0.000(2) O2 0.009(3) 0.015(3) 0.021(3) -0.014(2) 0.002(2) 0.000(2) O3 0.008(2) 0.009(3) 0.015(3) -0.008(2) 0.003(2) 0.000(2) O4 0.014(3) 0.010(3) 0.020(3) -0.007(2) -0.003(2) 0.005(2) O5 0.011(3) 0.025(3) 0.027(3) -0.021(3) 0.007(2) -0.004(2) O6 0.014(3) 0.013(3) 0.026(3) -0.017(2) -0.003(2) 0.003(2) O7 0.0305(19) 0.0306(19) 0.031(2) -0.0103(10) -0.0106(9) 0.0014(8) O8 0.021(7) 0.020(7) 0.015(6) -0.005(6) 0.006(5) -0.010(6) O9 0.010(5) 0.013(5) 0.013(5) -0.007(4) -0.004(4) 0.003(4) O10 0.008(5) 0.022(6) 0.020(6) -0.012(5) -0.001(4) 0.000(5) O11 0.007(5) 0.016(5) 0.014(5) -0.002(4) 0.001(4) -0.001(4) O12 0.017(6) 0.023(7) 0.031(8) -0.022(6) -0.006(5) 0.002(6) O13 0.017(3) 0.015(3) 0.034(3) 0.001(3) -0.014(3) 0.004(2) O14 0.019(3) 0.022(3) 0.011(3) 0.002(2) -0.007(2) -0.011(2) O15 0.0157(14) 0.0171(14) 0.0180(14) -0.0072(10) -0.0054(10) 0.0015(9) O16 0.012(3) 0.049(4) 0.016(3) -0.004(3) -0.003(2) -0.007(3) O17 0.017(6) 0.015(5) 0.026(6) -0.005(5) -0.010(5) 0.004(5) O18 0.012(6) 0.024(7) 0.019(6) -0.013(6) 0.008(5) -0.002(6) O19 0.007(5) 0.018(6) 0.019(6) 0.003(5) -0.006(4) -0.004(4) O20 0.0305(19) 0.0306(18) 0.030(2) -0.0103(10) -0.0105(9) 0.0015(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 Tb1 O7 2.27(2) . ? Tb1 O1 2.288(4) . ? Tb1 O4 2.344(5) 2_666 ? Tb1 O6 2.364(5) 2_656 ? Tb1 O14 2.376(5) . ? Tb1 O13 2.383(5) . ? Tb1 O5 2.394(5) 1_654 ? Tb1 O15 2.404(5) . ? Tb1 O20 2.524(13) . ? C1 O2 1.243(8) . ? C1 O1 1.250(8) . ? C1 C2 1.538(9) . ? C2 C3 1.333(9) . ? C2 O3 1.349(7) . ? C3 C4 1.444(9) . ? C3 H3A 0.9300 . ? C4 O6 1.257(8) . ? C4 C5 1.433(9) . ? C5 C6 1.346(9) . ? C5 H5A 0.9300 . ? C6 O3 1.361(8) . ? C6 C7 1.516(9) . ? C7 O5 1.234(8) . ? C7 O4 1.251(8) . ? C8 O20 1.145(19) . ? C8 O8 1.230(17) . ? C8 O7 1.30(3) . ? C8 C9 1.533(19) . ? C8 O18 1.575(17) . ? C9 C10 1.333(19) . ? C9 O9 1.368(15) . ? C10 C12 1.32(2) 2_655 ? C10 C11 1.42(2) . ? C10 H10A 0.9609 . ? C11 C13 0.68(2) 2_655 ? C11 C12 0.765(17) 2_655 ? C11 O12 1.26(2) . ? C11 C12 1.43(2) . ? C11 O9 1.87(2) 2_655 ? C12 C11 0.765(17) 2_655 ? C12 C12 1.14(3) 2_655 ? C12 C10 1.32(2) 2_655 ? C12 C13 1.35(3) . ? C12 H12A 0.9586 . ? C13 C11 0.68(2) 2_655 ? C13 O12 0.707(17) 2_655 ? C13 O9 1.36(2) . ? C13 C14 1.56(2) . ? C14 O10 1.190(16) . ? C14 O12 1.193(16) 2_655 ? C14 O11 1.258(16) . ? C14 O19 1.625(17) . ? O4 Tb1 2.344(5) 2_666 ? O5 Tb1 2.394(5) 1_456 ? O6 Tb1 2.364(5) 2_656 ? O8 O18 0.834(12) . ? O9 O12 1.341(13) 2_655 ? O9 C11 1.87(2) 2_655 ? O10 O19 1.340(12) . ? O10 O12 1.818(14) 2_655 ? O11 O19 1.782(14) . ? O12 C13 0.707(17) 2_655 ? O12 C14 1.193(16) 2_655 ? O12 O9 1.341(13) 2_655 ? O12 O10 1.818(14) 2_655 ? O13 H13A 0.8441 . ? O13 H13B 0.8434 . ? O14 H14B 0.8468 . ? O14 H14A 0.8490 . ? O15 H15A 0.8532 . ? O15 H15B 0.8423 . ? O16 H16A 0.8190 . ? O16 H16B 0.8432 . ? O17 O17 1.464(19) 2_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 O7 Tb1 O1 144.6(6) . . ? O7 Tb1 O4 75.8(6) . 2_666 ? O1 Tb1 O4 94.46(16) . 2_666 ? O7 Tb1 O6 81.9(6) . 2_656 ? O1 Tb1 O6 89.80(16) . 2_656 ? O4 Tb1 O6 147.05(16) 2_666 2_656 ? O7 Tb1 O14 126.7(6) . . ? O1 Tb1 O14 79.82(16) . . ? O4 Tb1 O14 72.30(16) 2_666 . ? O6 Tb1 O14 140.43(16) 2_656 . ? O7 Tb1 O13 131.8(6) . . ? O1 Tb1 O13 75.08(17) . . ? O4 Tb1 O13 142.87(17) 2_666 . ? O6 Tb1 O13 69.61(17) 2_656 . ? O14 Tb1 O13 70.82(17) . . ? O7 Tb1 O5 68.6(6) . 1_654 ? O1 Tb1 O5 146.17(18) . 1_654 ? O4 Tb1 O5 103.70(16) 2_666 1_654 ? O6 Tb1 O5 90.07(16) 2_656 1_654 ? O14 Tb1 O5 78.91(17) . 1_654 ? O13 Tb1 O5 73.22(18) . 1_654 ? O7 Tb1 O15 71.0(6) . . ? O1 Tb1 O15 73.60(16) . . ? O4 Tb1 O15 76.24(16) 2_666 . ? O6 Tb1 O15 73.70(16) 2_656 . ? O14 Tb1 O15 136.62(17) . . ? O13 Tb1 O15 131.10(17) . . ? O5 Tb1 O15 138.15(17) 1_654 . ? O7 Tb1 O20 1.6(9) . . ? O1 Tb1 O20 144.2(4) . . ? O4 Tb1 O20 74.2(4) 2_666 . ? O6 Tb1 O20 83.4(4) 2_656 . ? O14 Tb1 O20 125.8(4) . . ? O13 Tb1 O20 133.2(4) . . ? O5 Tb1 O20 69.2(4) 1_654 . ? O15 Tb1 O20 70.8(4) . . ? O2 C1 O1 127.1(6) . . ? O2 C1 C2 117.7(6) . . ? O1 C1 C2 115.2(6) . . ? C3 C2 O3 123.5(6) . . ? C3 C2 C1 124.5(6) . . ? O3 C2 C1 111.9(6) . . ? C2 C3 C4 120.9(7) . . ? C2 C3 H3A 119.5 . . ? C4 C3 H3A 119.5 . . ? O6 C4 C5 122.8(6) . . ? O6 C4 C3 123.1(6) . . ? C5 C4 C3 114.1(6) . . ? C6 C5 C4 120.8(6) . . ? C6 C5 H5A 119.6 . . ? C4 C5 H5A 119.6 . . ? C5 C6 O3 122.9(6) . . ? C5 C6 C7 124.8(6) . . ? O3 C6 C7 112.2(6) . . ? O5 C7 O4 126.2(6) . . ? O5 C7 C6 116.2(6) . . ? O4 C7 C6 117.6(6) . . ? O20 C8 O8 127.0(16) . . ? O20 C8 O7 9.9(16) . . ? O8 C8 O7 130.2(16) . . ? O20 C8 C9 115.6(14) . . ? O8 C8 C9 116.8(13) . . ? O7 C8 C9 113.0(14) . . ? O20 C8 O18 155.9(15) . . ? O8 C8 O18 31.7(7) . . ? O7 C8 O18 154.0(15) . . ? C9 C8 O18 87.9(10) . . ? C10 C9 O9 123.0(13) . . ? C10 C9 C8 123.5(12) . . ? O9 C9 C8 113.5(11) . . ? C10 C9 C12 44.7(9) . 2_655 ? O9 C9 C12 78.4(9) . 2_655 ? C8 C9 C12 167.9(11) . 2_655 ? C12 C10 C9 90.0(13) 2_655 . ? C12 C10 C11 32.2(8) 2_655 . ? C9 C10 C11 119.9(14) . . ? C12 C10 C13 44.2(11) 2_655 2_655 ? C9 C10 C13 134.0(13) . 2_655 ? C11 C10 C13 15.4(9) . 2_655 ? C12 C10 H10A 148.6 2_655 . ? C9 C10 H10A 120.1 . . ? C11 C10 H10A 119.8 . . ? C13 C10 H10A 105.7 2_655 . ? C13 C11 C12 138(4) 2_655 2_655 ? C13 C11 O12 25(2) 2_655 . ? C12 C11 O12 163(3) 2_655 . ? C13 C11 C10 131(3) 2_655 . ? C12 C11 C10 66.5(18) 2_655 . ? O12 C11 C10 122.1(14) . . ? C13 C11 C12 108(3) 2_655 . ? C12 C11 C12 53(2) 2_655 . ? O12 C11 C12 121.6(16) . . ? C10 C11 C12 116.3(19) . . ? C13 C11 O9 34(2) 2_655 2_655 ? C12 C11 O9 122(2) 2_655 2_655 ? O12 C11 O9 45.6(9) . 2_655 ? C10 C11 O9 164.0(14) . 2_655 ? C12 C11 O9 77.0(10) . 2_655 ? C13 C11 C14 46(2) 2_655 2_655 ? C12 C11 C14 142(2) 2_655 2_655 ? O12 C11 C14 36.3(8) . 2_655 ? C10 C11 C14 87.3(11) . 2_655 ? C12 C11 C14 154.4(15) . 2_655 ? O9 C11 C14 78.2(9) 2_655 2_655 ? C13 C11 C11 121(3) 2_655 2_655 ? C12 C11 C11 34.9(15) 2_655 2_655 ? O12 C11 C11 138.1(18) . 2_655 ? C10 C11 C11 99.5(17) . 2_655 ? C12 C11 C11 17.8(8) . 2_655 ? O9 C11 C11 92.6(12) 2_655 2_655 ? C14 C11 C11 162.3(15) 2_655 2_655 ? C11 C12 C12 95(3) 2_655 2_655 ? C11 C12 C10 81(2) 2_655 2_655 ? C12 C12 C10 160(2) 2_655 2_655 ? C11 C12 C13 19.5(18) 2_655 . ? C12 C12 C13 89.8(19) 2_655 . ? C10 C12 C13 92.8(14) 2_655 . ? C11 C12 C11 127(2) 2_655 . ? C12 C12 C11 32.2(10) 2_655 . ? C10 C12 C11 146.1(18) 2_655 . ? C13 C12 C11 120.1(15) . . ? C11 C12 C13 141(2) 2_655 2_655 ? C12 C12 C13 49.8(14) 2_655 2_655 ? C10 C12 C13 124.8(15) 2_655 2_655 ? C13 C12 C13 139.6(12) . 2_655 ? C11 C12 C13 21.3(8) . 2_655 ? C11 C12 C9 124(2) 2_655 2_655 ? C12 C12 C9 128(2) 2_655 2_655 ? C10 C12 C9 45.3(9) 2_655 2_655 ? C13 C12 C9 137.9(13) . 2_655 ? C11 C12 C9 101.0(14) . 2_655 ? C13 C12 C9 80.1(11) 2_655 2_655 ? C11 C12 H12A 109.1 2_655 . ? C12 C12 H12A 148.6 2_655 . ? C10 C12 H12A 27.7 2_655 . ? C13 C12 H12A 119.5 . . ? C11 C12 H12A 120.4 . . ? C13 C12 H12A 100.2 2_655 . ? C9 C12 H12A 21.0 2_655 . ? C11 C13 O12 132(4) 2_655 2_655 ? C11 C13 C12 22(2) 2_655 . ? O12 C13 C12 154(3) 2_655 . ? C11 C13 O9 130(3) 2_655 . ? O12 C13 O9 73(2) 2_655 . ? C12 C13 O9 122.3(15) . . ? C11 C13 C14 116(3) 2_655 . ? O12 C13 C14 46.9(17) 2_655 . ? C12 C13 C14 126.5(15) . . ? O9 C13 C14 111.0(16) . . ? C11 C13 C12 50(2) 2_655 2_655 ? O12 C13 C12 141(2) 2_655 2_655 ? C12 C13 C12 40.4(12) . 2_655 ? O9 C13 C12 82.7(11) . 2_655 ? C14 C13 C12 166.0(16) . 2_655 ? C11 C13 C10 34(2) 2_655 2_655 ? O12 C13 C10 118(2) 2_655 2_655 ? C12 C13 C10 43.0(9) . 2_655 ? O9 C13 C10 164.4(16) . 2_655 ? C14 C13 C10 84.3(10) . 2_655 ? C12 C13 C10 81.9(12) 2_655 2_655 ? O10 C14 O12 99.4(13) . 2_655 ? O10 C14 O11 129.4(14) . . ? O12 C14 O11 129.1(14) 2_655 . ? O10 C14 C13 119.2(14) . . ? O12 C14 C13 25.6(8) 2_655 . ? O11 C14 C13 111.5(13) . . ? O10 C14 O19 54.2(8) . . ? O12 C14 O19 149.0(13) 2_655 . ? O11 C14 O19 75.2(9) . . ? C13 C14 O19 173.4(14) . . ? O10 C14 C11 136.9(12) . 2_655 ? O12 C14 C11 38.8(8) 2_655 2_655 ? O11 C14 C11 93.7(11) . 2_655 ? C13 C14 C11 18.2(8) . 2_655 ? O19 C14 C11 168.1(11) . 2_655 ? C1 O1 Tb1 154.6(5) . . ? C2 O3 C6 117.6(5) . . ? C7 O4 Tb1 161.3(5) . 2_666 ? C7 O5 Tb1 123.1(4) . 1_456 ? C4 O6 Tb1 151.7(5) . 2_656 ? C8 O7 Tb1 144.8(16) . . ? O18 O8 C8 97.6(16) . . ? O12 O9 C13 30.3(7) 2_655 . ? O12 O9 C9 144.7(11) 2_655 . ? C13 O9 C9 118.0(12) . . ? O12 O9 C11 42.3(8) 2_655 2_655 ? C13 O9 C11 15.9(10) . 2_655 ? C9 O9 C11 103.5(9) . 2_655 ? C14 O10 O19 79.7(10) . . ? C14 O10 O12 40.3(8) . 2_655 ? O19 O10 O12 118.0(8) . 2_655 ? C14 O11 O19 61.8(8) . . ? C13 O12 C14 107(2) 2_655 2_655 ? C13 O12 C11 23.4(19) 2_655 . ? C14 O12 C11 104.9(13) 2_655 . ? C13 O12 O9 77(2) 2_655 2_655 ? C14 O12 O9 144.1(13) 2_655 2_655 ? C11 O12 O9 92.1(12) . 2_655 ? C13 O12 O10 136(2) 2_655 2_655 ? C14 O12 O10 40.2(8) 2_655 2_655 ? C11 O12 O10 143.6(11) . 2_655 ? O9 O12 O10 112.4(8) 2_655 2_655 ? Tb1 O13 H13A 135.3 . . ? Tb1 O13 H13B 130.5 . . ? H13A O13 H13B 93.1 . . ? Tb1 O14 H14B 131.0 . . ? Tb1 O14 H14A 128.0 . . ? H14B O14 H14A 99.1 . . ? Tb1 O15 H15A 124.9 . . ? Tb1 O15 H15B 130.6 . . ? H15A O15 H15B 96.6 . . ? H16A O16 H16B 111.6 . . ? O8 O18 C8 50.8(12) . . ? O10 O19 C14 46.1(7) . . ? O10 O19 O11 89.1(8) . . ? C14 O19 O11 43.0(6) . . ? C8 O20 Tb1 133.7(12) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 C1 C2 C3 -173.0(7) . . . . ? O1 C1 C2 C3 5.2(10) . . . . ? O2 C1 C2 O3 3.5(9) . . . . ? O1 C1 C2 O3 -178.3(6) . . . . ? O3 C2 C3 C4 -0.9(11) . . . . ? C1 C2 C3 C4 175.2(6) . . . . ? C2 C3 C4 O6 -175.1(7) . . . . ? C2 C3 C4 C5 2.4(10) . . . . ? O6 C4 C5 C6 176.8(7) . . . . ? C3 C4 C5 C6 -0.7(10) . . . . ? C4 C5 C6 O3 -2.6(11) . . . . ? C4 C5 C6 C7 179.3(7) . . . . ? C5 C6 C7 O5 14.2(10) . . . . ? O3 C6 C7 O5 -164.1(6) . . . . ? C5 C6 C7 O4 -164.2(7) . . . . ? O3 C6 C7 O4 17.6(9) . . . . ? O20 C8 C9 C10 -175.4(15) . . . . ? O8 C8 C9 C10 13(2) . . . . ? O7 C8 C9 C10 -164.9(16) . . . . ? O18 C8 C9 C10 -0.9(16) . . . . ? O20 C8 C9 O9 3.7(19) . . . . ? O8 C8 C9 O9 -168.2(12) . . . . ? O7 C8 C9 O9 14.2(19) . . . . ? O18 C8 C9 O9 178.2(11) . . . . ? O20 C8 C9 C12 174(5) . . . 2_655 ? O8 C8 C9 C12 2(6) . . . 2_655 ? O7 C8 C9 C12 -176(5) . . . 2_655 ? O18 C8 C9 C12 -12(6) . . . 2_655 ? O9 C9 C10 C12 4.2(17) . . . 2_655 ? C8 C9 C10 C12 -176.8(14) . . . 2_655 ? O9 C9 C10 C11 -8(2) . . . . ? C8 C9 C10 C11 170.8(13) . . . . ? C12 C9 C10 C11 -12.4(12) 2_655 . . . ? O9 C9 C10 C13 0(2) . . . 2_655 ? C8 C9 C10 C13 178.8(12) . . . 2_655 ? C12 C9 C10 C13 -4.4(13) 2_655 . . 2_655 ? C12 C10 C11 C13 134(5) 2_655 . . 2_655 ? C9 C10 C11 C13 158(3) . . . 2_655 ? C9 C10 C11 C12 24(2) . . . 2_655 ? C13 C10 C11 C12 -134(5) 2_655 . . 2_655 ? C12 C10 C11 O12 163(3) 2_655 . . . ? C9 C10 C11 O12 -173.2(15) . . . . ? C13 C10 C11 O12 29(3) 2_655 . . . ? C12 C10 C11 C12 -18(2) 2_655 . . . ? C9 C10 C11 C12 6(2) . . . . ? C13 C10 C11 C12 -152(5) 2_655 . . . ? C12 C10 C11 O9 127(6) 2_655 . . 2_655 ? C9 C10 C11 O9 151(4) . . . 2_655 ? C13 C10 C11 O9 -7(3) 2_655 . . 2_655 ? C12 C10 C11 C14 152(2) 2_655 . . 2_655 ? C9 C10 C11 C14 175.8(13) . . . 2_655 ? C13 C10 C11 C14 18(3) 2_655 . . 2_655 ? C12 C10 C11 C11 -11.5(14) 2_655 . . 2_655 ? C9 C10 C11 C11 12(2) . . . 2_655 ? C13 C10 C11 C11 -146(4) 2_655 . . 2_655 ? C13 C11 C12 C11 -137(4) 2_655 . . 2_655 ? C12 C11 C12 C11 -0.002(3) 2_655 . . 2_655 ? O12 C11 C12 C11 -160(3) . . . 2_655 ? C10 C11 C12 C11 21(2) . . . 2_655 ? O9 C11 C12 C11 -150(3) 2_655 . . 2_655 ? C14 C11 C12 C11 -135(4) 2_655 . . 2_655 ? C13 C11 C12 C12 -137(4) 2_655 . . 2_655 ? O12 C11 C12 C12 -160(3) . . . 2_655 ? C10 C11 C12 C12 21(2) . . . 2_655 ? O9 C11 C12 C12 -150(3) 2_655 . . 2_655 ? C14 C11 C12 C12 -135(4) 2_655 . . 2_655 ? C11 C11 C12 C12 0.002(2) 2_655 . . 2_655 ? C13 C11 C12 C10 5(4) 2_655 . . 2_655 ? C12 C11 C12 C10 143(4) 2_655 . . 2_655 ? O12 C11 C12 C10 -18(4) . . . 2_655 ? C10 C11 C12 C10 163(2) . . . 2_655 ? O9 C11 C12 C10 -7(3) 2_655 . . 2_655 ? C14 C11 C12 C10 7(5) 2_655 . . 2_655 ? C11 C11 C12 C10 143(4) 2_655 . . 2_655 ? C13 C11 C12 C13 -159(2) 2_655 . . . ? C12 C11 C12 C13 -22(2) 2_655 . . . ? O12 C11 C12 C13 177.9(17) . . . . ? C10 C11 C12 C13 -1(2) . . . . ? O9 C11 C12 C13 -171.9(16) 2_655 . . . ? C14 C11 C12 C13 -157(2) 2_655 . . . ? C11 C11 C12 C13 -22(2) 2_655 . . . ? C12 C11 C12 C13 137(4) 2_655 . . 2_655 ? O12 C11 C12 C13 -23(2) . . . 2_655 ? C10 C11 C12 C13 158(4) . . . 2_655 ? O9 C11 C12 C13 -13(2) 2_655 . . 2_655 ? C14 C11 C12 C13 2(2) 2_655 . . 2_655 ? C11 C11 C12 C13 137(4) 2_655 . . 2_655 ? C13 C11 C12 C9 12(3) 2_655 . . 2_655 ? C12 C11 C12 C9 149(3) 2_655 . . 2_655 ? O12 C11 C12 C9 -11.3(18) . . . 2_655 ? C10 C11 C12 C9 169.5(13) . . . 2_655 ? O9 C11 C12 C9 -1.0(8) 2_655 . . 2_655 ? C14 C11 C12 C9 14(3) 2_655 . . 2_655 ? C11 C11 C12 C9 149(3) 2_655 . . 2_655 ? C12 C12 C13 C11 106(6) 2_655 . . 2_655 ? C10 C12 C13 C11 -54(5) 2_655 . . 2_655 ? C11 C12 C13 C11 117(5) . . . 2_655 ? C13 C12 C13 C11 106(6) 2_655 . . 2_655 ? C9 C12 C13 C11 -49(5) 2_655 . . 2_655 ? C11 C12 C13 O12 2(6) 2_655 . . 2_655 ? C12 C12 C13 O12 108(6) 2_655 . . 2_655 ? C10 C12 C13 O12 -52(6) 2_655 . . 2_655 ? C11 C12 C13 O12 120(5) . . . 2_655 ? C13 C12 C13 O12 108(6) 2_655 . . 2_655 ? C9 C12 C13 O12 -47(7) 2_655 . . 2_655 ? C11 C12 C13 O9 -119(6) 2_655 . . . ? C12 C12 C13 O9 -13(2) 2_655 . . . ? C10 C12 C13 O9 -172.9(15) 2_655 . . . ? C11 C12 C13 O9 -1(3) . . . . ? C13 C12 C13 O9 -13(2) 2_655 . . . ? C9 C12 C13 O9 -168.0(14) 2_655 . . . ? C11 C12 C13 C14 67(5) 2_655 . . . ? C12 C12 C13 C14 173.1(17) 2_655 . . . ? C10 C12 C13 C14 13(2) 2_655 . . . ? C11 C12 C13 C14 -175.4(13) . . . . ? C13 C12 C13 C14 173.1(17) 2_655 . . . ? C9 C12 C13 C14 18(3) 2_655 . . . ? C11 C12 C13 C12 -106(6) 2_655 . . 2_655 ? C10 C12 C13 C12 -160(2) 2_655 . . 2_655 ? C11 C12 C13 C12 11.5(11) . . . 2_655 ? C13 C12 C13 C12 0.001(2) 2_655 . . 2_655 ? C9 C12 C13 C12 -155(3) 2_655 . . 2_655 ? C11 C12 C13 C10 54(5) 2_655 . . 2_655 ? C12 C12 C13 C10 160(2) 2_655 . . 2_655 ? C11 C12 C13 C10 171(2) . . . 2_655 ? C13 C12 C13 C10 160(2) 2_655 . . 2_655 ? C9 C12 C13 C10 4.9(14) 2_655 . . 2_655 ? C11 C13 C14 O10 -168(3) 2_655 . . . ? O12 C13 C14 O10 -43(3) 2_655 . . . ? C12 C13 C14 O10 169.4(16) . . . . ? O9 C13 C14 O10 -5.1(19) . . . . ? C12 C13 C14 O10 -172(5) 2_655 . . . ? C10 C13 C14 O10 178.4(12) 2_655 . . . ? C11 C13 C14 O12 -125(4) 2_655 . . 2_655 ? C12 C13 C14 O12 -147(4) . . . 2_655 ? O9 C13 C14 O12 38.1(19) . . . 2_655 ? C12 C13 C14 O12 -129(7) 2_655 . . 2_655 ? C10 C13 C14 O12 -138(3) 2_655 . . 2_655 ? C11 C13 C14 O11 14(3) 2_655 . . . ? O12 C13 C14 O11 138(3) 2_655 . . . ? C12 C13 C14 O11 -9(2) . . . . ? O9 C13 C14 O11 176.3(12) . . . . ? C12 C13 C14 O11 10(6) 2_655 . . . ? C10 C13 C14 O11 -0.2(12) 2_655 . . . ? C11 C13 C14 O19 -165(9) 2_655 . . . ? O12 C13 C14 O19 -40(11) 2_655 . . . ? C12 C13 C14 O19 172(9) . . . . ? O9 C13 C14 O19 -2(11) . . . . ? C12 C13 C14 O19 -169(7) 2_655 . . . ? C10 C13 C14 O19 -179(10) 2_655 . . . ? O12 C13 C14 C11 125(4) 2_655 . . 2_655 ? C12 C13 C14 C11 -23(2) . . . 2_655 ? O9 C13 C14 C11 163(4) . . . 2_655 ? C12 C13 C14 C11 -4(4) 2_655 . . 2_655 ? C10 C13 C14 C11 -14(3) 2_655 . . 2_655 ? O2 C1 O1 Tb1 -98.1(12) . . . . ? C2 C1 O1 Tb1 83.9(11) . . . . ? O7 Tb1 O1 C1 -13.9(15) . . . . ? O4 Tb1 O1 C1 57.7(10) 2_666 . . . ? O6 Tb1 O1 C1 -89.6(10) 2_656 . . . ? O14 Tb1 O1 C1 128.8(10) . . . . ? O13 Tb1 O1 C1 -158.5(10) . . . . ? O5 Tb1 O1 C1 -179.4(9) 1_654 . . . ? O15 Tb1 O1 C1 -16.6(10) . . . . ? O20 Tb1 O1 C1 -11.3(13) . . . . ? C3 C2 O3 C6 -2.4(10) . . . . ? C1 C2 O3 C6 -178.9(5) . . . . ? C5 C6 O3 C2 4.1(10) . . . . ? C7 C6 O3 C2 -177.6(5) . . . . ? O5 C7 O4 Tb1 -114.2(13) . . . 2_666 ? C6 C7 O4 Tb1 64.0(16) . . . 2_666 ? O4 C7 O5 Tb1 6.7(10) . . . 1_456 ? C6 C7 O5 Tb1 -171.5(4) . . . 1_456 ? C5 C4 O6 Tb1 5.2(15) . . . 2_656 ? C3 C4 O6 Tb1 -177.5(6) . . . 2_656 ? O20 C8 O7 Tb1 -169(13) . . . . ? O8 C8 O7 Tb1 -94(3) . . . . ? C9 C8 O7 Tb1 83(3) . . . . ? O18 C8 O7 Tb1 -58(5) . . . . ? O1 Tb1 O7 C8 -134(2) . . . . ? O4 Tb1 O7 C8 149(3) 2_666 . . . ? O6 Tb1 O7 C8 -56(3) 2_656 . . . ? O14 Tb1 O7 C8 94(3) . . . . ? O13 Tb1 O7 C8 -3(3) . . . . ? O5 Tb1 O7 C8 37(3) 1_654 . . . ? O15 Tb1 O7 C8 -131(3) . . . . ? O20 C8 O8 O18 162.6(19) . . . . ? O7 C8 O8 O18 151(2) . . . . ? C9 C8 O8 O18 -26(2) . . . . ? C11 C13 O9 O12 131(5) 2_655 . . 2_655 ? C12 C13 O9 O12 157(3) . . . 2_655 ? C14 C13 O9 O12 -28.1(15) . . . 2_655 ? C12 C13 O9 O12 149(2) 2_655 . . 2_655 ? C10 C13 O9 O12 139(6) 2_655 . . 2_655 ? C11 C13 O9 C9 -26(4) 2_655 . . . ? O12 C13 O9 C9 -157.3(19) 2_655 . . . ? C12 C13 O9 C9 0(2) . . . . ? C14 C13 O9 C9 174.6(11) . . . . ? C12 C13 O9 C9 -8.6(13) 2_655 . . . ? C10 C13 O9 C9 -18(6) 2_655 . . . ? O12 C13 O9 C11 -131(5) 2_655 . . 2_655 ? C12 C13 O9 C11 26(3) . . . 2_655 ? C14 C13 O9 C11 -159(5) . . . 2_655 ? C12 C13 O9 C11 17(3) 2_655 . . 2_655 ? C10 C13 O9 C11 8(3) 2_655 . . 2_655 ? C10 C9 O9 O12 -14(3) . . . 2_655 ? C8 C9 O9 O12 166.4(15) . . . 2_655 ? C12 C9 O9 O12 -11.5(19) 2_655 . . 2_655 ? C10 C9 O9 C13 5.2(19) . . . . ? C8 C9 O9 C13 -173.9(12) . . . . ? C12 C9 O9 C13 8.2(12) 2_655 . . . ? C10 C9 O9 C11 -1.9(16) . . . 2_655 ? C8 C9 O9 C11 179.0(10) . . . 2_655 ? C12 C9 O9 C11 1.1(9) 2_655 . . 2_655 ? O12 C14 O10 O19 162.1(11) 2_655 . . . ? O11 C14 O10 O19 -2.1(15) . . . . ? C13 C14 O10 O19 179.6(13) . . . . ? C11 C14 O10 O19 174.1(15) 2_655 . . . ? O11 C14 O10 O12 -164(2) . . . 2_655 ? C13 C14 O10 O12 17.5(10) . . . 2_655 ? O19 C14 O10 O12 -162.1(11) . . . 2_655 ? C11 C14 O10 O12 11.9(11) 2_655 . . 2_655 ? O10 C14 O11 O19 1.8(13) . . . . ? O12 C14 O11 O19 -158.0(18) 2_655 . . . ? C13 C14 O11 O19 -179.8(13) . . . . ? C11 C14 O11 O19 -175.6(9) 2_655 . . . ? C12 C11 O12 C13 -3(7) 2_655 . . 2_655 ? C10 C11 O12 C13 -118(5) . . . 2_655 ? C12 C11 O12 C13 63(5) . . . 2_655 ? O9 C11 O12 C13 49(5) 2_655 . . 2_655 ? C14 C11 O12 C13 -99(5) 2_655 . . 2_655 ? C11 C11 O12 C13 54(5) 2_655 . . 2_655 ? C13 C11 O12 C14 99(5) 2_655 . . 2_655 ? C12 C11 O12 C14 97(8) 2_655 . . 2_655 ? C10 C11 O12 C14 -19(2) . . . 2_655 ? C12 C11 O12 C14 162.0(14) . . . 2_655 ? O9 C11 O12 C14 148.0(15) 2_655 . . 2_655 ? C11 C11 O12 C14 153(2) 2_655 . . 2_655 ? C13 C11 O12 O9 -49(5) 2_655 . . 2_655 ? C12 C11 O12 O9 -51(8) 2_655 . . 2_655 ? C10 C11 O12 O9 -166.8(15) . . . 2_655 ? C12 C11 O12 O9 14.0(17) . . . 2_655 ? C14 C11 O12 O9 -148.0(15) 2_655 . . 2_655 ? C11 C11 O12 O9 5(3) 2_655 . . 2_655 ? C13 C11 O12 O10 85(5) 2_655 . . 2_655 ? C12 C11 O12 O10 82(9) 2_655 . . 2_655 ? C10 C11 O12 O10 -33(3) . . . 2_655 ? C12 C11 O12 O10 147.8(15) . . . 2_655 ? O9 C11 O12 O10 134(2) 2_655 . . 2_655 ? C14 C11 O12 O10 -14.2(14) 2_655 . . 2_655 ? C11 C11 O12 O10 138.9(18) 2_655 . . 2_655 ? O20 C8 O18 O8 -36(4) . . . . ? O7 C8 O18 O8 -59(4) . . . . ? C9 C8 O18 O8 156.5(19) . . . . ? O12 O10 O19 C14 13.0(8) 2_655 . . . ? C14 O10 O19 O11 1.2(8) . . . . ? O12 O10 O19 O11 14.2(9) 2_655 . . . ? O12 C14 O19 O10 -36(2) 2_655 . . . ? O11 C14 O19 O10 178.3(12) . . . . ? C13 C14 O19 O10 -3(10) . . . . ? C11 C14 O19 O10 -160(5) 2_655 . . . ? O10 C14 O19 O11 -178.3(12) . . . . ? O12 C14 O19 O11 146(3) 2_655 . . . ? C13 C14 O19 O11 179(11) . . . . ? C11 C14 O19 O11 22(4) 2_655 . . . ? C14 O11 O19 O10 -1.2(9) . . . . ? O8 C8 O20 Tb1 -104(2) . . . . ? O7 C8 O20 Tb1 8(9) . . . . ? C9 C8 O20 Tb1 84.6(19) . . . . ? O18 C8 O20 Tb1 -82(4) . . . . ? O1 Tb1 O20 C8 -132.8(15) . . . . ? O4 Tb1 O20 C8 152.0(18) 2_666 . . . ? O6 Tb1 O20 C8 -52.4(17) 2_656 . . . ? O14 Tb1 O20 C8 98.4(17) . . . . ? O13 Tb1 O20 C8 1(2) . . . . ? O5 Tb1 O20 C8 40.2(17) 1_654 . . . ? O15 Tb1 O20 C8 -127.4(18) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.825 _refine_diff_density_min -2.362 _refine_diff_density_rms 0.214 # Attachment 'Dy-5.cif' data_Dy-5 _database_code_depnum_ccdc_archive 'CCDC 716754' #TrackingRef 'Dy-5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H30 Dy2 O30' _chemical_formula_weight 1087.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.4832(19) _cell_length_b 9.6260(19) _cell_length_c 10.142(2) _cell_angle_alpha 69.53(3) _cell_angle_beta 68.52(3) _cell_angle_gamma 83.76(3) _cell_volume 806.9(3) _cell_formula_units_Z 1 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 2847 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 25 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.238 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 528 _exptl_absorpt_coefficient_mu 4.714 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6500 _exptl_absorpt_correction_T_max 0.7652 _exptl_absorpt_process_details Crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7676 _diffrn_reflns_av_R_equivalents 0.0669 _diffrn_reflns_av_sigmaI/netI 0.0814 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2847 _reflns_number_gt 2471 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. A few of restraints containing 'isor' and 'simu' have been used to restrict the disordered ligand and water molecules. ; _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^)+(0.0491P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2847 _refine_ls_number_parameters 316 _refine_ls_number_restraints 210 _refine_ls_R_factor_all 0.0454 _refine_ls_R_factor_gt 0.0405 _refine_ls_wR_factor_ref 0.0991 _refine_ls_wR_factor_gt 0.0965 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 0.993 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 0.82543(3) 0.30877(3) 0.21062(3) 0.01102(13) Uani 1 1 d . . . C1 C 0.6180(8) 0.3611(7) 0.5477(7) 0.0130(14) Uani 1 1 d U . . C2 C 0.4777(8) 0.2579(7) 0.6372(7) 0.0127(14) Uani 1 1 d U . . C3 C 0.4600(8) 0.1312(7) 0.6190(8) 0.0163(15) Uani 1 1 d U . . H3A H 0.5327 0.1037 0.5421 0.020 Uiso 1 1 calc R . . C4 C 0.3294(8) 0.0368(7) 0.7176(8) 0.0156(15) Uani 1 1 d U . . C5 C 0.2193(8) 0.0948(8) 0.8233(8) 0.0179(16) Uani 1 1 d U . . H5A H 0.1301 0.0409 0.8878 0.021 Uiso 1 1 calc R . . C6 C 0.2431(8) 0.2287(7) 0.8313(7) 0.0127(14) Uani 1 1 d U . . C7 C 0.1347(7) 0.3027(7) 0.9353(7) 0.0115(14) Uani 1 1 d U . . C8 C 0.8062(14) 0.2855(14) -0.1069(14) 0.009(3) Uani 0.50 1 d PU . . C9 C 0.6804(14) 0.1765(14) -0.0675(14) 0.009(3) Uani 0.50 1 d PU . . C10 C 0.6933(15) 0.0751(14) -0.1353(15) 0.013(3) Uani 0.50 1 d PU . . H10A H 0.7789 0.0798 -0.2244 0.015 Uiso 0.50 1 d PR . . C11 C 0.5820(17) -0.0377(17) -0.0749(16) 0.013(3) Uani 0.50 1 d PU . . C12 C 0.4514(16) -0.0288(16) 0.0530(15) 0.012(3) Uani 0.50 1 d PU . . H12A H 0.3703 -0.1006 0.0973 0.014 Uiso 0.50 1 d PR . . C13 C 0.4451(17) 0.0737(17) 0.1133(17) 0.014(3) Uani 0.50 1 d PU . . C14 C 0.3192(15) 0.0896(15) 0.2565(15) 0.013(3) Uani 0.50 1 d PU . . O1 O 0.7163(5) 0.3219(5) 0.4470(5) 0.0132(10) Uani 1 1 d U . . O2 O 0.6242(5) 0.4703(5) 0.5848(5) 0.0158(11) Uani 1 1 d U . . O3 O 0.3721(5) 0.3090(5) 0.7421(5) 0.0122(10) Uani 1 1 d U . . O4 O 0.1564(5) 0.4352(5) 0.9086(5) 0.0161(11) Uani 1 1 d U . . O5 O 0.0311(6) 0.2187(5) 1.0445(5) 0.0218(12) Uani 1 1 d U . . O6 O 0.3155(5) -0.0886(5) 0.7118(5) 0.0167(11) Uani 1 1 d U . . O7 O 0.7932(16) 0.3443(16) -0.0122(16) 0.0094(15) Uani 0.50 1 d PU . . O8 O 0.9074(12) 0.3016(12) -0.2280(11) 0.023(2) Uani 0.50 1 d PU . . O9 O 0.5574(10) 0.1812(9) 0.0541(9) 0.0101(19) Uani 0.50 1 d PU . . O10 O 0.3391(11) 0.1783(10) 0.3093(10) 0.016(2) Uani 0.50 1 d PU . . O11 O 0.2104(11) -0.0006(10) 0.3052(10) 0.018(2) Uani 0.50 1 d PU . . O12 O 0.5933(12) -0.1407(12) -0.1305(11) 0.022(2) Uani 0.50 1 d PU . . O13 O 0.9260(6) 0.1091(5) 0.3610(6) 0.0241(12) Uani 1 1 d U . . H13A H 0.8904 0.0436 0.4461 0.036 Uiso 1 1 d R . . H13B H 1.0163 0.0901 0.3554 0.036 Uiso 1 1 d R . . O14 O 1.0376(5) 0.3957(5) 0.2342(5) 0.0205(11) Uani 1 1 d U . . H14B H 1.0565 0.3894 0.3113 0.031 Uiso 1 1 d R . . H14A H 1.1023 0.4626 0.1693 0.031 Uiso 1 1 d R . . O15 O 0.5673(5) 0.3811(5) 0.2422(5) 0.0170(11) Uani 1 1 d U . . H15A H 0.5185 0.4391 0.2896 0.025 Uiso 1 1 d R . . H15B H 0.4917 0.3317 0.2569 0.025 Uiso 1 1 d R . . O16 O 0.8718(6) 0.6460(6) 0.5204(6) 0.0271(13) Uani 1 1 d U . . H16A H 0.9573 0.6610 0.4514 0.033 Uiso 1 1 d R . . H16B H 0.8050 0.6841 0.4839 0.033 Uiso 1 1 d R . . O17 O 0.5082(11) 0.5730(10) 0.0052(11) 0.019(2) Uani 0.50 1 d PU . . O18 O 0.9030(11) 0.2155(11) -0.2371(11) 0.022(2) Uani 0.50 1 d PU . . O19 O 0.2041(11) 0.1216(10) 0.4061(11) 0.019(2) Uani 0.50 1 d PU . . O20 O 0.7775(16) 0.3590(16) -0.0324(16) 0.0094(15) Uani 0.50 1 d PU . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.00973(19) 0.01065(19) 0.0110(2) -0.00772(15) 0.00305(14) -0.00311(13) C1 0.0131(17) 0.0131(17) 0.0127(17) -0.0050(10) -0.0038(10) 0.0001(10) C2 0.0125(17) 0.0128(17) 0.0125(17) -0.0048(10) -0.0037(10) 0.0004(10) C3 0.0166(18) 0.0160(17) 0.0163(18) -0.0069(11) -0.0046(10) 0.0003(10) C4 0.0155(17) 0.0154(17) 0.0160(17) -0.0062(10) -0.0048(10) -0.0004(10) C5 0.0178(18) 0.0175(18) 0.0183(18) -0.0066(11) -0.0056(11) -0.0003(10) C6 0.0125(17) 0.0130(17) 0.0125(17) -0.0044(10) -0.0041(10) 0.0000(10) C7 0.0110(17) 0.0119(16) 0.0114(16) -0.0042(10) -0.0036(10) 0.0003(10) C8 0.009(3) 0.009(3) 0.009(3) -0.0031(13) -0.0028(13) 0.0001(10) C9 0.009(3) 0.009(3) 0.009(3) -0.0028(13) -0.0030(13) 0.0001(10) C10 0.013(3) 0.013(3) 0.013(3) -0.0045(13) -0.0041(14) 0.0004(10) C11 0.013(3) 0.013(3) 0.013(3) -0.0044(14) -0.0044(14) 0.0002(10) C12 0.012(3) 0.012(3) 0.012(3) -0.0042(13) -0.0040(14) 0.0002(10) C13 0.014(3) 0.015(3) 0.014(3) -0.0046(14) -0.0049(15) 0.0004(10) C14 0.013(3) 0.013(3) 0.013(3) -0.0043(14) -0.0047(14) 0.0002(10) O1 0.0134(13) 0.0130(13) 0.0130(13) -0.0062(9) -0.0028(9) 0.0004(9) O2 0.0161(14) 0.0149(13) 0.0166(13) -0.0073(9) -0.0038(9) -0.0005(9) O3 0.0123(13) 0.0119(13) 0.0123(13) -0.0055(9) -0.0027(9) -0.0006(9) O4 0.0161(14) 0.0156(13) 0.0160(14) -0.0065(9) -0.0039(9) 0.0009(9) O5 0.0216(15) 0.0216(14) 0.0227(14) -0.0094(10) -0.0059(10) -0.0012(9) O6 0.0172(14) 0.0156(13) 0.0176(14) -0.0080(9) -0.0039(9) -0.0002(9) O7 0.0094(17) 0.0095(16) 0.0092(17) -0.0032(10) -0.0033(8) 0.0006(8) O8 0.023(3) 0.023(3) 0.023(3) -0.0081(12) -0.0077(12) -0.0002(10) O9 0.010(2) 0.010(2) 0.010(2) -0.0038(11) -0.0031(11) -0.0001(10) O10 0.016(2) 0.016(2) 0.016(2) -0.0059(12) -0.0053(12) 0.0003(10) O11 0.017(2) 0.018(2) 0.018(2) -0.0059(12) -0.0057(12) 0.0002(10) O12 0.023(3) 0.022(3) 0.022(3) -0.0080(13) -0.0078(13) 0.0000(10) O13 0.0229(15) 0.0232(15) 0.0248(15) -0.0067(10) -0.0083(10) 0.0012(9) O14 0.0196(14) 0.0211(14) 0.0204(14) -0.0055(10) -0.0075(10) -0.0017(9) O15 0.0174(14) 0.0175(14) 0.0175(14) -0.0086(9) -0.0050(9) -0.0002(9) O16 0.0265(15) 0.0289(15) 0.0259(15) -0.0092(10) -0.0089(10) -0.0011(9) O17 0.020(2) 0.019(2) 0.019(2) -0.0064(12) -0.0071(12) 0.0004(10) O18 0.022(2) 0.021(2) 0.021(2) -0.0080(12) -0.0068(12) 0.0005(10) O19 0.019(2) 0.019(2) 0.018(2) -0.0063(12) -0.0062(12) 0.0004(10) O20 0.0095(17) 0.0095(16) 0.0092(17) -0.0034(10) -0.0032(8) 0.0006(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 Dy1 O1 2.281(4) . ? Dy1 O7 2.294(14) . ? Dy1 O4 2.328(5) 2_666 ? Dy1 O13 2.355(5) . ? Dy1 O6 2.361(5) 2_656 ? Dy1 O5 2.376(5) 1_654 ? Dy1 O14 2.380(5) . ? Dy1 O15 2.407(5) . ? Dy1 O20 2.541(14) . ? C1 O1 1.245(8) . ? C1 O2 1.247(8) . ? C1 C2 1.535(9) . ? C2 C3 1.331(9) . ? C2 O3 1.362(8) . ? C3 C4 1.436(9) . ? C3 H3A 0.9300 . ? C4 O6 1.252(8) . ? C4 C5 1.423(10) . ? C5 C6 1.367(9) . ? C5 H5A 0.9300 . ? C6 O3 1.349(8) . ? C6 C7 1.500(9) . ? C7 O4 1.232(7) . ? C7 O5 1.263(8) . ? C8 O20 1.151(19) . ? C8 O8 1.221(15) . ? C8 O7 1.24(2) . ? C8 C9 1.521(17) . ? C8 O18 1.625(16) . ? C9 C10 1.349(18) . ? C9 O9 1.363(15) . ? C10 C12 1.346(19) 2_655 ? C10 C11 1.407(19) . ? C10 H10A 0.9592 . ? C11 C13 0.724(17) 2_655 ? C11 C12 0.750(16) 2_655 ? C11 O12 1.278(19) . ? C11 C12 1.45(2) . ? C11 O9 1.921(18) 2_655 ? C12 C11 0.750(16) 2_655 ? C12 C12 1.13(3) 2_655 ? C12 C13 1.32(2) . ? C12 C10 1.346(19) 2_655 ? C12 H12A 0.9572 . ? C13 C11 0.724(17) 2_655 ? C13 O12 0.748(15) 2_655 ? C13 O9 1.380(17) . ? C13 C14 1.55(2) . ? C14 O12 1.198(16) 2_655 ? C14 O10 1.216(16) . ? C14 O11 1.258(16) . ? C14 O19 1.622(16) . ? O4 Dy1 2.328(5) 2_666 ? O5 Dy1 2.376(5) 1_456 ? O6 Dy1 2.361(5) 2_656 ? O8 O18 0.872(12) . ? O9 O12 1.377(13) 2_655 ? O9 C11 1.921(18) 2_655 ? O10 O19 1.326(13) . ? O11 O19 1.793(13) . ? O12 C13 0.748(15) 2_655 ? O12 C14 1.199(16) 2_655 ? O12 O9 1.377(13) 2_655 ? O13 H13A 0.8422 . ? O13 H13B 0.8407 . ? O14 H14B 0.8456 . ? O14 H14A 0.8476 . ? O15 H15A 0.8513 . ? O15 H15B 0.8411 . ? O16 H16A 0.8415 . ? O16 H16B 0.8357 . ? O17 O17 1.474(18) 2_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 O1 Dy1 O7 145.8(4) . . ? O1 Dy1 O4 94.53(16) . 2_666 ? O7 Dy1 O4 75.4(4) . 2_666 ? O1 Dy1 O13 75.21(17) . . ? O7 Dy1 O13 131.2(4) . . ? O4 Dy1 O13 143.29(18) 2_666 . ? O1 Dy1 O6 89.93(16) . 2_656 ? O7 Dy1 O6 82.4(4) . 2_656 ? O4 Dy1 O6 146.54(17) 2_666 2_656 ? O13 Dy1 O6 69.72(17) . 2_656 ? O1 Dy1 O5 146.05(17) . 1_654 ? O7 Dy1 O5 67.6(4) . 1_654 ? O4 Dy1 O5 103.72(16) 2_666 1_654 ? O13 Dy1 O5 73.05(17) . 1_654 ? O6 Dy1 O5 90.21(16) 2_656 1_654 ? O1 Dy1 O14 80.25(16) . . ? O7 Dy1 O14 125.2(4) . . ? O4 Dy1 O14 72.67(16) 2_666 . ? O13 Dy1 O14 70.89(17) . . ? O6 Dy1 O14 140.62(17) 2_656 . ? O5 Dy1 O14 78.30(17) 1_654 . ? O1 Dy1 O15 73.01(16) . . ? O7 Dy1 O15 72.9(4) . . ? O4 Dy1 O15 76.06(16) 2_666 . ? O13 Dy1 O15 130.77(17) . . ? O6 Dy1 O15 73.63(16) 2_656 . ? O5 Dy1 O15 138.89(16) 1_654 . ? O14 Dy1 O15 136.62(16) . . ? O1 Dy1 O20 142.7(3) . . ? O7 Dy1 O20 3.4(7) . . ? O4 Dy1 O20 73.3(4) 2_666 . ? O13 Dy1 O20 134.3(4) . . ? O6 Dy1 O20 83.2(4) 2_656 . ? O5 Dy1 O20 70.9(3) 1_654 . ? O14 Dy1 O20 126.2(4) . . ? O15 Dy1 O20 69.8(3) . . ? O1 C1 O2 127.3(6) . . ? O1 C1 C2 114.6(6) . . ? O2 C1 C2 118.1(6) . . ? C3 C2 O3 123.0(6) . . ? C3 C2 C1 125.0(6) . . ? O3 C2 C1 111.9(5) . . ? C2 C3 C4 120.4(7) . . ? C2 C3 H3A 119.8 . . ? C4 C3 H3A 119.8 . . ? O6 C4 C5 122.7(7) . . ? O6 C4 C3 122.0(6) . . ? C5 C4 C3 115.2(6) . . ? C6 C5 C4 120.8(7) . . ? C6 C5 H5A 119.6 . . ? C4 C5 H5A 119.6 . . ? O3 C6 C5 121.6(6) . . ? O3 C6 C7 112.6(5) . . ? C5 C6 C7 125.8(6) . . ? O4 C7 O5 127.0(6) . . ? O4 C7 C6 118.1(6) . . ? O5 C7 C6 114.9(6) . . ? O20 C8 O8 129.1(14) . . ? O20 C8 O7 13.1(12) . . ? O8 C8 O7 129.0(14) . . ? O20 C8 C9 114.4(12) . . ? O8 C8 C9 114.8(11) . . ? O7 C8 C9 116.2(12) . . ? O20 C8 O18 159.5(13) . . ? O8 C8 O18 31.8(6) . . ? O7 C8 O18 153.5(13) . . ? C9 C8 O18 86.1(9) . . ? C10 C9 O9 122.7(11) . . ? C10 C9 C8 124.0(11) . . ? O9 C9 C8 112.9(10) . . ? C10 C9 C12 44.3(8) . 2_655 ? O9 C9 C12 78.8(8) . 2_655 ? C8 C9 C12 168.2(10) . 2_655 ? C12 C10 C9 91.2(12) 2_655 . ? C12 C10 C11 31.5(7) 2_655 . ? C9 C10 C11 120.1(13) . . ? C12 C10 C13 42.3(9) 2_655 2_655 ? C9 C10 C13 133.6(11) . 2_655 ? C11 C10 C13 16.7(8) . 2_655 ? C12 C10 H10A 146.5 2_655 . ? C9 C10 H10A 119.9 . . ? C11 C10 H10A 120.0 . . ? C13 C10 H10A 105.7 2_655 . ? C13 C11 C12 126(3) 2_655 2_655 ? C13 C11 O12 30.3(16) 2_655 . ? C12 C11 O12 157(2) 2_655 . ? C13 C11 C10 129(2) 2_655 . ? C12 C11 C10 69.8(17) 2_655 . ? O12 C11 C10 122.4(13) . . ? C13 C11 C12 106(2) 2_655 . ? C12 C11 C12 50.5(18) 2_655 . ? O12 C11 C12 121.7(13) . . ? C10 C11 C12 115.9(16) . . ? C13 C11 O9 33.8(15) 2_655 2_655 ? C12 C11 O9 117.0(19) 2_655 2_655 ? O12 C11 O9 45.7(8) . 2_655 ? C10 C11 O9 163.1(12) . 2_655 ? C12 C11 O9 77.1(9) . 2_655 ? C13 C11 C14 47.2(17) 2_655 2_655 ? C12 C11 C14 139.0(19) 2_655 2_655 ? O12 C11 C14 36.7(7) . 2_655 ? C10 C11 C14 87.6(10) . 2_655 ? C12 C11 C14 153.0(13) . 2_655 ? O9 C11 C14 77.5(8) 2_655 2_655 ? C13 C11 C11 115(2) 2_655 2_655 ? C12 C11 C11 33.8(13) 2_655 2_655 ? O12 C11 C11 136.1(15) . 2_655 ? C10 C11 C11 100.7(14) . 2_655 ? C12 C11 C11 16.7(7) . 2_655 ? O9 C11 C11 90.5(10) 2_655 2_655 ? C14 C11 C11 157.4(14) 2_655 2_655 ? C11 C12 C12 99(2) 2_655 2_655 ? C11 C12 C13 26.3(15) 2_655 . ? C12 C12 C13 93.6(17) 2_655 . ? C11 C12 C10 78.7(18) 2_655 2_655 ? C12 C12 C10 155(2) 2_655 2_655 ? C13 C12 C10 94.1(13) . 2_655 ? C11 C12 C11 129.5(18) 2_655 . ? C12 C12 C11 30.7(10) 2_655 . ? C13 C12 C11 120.8(13) . . ? C10 C12 C11 144.2(15) 2_655 . ? C11 C12 C13 139(2) 2_655 2_655 ? C12 C12 C13 47.2(13) 2_655 2_655 ? C13 C12 C13 140.8(11) . 2_655 ? C10 C12 C13 121.5(13) 2_655 2_655 ? C11 C12 C13 22.9(7) . 2_655 ? C11 C12 C9 119.7(19) 2_655 2_655 ? C12 C12 C9 123.7(17) 2_655 2_655 ? C13 C12 C9 138.5(12) . 2_655 ? C10 C12 C9 44.5(8) 2_655 2_655 ? C11 C12 C9 100.2(12) . 2_655 ? C13 C12 C9 78.5(9) 2_655 2_655 ? C11 C12 H12A 105.9 2_655 . ? C12 C12 H12A 145.1 2_655 . ? C13 C12 H12A 119.2 . . ? C10 C12 H12A 27.2 2_655 . ? C11 C12 H12A 119.9 . . ? C13 C12 H12A 99.2 2_655 . ? C9 C12 H12A 21.4 2_655 . ? C11 C13 O12 121(3) 2_655 2_655 ? C11 C13 C12 27.3(16) 2_655 . ? O12 C13 C12 148(2) 2_655 . ? C11 C13 O9 129(2) 2_655 . ? O12 C13 O9 74.0(16) 2_655 . ? C12 C13 O9 122.1(13) . . ? C11 C13 C14 113(2) 2_655 . ? O12 C13 C14 48.8(14) 2_655 . ? C12 C13 C14 126.6(13) . . ? O9 C13 C14 111.3(13) . . ? C11 C13 C12 51.3(17) 2_655 2_655 ? O12 C13 C12 136.0(18) 2_655 2_655 ? C12 C13 C12 39.2(11) . 2_655 ? O9 C13 C12 83.5(9) . 2_655 ? C14 C13 C12 164.0(13) . 2_655 ? C11 C13 C10 34.0(16) 2_655 2_655 ? O12 C13 C10 114.0(18) 2_655 2_655 ? C12 C13 C10 43.6(9) . 2_655 ? O9 C13 C10 163.1(13) . 2_655 ? C14 C13 C10 83.8(9) . 2_655 ? C12 C13 C10 80.7(10) 2_655 2_655 ? O12 C14 O10 99.3(12) 2_655 . ? O12 C14 O11 128.6(13) 2_655 . ? O10 C14 O11 129.2(13) . . ? O12 C14 C13 28.0(7) 2_655 . ? O10 C14 C13 118.6(12) . . ? O11 C14 C13 112.0(12) . . ? O12 C14 O19 147.0(13) 2_655 . ? O10 C14 O19 53.4(7) . . ? O11 C14 O19 75.9(9) . . ? C13 C14 O19 172.0(12) . . ? O12 C14 C11 39.6(8) 2_655 2_655 ? O10 C14 C11 137.4(11) . 2_655 ? O11 C14 C11 93.2(10) . 2_655 ? C13 C14 C11 20.0(7) . 2_655 ? O19 C14 C11 167.7(10) . 2_655 ? C1 O1 Dy1 154.4(5) . . ? C6 O3 C2 118.8(5) . . ? C7 O4 Dy1 160.6(5) . 2_666 ? C7 O5 Dy1 122.7(4) . 1_456 ? C4 O6 Dy1 151.4(5) . 2_656 ? C8 O7 Dy1 144.0(11) . . ? O18 O8 C8 100.6(13) . . ? C9 O9 O12 143.8(10) . 2_655 ? C9 O9 C13 118.1(11) . . ? O12 O9 C13 31.5(7) 2_655 . ? C9 O9 C11 103.9(8) . 2_655 ? O12 O9 C11 41.7(7) 2_655 2_655 ? C13 O9 C11 17.0(8) . 2_655 ? C14 O10 O19 79.1(9) . . ? C14 O11 O19 61.3(8) . . ? C13 O12 C14 103.2(18) 2_655 2_655 ? C13 O12 C11 29.2(15) 2_655 . ? C14 O12 C11 103.7(12) 2_655 . ? C13 O12 O9 74.5(16) 2_655 2_655 ? C14 O12 O9 140.2(12) 2_655 2_655 ? C11 O12 O9 92.6(10) . 2_655 ? Dy1 O13 H13A 135.2 . . ? Dy1 O13 H13B 130.3 . . ? H13A O13 H13B 93.2 . . ? Dy1 O14 H14B 130.8 . . ? Dy1 O14 H14A 128.0 . . ? H14B O14 H14A 99.1 . . ? Dy1 O15 H15A 125.4 . . ? Dy1 O15 H15B 130.2 . . ? H15A O15 H15B 96.7 . . ? H16A O16 H16B 109.6 . . ? O8 O18 C8 47.6(10) . . ? O10 O19 C14 47.5(7) . . ? O10 O19 O11 90.3(7) . . ? C14 O19 O11 42.9(6) . . ? C8 O20 Dy1 128.2(11) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 3.6(10) . . . . ? O2 C1 C2 C3 -174.4(7) . . . . ? O1 C1 C2 O3 -177.9(6) . . . . ? O2 C1 C2 O3 4.1(9) . . . . ? O3 C2 C3 C4 -3.6(11) . . . . ? C1 C2 C3 C4 174.7(6) . . . . ? C2 C3 C4 O6 -173.9(7) . . . . ? C2 C3 C4 C5 4.9(11) . . . . ? O6 C4 C5 C6 176.3(7) . . . . ? C3 C4 C5 C6 -2.5(10) . . . . ? C4 C5 C6 O3 -1.4(11) . . . . ? C4 C5 C6 C7 178.7(6) . . . . ? O3 C6 C7 O4 15.2(9) . . . . ? C5 C6 C7 O4 -164.8(7) . . . . ? O3 C6 C7 O5 -163.4(6) . . . . ? C5 C6 C7 O5 16.6(10) . . . . ? O20 C8 C9 C10 -176.4(14) . . . . ? O8 C8 C9 C10 17.2(19) . . . . ? O7 C8 C9 C10 -162.1(13) . . . . ? O18 C8 C9 C10 3.0(14) . . . . ? O20 C8 C9 O9 -2.5(17) . . . . ? O8 C8 C9 O9 -168.9(11) . . . . ? O7 C8 C9 O9 11.8(17) . . . . ? O18 C8 C9 O9 176.9(10) . . . . ? O20 C8 C9 C12 176(5) . . . 2_655 ? O8 C8 C9 C12 9(6) . . . 2_655 ? O7 C8 C9 C12 -170(5) . . . 2_655 ? O18 C8 C9 C12 -5(5) . . . 2_655 ? O9 C9 C10 C12 9.0(16) . . . 2_655 ? C8 C9 C10 C12 -177.8(13) . . . 2_655 ? O9 C9 C10 C11 -4(2) . . . . ? C8 C9 C10 C11 168.9(13) . . . . ? C12 C9 C10 C11 -13.3(11) 2_655 . . . ? O9 C9 C10 C13 8(2) . . . 2_655 ? C8 C9 C10 C13 -178.6(12) . . . 2_655 ? C12 C9 C10 C13 -0.9(11) 2_655 . . 2_655 ? C12 C10 C11 C13 121(4) 2_655 . . 2_655 ? C9 C10 C11 C13 147(3) . . . 2_655 ? C9 C10 C11 C12 26(2) . . . 2_655 ? C13 C10 C11 C12 -121(4) 2_655 . . 2_655 ? C12 C10 C11 O12 158(3) 2_655 . . . ? C9 C10 C11 O12 -176.2(13) . . . . ? C13 C10 C11 O12 37(2) 2_655 . . . ? C12 C10 C11 C12 -21.2(18) 2_655 . . . ? C9 C10 C11 C12 5(2) . . . . ? C13 C10 C11 C12 -142(4) 2_655 . . . ? C12 C10 C11 O9 117(5) 2_655 . . 2_655 ? C9 C10 C11 O9 143(4) . . . 2_655 ? C13 C10 C11 O9 -4(3) 2_655 . . 2_655 ? C12 C10 C11 C14 145.1(19) 2_655 . . 2_655 ? C9 C10 C11 C14 171.3(12) . . . 2_655 ? C13 C10 C11 C14 24(3) 2_655 . . 2_655 ? C12 C10 C11 C11 -13.8(12) 2_655 . . 2_655 ? C9 C10 C11 C11 12.4(18) . . . 2_655 ? C13 C10 C11 C11 -135(4) 2_655 . . 2_655 ? C13 C11 C12 C11 -124(3) 2_655 . . 2_655 ? C12 C11 C12 C11 -0.004(2) 2_655 . . 2_655 ? O12 C11 C12 C11 -153(3) . . . 2_655 ? C10 C11 C12 C11 26(2) . . . 2_655 ? O9 C11 C12 C11 -142(3) 2_655 . . 2_655 ? C14 C11 C12 C11 -122(4) 2_655 . . 2_655 ? C13 C11 C12 C12 -124(3) 2_655 . . 2_655 ? O12 C11 C12 C12 -153(3) . . . 2_655 ? C10 C11 C12 C12 26(2) . . . 2_655 ? O9 C11 C12 C12 -142(3) 2_655 . . 2_655 ? C14 C11 C12 C12 -122(4) 2_655 . . 2_655 ? C11 C11 C12 C12 0.004(2) 2_655 . . 2_655 ? C13 C11 C12 C13 -155.0(16) 2_655 . . . ? C12 C11 C12 C13 -31(2) 2_655 . . . ? O12 C11 C12 C13 176.7(15) . . . . ? C10 C11 C12 C13 -5(2) . . . . ? O9 C11 C12 C13 -173.1(15) 2_655 . . . ? C14 C11 C12 C13 -153(2) 2_655 . . . ? C11 C11 C12 C13 -31(2) 2_655 . . . ? C13 C11 C12 C10 11(4) 2_655 . . 2_655 ? C12 C11 C12 C10 135(4) 2_655 . . 2_655 ? O12 C11 C12 C10 -18(3) . . . 2_655 ? C10 C11 C12 C10 161.2(17) . . . 2_655 ? O9 C11 C12 C10 -7(2) 2_655 . . 2_655 ? C14 C11 C12 C10 13(5) 2_655 . . 2_655 ? C11 C11 C12 C10 135(4) 2_655 . . 2_655 ? C12 C11 C12 C13 124(3) 2_655 . . 2_655 ? O12 C11 C12 C13 -28.4(16) . . . 2_655 ? C10 C11 C12 C13 150(3) . . . 2_655 ? O9 C11 C12 C13 -18.1(19) 2_655 . . 2_655 ? C14 C11 C12 C13 1.9(19) 2_655 . . 2_655 ? C11 C11 C12 C13 124(3) 2_655 . . 2_655 ? C13 C11 C12 C9 19(2) 2_655 . . 2_655 ? C12 C11 C12 C9 143(3) 2_655 . . 2_655 ? O12 C11 C12 C9 -9.6(16) . . . 2_655 ? C10 C11 C12 C9 169.2(12) . . . 2_655 ? O9 C11 C12 C9 0.7(7) 2_655 . . 2_655 ? C14 C11 C12 C9 21(3) 2_655 . . 2_655 ? C11 C11 C12 C9 143(3) 2_655 . . 2_655 ? C12 C12 C13 C11 102(4) 2_655 . . 2_655 ? C10 C12 C13 C11 -54(3) 2_655 . . 2_655 ? C11 C12 C13 C11 118(3) . . . 2_655 ? C13 C12 C13 C11 103(4) 2_655 . . 2_655 ? C9 C12 C13 C11 -53(4) 2_655 . . 2_655 ? C11 C12 C13 O12 -2(4) 2_655 . . 2_655 ? C12 C12 C13 O12 101(4) 2_655 . . 2_655 ? C10 C12 C13 O12 -56(4) 2_655 . . 2_655 ? C11 C12 C13 O12 116(4) . . . 2_655 ? C13 C12 C13 O12 101(4) 2_655 . . 2_655 ? C9 C12 C13 O12 -55(5) 2_655 . . 2_655 ? C11 C12 C13 O9 -114(4) 2_655 . . . ? C12 C12 C13 O9 -12(2) 2_655 . . . ? C10 C12 C13 O9 -168.4(14) 2_655 . . . ? C11 C12 C13 O9 3(2) . . . . ? C13 C12 C13 O9 -12(2) 2_655 . . . ? C9 C12 C13 O9 -167.4(12) 2_655 . . . ? C11 C12 C13 C14 67(3) 2_655 . . . ? C12 C12 C13 C14 169.8(16) 2_655 . . . ? C10 C12 C13 C14 13.2(19) 2_655 . . . ? C11 C12 C13 C14 -175.1(12) . . . . ? C13 C12 C13 C14 169.8(16) 2_655 . . . ? C9 C12 C13 C14 14(3) 2_655 . . . ? C11 C12 C13 C12 -102(4) 2_655 . . 2_655 ? C10 C12 C13 C12 -157(2) 2_655 . . 2_655 ? C11 C12 C13 C12 15.1(10) . . . 2_655 ? C13 C12 C13 C12 0.004(2) 2_655 . . 2_655 ? C9 C12 C13 C12 -156(3) 2_655 . . 2_655 ? C11 C12 C13 C10 54(3) 2_655 . . 2_655 ? C12 C12 C13 C10 157(2) 2_655 . . 2_655 ? C11 C12 C13 C10 171.7(19) . . . 2_655 ? C13 C12 C13 C10 157(2) 2_655 . . 2_655 ? C9 C12 C13 C10 1.0(12) 2_655 . . 2_655 ? C11 C13 C14 O12 -111(3) 2_655 . . 2_655 ? C12 C13 C14 O12 -139(3) . . . 2_655 ? O9 C13 C14 O12 42.7(16) . . . 2_655 ? C12 C13 C14 O12 -115(5) 2_655 . . 2_655 ? C10 C13 C14 O12 -130(2) 2_655 . . 2_655 ? C11 C13 C14 O10 -162(2) 2_655 . . . ? O12 C13 C14 O10 -51(2) 2_655 . . . ? C12 C13 C14 O10 170.6(15) . . . . ? O9 C13 C14 O10 -8.0(18) . . . . ? C12 C13 C14 O10 -165(4) 2_655 . . . ? C10 C13 C14 O10 179.7(12) 2_655 . . . ? C11 C13 C14 O11 21(3) 2_655 . . . ? O12 C13 C14 O11 132(2) 2_655 . . . ? C12 C13 C14 O11 -6(2) . . . . ? O9 C13 C14 O11 175.0(11) . . . . ? C12 C13 C14 O11 18(5) 2_655 . . . ? C10 C13 C14 O11 2.6(12) 2_655 . . . ? C11 C13 C14 O19 -168(8) 2_655 . . . ? O12 C13 C14 O19 -57(9) 2_655 . . . ? C12 C13 C14 O19 165(8) . . . . ? O9 C13 C14 O19 -14(9) . . . . ? C12 C13 C14 O19 -171(6) 2_655 . . . ? C10 C13 C14 O19 174(8) 2_655 . . . ? O12 C13 C14 C11 111(3) 2_655 . . 2_655 ? C12 C13 C14 C11 -27.3(17) . . . 2_655 ? O9 C13 C14 C11 154(3) . . . 2_655 ? C12 C13 C14 C11 -3(3) 2_655 . . 2_655 ? C10 C13 C14 C11 -18(2) 2_655 . . 2_655 ? O2 C1 O1 Dy1 -96.4(11) . . . . ? C2 C1 O1 Dy1 85.8(11) . . . . ? O7 Dy1 O1 C1 -14.4(13) . . . . ? O4 Dy1 O1 C1 56.1(10) 2_666 . . . ? O13 Dy1 O1 C1 -159.7(10) . . . . ? O6 Dy1 O1 C1 -90.7(10) 2_656 . . . ? O5 Dy1 O1 C1 179.0(9) 1_654 . . . ? O14 Dy1 O1 C1 127.6(10) . . . . ? O15 Dy1 O1 C1 -17.8(10) . . . . ? O20 Dy1 O1 C1 -12.1(12) . . . . ? C5 C6 O3 C2 3.0(10) . . . . ? C7 C6 O3 C2 -177.0(6) . . . . ? C3 C2 O3 C6 -0.5(10) . . . . ? C1 C2 O3 C6 -179.0(5) . . . . ? O5 C7 O4 Dy1 -113.3(13) . . . 2_666 ? C6 C7 O4 Dy1 68.2(16) . . . 2_666 ? O4 C7 O5 Dy1 9.3(10) . . . 1_456 ? C6 C7 O5 Dy1 -172.2(4) . . . 1_456 ? C5 C4 O6 Dy1 6.1(15) . . . 2_656 ? C3 C4 O6 Dy1 -175.1(6) . . . 2_656 ? O20 C8 O7 Dy1 165(7) . . . . ? O8 C8 O7 Dy1 -100(2) . . . . ? C9 C8 O7 Dy1 80(2) . . . . ? O18 C8 O7 Dy1 -65(4) . . . . ? O1 Dy1 O7 C8 -129.2(17) . . . . ? O4 Dy1 O7 C8 155(2) 2_666 . . . ? O13 Dy1 O7 C8 4(2) . . . . ? O6 Dy1 O7 C8 -50.6(19) 2_656 . . . ? O5 Dy1 O7 C8 42.8(18) 1_654 . . . ? O14 Dy1 O7 C8 98.8(19) . . . . ? O15 Dy1 O7 C8 -126(2) . . . . ? O20 Dy1 O7 C8 -153(13) . . . . ? O20 C8 O8 O18 168.4(17) . . . . ? O7 C8 O8 O18 151.6(16) . . . . ? C9 C8 O8 O18 -27.6(17) . . . . ? C10 C9 O9 O12 -22(2) . . . 2_655 ? C8 C9 O9 O12 163.9(14) . . . 2_655 ? C12 C9 O9 O12 -15.8(17) 2_655 . . 2_655 ? C10 C9 O9 C13 2.8(18) . . . . ? C8 C9 O9 C13 -171.2(11) . . . . ? C12 C9 O9 C13 9.2(11) 2_655 . . . ? C10 C9 O9 C11 -7.1(15) . . . 2_655 ? C8 C9 O9 C11 178.9(9) . . . 2_655 ? C12 C9 O9 C11 -0.8(8) 2_655 . . 2_655 ? C11 C13 O9 C9 -35(3) 2_655 . . . ? O12 C13 O9 C9 -151.6(16) 2_655 . . . ? C12 C13 O9 C9 -2(2) . . . . ? C14 C13 O9 C9 176.4(11) . . . . ? C12 C13 O9 C9 -9.8(12) 2_655 . . . ? C10 C13 O9 C9 -31(5) 2_655 . . . ? C11 C13 O9 O12 117(4) 2_655 . . 2_655 ? C12 C13 O9 O12 149(3) . . . 2_655 ? C14 C13 O9 O12 -32.1(12) . . . 2_655 ? C12 C13 O9 O12 141.8(18) 2_655 . . 2_655 ? C10 C13 O9 O12 121(5) 2_655 . . 2_655 ? O12 C13 O9 C11 -117(4) 2_655 . . 2_655 ? C12 C13 O9 C11 33(2) . . . 2_655 ? C14 C13 O9 C11 -149(4) . . . 2_655 ? C12 C13 O9 C11 25(3) 2_655 . . 2_655 ? C10 C13 O9 C11 4(2) 2_655 . . 2_655 ? O12 C14 O10 O19 159.4(12) 2_655 . . . ? O11 C14 O10 O19 -2.5(16) . . . . ? C13 C14 O10 O19 -179.0(13) . . . . ? C11 C14 O10 O19 172.1(16) 2_655 . . . ? O12 C14 O11 O19 -154.9(18) 2_655 . . . ? O10 C14 O11 O19 2.1(13) . . . . ? C13 C14 O11 O19 178.7(13) . . . . ? C11 C14 O11 O19 -174.3(9) 2_655 . . . ? C12 C11 O12 C13 2(5) 2_655 . . 2_655 ? C10 C11 O12 C13 -114(3) . . . 2_655 ? C12 C11 O12 C13 65(3) . . . 2_655 ? O9 C11 O12 C13 51(3) 2_655 . . 2_655 ? C14 C11 O12 C13 -93(3) 2_655 . . 2_655 ? C11 C11 O12 C13 54(3) 2_655 . . 2_655 ? C13 C11 O12 C14 93(3) 2_655 . . 2_655 ? C12 C11 O12 C14 94(5) 2_655 . . 2_655 ? C10 C11 O12 C14 -21(2) . . . 2_655 ? C12 C11 O12 C14 157.5(13) . . . 2_655 ? O9 C11 O12 C14 143.4(14) 2_655 . . 2_655 ? C11 C11 O12 C14 146.5(19) 2_655 . . 2_655 ? C13 C11 O12 O9 -51(3) 2_655 . . 2_655 ? C12 C11 O12 O9 -49(5) 2_655 . . 2_655 ? C10 C11 O12 O9 -164.6(14) . . . 2_655 ? C12 C11 O12 O9 14.1(15) . . . 2_655 ? C14 C11 O12 O9 -143.4(14) 2_655 . . 2_655 ? C11 C11 O12 O9 3(2) 2_655 . . 2_655 ? O20 C8 O18 O8 -26(4) . . . . ? O7 C8 O18 O8 -56(3) . . . . ? C9 C8 O18 O8 155.0(16) . . . . ? C14 O10 O19 O11 1.4(9) . . . . ? O12 C14 O19 O10 -40(2) 2_655 . . . ? O11 C14 O19 O10 178.0(13) . . . . ? C13 C14 O19 O10 7(8) . . . . ? C11 C14 O19 O10 -154(5) 2_655 . . . ? O12 C14 O19 O11 142(3) 2_655 . . . ? O10 C14 O19 O11 -178.0(13) . . . . ? C13 C14 O19 O11 -171(9) . . . . ? C11 C14 O19 O11 28(4) 2_655 . . . ? C14 O11 O19 O10 -1.5(9) . . . . ? O8 C8 O20 Dy1 -105.3(17) . . . . ? O7 C8 O20 Dy1 -10(5) . . . . ? C9 C8 O20 Dy1 90.7(15) . . . . ? O18 C8 O20 Dy1 -88(4) . . . . ? O1 Dy1 O20 C8 -136.6(12) . . . . ? O7 Dy1 O20 C8 21(10) . . . . ? O4 Dy1 O20 C8 148.3(15) 2_666 . . . ? O13 Dy1 O20 C8 -3.0(17) . . . . ? O6 Dy1 O20 C8 -55.8(14) 2_656 . . . ? O5 Dy1 O20 C8 36.8(14) 1_654 . . . ? O14 Dy1 O20 C8 95.5(14) . . . . ? O15 Dy1 O20 C8 -130.8(15) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.101 _refine_diff_density_min -2.305 _refine_diff_density_rms 0.223 # Attachment 'Ho-6.cif' data_Ho-6 _database_code_depnum_ccdc_archive 'CCDC 716755' #TrackingRef 'Ho-6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H30 Ho2 O30' _chemical_formula_weight 1092.31 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' Ho Ho -0.2175 4.6783 '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 9.4966(19) _cell_length_b 9.6020(19) _cell_length_c 10.144(2) _cell_angle_alpha 69.48(3) _cell_angle_beta 68.52(3) _cell_angle_gamma 83.79(3) _cell_volume 805.9(3) _cell_formula_units_Z 1 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 25.15 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.251 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 530 _exptl_absorpt_coefficient_mu 4.992 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4351 _exptl_absorpt_correction_T_max 0.7884 _exptl_absorpt_process_details Crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4992 _diffrn_reflns_av_R_equivalents 0.0918 _diffrn_reflns_av_sigmaI/netI 0.1333 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 25.15 _reflns_number_total 2871 _reflns_number_gt 2460 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. A few of restraints containing 'isor' and 'simu' have been used to restrict the disordered ligand and water molecules. ; _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^)+(0.0845P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.008(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2871 _refine_ls_number_parameters 317 _refine_ls_number_restraints 114 _refine_ls_R_factor_all 0.0704 _refine_ls_R_factor_gt 0.0642 _refine_ls_wR_factor_ref 0.1611 _refine_ls_wR_factor_gt 0.1588 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.024 _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 Ho1 Ho 0.82480(5) 0.30862(5) 0.21095(5) 0.0095(3) Uani 1 1 d . . . C1 C 0.6195(12) 0.3610(12) 0.5474(12) 0.014(2) Uani 1 1 d . . . C2 C 0.4786(11) 0.2594(11) 0.6380(11) 0.009(2) Uani 1 1 d U . . C3 C 0.4601(12) 0.1318(13) 0.6192(12) 0.015(2) Uani 1 1 d . . . H3A H 0.5327 0.1040 0.5425 0.018 Uiso 1 1 calc R . . C4 C 0.3288(12) 0.0382(11) 0.7171(11) 0.010(2) Uani 1 1 d U . . C5 C 0.2191(12) 0.0954(12) 0.8245(12) 0.013(2) Uani 1 1 d U . . H5A H 0.1302 0.0414 0.8896 0.015 Uiso 1 1 calc R . . C6 C 0.2444(12) 0.2278(13) 0.8319(13) 0.016(2) Uani 1 1 d . . . C7 C 0.1362(11) 0.3023(12) 0.9375(12) 0.011(2) Uani 1 1 d . . . C8 C 0.807(2) 0.287(2) -0.108(2) 0.008(4) Uani 0.50 1 d PU . . C9 C 0.681(2) 0.177(2) -0.071(2) 0.010(4) Uani 0.50 1 d PU . . C10 C 0.690(3) 0.079(3) -0.137(3) 0.019(5) Uani 0.50 1 d P . . H10A H 0.7752 0.0834 -0.2265 0.023 Uiso 0.50 1 d PR . . C11 C 0.576(3) -0.040(3) -0.076(3) 0.016(5) Uani 0.50 1 d PU . . C12 C 0.449(2) -0.034(3) 0.055(2) 0.013(4) Uani 0.50 1 d PU . . H12A H 0.3683 -0.1058 0.0995 0.016 Uiso 0.50 1 d PR . . C13 C 0.445(3) 0.076(3) 0.113(3) 0.017(5) Uani 0.50 1 d PU . . C14 C 0.319(2) 0.085(2) 0.257(2) 0.008(4) Uani 0.50 1 d PU . . O1 O 0.7182(8) 0.3220(8) 0.4466(8) 0.0125(16) Uani 1 1 d U . . O2 O 0.6252(8) 0.4712(8) 0.5845(9) 0.0160(17) Uani 1 1 d . . . O3 O 0.3737(8) 0.3107(8) 0.7397(8) 0.0135(16) Uani 1 1 d . . . O4 O 0.1588(9) 0.4384(9) 0.9070(9) 0.0194(18) Uani 1 1 d . . . O5 O 0.0296(9) 0.2206(9) 1.0451(9) 0.023(2) Uani 1 1 d . . . O6 O 0.3153(8) -0.0878(8) 0.7105(8) 0.0161(17) Uani 1 1 d . . . O7 O 0.780(3) 0.361(3) -0.029(3) 0.012(2) Uani 0.50 1 d PU . . O8 O 0.9095(19) 0.304(2) -0.233(2) 0.026(4) Uani 0.50 1 d PU . . O9 O 0.5555(18) 0.1821(16) 0.0537(16) 0.015(3) Uani 0.50 1 d P . . O10 O 0.3381(18) 0.1778(19) 0.3083(18) 0.021(4) Uani 0.50 1 d P . . O11 O 0.2099(17) -0.0008(17) 0.3037(17) 0.017(3) Uani 0.50 1 d P . . O12 O 0.5921(19) -0.141(2) -0.1327(19) 0.023(4) Uani 0.50 1 d PU . . O13 O 0.9274(9) 0.1097(9) 0.3595(10) 0.0246(19) Uani 1 1 d . . . H13A H 0.8918 0.0441 0.4446 0.037 Uiso 1 1 d R . . H13B H 1.0176 0.0907 0.3539 0.037 Uiso 1 1 d R . . O14 O 1.0328(9) 0.3988(9) 0.2337(9) 0.0191(18) Uani 1 1 d . . . H14B H 1.0517 0.3925 0.3108 0.029 Uiso 1 1 d R . . H14A H 1.0976 0.4657 0.1687 0.029 Uiso 1 1 d R . . O15 O 0.5687(9) 0.3785(9) 0.2422(8) 0.0193(19) Uani 1 1 d . . . H15A H 0.5199 0.4364 0.2896 0.029 Uiso 1 1 d R . . H15B H 0.4931 0.3291 0.2569 0.029 Uiso 1 1 d R . . O16 O 0.8739(9) 0.6457(9) 0.5209(9) 0.0235(19) Uani 1 1 d U . . H16A H 0.9544 0.6608 0.4545 0.028 Uiso 1 1 d R . . H16B H 0.8020 0.6838 0.4871 0.028 Uiso 1 1 d R . . O17 O 0.514(2) 0.5735(19) 0.9985(19) 0.023(4) Uani 0.50 1 d P . . O18 O 0.9022(18) 0.222(2) -0.2382(18) 0.022(4) Uani 0.50 1 d PU . . O19 O 0.2032(17) 0.1194(17) 0.4092(17) 0.015(3) Uani 0.50 1 d PU . . O20 O 0.792(3) 0.340(3) -0.015(3) 0.012(2) Uani 0.50 1 d PU . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ho1 0.0098(4) 0.0094(4) 0.0091(4) -0.0069(2) 0.0015(2) -0.0039(2) C1 0.012(5) 0.016(6) 0.017(6) -0.011(5) -0.002(5) 0.000(4) C2 0.009(2) 0.010(2) 0.009(2) -0.0033(12) -0.0032(12) 0.0000(10) C3 0.012(5) 0.020(6) 0.015(6) -0.014(5) -0.001(5) 0.002(4) C4 0.010(2) 0.011(2) 0.010(2) -0.0038(12) -0.0037(12) -0.0002(10) C5 0.013(2) 0.013(2) 0.013(2) -0.0044(12) -0.0042(12) -0.0003(10) C6 0.007(5) 0.022(6) 0.019(6) -0.013(5) 0.002(5) -0.007(4) C7 0.010(5) 0.013(6) 0.015(5) -0.010(5) -0.008(5) 0.003(4) C8 0.008(4) 0.007(4) 0.008(4) -0.0025(17) -0.0027(17) 0.0003(10) C9 0.010(4) 0.010(4) 0.009(4) -0.0033(17) -0.0033(17) 0.0001(10) C10 0.023(12) 0.020(13) 0.018(12) -0.009(10) -0.010(11) 0.002(10) C11 0.016(5) 0.016(5) 0.016(5) -0.0056(19) -0.006(2) 0.0003(10) C12 0.013(4) 0.014(4) 0.014(4) -0.0046(16) -0.0048(17) 0.0003(7) C13 0.017(5) 0.017(5) 0.017(5) -0.006(2) -0.006(2) 0.0004(10) C14 0.008(4) 0.008(4) 0.008(4) -0.0027(17) -0.0027(17) 0.0000(10) O1 0.0130(18) 0.0127(18) 0.0121(18) -0.0050(11) -0.0038(11) -0.0001(10) O2 0.007(4) 0.017(4) 0.025(4) -0.015(4) 0.001(3) -0.003(3) O3 0.015(4) 0.010(4) 0.013(4) -0.009(3) 0.003(3) -0.004(3) O4 0.020(4) 0.019(5) 0.022(4) -0.015(4) -0.004(4) 0.004(3) O5 0.017(4) 0.026(5) 0.026(5) -0.020(4) 0.005(4) -0.010(3) O6 0.022(4) 0.012(4) 0.020(4) -0.008(3) -0.009(4) -0.006(3) O7 0.012(2) 0.012(2) 0.011(2) -0.0040(12) -0.0039(11) 0.0005(8) O8 0.026(4) 0.026(4) 0.025(4) -0.0086(16) -0.0088(17) 0.0003(10) O9 0.030(9) 0.005(7) 0.011(7) 0.000(6) -0.007(7) -0.004(6) O10 0.022(9) 0.026(9) 0.019(8) -0.014(8) -0.007(8) 0.006(7) O11 0.018(8) 0.011(8) 0.015(8) -0.004(7) 0.004(7) -0.006(6) O12 0.023(4) 0.023(4) 0.023(4) -0.0079(16) -0.0078(16) 0.0002(10) O13 0.025(4) 0.012(4) 0.036(5) -0.002(4) -0.015(4) 0.001(3) O14 0.016(4) 0.028(5) 0.017(4) -0.010(4) -0.004(4) -0.012(3) O15 0.015(4) 0.026(5) 0.018(4) -0.016(4) 0.004(4) -0.010(3) O16 0.023(2) 0.024(2) 0.023(2) -0.0074(11) -0.0083(11) -0.0007(10) O17 0.035(10) 0.023(9) 0.027(9) -0.009(8) -0.027(9) 0.002(8) O18 0.022(4) 0.022(4) 0.022(4) -0.0078(16) -0.0074(16) 0.0004(10) O19 0.015(3) 0.015(3) 0.015(3) -0.0050(15) -0.0053(15) 0.0000(10) O20 0.012(2) 0.012(2) 0.012(2) -0.0040(12) -0.0039(11) 0.0005(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 Ho1 O1 2.274(7) . ? Ho1 O4 2.295(8) 2_666 ? Ho1 O20 2.34(3) . ? Ho1 O13 2.350(8) . ? Ho1 O14 2.356(7) . ? Ho1 O6 2.356(7) 2_656 ? Ho1 O5 2.360(7) 1_654 ? Ho1 O15 2.387(8) . ? Ho1 O7 2.49(3) . ? C1 O1 1.247(12) . ? C1 O2 1.253(12) . ? C1 C2 1.530(14) . ? C2 O3 1.341(12) . ? C2 C3 1.342(15) . ? C3 C4 1.435(15) . ? C3 H3A 0.9300 . ? C4 O6 1.258(12) . ? C4 C5 1.427(14) . ? C5 C6 1.351(15) . ? C5 H5A 0.9300 . ? C6 O3 1.366(12) . ? C6 C7 1.513(14) . ? C7 O4 1.255(13) . ? C7 O5 1.263(13) . ? C8 O20 1.18(3) . ? C8 O7 1.19(3) . ? C8 O8 1.25(3) . ? C8 C9 1.53(3) . ? C8 O18 1.59(2) . ? C9 C10 1.32(3) . ? C9 O9 1.40(2) . ? C10 C12 1.30(3) 2_655 ? C10 C11 1.46(3) . ? C10 H10A 0.9599 . ? C11 C13 0.67(3) 2_655 ? C11 C12 0.80(3) 2_655 ? C11 O12 1.25(3) . ? C11 C12 1.44(3) . ? C11 O9 1.84(3) 2_655 ? C12 C11 0.80(3) 2_655 ? C12 C12 1.20(4) 2_655 ? C12 C10 1.30(3) 2_655 ? C12 C13 1.36(4) . ? C12 H12A 0.9562 . ? C13 C11 0.67(3) 2_655 ? C13 O12 0.73(3) 2_655 ? C13 O9 1.36(3) . ? C13 C14 1.53(3) . ? C14 O12 1.19(3) 2_655 ? C14 O11 1.24(2) . ? C14 O10 1.24(2) . ? C14 O19 1.66(2) . ? O4 Ho1 2.295(8) 2_666 ? O5 Ho1 2.360(7) 1_456 ? O6 Ho1 2.356(7) 2_656 ? O8 O18 0.822(19) . ? O9 O12 1.36(2) 2_655 ? O9 C11 1.84(3) 2_655 ? O10 O19 1.34(2) . ? O10 O12 1.81(2) 2_655 ? O11 O19 1.81(2) . ? O12 C13 0.73(3) 2_655 ? O12 C14 1.19(3) 2_655 ? O12 O9 1.36(2) 2_655 ? O12 O10 1.81(2) 2_655 ? O13 H13A 0.8411 . ? O13 H13B 0.8419 . ? O14 H14B 0.8458 . ? O14 H14A 0.8465 . ? O15 H15A 0.8508 . ? O15 H15B 0.8410 . ? O16 H16A 0.7985 . ? O16 H16B 0.8642 . ? O17 O17 1.45(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 Ho1 O4 94.5(3) . 2_666 ? O1 Ho1 O20 146.6(6) . . ? O4 Ho1 O20 76.1(6) 2_666 . ? O1 Ho1 O13 75.3(3) . . ? O4 Ho1 O13 143.3(3) 2_666 . ? O20 Ho1 O13 130.1(6) . . ? O1 Ho1 O14 79.5(3) . . ? O4 Ho1 O14 72.2(3) 2_666 . ? O20 Ho1 O14 125.5(7) . . ? O13 Ho1 O14 71.3(3) . . ? O1 Ho1 O6 90.1(2) . 2_656 ? O4 Ho1 O6 146.4(3) 2_666 2_656 ? O20 Ho1 O6 81.8(7) . 2_656 ? O13 Ho1 O6 69.9(3) . 2_656 ? O14 Ho1 O6 141.2(3) . 2_656 ? O1 Ho1 O5 145.7(3) . 1_654 ? O4 Ho1 O5 103.5(3) 2_666 1_654 ? O20 Ho1 O5 67.1(6) . 1_654 ? O13 Ho1 O5 72.8(3) . 1_654 ? O14 Ho1 O5 78.7(3) . 1_654 ? O6 Ho1 O5 90.6(3) 2_656 1_654 ? O1 Ho1 O15 73.7(3) . . ? O4 Ho1 O15 76.1(3) 2_666 . ? O20 Ho1 O15 73.0(6) . . ? O13 Ho1 O15 131.1(3) . . ? O14 Ho1 O15 136.2(3) . . ? O6 Ho1 O15 73.3(3) 2_656 . ? O5 Ho1 O15 138.7(3) 1_654 . ? O1 Ho1 O7 143.2(6) . . ? O4 Ho1 O7 72.3(6) 2_666 . ? O20 Ho1 O7 4.6(10) . . ? O13 Ho1 O7 134.6(6) . . ? O14 Ho1 O7 125.3(7) . . ? O6 Ho1 O7 84.2(6) 2_656 . ? O5 Ho1 O7 70.8(6) 1_654 . ? O15 Ho1 O7 69.9(6) . . ? O1 C1 O2 127.2(10) . . ? O1 C1 C2 115.7(9) . . ? O2 C1 C2 117.0(9) . . ? O3 C2 C3 122.8(9) . . ? O3 C2 C1 112.9(8) . . ? C3 C2 C1 124.3(9) . . ? C2 C3 C4 120.2(9) . . ? C2 C3 H3A 119.9 . . ? C4 C3 H3A 119.9 . . ? O6 C4 C5 123.0(10) . . ? O6 C4 C3 121.4(9) . . ? C5 C4 C3 115.6(9) . . ? C6 C5 C4 120.1(10) . . ? C6 C5 H5A 119.9 . . ? C4 C5 H5A 119.9 . . ? C5 C6 O3 122.2(9) . . ? C5 C6 C7 125.4(10) . . ? O3 C6 C7 112.4(9) . . ? O4 C7 O5 127.1(9) . . ? O4 C7 C6 117.2(9) . . ? O5 C7 C6 115.7(9) . . ? O20 C8 O7 12(2) . . ? O20 C8 O8 131(2) . . ? O7 C8 O8 130(2) . . ? O20 C8 C9 115(2) . . ? O7 C8 C9 116(2) . . ? O8 C8 C9 113.3(17) . . ? O20 C8 O18 155(2) . . ? O7 C8 O18 159(2) . . ? O8 C8 O18 30.7(10) . . ? C9 C8 O18 85.8(13) . . ? C10 C9 O9 121.6(19) . . ? C10 C9 C8 126.2(19) . . ? O9 C9 C8 112.0(15) . . ? C10 C9 C12 43.7(14) . 2_655 ? O9 C9 C12 78.1(12) . 2_655 ? C8 C9 C12 169.8(16) . 2_655 ? C12 C10 C9 92(2) 2_655 . ? C12 C10 C11 33.0(12) 2_655 . ? C9 C10 C11 122(2) . . ? C12 C10 C13 44.1(15) 2_655 2_655 ? C9 C10 C13 136(2) . 2_655 ? C11 C10 C13 15.6(12) . 2_655 ? C12 C10 H10A 147.8 2_655 . ? C9 C10 H10A 118.8 . . ? C11 C10 H10A 119.1 . . ? C13 C10 H10A 105.3 2_655 . ? C13 C11 C12 135(5) 2_655 2_655 ? C13 C11 O12 28(3) 2_655 . ? C12 C11 O12 163(4) 2_655 . ? C13 C11 C12 110(4) 2_655 . ? C12 C11 C12 56(3) 2_655 . ? O12 C11 C12 124(2) . . ? C13 C11 C10 129(4) 2_655 . ? C12 C11 C10 62(2) 2_655 . ? O12 C11 C10 121(2) . . ? C12 C11 C10 115(3) . . ? C13 C11 O9 36(3) 2_655 2_655 ? C12 C11 O9 125(3) 2_655 2_655 ? O12 C11 O9 47.3(13) . 2_655 ? C12 C11 O9 78.2(15) . 2_655 ? C10 C11 O9 164(2) . 2_655 ? C13 C11 C14 47(3) 2_655 2_655 ? C12 C11 C14 135(3) 2_655 2_655 ? O12 C11 C14 37.6(12) . 2_655 ? C12 C11 C14 157(2) . 2_655 ? C10 C11 C14 85.6(15) . 2_655 ? O9 C11 C14 80.3(13) 2_655 2_655 ? C13 C11 C11 122(4) 2_655 2_655 ? C12 C11 C11 36.8(19) 2_655 2_655 ? O12 C11 C11 142(3) . 2_655 ? C12 C11 C11 19.4(11) . 2_655 ? C10 C11 C11 96(2) . 2_655 ? O9 C11 C11 94.7(17) 2_655 2_655 ? C14 C11 C11 162(2) 2_655 2_655 ? C11 C12 C12 90(3) 2_655 2_655 ? C11 C12 C10 85(3) 2_655 2_655 ? C12 C12 C10 156(3) 2_655 2_655 ? C11 C12 C13 20(2) 2_655 . ? C12 C12 C13 89(3) 2_655 . ? C10 C12 C13 94(2) 2_655 . ? C11 C12 C11 124(3) 2_655 . ? C12 C12 C11 33.7(14) 2_655 . ? C10 C12 C11 144(3) 2_655 . ? C13 C12 C11 120(2) . . ? C11 C12 C13 136(3) 2_655 2_655 ? C12 C12 C13 49.5(19) 2_655 2_655 ? C10 C12 C13 124(2) 2_655 2_655 ? C13 C12 C13 138.0(17) . 2_655 ? C11 C12 C13 20.6(12) . 2_655 ? C11 C12 C9 126(3) 2_655 2_655 ? C12 C12 C9 127(3) 2_655 2_655 ? C10 C12 C9 44.7(13) 2_655 2_655 ? C13 C12 C9 138.9(19) . 2_655 ? C11 C12 C9 100.1(19) . 2_655 ? C13 C12 C9 80.2(14) 2_655 2_655 ? C11 C12 H12A 112.5 2_655 . ? C12 C12 H12A 147.8 2_655 . ? C10 C12 H12A 27.7 2_655 . ? C13 C12 H12A 120.7 . . ? C11 C12 H12A 119.4 . . ? C13 C12 H12A 100.3 2_655 . ? C9 C12 H12A 20.9 2_655 . ? C11 C13 O12 126(5) 2_655 2_655 ? C11 C13 O9 127(4) 2_655 . ? O12 C13 O9 74(3) 2_655 . ? C11 C13 C12 24(3) 2_655 . ? O12 C13 C12 151(4) 2_655 . ? O9 C13 C12 123(2) . . ? C11 C13 C14 114(4) 2_655 . ? O12 C13 C14 50(2) 2_655 . ? O9 C13 C14 114(2) . . ? C12 C13 C14 123(2) . . ? C11 C13 C12 49(3) 2_655 2_655 ? O12 C13 C12 138(3) 2_655 2_655 ? O9 C13 C12 82.2(15) . 2_655 ? C12 C13 C12 42.0(17) . 2_655 ? C14 C13 C12 163(2) . 2_655 ? C11 C13 C10 36(3) 2_655 2_655 ? O12 C13 C10 116(3) 2_655 2_655 ? O9 C13 C10 163(2) . 2_655 ? C12 C13 C10 41.5(14) . 2_655 ? C14 C13 C10 82.3(15) . 2_655 ? C12 C13 C10 81.4(16) 2_655 2_655 ? O12 C14 O11 131(2) 2_655 . ? O12 C14 O10 95.9(18) 2_655 . ? O11 C14 O10 128.5(19) . . ? O12 C14 C13 27.8(12) 2_655 . ? O11 C14 C13 114.8(19) . . ? O10 C14 C13 116.7(19) . . ? O12 C14 O19 143.7(19) 2_655 . ? O11 C14 O19 75.9(13) . . ? O10 C14 O19 52.6(11) . . ? C13 C14 O19 169.3(19) . . ? O12 C14 C11 39.8(13) 2_655 2_655 ? O11 C14 C11 96.7(15) . 2_655 ? O10 C14 C11 134.4(17) . 2_655 ? C13 C14 C11 18.7(11) . 2_655 ? O19 C14 C11 170.8(16) . 2_655 ? C1 O1 Ho1 153.9(7) . . ? C2 O3 C6 118.9(8) . . ? C7 O4 Ho1 161.5(7) . 2_666 ? C7 O5 Ho1 124.2(7) . 1_456 ? C4 O6 Ho1 151.0(7) . 2_656 ? C8 O7 Ho1 129.4(18) . . ? O18 O8 C8 98(2) . . ? O12 O9 C13 31.3(11) 2_655 . ? O12 O9 C9 145.0(16) 2_655 . ? C13 O9 C9 118.3(18) . . ? O12 O9 C11 42.8(12) 2_655 2_655 ? C13 O9 C11 16.8(13) . 2_655 ? C9 O9 C11 103.6(13) . 2_655 ? C14 O10 O19 80.0(14) . . ? C14 O10 O12 41.1(11) . 2_655 ? O19 O10 O12 118.5(13) . 2_655 ? C14 O11 O19 62.7(12) . . ? C13 O12 C14 103(3) 2_655 2_655 ? C13 O12 C11 26(3) 2_655 . ? C14 O12 C11 102.6(19) 2_655 . ? C13 O12 O9 74(3) 2_655 2_655 ? C14 O12 O9 143.4(19) 2_655 2_655 ? C11 O12 O9 89.8(17) . 2_655 ? C13 O12 O10 132(3) 2_655 2_655 ? C14 O12 O10 43.0(12) 2_655 2_655 ? C11 O12 O10 143.8(17) . 2_655 ? O9 O12 O10 112.4(13) 2_655 2_655 ? Ho1 O13 H13A 134.6 . . ? Ho1 O13 H13B 130.9 . . ? H13A O13 H13B 93.3 . . ? Ho1 O14 H14B 130.7 . . ? Ho1 O14 H14A 128.5 . . ? H14B O14 H14A 99.0 . . ? Ho1 O15 H15A 125.0 . . ? Ho1 O15 H15B 130.8 . . ? H15A O15 H15B 96.5 . . ? H16A O16 H16B 111.2 . . ? O8 O18 C8 51.0(17) . . ? O10 O19 C14 47.4(11) . . ? O10 O19 O11 88.8(11) . . ? C14 O19 O11 41.4(9) . . ? C8 O20 Ho1 146(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 O3 -177.1(9) . . . . ? O2 C1 C2 O3 4.8(15) . . . . ? O1 C1 C2 C3 2.9(17) . . . . ? O2 C1 C2 C3 -175.1(11) . . . . ? O3 C2 C3 C4 -4.6(17) . . . . ? C1 C2 C3 C4 175.4(10) . . . . ? C2 C3 C4 O6 -173.6(11) . . . . ? C2 C3 C4 C5 4.1(16) . . . . ? O6 C4 C5 C6 176.0(11) . . . . ? C3 C4 C5 C6 -1.7(16) . . . . ? C4 C5 C6 O3 -0.5(18) . . . . ? C4 C5 C6 C7 178.5(10) . . . . ? C5 C6 C7 O4 -163.3(12) . . . . ? O3 C6 C7 O4 15.8(15) . . . . ? C5 C6 C7 O5 14.6(17) . . . . ? O3 C6 C7 O5 -166.3(9) . . . . ? O20 C8 C9 C10 -163(2) . . . . ? O7 C8 C9 C10 -176(2) . . . . ? O8 C8 C9 C10 16(3) . . . . ? O18 C8 C9 C10 3(3) . . . . ? O20 C8 C9 O9 12(3) . . . . ? O7 C8 C9 O9 -1(3) . . . . ? O8 C8 C9 O9 -168.2(18) . . . . ? O18 C8 C9 O9 177.9(16) . . . . ? O20 C8 C9 C12 -170(9) . . . 2_655 ? O7 C8 C9 C12 177(9) . . . 2_655 ? O8 C8 C9 C12 9(11) . . . 2_655 ? O18 C8 C9 C12 -5(10) . . . 2_655 ? O9 C9 C10 C12 7(3) . . . 2_655 ? C8 C9 C10 C12 -178(2) . . . 2_655 ? O9 C9 C10 C11 -7(4) . . . . ? C8 C9 C10 C11 168(2) . . . . ? C12 C9 C10 C11 -13.8(18) 2_655 . . . ? O9 C9 C10 C13 3(4) . . . 2_655 ? C8 C9 C10 C13 178(2) . . . 2_655 ? C12 C9 C10 C13 -4(2) 2_655 . . 2_655 ? C12 C10 C11 C13 128(7) 2_655 . . 2_655 ? C9 C10 C11 C13 153(5) . . . 2_655 ? C9 C10 C11 C12 26(3) . . . 2_655 ? C13 C10 C11 C12 -128(7) 2_655 . . 2_655 ? C12 C10 C11 O12 161(4) 2_655 . . . ? C9 C10 C11 O12 -173(2) . . . . ? C13 C10 C11 O12 33(4) 2_655 . . . ? C12 C10 C11 C12 -21(3) 2_655 . . . ? C9 C10 C11 C12 5(3) . . . . ? C13 C10 C11 C12 -149(7) 2_655 . . . ? C12 C10 C11 O9 121(8) 2_655 . . 2_655 ? C9 C10 C11 O9 147(6) . . . 2_655 ? C13 C10 C11 O9 -7(5) 2_655 . . 2_655 ? C12 C10 C11 C14 148(3) 2_655 . . 2_655 ? C9 C10 C11 C14 174(2) . . . 2_655 ? C13 C10 C11 C14 20(5) 2_655 . . 2_655 ? C12 C10 C11 C11 -14(2) 2_655 . . 2_655 ? C9 C10 C11 C11 12(3) . . . 2_655 ? C13 C10 C11 C11 -141(7) 2_655 . . 2_655 ? C13 C11 C12 C11 -132(6) 2_655 . . 2_655 ? C12 C11 C12 C11 0.001(3) 2_655 . . 2_655 ? O12 C11 C12 C11 -159(4) . . . 2_655 ? C10 C11 C12 C11 22(3) . . . 2_655 ? O9 C11 C12 C11 -148(4) 2_655 . . 2_655 ? C14 C11 C12 C11 -128(6) 2_655 . . 2_655 ? C13 C11 C12 C12 -132(6) 2_655 . . 2_655 ? O12 C11 C12 C12 -159(4) . . . 2_655 ? C10 C11 C12 C12 22(3) . . . 2_655 ? O9 C11 C12 C12 -148(4) 2_655 . . 2_655 ? C14 C11 C12 C12 -128(6) 2_655 . . 2_655 ? C11 C11 C12 C12 -0.001(3) 2_655 . . 2_655 ? C13 C11 C12 C10 6(7) 2_655 . . 2_655 ? C12 C11 C12 C10 138(6) 2_655 . . 2_655 ? O12 C11 C12 C10 -21(6) . . . 2_655 ? C10 C11 C12 C10 160(3) . . . 2_655 ? O9 C11 C12 C10 -10(4) 2_655 . . 2_655 ? C14 C11 C12 C10 10(9) 2_655 . . 2_655 ? C11 C11 C12 C10 138(6) 2_655 . . 2_655 ? C13 C11 C12 C13 -155(3) 2_655 . . . ? C12 C11 C12 C13 -23(3) 2_655 . . . ? O12 C11 C12 C13 177(2) . . . . ? C10 C11 C12 C13 -1(4) . . . . ? O9 C11 C12 C13 -171(2) 2_655 . . . ? C14 C11 C12 C13 -152(4) 2_655 . . . ? C11 C11 C12 C13 -23(3) 2_655 . . . ? C12 C11 C12 C13 132(6) 2_655 . . 2_655 ? O12 C11 C12 C13 -28(3) . . . 2_655 ? C10 C11 C12 C13 154(6) . . . 2_655 ? O9 C11 C12 C13 -16(4) 2_655 . . 2_655 ? C14 C11 C12 C13 4(4) 2_655 . . 2_655 ? C11 C11 C12 C13 132(6) 2_655 . . 2_655 ? C13 C11 C12 C9 15(5) 2_655 . . 2_655 ? C12 C11 C12 C9 147(4) 2_655 . . 2_655 ? O12 C11 C12 C9 -13(3) . . . 2_655 ? C10 C11 C12 C9 169.1(19) . . . 2_655 ? O9 C11 C12 C9 -1.0(13) 2_655 . . 2_655 ? C14 C11 C12 C9 18(6) 2_655 . . 2_655 ? C11 C11 C12 C9 147(4) 2_655 . . 2_655 ? C12 C12 C13 C11 94(7) 2_655 . . 2_655 ? C10 C12 C13 C11 -62(6) 2_655 . . 2_655 ? C11 C12 C13 C11 107(7) . . . 2_655 ? C13 C12 C13 C11 94(7) 2_655 . . 2_655 ? C9 C12 C13 C11 -58(7) 2_655 . . 2_655 ? C11 C12 C13 O12 12(7) 2_655 . . 2_655 ? C12 C12 C13 O12 107(7) 2_655 . . 2_655 ? C10 C12 C13 O12 -50(7) 2_655 . . 2_655 ? C11 C12 C13 O12 119(7) . . . 2_655 ? C13 C12 C13 O12 107(7) 2_655 . . 2_655 ? C9 C12 C13 O12 -46(9) 2_655 . . 2_655 ? C11 C12 C13 O9 -108(7) 2_655 . . . ? C12 C12 C13 O9 -14(4) 2_655 . . . ? C10 C12 C13 O9 -170(2) 2_655 . . . ? C11 C12 C13 O9 -1(4) . . . . ? C13 C12 C13 O9 -14(4) 2_655 . . . ? C9 C12 C13 O9 -166(2) 2_655 . . . ? C11 C12 C13 C14 77(7) 2_655 . . . ? C12 C12 C13 C14 171(3) 2_655 . . . ? C10 C12 C13 C14 15(3) 2_655 . . . ? C11 C12 C13 C14 -176(2) . . . . ? C13 C12 C13 C14 171(3) 2_655 . . . ? C9 C12 C13 C14 19(4) 2_655 . . . ? C11 C12 C13 C12 -94(7) 2_655 . . 2_655 ? C10 C12 C13 C12 -156(3) 2_655 . . 2_655 ? C11 C12 C13 C12 12.7(16) . . . 2_655 ? C13 C12 C13 C12 -0.001(3) 2_655 . . 2_655 ? C9 C12 C13 C12 -152(5) 2_655 . . 2_655 ? C11 C12 C13 C10 62(6) 2_655 . . 2_655 ? C12 C12 C13 C10 156(3) 2_655 . . 2_655 ? C11 C12 C13 C10 169(3) . . . 2_655 ? C13 C12 C13 C10 156(3) 2_655 . . 2_655 ? C9 C12 C13 C10 4(2) 2_655 . . 2_655 ? C11 C13 C14 O12 -118(6) 2_655 . . 2_655 ? O9 C13 C14 O12 40(3) . . . 2_655 ? C12 C13 C14 O12 -144(5) . . . 2_655 ? C12 C13 C14 O12 -123(8) 2_655 . . 2_655 ? C10 C13 C14 O12 -135(3) 2_655 . . 2_655 ? C11 C13 C14 O11 15(5) 2_655 . . . ? O12 C13 C14 O11 133(3) 2_655 . . . ? O9 C13 C14 O11 172.9(19) . . . . ? C12 C13 C14 O11 -11(3) . . . . ? C12 C13 C14 O11 10(8) 2_655 . . . ? C10 C13 C14 O11 -2(2) 2_655 . . . ? C11 C13 C14 O10 -163(4) 2_655 . . . ? O12 C13 C14 O10 -45(3) 2_655 . . . ? O9 C13 C14 O10 -5(3) . . . . ? C12 C13 C14 O10 171(2) . . . . ? C12 C13 C14 O10 -168(7) 2_655 . . . ? C10 C13 C14 O10 -180(2) 2_655 . . . ? C11 C13 C14 O19 -161(9) 2_655 . . . ? O12 C13 C14 O19 -43(11) 2_655 . . . ? O9 C13 C14 O19 -3(11) . . . . ? C12 C13 C14 O19 173(9) . . . . ? C12 C13 C14 O19 -166(7) 2_655 . . . ? C10 C13 C14 O19 -177(10) 2_655 . . . ? O12 C13 C14 C11 118(6) 2_655 . . 2_655 ? O9 C13 C14 C11 158(6) . . . 2_655 ? C12 C13 C14 C11 -26(3) . . . 2_655 ? C12 C13 C14 C11 -5(5) 2_655 . . 2_655 ? C10 C13 C14 C11 -16(4) 2_655 . . 2_655 ? O2 C1 O1 Ho1 -97.5(18) . . . . ? C2 C1 O1 Ho1 84.7(18) . . . . ? O4 Ho1 O1 C1 56.9(16) 2_666 . . . ? O20 Ho1 O1 C1 -15(2) . . . . ? O13 Ho1 O1 C1 -158.9(16) . . . . ? O14 Ho1 O1 C1 127.8(16) . . . . ? O6 Ho1 O1 C1 -89.8(16) 2_656 . . . ? O5 Ho1 O1 C1 179.0(14) 1_654 . . . ? O15 Ho1 O1 C1 -17.2(15) . . . . ? O7 Ho1 O1 C1 -9(2) . . . . ? C3 C2 O3 C6 2.3(16) . . . . ? C1 C2 O3 C6 -177.7(9) . . . . ? C5 C6 O3 C2 0.4(17) . . . . ? C7 C6 O3 C2 -178.7(9) . . . . ? O5 C7 O4 Ho1 -108(2) . . . 2_666 ? C6 C7 O4 Ho1 70(3) . . . 2_666 ? O4 C7 O5 Ho1 5.9(16) . . . 1_456 ? C6 C7 O5 Ho1 -171.8(7) . . . 1_456 ? C5 C4 O6 Ho1 6(2) . . . 2_656 ? C3 C4 O6 Ho1 -176.6(10) . . . 2_656 ? O20 C8 O7 Ho1 -3(10) . . . . ? O8 C8 O7 Ho1 -106(3) . . . . ? C9 C8 O7 Ho1 89(3) . . . . ? O18 C8 O7 Ho1 -87(6) . . . . ? O1 Ho1 O7 C8 -137(2) . . . . ? O4 Ho1 O7 C8 150(3) 2_666 . . . ? O20 Ho1 O7 C8 4(14) . . . . ? O13 Ho1 O7 C8 -1(3) . . . . ? O14 Ho1 O7 C8 98(2) . . . . ? O6 Ho1 O7 C8 -55(2) 2_656 . . . ? O5 Ho1 O7 C8 38(2) 1_654 . . . ? O15 Ho1 O7 C8 -129(3) . . . . ? O20 C8 O8 O18 151(3) . . . . ? O7 C8 O8 O18 167(3) . . . . ? C9 C8 O8 O18 -28(3) . . . . ? C11 C13 O9 O12 124(7) 2_655 . . 2_655 ? C12 C13 O9 O12 154(4) . . . 2_655 ? C14 C13 O9 O12 -31(2) . . . 2_655 ? C12 C13 O9 O12 145(3) 2_655 . . 2_655 ? C10 C13 O9 O12 131(9) 2_655 . . 2_655 ? C11 C13 O9 C9 -30(6) 2_655 . . . ? O12 C13 O9 C9 -155(3) 2_655 . . . ? C12 C13 O9 C9 -1(3) . . . . ? C14 C13 O9 C9 174.8(18) . . . . ? C12 C13 O9 C9 -10(2) 2_655 . . . ? C10 C13 O9 C9 -24(8) 2_655 . . . ? O12 C13 O9 C11 -124(7) 2_655 . . 2_655 ? C12 C13 O9 C11 30(4) . . . 2_655 ? C14 C13 O9 C11 -155(7) . . . 2_655 ? C12 C13 O9 C11 20(5) 2_655 . . 2_655 ? C10 C13 O9 C11 6(4) 2_655 . . 2_655 ? C10 C9 O9 O12 -18(4) . . . 2_655 ? C8 C9 O9 O12 166(2) . . . 2_655 ? C12 C9 O9 O12 -13(3) 2_655 . . 2_655 ? C10 C9 O9 C13 5(3) . . . . ? C8 C9 O9 C13 -170.8(19) . . . . ? C12 C9 O9 C13 9.7(19) 2_655 . . . ? C10 C9 O9 C11 -4(2) . . . 2_655 ? C8 C9 O9 C11 -179.5(16) . . . 2_655 ? C12 C9 O9 C11 1.0(14) 2_655 . . 2_655 ? O12 C14 O10 O19 160.2(17) 2_655 . . . ? O11 C14 O10 O19 2(3) . . . . ? C13 C14 O10 O19 180(2) . . . . ? C11 C14 O10 O19 172(2) 2_655 . . . ? O11 C14 O10 O12 -158(3) . . . 2_655 ? C13 C14 O10 O12 19.4(15) . . . 2_655 ? O19 C14 O10 O12 -160.2(17) . . . 2_655 ? C11 C14 O10 O12 11.9(18) 2_655 . . 2_655 ? O12 C14 O11 O19 -152(3) 2_655 . . . ? O10 C14 O11 O19 -2(2) . . . . ? C13 C14 O11 O19 -179(2) . . . . ? C11 C14 O11 O19 -174.5(15) 2_655 . . . ? C12 C11 O12 C13 -18(11) 2_655 . . 2_655 ? C12 C11 O12 C13 68(6) . . . 2_655 ? C10 C11 O12 C13 -114(7) . . . 2_655 ? O9 C11 O12 C13 52(6) 2_655 . . 2_655 ? C14 C11 O12 C13 -93(6) 2_655 . . 2_655 ? C11 C11 O12 C13 57(6) 2_655 . . 2_655 ? C13 C11 O12 C14 93(6) 2_655 . . 2_655 ? C12 C11 O12 C14 75(11) 2_655 . . 2_655 ? C12 C11 O12 C14 161(2) . . . 2_655 ? C10 C11 O12 C14 -21(3) . . . 2_655 ? O9 C11 O12 C14 145(2) 2_655 . . 2_655 ? C11 C11 O12 C14 150(4) 2_655 . . 2_655 ? C13 C11 O12 O9 -52(6) 2_655 . . 2_655 ? C12 C11 O12 O9 -70(11) 2_655 . . 2_655 ? C12 C11 O12 O9 16(3) . . . 2_655 ? C10 C11 O12 O9 -166(2) . . . 2_655 ? C14 C11 O12 O9 -145(2) 2_655 . . 2_655 ? C11 C11 O12 O9 5(4) 2_655 . . 2_655 ? C13 C11 O12 O10 78(7) 2_655 . . 2_655 ? C12 C11 O12 O10 60(12) 2_655 . . 2_655 ? C12 C11 O12 O10 145(2) . . . 2_655 ? C10 C11 O12 O10 -36(5) . . . 2_655 ? O9 C11 O12 O10 130(3) 2_655 . . 2_655 ? C14 C11 O12 O10 -15(2) 2_655 . . 2_655 ? C11 C11 O12 O10 134(3) 2_655 . . 2_655 ? O20 C8 O18 O8 -58(5) . . . . ? O7 C8 O18 O8 -29(6) . . . . ? C9 C8 O18 O8 154(2) . . . . ? O12 O10 O19 C14 14.7(13) 2_655 . . . ? C14 O10 O19 O11 -1.0(13) . . . . ? O12 O10 O19 O11 13.7(15) 2_655 . . . ? O12 C14 O19 O10 -35(3) 2_655 . . . ? O11 C14 O19 O10 -178(2) . . . . ? C13 C14 O19 O10 -2(10) . . . . ? C11 C14 O19 O10 -142(10) 2_655 . . . ? O12 C14 O19 O11 144(4) 2_655 . . . ? O10 C14 O19 O11 178(2) . . . . ? C13 C14 O19 O11 176(11) . . . . ? C11 C14 O19 O11 37(9) 2_655 . . . ? C14 O11 O19 O10 1.1(15) . . . . ? O7 C8 O20 Ho1 176(15) . . . . ? O8 C8 O20 Ho1 -97(4) . . . . ? C9 C8 O20 Ho1 82(4) . . . . ? O18 C8 O20 Ho1 -62(7) . . . . ? O1 Ho1 O20 C8 -131(3) . . . . ? O4 Ho1 O20 C8 152(4) 2_666 . . . ? O13 Ho1 O20 C8 1(4) . . . . ? O14 Ho1 O20 C8 96(4) . . . . ? O6 Ho1 O20 C8 -54(4) 2_656 . . . ? O5 Ho1 O20 C8 40(4) 1_654 . . . ? O15 Ho1 O20 C8 -129(4) . . . . ? O7 Ho1 O20 C8 -175(19) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.15 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 3.600 _refine_diff_density_min -2.224 _refine_diff_density_rms 0.388 # Attachment 'Ho-11.cif' data_Ho-11 _database_code_depnum_ccdc_archive 'CCDC 716756' #TrackingRef 'Ho-11.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H24 Ho2 O26' _chemical_formula_weight 962.22 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' Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.1814(4) _cell_length_b 10.0963(7) _cell_length_c 10.8666(7) _cell_angle_alpha 97.249(6) _cell_angle_beta 95.999(5) _cell_angle_gamma 103.840(6) _cell_volume 646.81(7) _cell_formula_units_Z 1 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 2644 _cell_measurement_theta_min 2.61 _cell_measurement_theta_max 26.37 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.470 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 462 _exptl_absorpt_coefficient_mu 6.191 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.3707 _exptl_absorpt_correction_T_max 0.5764 _exptl_absorpt_process_details Crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(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 ? _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4424 _diffrn_reflns_av_R_equivalents 0.0159 _diffrn_reflns_av_sigmaI/netI 0.0197 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 26.37 _reflns_number_total 2644 _reflns_number_gt 2569 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0281P)^2^+1.6956P] 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 2644 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0205 _refine_ls_R_factor_gt 0.0197 _refine_ls_wR_factor_ref 0.0496 _refine_ls_wR_factor_gt 0.0492 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _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 0.5661(6) 1.1605(3) 0.1506(3) 0.0077(6) Uani 1 1 d . . . C2 C 0.6937(6) 1.0610(4) 0.1192(3) 0.0078(6) Uani 1 1 d . . . H2 H 0.8139 1.0838 0.0744 0.009 Uiso 1 1 calc R . . C3 C 0.6392(5) 0.9365(3) 0.1545(3) 0.0065(6) Uani 1 1 d . . . C4 C 0.3446(6) 0.9899(4) 0.2567(3) 0.0072(6) Uani 1 1 d . . . C5 C 0.3875(6) 1.1169(4) 0.2247(3) 0.0079(6) Uani 1 1 d . . . H5 H 0.3023 1.1771 0.2502 0.009 Uiso 1 1 calc R . . C6 C 0.1577(5) 0.9222(3) 0.3260(3) 0.0064(6) Uani 1 1 d . . . C7 C 0.7447(5) 0.8177(3) 0.1233(3) 0.0064(6) Uani 1 1 d . . . C8 C 0.4182(5) 0.5282(3) 0.5389(3) 0.0065(6) Uani 1 1 d . . . Ho1 Ho 0.36312(2) 0.647240(14) 0.278697(13) 0.00441(6) Uani 1 1 d . . . O1 O 0.6027(4) 1.2739(2) 0.1122(2) 0.0103(5) Uani 1 1 d . . . O2 O 0.4682(4) 0.8996(2) 0.2229(2) 0.0069(5) Uani 1 1 d . . . O3 O 0.9057(4) 0.8400(3) 0.0634(2) 0.0100(5) Uani 1 1 d . . . O4 O 0.6578(4) 0.7068(2) 0.1612(2) 0.0084(5) Uani 1 1 d . . . O5 O 0.0189(4) 0.9877(2) 0.3541(2) 0.0078(5) Uani 1 1 d . . . O6 O 0.1567(4) 0.8015(2) 0.3457(2) 0.0082(5) Uani 1 1 d . . . O7 O 0.1600(4) 0.6621(3) 0.0826(2) 0.0094(5) Uani 1 1 d . . . H7A H 0.0686 0.7166 0.0794 0.011 Uiso 1 1 d R . . H7B H 0.2161 0.6677 0.0188 0.011 Uiso 1 1 d R . . O8 O 0.0029(4) 0.4993(3) 0.2731(2) 0.0117(5) Uani 1 1 d . . . H8A H -0.0546 0.4350 0.2117 0.014 Uiso 1 1 d R . . H8B H 0.0427 0.4622 0.3347 0.014 Uiso 1 1 d R . . O9 O 0.3236(4) 0.4426(3) 0.1350(2) 0.0137(5) Uani 1 1 d . . . H9A H 0.3552 0.3715 0.0986 0.016 Uiso 1 1 d R . . H9B H 0.2047 0.4516 0.0938 0.016 Uiso 1 1 d R . . O10 O 0.3179(4) 0.6071(2) 0.4921(2) 0.0080(5) Uani 1 1 d . . . O11 O 0.5954(4) 0.5104(3) 0.3552(2) 0.0094(5) Uani 1 1 d . . . O12 O 0.6546(4) 0.8095(3) 0.4249(2) 0.0104(5) Uani 1 1 d . . . H12A H 0.7612 0.8719 0.3964 0.012 Uiso 1 1 d R . . H12B H 0.7156 0.7819 0.4910 0.012 Uiso 1 1 d R . . O13 O 1.0276(4) 0.2692(3) 0.3946(2) 0.0136(5) Uani 1 1 d . . . H13A H 0.9849 0.1823 0.3712 0.016 Uiso 1 1 d R . . H13B H 0.9698 0.2877 0.4602 0.016 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0089(16) 0.0063(16) 0.0052(15) -0.0014(12) -0.0016(12) -0.0009(13) C2 0.0070(15) 0.0107(16) 0.0048(15) 0.0014(13) -0.0008(12) 0.0013(13) C3 0.0056(15) 0.0091(16) 0.0042(15) 0.0007(12) 0.0003(12) 0.0011(13) C4 0.0072(15) 0.0098(16) 0.0053(15) -0.0002(12) 0.0009(12) 0.0040(13) C5 0.0092(16) 0.0079(16) 0.0076(16) 0.0008(13) 0.0019(13) 0.0040(13) C6 0.0051(15) 0.0076(15) 0.0047(15) -0.0014(12) -0.0012(12) 0.0006(12) C7 0.0054(15) 0.0098(16) 0.0035(14) -0.0015(12) -0.0026(12) 0.0035(13) C8 0.0041(14) 0.0052(15) 0.0078(15) -0.0015(12) 0.0001(12) -0.0014(12) Ho1 0.00421(9) 0.00415(9) 0.00515(9) 0.00098(6) 0.00067(6) 0.00149(6) O1 0.0141(12) 0.0059(12) 0.0124(12) 0.0028(10) 0.0044(10) 0.0038(10) O2 0.0056(11) 0.0071(11) 0.0089(12) 0.0011(9) 0.0030(9) 0.0025(9) O3 0.0080(11) 0.0115(12) 0.0133(12) 0.0051(10) 0.0048(10) 0.0046(10) O4 0.0078(11) 0.0093(12) 0.0099(12) 0.0029(9) 0.0035(9) 0.0038(9) O5 0.0083(11) 0.0077(11) 0.0075(12) 0.0000(9) 0.0013(9) 0.0027(9) O6 0.0083(11) 0.0073(11) 0.0106(12) 0.0027(9) 0.0028(9) 0.0035(9) O7 0.0114(12) 0.0135(12) 0.0061(11) 0.0034(9) 0.0032(9) 0.0063(10) O8 0.0099(12) 0.0092(12) 0.0144(13) 0.0017(10) 0.0007(10) -0.0001(10) O9 0.0132(12) 0.0096(12) 0.0166(13) -0.0063(10) -0.0034(10) 0.0064(10) O10 0.0085(11) 0.0092(12) 0.0082(11) 0.0042(9) 0.0017(9) 0.0041(9) O11 0.0105(12) 0.0128(12) 0.0072(11) 0.0041(10) 0.0034(9) 0.0052(10) O12 0.0092(11) 0.0104(12) 0.0083(12) 0.0011(9) -0.0021(9) -0.0021(10) O13 0.0160(13) 0.0095(12) 0.0153(13) 0.0013(10) 0.0049(10) 0.0023(10) _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 1.247(4) . ? C1 C2 1.448(5) . ? C1 C5 1.450(5) . ? C2 C3 1.337(5) . ? C2 H2 0.9300 . ? C3 O2 1.362(4) . ? C3 C7 1.515(4) . ? C4 C5 1.343(5) . ? C4 O2 1.363(4) . ? C4 C6 1.518(4) . ? C5 H5 0.9300 . ? C6 O5 1.242(4) . ? C6 O6 1.262(4) . ? C7 O3 1.237(4) . ? C7 O4 1.260(4) . ? C8 O10 1.245(4) . ? C8 O11 1.265(4) 2_666 ? C8 C8 1.547(6) 2_666 ? Ho1 O6 2.333(2) . ? Ho1 O4 2.338(2) . ? Ho1 O8 2.356(2) . ? Ho1 O9 2.373(2) . ? Ho1 O11 2.378(2) . ? Ho1 O7 2.398(2) . ? Ho1 O12 2.406(2) . ? Ho1 O10 2.437(2) . ? Ho1 O2 2.638(2) . ? Ho1 H8B 2.5595 . ? O7 H7A 0.8792 . ? O7 H7B 0.8088 . ? O8 H8A 0.8500 . ? O8 H8B 0.8500 . ? O9 H9A 0.8501 . ? O9 H9B 0.8500 . ? O11 C8 1.265(4) 2_666 ? O12 H12A 0.9056 . ? O12 H12B 0.8832 . ? O13 H13A 0.8500 . ? O13 H13B 0.8500 . ? 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 C2 121.8(3) . . ? O1 C1 C5 122.5(3) . . ? C2 C1 C5 115.6(3) . . ? C3 C2 C1 120.2(3) . . ? C3 C2 H2 119.9 . . ? C1 C2 H2 119.9 . . ? C2 C3 O2 122.0(3) . . ? C2 C3 C7 127.2(3) . . ? O2 C3 C7 110.8(3) . . ? C5 C4 O2 121.6(3) . . ? C5 C4 C6 128.3(3) . . ? O2 C4 C6 110.1(3) . . ? C4 C5 C1 120.3(3) . . ? C4 C5 H5 119.9 . . ? C1 C5 H5 119.9 . . ? O5 C6 O6 126.7(3) . . ? O5 C6 C4 117.8(3) . . ? O6 C6 C4 115.5(3) . . ? O3 C7 O4 127.2(3) . . ? O3 C7 C3 116.7(3) . . ? O4 C7 C3 116.1(3) . . ? O10 C8 O11 127.3(3) . 2_666 ? O10 C8 C8 117.2(4) . 2_666 ? O11 C8 C8 115.5(4) 2_666 2_666 ? O6 Ho1 O4 122.44(8) . . ? O6 Ho1 O8 77.89(8) . . ? O4 Ho1 O8 143.47(9) . . ? O6 Ho1 O9 140.55(9) . . ? O4 Ho1 O9 76.53(9) . . ? O8 Ho1 O9 70.53(9) . . ? O6 Ho1 O11 142.02(8) . . ? O4 Ho1 O11 81.02(8) . . ? O8 Ho1 O11 100.88(9) . . ? O9 Ho1 O11 68.86(9) . . ? O6 Ho1 O7 79.55(8) . . ? O4 Ho1 O7 79.06(8) . . ? O8 Ho1 O7 75.36(9) . . ? O9 Ho1 O7 70.20(9) . . ? O11 Ho1 O7 137.54(8) . . ? O6 Ho1 O12 81.28(8) . . ? O4 Ho1 O12 76.15(8) . . ? O8 Ho1 O12 140.08(9) . . ? O9 Ho1 O12 138.10(9) . . ? O11 Ho1 O12 75.97(9) . . ? O7 Ho1 O12 133.26(9) . . ? O6 Ho1 O10 76.73(8) . . ? O4 Ho1 O10 137.74(8) . . ? O8 Ho1 O10 72.34(9) . . ? O9 Ho1 O10 113.87(9) . . ? O11 Ho1 O10 67.08(8) . . ? O7 Ho1 O10 143.12(8) . . ? O12 Ho1 O10 69.91(8) . . ? O6 Ho1 O2 60.94(8) . . ? O4 Ho1 O2 61.50(8) . . ? O8 Ho1 O2 128.36(8) . . ? O9 Ho1 O2 124.78(8) . . ? O11 Ho1 O2 130.71(8) . . ? O7 Ho1 O2 68.07(8) . . ? O12 Ho1 O2 65.32(8) . . ? O10 Ho1 O2 121.27(8) . . ? O6 Ho1 H8B 85.1 . . ? O4 Ho1 H8B 149.1 . . ? O8 Ho1 H8B 19.3 . . ? O9 Ho1 H8B 72.9 . . ? O11 Ho1 H8B 84.2 . . ? O7 Ho1 H8B 94.3 . . ? O12 Ho1 H8B 126.0 . . ? O10 Ho1 H8B 56.1 . . ? O2 Ho1 H8B 143.4 . . ? C3 O2 C4 120.2(3) . . ? C3 O2 Ho1 119.48(19) . . ? C4 O2 Ho1 120.19(19) . . ? C7 O4 Ho1 132.1(2) . . ? C6 O6 Ho1 132.9(2) . . ? Ho1 O7 H7A 120.5 . . ? Ho1 O7 H7B 123.5 . . ? H7A O7 H7B 103.8 . . ? Ho1 O8 H8A 121.3 . . ? Ho1 O8 H8B 94.0 . . ? H8A O8 H8B 107.7 . . ? Ho1 O9 H9A 159.2 . . ? Ho1 O9 H9B 92.9 . . ? H9A O9 H9B 107.7 . . ? C8 O10 Ho1 118.7(2) . . ? C8 O11 Ho1 121.1(2) 2_666 . ? Ho1 O12 H12A 119.8 . . ? Ho1 O12 H12B 119.5 . . ? H12A O12 H12B 109.6 . . ? H13A O13 H13B 107.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 -175.2(3) . . . . ? C5 C1 C2 C3 2.2(5) . . . . ? C1 C2 C3 O2 -1.6(5) . . . . ? C1 C2 C3 C7 176.1(3) . . . . ? O2 C4 C5 C1 1.1(5) . . . . ? C6 C4 C5 C1 -175.8(3) . . . . ? O1 C1 C5 C4 175.4(3) . . . . ? C2 C1 C5 C4 -2.0(5) . . . . ? C5 C4 C6 O5 3.0(5) . . . . ? O2 C4 C6 O5 -174.3(3) . . . . ? C5 C4 C6 O6 -179.2(3) . . . . ? O2 C4 C6 O6 3.6(4) . . . . ? C2 C3 C7 O3 3.5(5) . . . . ? O2 C3 C7 O3 -178.5(3) . . . . ? C2 C3 C7 O4 -176.3(3) . . . . ? O2 C3 C7 O4 1.7(4) . . . . ? C2 C3 O2 C4 0.7(5) . . . . ? C7 C3 O2 C4 -177.4(3) . . . . ? C2 C3 O2 Ho1 177.2(2) . . . . ? C7 C3 O2 Ho1 -0.8(3) . . . . ? C5 C4 O2 C3 -0.4(5) . . . . ? C6 C4 O2 C3 177.1(3) . . . . ? C5 C4 O2 Ho1 -176.9(2) . . . . ? C6 C4 O2 Ho1 0.5(3) . . . . ? O6 Ho1 O2 C3 -179.1(2) . . . . ? O4 Ho1 O2 C3 0.0(2) . . . . ? O8 Ho1 O2 C3 -137.4(2) . . . . ? O9 Ho1 O2 C3 -45.6(2) . . . . ? O11 Ho1 O2 C3 45.5(3) . . . . ? O7 Ho1 O2 C3 -89.2(2) . . . . ? O12 Ho1 O2 C3 87.2(2) . . . . ? O10 Ho1 O2 C3 131.0(2) . . . . ? O6 Ho1 O2 C4 -2.6(2) . . . . ? O4 Ho1 O2 C4 176.6(2) . . . . ? O8 Ho1 O2 C4 39.2(3) . . . . ? O9 Ho1 O2 C4 131.0(2) . . . . ? O11 Ho1 O2 C4 -137.9(2) . . . . ? O7 Ho1 O2 C4 87.4(2) . . . . ? O12 Ho1 O2 C4 -96.3(2) . . . . ? O10 Ho1 O2 C4 -52.5(2) . . . . ? O3 C7 O4 Ho1 178.2(2) . . . . ? C3 C7 O4 Ho1 -2.1(4) . . . . ? O6 Ho1 O4 C7 2.0(3) . . . . ? O8 Ho1 O4 C7 118.2(3) . . . . ? O9 Ho1 O4 C7 144.1(3) . . . . ? O11 Ho1 O4 C7 -145.7(3) . . . . ? O7 Ho1 O4 C7 72.0(3) . . . . ? O12 Ho1 O4 C7 -68.0(3) . . . . ? O10 Ho1 O4 C7 -105.1(3) . . . . ? O2 Ho1 O4 C7 1.2(3) . . . . ? O5 C6 O6 Ho1 170.0(2) . . . . ? C4 C6 O6 Ho1 -7.6(4) . . . . ? O4 Ho1 O6 C6 4.9(3) . . . . ? O8 Ho1 O6 C6 -141.9(3) . . . . ? O9 Ho1 O6 C6 -104.8(3) . . . . ? O11 Ho1 O6 C6 125.8(3) . . . . ? O7 Ho1 O6 C6 -64.8(3) . . . . ? O12 Ho1 O6 C6 72.3(3) . . . . ? O10 Ho1 O6 C6 143.6(3) . . . . ? O2 Ho1 O6 C6 5.8(3) . . . . ? O11 C8 O10 Ho1 -175.8(3) 2_666 . . . ? C8 C8 O10 Ho1 5.4(5) 2_666 . . . ? O6 Ho1 O10 C8 -173.6(3) . . . . ? O4 Ho1 O10 C8 -49.5(3) . . . . ? O8 Ho1 O10 C8 105.1(2) . . . . ? O9 Ho1 O10 C8 46.7(3) . . . . ? O11 Ho1 O10 C8 -5.4(2) . . . . ? O7 Ho1 O10 C8 135.1(2) . . . . ? O12 Ho1 O10 C8 -88.1(2) . . . . ? O2 Ho1 O10 C8 -130.2(2) . . . . ? O6 Ho1 O11 C8 23.7(3) . . . 2_666 ? O4 Ho1 O11 C8 156.5(3) . . . 2_666 ? O8 Ho1 O11 C8 -60.5(3) . . . 2_666 ? O9 Ho1 O11 C8 -124.5(3) . . . 2_666 ? O7 Ho1 O11 C8 -140.7(2) . . . 2_666 ? O12 Ho1 O11 C8 78.7(2) . . . 2_666 ? O10 Ho1 O11 C8 4.9(2) . . . 2_666 ? O2 Ho1 O11 C8 117.2(2) . . . 2_666 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.886 _refine_diff_density_min -0.931 _refine_diff_density_rms 0.135 # Attachment 'Er-7.cif' data_Er-7 _database_code_depnum_ccdc_archive 'CCDC 716757' #TrackingRef 'Er-7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H32 Er2 O30' _chemical_formula_weight 1038.92 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' Er Er -0.2586 4.9576 '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' _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 6.3385(13) _cell_length_b 10.340(2) _cell_length_c 13.700(3) _cell_angle_alpha 108.60(3) _cell_angle_beta 94.42(3) _cell_angle_gamma 106.38(3) _cell_volume 802.6(3) _cell_formula_units_Z 1 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 2855 _cell_measurement_theta_min 1.60 _cell_measurement_theta_max 25.15 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.112 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 494 _exptl_absorpt_coefficient_mu 5.301 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4170 _exptl_absorpt_correction_T_max 0.7775 _exptl_absorpt_process_details Crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4162 _diffrn_reflns_av_R_equivalents 0.0174 _diffrn_reflns_av_sigmaI/netI 0.0306 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 25.15 _reflns_number_total 2855 _reflns_number_gt 2696 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Isor has been used to restrict the disordered water molecules. ; _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^)+(0.0440P)^2^+0.5958P] 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 2855 _refine_ls_number_parameters 238 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0272 _refine_ls_R_factor_gt 0.0255 _refine_ls_wR_factor_ref 0.0665 _refine_ls_wR_factor_gt 0.0653 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _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 O11 O 0.1351(5) 0.0526(4) -0.0953(2) 0.0309(7) Uani 1 1 d . . . Er1 Er 0.20521(3) -0.002641(19) 0.213307(13) 0.02044(9) Uani 1 1 d . . . C1 C 0.4655(8) 0.4032(5) 0.6134(4) 0.0318(10) Uani 1 1 d . . . C2 C 0.2389(8) 0.2987(5) 0.5755(4) 0.0288(10) Uani 1 1 d . . . H2 H 0.1338 0.3002 0.6192 0.035 Uiso 1 1 calc R . . C3 C 0.1826(7) 0.2005(5) 0.4772(3) 0.0224(9) Uani 1 1 d . . . C4 C 0.5472(7) 0.2902(5) 0.4406(3) 0.0229(9) Uani 1 1 d . . . C5 C 0.6195(7) 0.3921(5) 0.5381(4) 0.0282(10) Uani 1 1 d . . . H5 H 0.7659 0.4548 0.5574 0.034 Uiso 1 1 calc R . . C6 C 0.6803(7) 0.2650(5) 0.3504(3) 0.0233(9) Uani 1 1 d . . . C7 C -0.0449(7) 0.0841(5) 0.4210(3) 0.0214(9) Uani 1 1 d . . . C8 C 0.1205(7) 0.0249(5) -0.0117(3) 0.0257(9) Uani 1 1 d . . . O1 O 0.5235(7) 0.5001(4) 0.7042(3) 0.0483(10) Uani 1 1 d . . . O2 O 0.3330(5) 0.1941(3) 0.4093(2) 0.0253(7) Uani 1 1 d . . . O3 O -0.2022(5) 0.0753(4) 0.4722(2) 0.0292(7) Uani 1 1 d . . . O4 O -0.0553(5) 0.0060(3) 0.3271(2) 0.0262(7) Uani 1 1 d . . . O5 O 0.8783(5) 0.3409(4) 0.3678(3) 0.0348(8) Uani 1 1 d . . . O6 O 0.5687(5) 0.1648(3) 0.2635(2) 0.0277(7) Uani 1 1 d . . . O7 O 0.3585(5) -0.0929(4) 0.3401(2) 0.0327(7) Uani 1 1 d . . . H7A H 0.2965 -0.0916 0.3956 0.039 Uiso 1 1 d R . . H7B H 0.4960 -0.0453 0.3613 0.039 Uiso 1 1 d R . . O8 O 0.4372(6) -0.1429(4) 0.1350(3) 0.0391(8) Uani 1 1 d . . . H8A H 0.5460 -0.1334 0.1800 0.047 Uiso 1 1 d R . . H8B H 0.4582 -0.1881 0.0748 0.047 Uiso 1 1 d R . . O9 O -0.0059(6) -0.2478(4) 0.1615(4) 0.0528(11) Uani 1 1 d . . . H9A H 0.0684 -0.3061 0.1483 0.063 Uiso 1 1 d R . . H9B H -0.1433 -0.2967 0.1379 0.063 Uiso 1 1 d R . . O10 O 0.2791(5) 0.0337(4) 0.0543(2) 0.0347(8) Uani 1 1 d . . . O12 O 0.1423(5) 0.2240(4) 0.2268(3) 0.0329(7) Uani 1 1 d . . . H12B H 0.2363 0.3013 0.2461 0.040 Uiso 1 1 d R . . H12A H 0.0468 0.2421 0.2533 0.040 Uiso 1 1 d R . . O13 O 0.3061(9) 0.7057(6) 0.9031(4) 0.0769(15) Uani 1 1 d . . . H13A H 0.2993 0.6177 0.8781 0.092 Uiso 1 1 d R . . H13B H 0.2502 0.7262 0.8539 0.092 Uiso 1 1 d R . . O14 O 0.117(8) 0.506(4) 0.121(7) 0.17(3) Uani 0.25(4) 1 d P A 1 O14' O 0.072(3) 0.5276(14) 0.191(2) 0.164(12) Uani 0.75(4) 1 d P A 1 O15 O 0.5453(14) 0.5827(12) 0.1096(9) 0.140(6) Uani 0.82(2) 1 d P B 2 O16 O 0.643(3) 0.602(2) 0.9753(18) 0.140(12) Uani 0.40(2) 1 d P C 3 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 O11 0.0207(16) 0.046(2) 0.0237(16) 0.0148(15) 0.0050(12) 0.0050(15) Er1 0.01479(12) 0.02510(13) 0.01939(12) 0.00719(9) 0.00328(8) 0.00423(8) C1 0.032(2) 0.032(3) 0.027(2) 0.007(2) 0.0030(19) 0.008(2) C2 0.028(2) 0.032(3) 0.025(2) 0.0085(19) 0.0088(18) 0.009(2) C3 0.019(2) 0.028(2) 0.024(2) 0.0116(18) 0.0054(17) 0.0092(18) C4 0.019(2) 0.022(2) 0.027(2) 0.0089(18) 0.0027(17) 0.0050(18) C5 0.020(2) 0.026(2) 0.031(2) 0.0060(19) -0.0006(18) 0.0027(19) C6 0.017(2) 0.022(2) 0.030(2) 0.0091(18) 0.0044(17) 0.0049(18) C7 0.0163(19) 0.027(2) 0.024(2) 0.0133(18) 0.0039(16) 0.0064(17) C8 0.019(2) 0.031(2) 0.024(2) 0.0071(19) 0.0071(18) 0.0072(19) O1 0.046(2) 0.045(2) 0.0306(18) -0.0031(17) 0.0082(16) -0.0016(19) O2 0.0148(14) 0.0325(17) 0.0221(15) 0.0049(13) 0.0042(12) 0.0033(13) O3 0.0195(15) 0.0404(19) 0.0268(16) 0.0127(14) 0.0087(13) 0.0064(14) O4 0.0182(14) 0.0339(18) 0.0224(15) 0.0082(13) 0.0031(12) 0.0043(13) O5 0.0167(15) 0.041(2) 0.0336(18) 0.0066(15) 0.0061(13) -0.0024(14) O6 0.0202(15) 0.0331(18) 0.0253(16) 0.0068(14) 0.0063(12) 0.0054(14) O7 0.0261(16) 0.041(2) 0.0316(17) 0.0143(15) 0.0060(14) 0.0102(15) O8 0.0341(19) 0.038(2) 0.049(2) 0.0122(17) 0.0216(16) 0.0162(17) O9 0.031(2) 0.031(2) 0.084(3) 0.012(2) 0.0025(19) 0.0038(17) O10 0.0154(15) 0.060(2) 0.0262(16) 0.0157(16) 0.0029(13) 0.0086(16) O12 0.0269(17) 0.0295(18) 0.0418(19) 0.0136(15) 0.0087(14) 0.0067(14) O13 0.090(4) 0.067(3) 0.056(3) 0.020(2) 0.011(3) 0.002(3) O14 0.13(3) 0.07(2) 0.36(7) 0.09(3) 0.16(4) 0.07(2) O14' 0.129(13) 0.063(7) 0.26(2) 0.075(10) -0.114(13) -0.016(7) O15 0.082(6) 0.172(11) 0.173(11) 0.116(9) -0.011(6) -0.002(6) O16 0.113(16) 0.076(13) 0.18(2) 0.002(12) -0.052(14) 0.023(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O11 C8 1.270(5) . ? O11 Er1 2.416(3) 2 ? Er1 O9 2.348(4) . ? Er1 O6 2.350(3) . ? Er1 O4 2.357(3) . ? Er1 O10 2.384(3) . ? Er1 O11 2.416(3) 2 ? Er1 O8 2.423(3) . ? Er1 O12 2.439(3) . ? Er1 O7 2.474(3) . ? Er1 O2 2.694(3) . ? C1 O1 1.270(6) . ? C1 C2 1.467(7) . ? C1 C5 1.474(7) . ? C2 C3 1.349(6) . ? C2 H2 0.9300 . ? C3 O2 1.383(5) . ? C3 C7 1.543(6) . ? C4 C5 1.356(6) . ? C4 O2 1.376(5) . ? C4 C6 1.545(6) . ? C5 H5 0.9300 . ? C6 O5 1.236(5) . ? C6 O6 1.289(5) . ? C7 O3 1.262(5) . ? C7 O4 1.268(5) . ? C8 O10 1.262(5) . ? C8 C8 1.561(8) 2 ? O7 H7A 0.8803 . ? O7 H7B 0.8451 . ? O8 H8A 0.8501 . ? O8 H8B 0.8499 . ? O9 H9A 0.8499 . ? O9 H9B 0.8500 . ? O12 H12B 0.7977 . ? O12 H12A 0.7663 . ? O13 H13A 0.8501 . ? O13 H13B 0.8499 . ? O14 O14' 0.99(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C8 O11 Er1 118.7(3) . 2 ? O9 Er1 O6 144.89(13) . . ? O9 Er1 O4 78.73(13) . . ? O6 Er1 O4 121.55(10) . . ? O9 Er1 O10 104.82(15) . . ? O6 Er1 O10 77.22(11) . . ? O4 Er1 O10 142.02(10) . . ? O9 Er1 O11 70.45(14) . 2 ? O6 Er1 O11 137.41(11) . 2 ? O4 Er1 O11 78.19(10) . 2 ? O10 Er1 O11 68.12(10) . 2 ? O9 Er1 O8 72.12(13) . . ? O6 Er1 O8 75.91(12) . . ? O4 Er1 O8 142.07(12) . . ? O10 Er1 O8 70.55(12) . . ? O11 Er1 O8 112.88(12) 2 . ? O9 Er1 O12 138.09(12) . . ? O6 Er1 O12 76.79(11) . . ? O4 Er1 O12 78.37(11) . . ? O10 Er1 O12 74.48(12) . . ? O11 Er1 O12 70.79(12) 2 . ? O8 Er1 O12 139.38(12) . . ? O9 Er1 O7 74.00(14) . . ? O6 Er1 O7 81.74(11) . . ? O4 Er1 O7 79.33(11) . . ? O10 Er1 O7 138.48(11) . . ? O11 Er1 O7 140.85(11) 2 . ? O8 Er1 O7 69.79(12) . . ? O12 Er1 O7 134.19(11) . . ? O9 Er1 O2 127.46(13) . . ? O6 Er1 O2 60.99(10) . . ? O4 Er1 O2 60.64(10) . . ? O10 Er1 O2 127.72(11) . . ? O11 Er1 O2 125.15(11) 2 . ? O8 Er1 O2 121.93(11) . . ? O12 Er1 O2 66.89(11) . . ? O7 Er1 O2 67.30(11) . . ? O1 C1 C2 122.2(4) . . ? O1 C1 C5 122.0(4) . . ? C2 C1 C5 115.8(4) . . ? C3 C2 C1 120.2(4) . . ? C3 C2 H2 119.9 . . ? C1 C2 H2 119.9 . . ? C2 C3 O2 122.0(4) . . ? C2 C3 C7 128.7(4) . . ? O2 C3 C7 109.2(3) . . ? C5 C4 O2 122.0(4) . . ? C5 C4 C6 127.4(4) . . ? O2 C4 C6 110.6(3) . . ? C4 C5 C1 119.9(4) . . ? C4 C5 H5 120.1 . . ? C1 C5 H5 120.1 . . ? O5 C6 O6 126.9(4) . . ? O5 C6 C4 118.1(4) . . ? O6 C6 C4 115.0(3) . . ? O3 C7 O4 126.2(4) . . ? O3 C7 C3 117.5(4) . . ? O4 C7 C3 116.3(4) . . ? O10 C8 O11 127.1(4) . . ? O10 C8 C8 116.8(5) . 2 ? O11 C8 C8 116.1(5) . 2 ? C4 O2 C3 120.2(3) . . ? C4 O2 Er1 119.6(2) . . ? C3 O2 Er1 120.2(2) . . ? C7 O4 Er1 133.6(3) . . ? C6 O6 Er1 133.7(3) . . ? Er1 O7 H7A 118.3 . . ? Er1 O7 H7B 108.5 . . ? H7A O7 H7B 107.8 . . ? Er1 O8 H8A 111.6 . . ? Er1 O8 H8B 139.7 . . ? H8A O8 H8B 107.7 . . ? Er1 O9 H9A 115.5 . . ? Er1 O9 H9B 134.8 . . ? H9A O9 H9B 107.7 . . ? C8 O10 Er1 119.7(3) . . ? Er1 O12 H12B 125.7 . . ? Er1 O12 H12A 119.0 . . ? H12B O12 H12A 101.6 . . ? H13A O13 H13B 107.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 177.9(5) . . . . ? C5 C1 C2 C3 0.1(7) . . . . ? C1 C2 C3 O2 0.0(7) . . . . ? C1 C2 C3 C7 -178.6(4) . . . . ? O2 C4 C5 C1 -0.9(7) . . . . ? C6 C4 C5 C1 178.0(4) . . . . ? O1 C1 C5 C4 -177.4(5) . . . . ? C2 C1 C5 C4 0.4(7) . . . . ? C5 C4 C6 O5 3.1(7) . . . . ? O2 C4 C6 O5 -178.0(4) . . . . ? C5 C4 C6 O6 -176.8(4) . . . . ? O2 C4 C6 O6 2.1(5) . . . . ? C2 C3 C7 O3 -1.1(7) . . . . ? O2 C3 C7 O3 -179.9(4) . . . . ? C2 C3 C7 O4 178.9(5) . . . . ? O2 C3 C7 O4 0.1(5) . . . . ? Er1 O11 C8 O10 174.2(4) 2 . . . ? Er1 O11 C8 C8 -6.1(6) 2 . . 2 ? C5 C4 O2 C3 1.0(6) . . . . ? C6 C4 O2 C3 -178.0(3) . . . . ? C5 C4 O2 Er1 179.5(3) . . . . ? C6 C4 O2 Er1 0.5(4) . . . . ? C2 C3 O2 C4 -0.5(6) . . . . ? C7 C3 O2 C4 178.3(3) . . . . ? C2 C3 O2 Er1 -179.0(3) . . . . ? C7 C3 O2 Er1 -0.2(4) . . . . ? O9 Er1 O2 C4 137.1(3) . . . . ? O6 Er1 O2 C4 -1.8(3) . . . . ? O4 Er1 O2 C4 -178.4(3) . . . . ? O10 Er1 O2 C4 -43.3(3) . . . . ? O11 Er1 O2 C4 -131.5(3) 2 . . . ? O8 Er1 O2 C4 45.9(3) . . . . ? O12 Er1 O2 C4 -89.0(3) . . . . ? O7 Er1 O2 C4 91.3(3) . . . . ? O9 Er1 O2 C3 -44.3(3) . . . . ? O6 Er1 O2 C3 176.8(3) . . . . ? O4 Er1 O2 C3 0.1(3) . . . . ? O10 Er1 O2 C3 135.2(3) . . . . ? O11 Er1 O2 C3 47.0(3) 2 . . . ? O8 Er1 O2 C3 -135.6(3) . . . . ? O12 Er1 O2 C3 89.5(3) . . . . ? O7 Er1 O2 C3 -90.1(3) . . . . ? O3 C7 O4 Er1 -180.0(3) . . . . ? C3 C7 O4 Er1 0.0(6) . . . . ? O9 Er1 O4 C7 145.4(4) . . . . ? O6 Er1 O4 C7 -3.6(4) . . . . ? O10 Er1 O4 C7 -114.9(4) . . . . ? O11 Er1 O4 C7 -142.5(4) 2 . . . ? O8 Er1 O4 C7 105.3(4) . . . . ? O12 Er1 O4 C7 -70.0(4) . . . . ? O7 Er1 O4 C7 69.8(4) . . . . ? O2 Er1 O4 C7 -0.1(4) . . . . ? O5 C6 O6 Er1 175.3(3) . . . . ? C4 C6 O6 Er1 -4.8(6) . . . . ? O9 Er1 O6 C6 -111.1(4) . . . . ? O4 Er1 O6 C6 7.2(4) . . . . ? O10 Er1 O6 C6 151.2(4) . . . . ? O11 Er1 O6 C6 115.4(4) 2 . . . ? O8 Er1 O6 C6 -136.0(4) . . . . ? O12 Er1 O6 C6 74.4(4) . . . . ? O7 Er1 O6 C6 -64.8(4) . . . . ? O2 Er1 O6 C6 3.7(4) . . . . ? O11 C8 O10 Er1 173.9(4) . . . . ? C8 C8 O10 Er1 -5.9(7) 2 . . . ? O9 Er1 O10 C8 67.8(4) . . . . ? O6 Er1 O10 C8 -148.3(4) . . . . ? O4 Er1 O10 C8 -22.8(5) . . . . ? O11 Er1 O10 C8 6.4(3) 2 . . . ? O8 Er1 O10 C8 132.3(4) . . . . ? O12 Er1 O10 C8 -68.7(4) . . . . ? O7 Er1 O10 C8 150.2(3) . . . . ? O2 Er1 O10 C8 -111.9(3) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.15 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.165 _refine_diff_density_min -1.216 _refine_diff_density_rms 0.141 # Attachment 'Tm-8.cif' data_Tm-8 _database_code_depnum_ccdc_archive 'CCDC 716758' #TrackingRef 'Tm-8.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H32 O30 Tm2' _chemical_formula_weight 1042.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tm Tm -0.3139 5.2483 '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 6.2356(12) _cell_length_b 10.183(2) _cell_length_c 13.466(3) _cell_angle_alpha 108.55(3) _cell_angle_beta 94.37(3) _cell_angle_gamma 106.45(3) _cell_volume 764.3(3) _cell_formula_units_Z 1 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 2641 _cell_measurement_theta_min 1.62 _cell_measurement_theta_max 25.01 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.238 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 494 _exptl_absorpt_coefficient_mu 5.884 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5907 _exptl_absorpt_correction_T_max 0.8914 _exptl_absorpt_process_details Crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4566 _diffrn_reflns_av_R_equivalents 0.0207 _diffrn_reflns_av_sigmaI/netI 0.0324 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 25.01 _reflns_number_total 2641 _reflns_number_gt 2494 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0316P)^2^+0.8752P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0031(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2641 _refine_ls_number_parameters 238 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0215 _refine_ls_R_factor_gt 0.0203 _refine_ls_wR_factor_ref 0.0556 _refine_ls_wR_factor_gt 0.0551 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _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 Tm1 Tm 0.70509(2) -0.002411(17) 0.213176(12) 0.01720(11) Uani 1 1 d . . . C1 C 0.9655(7) 0.4037(5) 0.6130(3) 0.0258(9) Uani 1 1 d . . . C2 C 0.7401(7) 0.2987(5) 0.5753(3) 0.0254(9) Uani 1 1 d . . . H2 H 0.6338 0.2998 0.6201 0.030 Uiso 1 1 calc R . . C3 C 0.6823(7) 0.2002(4) 0.4769(3) 0.0199(8) Uani 1 1 d . . . C4 C 1.0466(6) 0.2900(4) 0.4406(3) 0.0191(8) Uani 1 1 d . . . C5 C 1.1201(7) 0.3918(4) 0.5380(3) 0.0237(9) Uani 1 1 d . . . H5 H 1.2695 0.4547 0.5577 0.028 Uiso 1 1 calc R . . C6 C 1.1792(6) 0.2644(4) 0.3493(3) 0.0202(8) Uani 1 1 d . . . C7 C 0.4550(6) 0.0838(4) 0.4208(3) 0.0190(8) Uani 1 1 d . . . C8 C 0.3781(7) -0.0249(4) 0.0119(3) 0.0220(8) Uani 1 1 d . . . O1 O 1.0230(6) 0.5000(4) 0.7042(3) 0.0436(9) Uani 1 1 d . . . O2 O 0.8333(4) 0.1944(3) 0.4092(2) 0.0207(6) Uani 1 1 d . . . O3 O 0.2971(5) 0.0750(3) 0.4713(2) 0.0261(6) Uani 1 1 d . . . O4 O 0.4448(4) 0.0056(3) 0.3264(2) 0.0224(6) Uani 1 1 d . . . O5 O 1.3787(5) 0.3401(3) 0.3674(3) 0.0312(7) Uani 1 1 d . . . O6 O 1.0680(5) 0.1641(3) 0.2634(2) 0.0234(6) Uani 1 1 d . . . O7 O 0.8580(5) -0.0925(3) 0.3401(2) 0.0280(7) Uani 1 1 d . . . O8 O 0.9380(5) -0.1425(3) 0.1356(3) 0.0341(8) Uani 1 1 d . . . O9 O 0.4921(6) -0.2482(4) 0.1607(3) 0.0438(9) Uani 1 1 d . . . O10 O 0.3646(5) -0.0519(3) 0.0956(2) 0.0263(6) Uani 1 1 d . . . O11 O 0.2219(5) -0.0331(4) -0.0541(2) 0.0304(7) Uani 1 1 d . . . O12 O 0.6442(5) 0.2252(3) 0.2274(2) 0.0274(6) Uani 1 1 d . . . O13 O 0.1940(8) 0.2965(5) 0.0975(4) 0.0682(13) Uani 1 1 d . . . H13A H 0.1278 0.2340 0.0362 0.082 Uiso 1 1 d R . . H13B H 0.1895 0.2508 0.1407 0.082 Uiso 1 1 d R . . O14 O 0.530(4) 0.539(2) 0.219(2) 0.054(9) Uani 0.30(5) 1 d P A 1 O14' O 0.610(4) 0.5178(12) 0.160(3) 0.123(11) Uani 0.70(5) 1 d P A 2 O15 O 0.0427(13) 0.5841(12) 0.1081(9) 0.116(5) Uani 0.681(12) 1 d P B 3 O15' O 0.862(3) 0.3977(16) 0.0260(14) 0.083(7) Uani 0.319(12) 1 d P B 4 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 Tm1 0.01371(13) 0.02326(14) 0.01444(13) 0.00736(8) 0.00435(7) 0.00450(8) C1 0.027(2) 0.030(2) 0.020(2) 0.0095(18) 0.0044(17) 0.0064(18) C2 0.025(2) 0.030(2) 0.021(2) 0.0085(17) 0.0114(17) 0.0080(18) C3 0.020(2) 0.026(2) 0.021(2) 0.0135(17) 0.0083(16) 0.0095(17) C4 0.0152(19) 0.0236(19) 0.021(2) 0.0131(17) 0.0041(15) 0.0046(16) C5 0.021(2) 0.0224(19) 0.025(2) 0.0081(17) 0.0039(17) 0.0023(16) C6 0.0154(19) 0.0244(19) 0.025(2) 0.0133(17) 0.0082(16) 0.0063(16) C7 0.0162(19) 0.0256(19) 0.020(2) 0.0137(17) 0.0051(15) 0.0080(16) C8 0.023(2) 0.027(2) 0.0122(19) 0.0021(16) 0.0056(16) 0.0065(17) O1 0.044(2) 0.0388(18) 0.0232(17) -0.0059(14) 0.0086(15) -0.0051(16) O2 0.0133(13) 0.0273(14) 0.0172(14) 0.0054(11) 0.0053(11) 0.0023(11) O3 0.0199(15) 0.0379(16) 0.0233(15) 0.0143(13) 0.0103(12) 0.0081(13) O4 0.0155(13) 0.0304(15) 0.0166(14) 0.0067(12) 0.0055(11) 0.0019(12) O5 0.0152(15) 0.0369(17) 0.0304(17) 0.0058(14) 0.0066(12) -0.0017(13) O6 0.0178(14) 0.0303(15) 0.0176(14) 0.0051(12) 0.0047(11) 0.0047(12) O7 0.0291(16) 0.0374(17) 0.0244(16) 0.0168(13) 0.0083(13) 0.0136(14) O8 0.0316(17) 0.0318(16) 0.044(2) 0.0137(15) 0.0242(15) 0.0142(14) O9 0.0308(18) 0.0279(17) 0.064(3) 0.0116(16) 0.0050(17) 0.0027(14) O10 0.0169(14) 0.0422(17) 0.0186(15) 0.0144(13) 0.0038(11) 0.0033(13) O11 0.0166(15) 0.059(2) 0.0172(15) 0.0172(14) 0.0062(12) 0.0103(14) O12 0.0244(15) 0.0284(15) 0.0330(17) 0.0137(13) 0.0084(13) 0.0099(12) O13 0.081(3) 0.059(3) 0.045(2) 0.016(2) 0.011(2) -0.003(2) O14 0.036(11) 0.050(9) 0.078(17) 0.027(9) -0.006(8) 0.015(7) O14' 0.093(10) 0.055(5) 0.21(2) 0.048(8) -0.019(14) 0.020(6) O15 0.053(5) 0.153(9) 0.160(10) 0.115(8) -0.006(5) -0.001(5) O15' 0.075(11) 0.059(9) 0.093(13) 0.004(8) -0.025(9) 0.025(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 Tm1 O6 2.306(3) . ? Tm1 O4 2.311(3) . ? Tm1 O9 2.319(3) . ? Tm1 O11 2.339(3) 2_655 ? Tm1 O10 2.376(3) . ? Tm1 O8 2.386(3) . ? Tm1 O12 2.404(3) . ? Tm1 O7 2.432(3) . ? Tm1 O2 2.651(3) . ? C1 O1 1.252(5) . ? C1 C2 1.439(6) . ? C1 C5 1.449(6) . ? C2 C3 1.329(6) . ? C2 H2 0.9300 . ? C3 O2 1.360(5) . ? C3 C7 1.517(6) . ? C4 C5 1.334(6) . ? C4 O2 1.347(5) . ? C4 C6 1.529(5) . ? C5 H5 0.9300 . ? C6 O5 1.222(5) . ? C6 O6 1.259(5) . ? C7 O3 1.237(5) . ? C7 O4 1.253(5) . ? C8 O11 1.234(5) . ? C8 O10 1.245(5) . ? C8 C8 1.553(8) 2_655 ? O11 Tm1 2.339(3) 2_655 ? O13 H13A 0.8499 . ? O13 H13B 0.8501 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Tm1 O4 121.64(10) . . ? O6 Tm1 O9 144.93(11) . . ? O4 Tm1 O9 78.65(12) . . ? O6 Tm1 O11 77.49(11) . 2_655 ? O4 Tm1 O11 141.97(10) . 2_655 ? O9 Tm1 O11 104.46(13) . 2_655 ? O6 Tm1 O10 137.55(10) . . ? O4 Tm1 O10 77.98(10) . . ? O9 Tm1 O10 70.31(12) . . ? O11 Tm1 O10 68.11(10) 2_655 . ? O6 Tm1 O8 75.77(11) . . ? O4 Tm1 O8 141.84(11) . . ? O9 Tm1 O8 72.18(12) . . ? O11 Tm1 O8 70.74(11) 2_655 . ? O10 Tm1 O8 113.28(12) . . ? O6 Tm1 O12 76.62(10) . . ? O4 Tm1 O12 78.48(10) . . ? O9 Tm1 O12 138.23(11) . . ? O11 Tm1 O12 74.71(11) 2_655 . ? O10 Tm1 O12 71.02(11) . . ? O8 Tm1 O12 139.45(11) . . ? O6 Tm1 O7 81.60(11) . . ? O4 Tm1 O7 79.31(10) . . ? O9 Tm1 O7 74.24(13) . . ? O11 Tm1 O7 138.51(10) 2_655 . ? O10 Tm1 O7 140.85(10) . . ? O8 Tm1 O7 69.56(11) . . ? O12 Tm1 O7 133.88(11) . . ? O6 Tm1 O2 60.90(9) . . ? O4 Tm1 O2 60.81(9) . . ? O9 Tm1 O2 127.69(12) . . ? O11 Tm1 O2 127.85(10) 2_655 . ? O10 Tm1 O2 125.00(10) . . ? O8 Tm1 O2 121.68(10) . . ? O12 Tm1 O2 66.59(10) . . ? O7 Tm1 O2 67.30(10) . . ? O1 C1 C2 122.1(4) . . ? O1 C1 C5 122.3(4) . . ? C2 C1 C5 115.6(4) . . ? C3 C2 C1 120.6(4) . . ? C3 C2 H2 119.7 . . ? C1 C2 H2 119.7 . . ? C2 C3 O2 121.5(4) . . ? C2 C3 C7 129.1(4) . . ? O2 C3 C7 109.4(3) . . ? C5 C4 O2 122.4(4) . . ? C5 C4 C6 127.4(4) . . ? O2 C4 C6 110.2(3) . . ? C4 C5 C1 119.5(4) . . ? C4 C5 H5 120.2 . . ? C1 C5 H5 120.2 . . ? O5 C6 O6 127.4(4) . . ? O5 C6 C4 117.5(4) . . ? O6 C6 C4 115.1(3) . . ? O3 C7 O4 126.0(4) . . ? O3 C7 C3 117.7(4) . . ? O4 C7 C3 116.3(3) . . ? O11 C8 O10 128.0(4) . . ? O11 C8 C8 116.3(4) . 2_655 ? O10 C8 C8 115.8(4) . 2_655 ? C4 O2 C3 120.3(3) . . ? C4 O2 Tm1 119.8(2) . . ? C3 O2 Tm1 119.9(2) . . ? C7 O4 Tm1 133.6(2) . . ? C6 O6 Tm1 134.0(2) . . ? C8 O10 Tm1 118.9(2) . . ? C8 O11 Tm1 120.4(2) . 2_655 ? H13A O13 H13B 107.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 178.2(4) . . . . ? C5 C1 C2 C3 -1.0(6) . . . . ? C1 C2 C3 O2 0.5(6) . . . . ? C1 C2 C3 C7 -178.2(4) . . . . ? O2 C4 C5 C1 -1.5(6) . . . . ? C6 C4 C5 C1 177.2(4) . . . . ? O1 C1 C5 C4 -177.7(4) . . . . ? C2 C1 C5 C4 1.4(6) . . . . ? C5 C4 C6 O5 3.7(6) . . . . ? O2 C4 C6 O5 -177.5(3) . . . . ? C5 C4 C6 O6 -177.4(4) . . . . ? O2 C4 C6 O6 1.4(5) . . . . ? C2 C3 C7 O3 -0.6(6) . . . . ? O2 C3 C7 O3 -179.4(3) . . . . ? C2 C3 C7 O4 178.9(4) . . . . ? O2 C3 C7 O4 0.1(5) . . . . ? C5 C4 O2 C3 0.9(6) . . . . ? C6 C4 O2 C3 -177.9(3) . . . . ? C5 C4 O2 Tm1 179.6(3) . . . . ? C6 C4 O2 Tm1 0.8(4) . . . . ? C2 C3 O2 C4 -0.4(6) . . . . ? C7 C3 O2 C4 178.5(3) . . . . ? C2 C3 O2 Tm1 -179.1(3) . . . . ? C7 C3 O2 Tm1 -0.2(4) . . . . ? O6 Tm1 O2 C4 -1.7(2) . . . . ? O4 Tm1 O2 C4 -178.5(3) . . . . ? O9 Tm1 O2 C4 137.2(3) . . . . ? O11 Tm1 O2 C4 -43.4(3) 2_655 . . . ? O10 Tm1 O2 C4 -131.6(2) . . . . ? O8 Tm1 O2 C4 45.9(3) . . . . ? O12 Tm1 O2 C4 -89.0(3) . . . . ? O7 Tm1 O2 C4 91.3(3) . . . . ? O6 Tm1 O2 C3 177.0(3) . . . . ? O4 Tm1 O2 C3 0.2(2) . . . . ? O9 Tm1 O2 C3 -44.1(3) . . . . ? O11 Tm1 O2 C3 135.3(3) 2_655 . . . ? O10 Tm1 O2 C3 47.2(3) . . . . ? O8 Tm1 O2 C3 -135.3(2) . . . . ? O12 Tm1 O2 C3 89.8(3) . . . . ? O7 Tm1 O2 C3 -90.0(3) . . . . ? O3 C7 O4 Tm1 179.5(3) . . . . ? C3 C7 O4 Tm1 0.1(5) . . . . ? O6 Tm1 O4 C7 -3.4(4) . . . . ? O9 Tm1 O4 C7 145.6(4) . . . . ? O11 Tm1 O4 C7 -115.4(4) 2_655 . . . ? O10 Tm1 O4 C7 -142.4(4) . . . . ? O8 Tm1 O4 C7 105.1(4) . . . . ? O12 Tm1 O4 C7 -69.6(3) . . . . ? O7 Tm1 O4 C7 69.7(3) . . . . ? O2 Tm1 O4 C7 -0.2(3) . . . . ? O5 C6 O6 Tm1 174.9(3) . . . . ? C4 C6 O6 Tm1 -3.8(5) . . . . ? O4 Tm1 O6 C6 6.3(4) . . . . ? O9 Tm1 O6 C6 -112.0(4) . . . . ? O11 Tm1 O6 C6 150.5(4) 2_655 . . . ? O10 Tm1 O6 C6 114.5(4) . . . . ? O8 Tm1 O6 C6 -136.5(4) . . . . ? O12 Tm1 O6 C6 73.5(4) . . . . ? O7 Tm1 O6 C6 -65.5(4) . . . . ? O2 Tm1 O6 C6 3.1(3) . . . . ? O11 C8 O10 Tm1 -174.2(3) . . . . ? C8 C8 O10 Tm1 5.9(6) 2_655 . . . ? O6 Tm1 O10 C8 31.8(4) . . . . ? O4 Tm1 O10 C8 156.0(3) . . . . ? O9 Tm1 O10 C8 -121.9(3) . . . . ? O11 Tm1 O10 C8 -6.4(3) 2_655 . . . ? O8 Tm1 O10 C8 -62.4(3) . . . . ? O12 Tm1 O10 C8 74.2(3) . . . . ? O7 Tm1 O10 C8 -148.2(3) . . . . ? O2 Tm1 O10 C8 115.3(3) . . . . ? O10 C8 O11 Tm1 -173.9(3) . . . 2_655 ? C8 C8 O11 Tm1 5.9(6) 2_655 . . 2_655 ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.670 _refine_diff_density_min -1.241 _refine_diff_density_rms 0.110 # Attachment 'Yb-9.cif' data_Yb-9 _database_code_depnum_ccdc_archive 'CCDC 716759' #TrackingRef 'Yb-9.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H26 O27 Yb2' _chemical_formula_weight 996.45 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' Yb Yb -0.3850 5.5486 '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 7.4895(15) _cell_length_b 11.093(2) _cell_length_c 16.875(3) _cell_angle_alpha 86.68(3) _cell_angle_beta 80.69(3) _cell_angle_gamma 77.65(3) _cell_volume 1351.1(4) _cell_formula_units_Z 2 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 4711 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 25.15 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.449 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 956 _exptl_absorpt_coefficient_mu 6.998 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.3350 _exptl_absorpt_correction_T_max 0.7211 _exptl_absorpt_process_details Crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7680 _diffrn_reflns_av_R_equivalents 0.0347 _diffrn_reflns_av_sigmaI/netI 0.0564 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 25.15 _reflns_number_total 4711 _reflns_number_gt 3887 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0571P)^2^+4.1770P] 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 4711 _refine_ls_number_parameters 406 _refine_ls_number_restraints 72 _refine_ls_R_factor_all 0.0414 _refine_ls_R_factor_gt 0.0360 _refine_ls_wR_factor_ref 0.1027 _refine_ls_wR_factor_gt 0.1005 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.061 _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 O24 O -0.2166(7) 1.0122(5) 0.4714(3) 0.0099(11) Uani 1 1 d U . . Yb1 Yb 0.29726(4) 0.76792(3) 0.518300(18) 0.00582(11) Uani 1 1 d . . . Yb2 Yb 0.47624(4) -0.28048(3) 0.167932(18) 0.00481(11) Uani 1 1 d . . . C1 C 0.6524(10) -0.0228(7) 0.2114(5) 0.0107(16) Uani 1 1 d . . . C2 C 0.6145(10) 0.0868(7) 0.1549(5) 0.0110(16) Uani 1 1 d . . . C3 C 0.5738(10) 0.0790(7) 0.0808(5) 0.0094(16) Uani 1 1 d . . . H3 H 0.5633 0.0031 0.0634 0.011 Uiso 1 1 calc R . . C4 C 0.5464(9) 0.1854(7) 0.0281(4) 0.0061(15) Uani 1 1 d . . . C5 C 0.5493(10) 0.3006(7) 0.0638(5) 0.0083(15) Uani 1 1 d . . . H5 H 0.5221 0.3748 0.0353 0.010 Uiso 1 1 calc R . . C6 C 0.5915(10) 0.2997(7) 0.1383(5) 0.0096(16) Uani 1 1 d . . . C7 C 0.6079(10) 0.4142(7) 0.1796(4) 0.0072(15) Uani 1 1 d . . . C8 C 0.2033(10) -0.0169(7) 0.2312(5) 0.0093(16) Uani 1 1 d . . . C9 C 0.1367(10) 0.0843(7) 0.1721(5) 0.0089(16) Uani 1 1 d . . . C10 C 0.0854(10) 0.0685(7) 0.1015(5) 0.0076(15) Uani 1 1 d . . . H10 H 0.0814 -0.0104 0.0869 0.009 Uiso 1 1 calc R . . C11 C 0.0366(10) 0.1711(7) 0.0483(5) 0.0101(16) Uani 1 1 d . . . C12 C 0.0362(10) 0.2903(7) 0.0801(5) 0.0103(16) Uani 1 1 d . . . H12 H -0.0008 0.3623 0.0508 0.012 Uiso 1 1 calc R . . C13 C 0.0897(10) 0.2964(7) 0.1525(4) 0.0072(15) Uani 1 1 d U . . C14 C 0.1152(10) 0.4161(7) 0.1839(5) 0.0104(16) Uani 1 1 d . . . C15 C 0.5299(10) 0.5016(7) 0.5419(4) 0.0061(15) Uani 1 1 d . . . C16 C -0.0594(10) 0.9594(7) 0.4855(4) 0.0078(15) Uani 1 1 d . . . O1 O 0.7295(7) -0.0109(5) 0.2693(3) 0.0128(12) Uani 1 1 d U . . O2 O 0.6040(7) -0.1172(5) 0.1921(3) 0.0111(11) Uani 1 1 d U . . O3 O 0.6263(7) 0.1963(4) 0.1842(3) 0.0070(10) Uani 1 1 d . . . O4 O 0.6758(7) 0.4011(5) 0.2426(3) 0.0101(11) Uani 1 1 d . . . O5 O 0.5530(7) 0.5132(5) 0.1427(3) 0.0088(11) Uani 1 1 d U . . O6 O 0.5221(7) 0.1764(4) -0.0425(3) 0.0076(11) Uani 1 1 d U . . O7 O 0.6447(6) -0.3495(4) 0.2719(3) 0.0064(10) Uani 1 1 d U . . H7A H 0.6513 -0.4227 0.2909 0.008 Uiso 1 1 d R . . H7B H 0.7481 -0.3301 0.2730 0.008 Uiso 1 1 d R . . O8 O 0.2915(7) -0.3742(5) 0.2743(3) 0.0079(11) Uani 1 1 d . . . H8A H 0.2219 -0.4255 0.2882 0.009 Uiso 1 1 d R . . H8B H 0.2601 -0.3164 0.3079 0.009 Uiso 1 1 d R . . O9 O 0.7741(7) -0.3239(5) 0.0984(3) 0.0125(12) Uani 1 1 d . . . H9A H 0.8231 -0.2681 0.0724 0.015 Uiso 1 1 d R . . H9B H 0.8575 -0.3892 0.0984 0.015 Uiso 1 1 d R . . O10 O 0.2428(7) -0.3218(5) 0.1077(3) 0.0101(11) Uani 1 1 d . . . H10A H 0.2131 -0.3981 0.1140 0.012 Uiso 1 1 d R . . H10B H 0.1483 -0.2735 0.0952 0.012 Uiso 1 1 d R . . O11 O 0.2312(7) -0.1241(5) 0.2054(3) 0.0112(11) Uani 1 1 d . . . O12 O 0.2256(7) 0.0131(5) 0.2975(3) 0.0154(12) Uani 1 1 d U . . O13 O 0.0008(8) 0.1605(5) -0.0206(3) 0.0145(12) Uani 1 1 d . . . O14 O 0.2101(7) 0.4098(5) 0.2378(3) 0.0125(12) Uani 1 1 d U . . O15 O 0.0458(7) 0.5101(5) 0.1474(4) 0.0177(13) Uani 1 1 d . . . O16 O 0.1408(7) 0.1969(5) 0.1980(3) 0.0098(11) Uani 1 1 d . . . O17 O 0.2383(7) 0.2342(5) 0.3574(3) 0.0135(12) Uani 1 1 d . . . H17A H 0.2265 0.2094 0.3121 0.016 Uiso 1 1 d R . . H17B H 0.2856 0.2978 0.3488 0.016 Uiso 1 1 d R . . O18 O 0.0870(7) 0.2477(5) 0.6983(4) 0.0139(12) Uani 1 1 d . . . H18A H 0.0908 0.1896 0.7336 0.017 Uiso 1 1 d R . . H18B H 0.0732 0.2188 0.6546 0.017 Uiso 1 1 d R . . O19 O 0.1220(10) 0.4000(5) 0.5650(4) 0.0279(15) Uani 1 1 d . . . H19A H 0.0181 0.3984 0.5515 0.033 Uiso 1 1 d R . . H19B H 0.2059 0.3618 0.5298 0.033 Uiso 1 1 d R . . O20 O 0.4843(7) 0.6016(5) 0.5769(3) 0.0115(11) Uani 1 1 d U . . O21 O 0.6223(7) 0.4013(5) 0.5662(3) 0.0097(11) Uani 1 1 d . . . O22 O 0.3922(7) 0.8330(5) 0.3881(3) 0.0153(12) Uani 1 1 d U . . H22A H 0.4888 0.7950 0.3643 0.018 Uiso 1 1 d R . . H22B H 0.3676 0.8896 0.3650 0.018 Uiso 1 1 d R . . O23 O 0.0098(7) 0.8471(5) 0.4799(3) 0.0112(11) Uani 1 1 d U . . O25 O 0.5705(7) 0.8254(5) 0.5220(3) 0.0123(12) Uani 1 1 d . . . O26 O 0.2390(7) 0.8047(5) 0.6530(3) 0.0123(11) Uani 1 1 d . . . H26A H 0.2323 0.8691 0.6792 0.015 Uiso 1 1 d R . . H26B H 0.2598 0.7427 0.6847 0.015 Uiso 1 1 d R . . O27 O 0.0912(7) 0.6423(5) 0.5698(4) 0.0151(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O24 0.0092(13) 0.0100(14) 0.0101(14) 0.0001(9) -0.0020(9) -0.0010(9) Yb1 0.00665(18) 0.00256(18) 0.00758(19) 0.00059(13) -0.00315(13) 0.00189(13) Yb2 0.00762(18) 0.00133(18) 0.00579(19) 0.00047(12) -0.00326(13) -0.00009(13) C1 0.010(4) 0.010(4) 0.013(4) 0.001(3) -0.005(3) -0.002(3) C2 0.011(4) 0.008(4) 0.016(4) -0.003(3) -0.005(3) -0.004(3) C3 0.007(3) 0.010(4) 0.012(4) 0.001(3) -0.002(3) -0.002(3) C4 0.004(3) 0.005(3) 0.009(4) -0.004(3) 0.002(3) -0.002(3) C5 0.010(3) 0.004(4) 0.010(4) -0.003(3) -0.002(3) 0.002(3) C6 0.003(3) 0.012(4) 0.013(4) 0.000(3) 0.000(3) -0.001(3) C7 0.010(3) 0.009(4) 0.002(4) 0.000(3) -0.002(3) -0.002(3) C8 0.009(3) 0.006(4) 0.011(4) -0.002(3) -0.003(3) 0.003(3) C9 0.010(4) 0.010(4) 0.005(4) -0.001(3) 0.002(3) 0.001(3) C10 0.007(3) 0.006(4) 0.010(4) -0.001(3) -0.005(3) 0.000(3) C11 0.009(3) 0.006(4) 0.017(5) 0.001(3) -0.006(3) -0.003(3) C12 0.009(3) 0.007(4) 0.015(4) 0.006(3) -0.004(3) 0.000(3) C13 0.0074(17) 0.0067(17) 0.0075(17) -0.0001(10) -0.0015(10) -0.0015(10) C14 0.009(3) 0.007(4) 0.014(4) 0.000(3) 0.002(3) 0.000(3) C15 0.006(3) 0.005(4) 0.007(4) -0.002(3) 0.001(3) -0.001(3) C16 0.007(3) 0.005(4) 0.011(4) 0.000(3) -0.004(3) 0.001(3) O1 0.0140(14) 0.0120(14) 0.0127(14) 0.0000(9) -0.0038(9) -0.0020(10) O2 0.0123(14) 0.0103(14) 0.0115(14) -0.0003(9) -0.0033(9) -0.0027(9) O3 0.011(2) 0.002(2) 0.007(3) 0.000(2) -0.004(2) 0.001(2) O4 0.013(3) 0.004(3) 0.014(3) 0.000(2) -0.005(2) -0.003(2) O5 0.0097(13) 0.0077(14) 0.0092(14) -0.0008(9) -0.0017(9) -0.0017(9) O6 0.0085(13) 0.0071(13) 0.0073(14) 0.0002(9) -0.0022(9) -0.0016(9) O7 0.0072(13) 0.0056(13) 0.0069(13) -0.0005(9) -0.0016(9) -0.0016(9) O8 0.007(2) 0.008(3) 0.010(3) 0.001(2) -0.003(2) -0.003(2) O9 0.011(3) 0.008(3) 0.014(3) 0.006(2) 0.002(2) 0.001(2) O10 0.012(3) 0.007(3) 0.015(3) 0.005(2) -0.011(2) -0.005(2) O11 0.013(3) 0.002(3) 0.019(3) -0.001(2) -0.007(2) 0.001(2) O12 0.0166(14) 0.0143(15) 0.0149(15) 0.0000(9) -0.0029(10) -0.0019(10) O13 0.025(3) 0.010(3) 0.012(3) 0.004(2) -0.009(2) -0.006(2) O14 0.0133(14) 0.0114(14) 0.0134(15) -0.0002(9) -0.0028(9) -0.0034(10) O15 0.014(3) 0.004(3) 0.038(4) 0.003(2) -0.012(3) -0.003(2) O16 0.010(2) 0.002(3) 0.016(3) 0.002(2) -0.002(2) 0.001(2) O17 0.017(3) 0.014(3) 0.011(3) 0.001(2) -0.005(2) -0.005(2) O18 0.018(3) 0.005(3) 0.019(3) 0.001(2) -0.007(2) -0.003(2) O19 0.045(4) 0.012(3) 0.028(4) 0.001(3) -0.008(3) -0.006(3) O20 0.0123(14) 0.0109(14) 0.0108(14) -0.0011(9) -0.0026(9) -0.0008(9) O21 0.013(3) 0.005(3) 0.011(3) -0.001(2) -0.004(2) 0.002(2) O22 0.0155(14) 0.0143(14) 0.0150(15) 0.0010(9) -0.0017(10) -0.0014(10) O23 0.0110(14) 0.0109(14) 0.0112(14) 0.0002(9) -0.0029(9) -0.0005(9) O25 0.008(2) 0.009(3) 0.021(3) 0.005(2) -0.007(2) -0.002(2) O26 0.025(3) 0.005(3) 0.009(3) -0.001(2) -0.005(2) -0.004(2) O27 0.014(3) 0.011(3) 0.020(3) 0.002(2) 0.001(2) -0.006(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O24 C16 1.251(9) . ? O24 Yb1 2.394(5) 2_576 ? Yb1 O25 2.281(5) . ? Yb1 O26 2.287(5) . ? Yb1 O22 2.320(6) . ? Yb1 O23 2.325(5) . ? Yb1 O27 2.329(5) . ? Yb1 O21 2.339(5) 2_666 ? Yb1 O20 2.340(5) . ? Yb1 O24 2.394(5) 2_576 ? Yb1 C15 3.149(7) 2_666 ? Yb1 C16 3.169(7) 2_576 ? Yb2 O11 2.273(5) . ? Yb2 O5 2.285(5) 1_545 ? Yb2 O10 2.295(5) . ? Yb2 O2 2.306(5) . ? Yb2 O9 2.312(5) . ? Yb2 O7 2.325(5) . ? Yb2 O6 2.351(5) 2_655 ? Yb2 O8 2.411(5) . ? Yb2 H8B 2.7003 . ? C1 O1 1.239(10) . ? C1 O2 1.254(9) . ? C1 C2 1.508(10) . ? C2 C3 1.345(12) . ? C2 O3 1.364(9) . ? C3 C4 1.436(10) . ? C3 H3 0.9300 . ? C4 O6 1.246(9) . ? C4 C5 1.449(10) . ? C5 C6 1.344(11) . ? C5 H5 0.9300 . ? C6 O3 1.348(9) . ? C6 C7 1.521(11) . ? C7 O4 1.239(9) . ? C7 O5 1.255(9) . ? C8 O12 1.232(10) . ? C8 O11 1.253(9) . ? C8 C9 1.516(10) . ? C9 C10 1.341(11) . ? C9 O16 1.355(9) . ? C10 C11 1.430(10) . ? C10 H10 0.9300 . ? C11 O13 1.252(9) . ? C11 C12 1.454(11) . ? C12 C13 1.355(11) . ? C12 H12 0.9300 . ? C13 O16 1.331(9) . ? C13 C14 1.518(10) . ? C14 O14 1.233(10) . ? C14 O15 1.238(9) . ? C15 O20 1.243(9) . ? C15 O21 1.263(9) . ? C15 C15 1.554(15) 2_666 ? C15 Yb1 3.149(7) 2_666 ? C16 O23 1.245(9) . ? C16 C16 1.543(14) 2_576 ? C16 Yb1 3.168(7) 2_576 ? O5 Yb2 2.285(5) 1_565 ? O6 Yb2 2.352(5) 2_655 ? O7 H7A 0.8499 . ? O7 H7B 0.8500 . ? O8 H8A 0.8501 . ? O8 H8B 0.8500 . ? O9 H9A 0.8500 . ? O9 H9B 0.8500 . ? O10 H10A 0.9163 . ? O10 H10B 0.8402 . ? O17 H17A 0.8501 . ? O17 H17B 0.8500 . ? O18 H18A 0.8500 . ? O18 H18B 0.8502 . ? O19 H19A 0.8500 . ? O19 H19B 0.8500 . ? O21 Yb1 2.339(5) 2_666 ? O22 H22A 0.8114 . ? O22 H22B 0.7252 . ? O26 H26A 0.8501 . ? O26 H26B 0.8500 . ? 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 C16 O24 Yb1 117.3(4) . 2_576 ? O25 Yb1 O26 84.9(2) . . ? O25 Yb1 O22 74.7(2) . . ? O26 Yb1 O22 149.10(19) . . ? O25 Yb1 O23 139.85(18) . . ? O26 Yb1 O23 101.83(19) . . ? O22 Yb1 O23 80.61(19) . . ? O25 Yb1 O27 148.16(19) . . ? O26 Yb1 O27 76.0(2) . . ? O22 Yb1 O27 131.8(2) . . ? O23 Yb1 O27 70.11(19) . . ? O25 Yb1 O21 104.31(19) . 2_666 ? O26 Yb1 O21 138.40(18) . 2_666 ? O22 Yb1 O21 70.47(19) . 2_666 ? O23 Yb1 O21 96.47(19) . 2_666 ? O27 Yb1 O21 75.68(19) . 2_666 ? O25 Yb1 O20 73.60(18) . . ? O26 Yb1 O20 74.81(19) . . ? O22 Yb1 O20 119.58(19) . . ? O23 Yb1 O20 146.51(18) . . ? O27 Yb1 O20 76.87(19) . . ? O21 Yb1 O20 69.50(18) 2_666 . ? O25 Yb1 O24 75.34(18) . 2_576 ? O26 Yb1 O24 74.50(18) . 2_576 ? O22 Yb1 O24 77.94(19) . 2_576 ? O23 Yb1 O24 68.78(18) . 2_576 ? O27 Yb1 O24 122.08(18) . 2_576 ? O21 Yb1 O24 147.06(18) 2_666 2_576 ? O20 Yb1 O24 137.69(18) . 2_576 ? O25 Yb1 C15 96.59(19) . 2_666 ? O26 Yb1 C15 119.70(19) . 2_666 ? O22 Yb1 C15 86.10(19) . 2_666 ? O23 Yb1 C15 112.97(19) . 2_666 ? O27 Yb1 C15 72.10(19) . 2_666 ? O21 Yb1 C15 20.56(19) 2_666 2_666 ? O20 Yb1 C15 49.00(19) . 2_666 ? O24 Yb1 C15 163.50(18) 2_576 2_666 ? O25 Yb1 C16 95.32(19) . 2_576 ? O26 Yb1 C16 80.67(19) . 2_576 ? O22 Yb1 C16 78.4(2) . 2_576 ? O23 Yb1 C16 48.31(18) . 2_576 ? O27 Yb1 C16 106.26(19) . 2_576 ? O21 Yb1 C16 136.73(19) 2_666 2_576 ? O20 Yb1 C16 153.77(19) . 2_576 ? O24 Yb1 C16 20.55(17) 2_576 2_576 ? C15 Yb1 C16 157.20(19) 2_666 2_576 ? O11 Yb2 O5 142.59(17) . 1_545 ? O11 Yb2 O10 75.53(19) . . ? O5 Yb2 O10 73.97(18) 1_545 . ? O11 Yb2 O2 74.80(18) . . ? O5 Yb2 O2 141.83(18) 1_545 . ? O10 Yb2 O2 140.41(18) . . ? O11 Yb2 O9 143.29(18) . . ? O5 Yb2 O9 71.93(18) 1_545 . ? O10 Yb2 O9 118.1(2) . . ? O2 Yb2 O9 75.00(19) . . ? O11 Yb2 O7 112.32(19) . . ? O5 Yb2 O7 80.47(18) 1_545 . ? O10 Yb2 O7 141.55(17) . . ? O2 Yb2 O7 74.98(18) . . ? O9 Yb2 O7 79.02(18) . . ? O11 Yb2 O6 83.00(19) . 2_655 ? O5 Yb2 O6 106.66(18) 1_545 2_655 ? O10 Yb2 O6 71.05(17) . 2_655 ? O2 Yb2 O6 79.83(18) . 2_655 ? O9 Yb2 O6 71.54(18) . 2_655 ? O7 Yb2 O6 145.25(16) . 2_655 ? O11 Yb2 O8 76.99(18) . . ? O5 Yb2 O8 75.11(18) 1_545 . ? O10 Yb2 O8 76.11(17) . . ? O2 Yb2 O8 121.10(18) . . ? O9 Yb2 O8 137.60(17) . . ? O7 Yb2 O8 69.80(16) . . ? O6 Yb2 O8 144.87(16) 2_655 . ? O11 Yb2 H8B 64.0 . . ? O5 Yb2 H8B 92.4 1_545 . ? O10 Yb2 H8B 85.6 . . ? O2 Yb2 H8B 104.1 . . ? O9 Yb2 H8B 144.7 . . ? O7 Yb2 H8B 67.1 . . ? O6 Yb2 H8B 143.7 2_655 . ? O8 Yb2 H8B 18.0 . . ? O1 C1 O2 127.9(7) . . ? O1 C1 C2 117.6(7) . . ? O2 C1 C2 114.5(7) . . ? C3 C2 O3 121.7(7) . . ? C3 C2 C1 123.5(7) . . ? O3 C2 C1 114.7(7) . . ? C2 C3 C4 121.3(7) . . ? C2 C3 H3 119.4 . . ? C4 C3 H3 119.4 . . ? O6 C4 C3 121.2(7) . . ? O6 C4 C5 124.1(7) . . ? C3 C4 C5 114.7(7) . . ? C6 C5 C4 119.8(7) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? C5 C6 O3 123.4(7) . . ? C5 C6 C7 124.0(7) . . ? O3 C6 C7 112.6(7) . . ? O4 C7 O5 127.6(7) . . ? O4 C7 C6 118.7(7) . . ? O5 C7 C6 113.7(6) . . ? O12 C8 O11 127.2(7) . . ? O12 C8 C9 118.3(7) . . ? O11 C8 C9 114.5(7) . . ? C10 C9 O16 122.6(7) . . ? C10 C9 C8 126.2(7) . . ? O16 C9 C8 111.1(6) . . ? C9 C10 C11 121.0(7) . . ? C9 C10 H10 119.5 . . ? C11 C10 H10 119.5 . . ? O13 C11 C10 123.5(7) . . ? O13 C11 C12 122.2(7) . . ? C10 C11 C12 114.3(7) . . ? C13 C12 C11 120.1(7) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? O16 C13 C12 122.8(7) . . ? O16 C13 C14 114.6(6) . . ? C12 C13 C14 122.3(7) . . ? O14 C14 O15 127.4(7) . . ? O14 C14 C13 118.1(7) . . ? O15 C14 C13 114.3(7) . . ? O20 C15 O21 127.3(7) . . ? O20 C15 C15 117.1(8) . 2_666 ? O21 C15 C15 115.6(8) . 2_666 ? O20 C15 Yb1 167.5(5) . 2_666 ? O21 C15 Yb1 40.6(3) . 2_666 ? C15 C15 Yb1 75.1(5) 2_666 2_666 ? O23 C16 O24 126.5(7) . . ? O23 C16 C16 116.5(8) . 2_576 ? O24 C16 C16 116.9(8) . 2_576 ? O23 C16 Yb1 168.5(5) . 2_576 ? O24 C16 Yb1 42.2(3) . 2_576 ? C16 C16 Yb1 74.9(5) 2_576 2_576 ? C1 O2 Yb2 172.0(5) . . ? C6 O3 C2 118.9(6) . . ? C7 O5 Yb2 137.7(5) . 1_565 ? C4 O6 Yb2 143.4(4) . 2_655 ? Yb2 O7 H7A 120.4 . . ? Yb2 O7 H7B 121.1 . . ? H7A O7 H7B 107.7 . . ? Yb2 O8 H8A 148.1 . . ? Yb2 O8 H8B 100.6 . . ? H8A O8 H8B 107.7 . . ? Yb2 O9 H9A 121.8 . . ? Yb2 O9 H9B 130.0 . . ? H9A O9 H9B 107.7 . . ? Yb2 O10 H10A 120.3 . . ? Yb2 O10 H10B 129.4 . . ? H10A O10 H10B 105.6 . . ? C8 O11 Yb2 137.9(5) . . ? C13 O16 C9 119.1(6) . . ? H17A O17 H17B 107.7 . . ? H18A O18 H18B 107.7 . . ? H19A O19 H19B 107.7 . . ? C15 O20 Yb1 118.7(5) . . ? C15 O21 Yb1 118.9(5) . 2_666 ? Yb1 O22 H22A 117.7 . . ? Yb1 O22 H22B 134.2 . . ? H22A O22 H22B 106.4 . . ? C16 O23 Yb1 120.2(5) . . ? Yb1 O26 H26A 132.0 . . ? Yb1 O26 H26B 117.2 . . ? H26A O26 H26B 107.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 163.5(7) . . . . ? O2 C1 C2 C3 -15.0(11) . . . . ? O1 C1 C2 O3 -15.9(10) . . . . ? O2 C1 C2 O3 165.6(6) . . . . ? O3 C2 C3 C4 1.9(11) . . . . ? C1 C2 C3 C4 -177.4(7) . . . . ? C2 C3 C4 O6 174.7(7) . . . . ? C2 C3 C4 C5 -5.4(10) . . . . ? O6 C4 C5 C6 -174.6(7) . . . . ? C3 C4 C5 C6 5.5(10) . . . . ? C4 C5 C6 O3 -2.3(11) . . . . ? C4 C5 C6 C7 176.8(6) . . . . ? C5 C6 C7 O4 -168.6(7) . . . . ? O3 C6 C7 O4 10.6(10) . . . . ? C5 C6 C7 O5 9.5(10) . . . . ? O3 C6 C7 O5 -171.3(6) . . . . ? O12 C8 C9 C10 -172.0(7) . . . . ? O11 C8 C9 C10 8.7(11) . . . . ? O12 C8 C9 O16 10.2(9) . . . . ? O11 C8 C9 O16 -169.1(6) . . . . ? O16 C9 C10 C11 1.8(11) . . . . ? C8 C9 C10 C11 -175.8(7) . . . . ? C9 C10 C11 O13 174.6(7) . . . . ? C9 C10 C11 C12 -3.9(10) . . . . ? O13 C11 C12 C13 -174.9(7) . . . . ? C10 C11 C12 C13 3.7(10) . . . . ? C11 C12 C13 O16 -1.3(11) . . . . ? C11 C12 C13 C14 172.1(6) . . . . ? O16 C13 C14 O14 13.5(10) . . . . ? C12 C13 C14 O14 -160.5(7) . . . . ? O16 C13 C14 O15 -171.1(6) . . . . ? C12 C13 C14 O15 15.0(11) . . . . ? Yb1 O24 C16 O23 -176.8(6) 2_576 . . . ? Yb1 O24 C16 C16 4.8(10) 2_576 . . 2_576 ? O1 C1 O2 Yb2 90(4) . . . . ? C2 C1 O2 Yb2 -92(4) . . . . ? O11 Yb2 O2 C1 23(4) . . . . ? O5 Yb2 O2 C1 -147(4) 1_545 . . . ? O10 Yb2 O2 C1 66(4) . . . . ? O9 Yb2 O2 C1 -178(4) . . . . ? O7 Yb2 O2 C1 -95(4) . . . . ? O6 Yb2 O2 C1 109(4) 2_655 . . . ? O8 Yb2 O2 C1 -41(4) . . . . ? C5 C6 O3 C2 -1.5(11) . . . . ? C7 C6 O3 C2 179.3(6) . . . . ? C3 C2 O3 C6 1.7(11) . . . . ? C1 C2 O3 C6 -178.9(6) . . . . ? O4 C7 O5 Yb2 -16.6(12) . . . 1_565 ? C6 C7 O5 Yb2 165.5(5) . . . 1_565 ? C3 C4 O6 Yb2 -164.1(5) . . . 2_655 ? C5 C4 O6 Yb2 16.0(12) . . . 2_655 ? O12 C8 O11 Yb2 -68.9(11) . . . . ? C9 C8 O11 Yb2 110.4(7) . . . . ? O5 Yb2 O11 C8 164.3(7) 1_545 . . . ? O10 Yb2 O11 C8 -159.5(8) . . . . ? O2 Yb2 O11 C8 -6.1(7) . . . . ? O9 Yb2 O11 C8 -41.7(9) . . . . ? O7 Yb2 O11 C8 60.2(8) . . . . ? O6 Yb2 O11 C8 -87.4(8) 2_655 . . . ? O8 Yb2 O11 C8 121.7(8) . . . . ? C12 C13 O16 C9 -1.1(10) . . . . ? C14 C13 O16 C9 -175.0(6) . . . . ? C10 C9 O16 C13 0.9(10) . . . . ? C8 C9 O16 C13 178.8(6) . . . . ? O21 C15 O20 Yb1 -176.5(5) . . . . ? C15 C15 O20 Yb1 4.4(10) 2_666 . . . ? Yb1 C15 O20 Yb1 171(2) 2_666 . . . ? O25 Yb1 O20 C15 -117.0(5) . . . . ? O26 Yb1 O20 C15 153.8(5) . . . . ? O22 Yb1 O20 C15 -55.9(5) . . . . ? O23 Yb1 O20 C15 65.3(6) . . . . ? O27 Yb1 O20 C15 75.0(5) . . . . ? O21 Yb1 O20 C15 -4.4(5) 2_666 . . . ? O24 Yb1 O20 C15 -161.4(4) 2_576 . . . ? C15 Yb1 O20 C15 -2.6(6) 2_666 . . . ? C16 Yb1 O20 C15 175.2(4) 2_576 . . . ? O20 C15 O21 Yb1 -175.9(6) . . . 2_666 ? C15 C15 O21 Yb1 3.3(9) 2_666 . . 2_666 ? O24 C16 O23 Yb1 -175.5(6) . . . . ? C16 C16 O23 Yb1 2.9(11) 2_576 . . . ? Yb1 C16 O23 Yb1 174(2) 2_576 . . . ? O25 Yb1 O23 C16 -32.0(7) . . . . ? O26 Yb1 O23 C16 64.2(6) . . . . ? O22 Yb1 O23 C16 -84.5(5) . . . . ? O27 Yb1 O23 C16 134.4(6) . . . . ? O21 Yb1 O23 C16 -153.4(5) 2_666 . . . ? O20 Yb1 O23 C16 144.5(5) . . . . ? O24 Yb1 O23 C16 -3.9(5) 2_576 . . . ? C15 Yb1 O23 C16 -166.1(5) 2_666 . . . ? C16 Yb1 O23 C16 -1.7(6) 2_576 . . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 25.15 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 1.683 _refine_diff_density_min -2.279 _refine_diff_density_rms 0.242 # Attachment 'Ba-10.cif' data_Ba-10 _database_code_depnum_ccdc_archive 'CCDC 754686' #TrackingRef 'Ba-10.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C7 H4 Ba O7' _chemical_formula_weight 337.43 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' Ba Ba -0.3244 2.2819 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 19.441(2) _cell_length_b 10.0363(12) _cell_length_c 4.3190(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 842.70(16) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 778 _cell_measurement_theta_min 4.06 _cell_measurement_theta_max 24.96 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.660 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 632 _exptl_absorpt_coefficient_mu 4.728 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6492 _exptl_absorpt_correction_T_max 0.7979 _exptl_absorpt_process_details Crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(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 ? _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6384 _diffrn_reflns_av_R_equivalents 0.0326 _diffrn_reflns_av_sigmaI/netI 0.0168 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_theta_min 4.06 _diffrn_reflns_theta_max 24.96 _reflns_number_total 778 _reflns_number_gt 738 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0199P)^2^+0.5917P] 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 778 _refine_ls_number_parameters 74 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0206 _refine_ls_R_factor_gt 0.0184 _refine_ls_wR_factor_ref 0.0412 _refine_ls_wR_factor_gt 0.0406 _refine_ls_goodness_of_fit_ref 1.179 _refine_ls_restrained_S_all 1.179 _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 Ba1 Ba 0.162525(13) 0.2500 0.55238(6) 0.01831(11) Uani 1 2 d S . . O1 O 0.18051(12) 0.5268(2) 0.3600(6) 0.0326(6) Uani 1 1 d . . . C3 C 0.05177(16) 0.6304(3) -0.1889(7) 0.0218(7) Uani 1 1 d . . . H3 H 0.0350 0.5483 -0.2541 0.026 Uiso 1 1 calc R . . C4 C 0.0217(2) 0.7500 -0.3080(10) 0.0230(10) Uani 1 2 d S . . C2 C 0.10356(16) 0.6345(3) 0.0143(7) 0.0189(7) Uani 1 1 d . . . O5 O 0.12965(16) 0.7500 0.1255(7) 0.0200(7) Uani 1 2 d S . . O2 O 0.12036(12) 0.4042(2) 0.0334(5) 0.0253(5) Uani 1 1 d . . . C1 C 0.13844(17) 0.5127(3) 0.1464(7) 0.0213(7) Uani 1 1 d . . . O4 O 0.25810(12) 0.2500 0.0791(5) 0.0285(8) Uani 1 2 d S . . H4A H 0.2753 0.3279 0.0744 0.034 Uiso 0.50 1 d PR . . H4B H 0.2913 0.1947 0.0723 0.034 Uiso 0.50 1 d PR . . O3 O -0.02492(12) 0.7500 -0.5035(5) 0.0312(8) Uani 1 2 d SR . . 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 Ba1 0.02484(17) 0.01582(16) 0.01425(16) 0.000 -0.00019(11) 0.000 O1 0.0442(15) 0.0210(13) 0.0327(14) -0.0001(11) -0.0152(12) 0.0038(10) C3 0.0248(17) 0.0201(17) 0.0206(16) -0.0024(14) -0.0005(14) -0.0032(13) C4 0.019(2) 0.032(3) 0.017(2) 0.000 0.0028(19) 0.000 C2 0.0247(16) 0.0127(15) 0.0192(16) -0.0018(12) 0.0042(13) -0.0029(13) O5 0.0270(17) 0.0127(16) 0.0202(16) 0.000 -0.0042(14) 0.000 O2 0.0371(13) 0.0129(12) 0.0259(12) -0.0027(9) -0.0010(10) -0.0004(10) C1 0.0267(17) 0.0186(17) 0.0187(16) 0.0004(13) 0.0064(14) 0.0024(13) O4 0.0215(17) 0.0251(18) 0.039(2) 0.000 0.0066(15) 0.000 O3 0.0223(18) 0.042(2) 0.0294(19) 0.000 -0.0047(15) 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 Ba1 O3 2.683(2) 5_565 ? Ba1 O2 2.717(2) 1_556 ? Ba1 O2 2.717(2) 8_566 ? Ba1 O4 2.762(2) . ? Ba1 O2 2.844(2) 8_565 ? Ba1 O2 2.844(2) . ? Ba1 O1 2.920(2) 8_565 ? Ba1 O1 2.920(2) . ? Ba1 O4 2.937(2) 1_556 ? Ba1 C1 3.201(3) 8_565 ? O1 C1 1.241(4) . ? C3 C2 1.336(4) . ? C3 C4 1.431(4) . ? C3 H3 0.9300 . ? C4 O3 1.238(5) . ? C4 C3 1.431(4) 8_575 ? C2 O5 1.353(3) . ? C2 C1 1.510(4) . ? O5 C2 1.353(3) 8_575 ? O2 C1 1.244(4) . ? O2 Ba1 2.717(2) 1_554 ? O4 Ba1 2.937(2) 1_554 ? O4 H4A 0.8510 . ? O4 H4B 0.8520 . ? O3 Ba1 2.683(2) 5_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Ba1 O2 76.08(6) 5_565 1_556 ? O3 Ba1 O2 76.08(6) 5_565 8_566 ? O2 Ba1 O2 69.43(9) 1_556 8_566 ? O3 Ba1 O4 127.76(4) 5_565 . ? O2 Ba1 O4 140.24(5) 1_556 . ? O2 Ba1 O4 140.24(5) 8_566 . ? O3 Ba1 O2 69.56(6) 5_565 8_565 ? O2 Ba1 O2 145.63(9) 1_556 8_565 ? O2 Ba1 O2 101.87(7) 8_566 8_565 ? O4 Ba1 O2 67.09(6) . 8_565 ? O3 Ba1 O2 69.56(6) 5_565 . ? O2 Ba1 O2 101.87(7) 1_556 . ? O2 Ba1 O2 145.63(9) 8_566 . ? O4 Ba1 O2 67.09(6) . . ? O2 Ba1 O2 65.92(9) 8_565 . ? O3 Ba1 O1 95.56(5) 5_565 8_565 ? O2 Ba1 O1 142.69(7) 1_556 8_565 ? O2 Ba1 O1 73.26(7) 8_566 8_565 ? O4 Ba1 O1 73.08(5) . 8_565 ? O2 Ba1 O1 44.99(6) 8_565 8_565 ? O2 Ba1 O1 109.13(6) . 8_565 ? O3 Ba1 O1 95.56(5) 5_565 . ? O2 Ba1 O1 73.26(7) 1_556 . ? O2 Ba1 O1 142.69(7) 8_566 . ? O4 Ba1 O1 73.08(5) . . ? O2 Ba1 O1 109.13(6) 8_565 . ? O2 Ba1 O1 44.99(6) . . ? O1 Ba1 O1 144.04(10) 8_565 . ? O3 Ba1 O4 133.75(4) 5_565 1_556 ? O2 Ba1 O4 66.34(6) 1_556 1_556 ? O2 Ba1 O4 66.34(6) 8_566 1_556 ? O4 Ba1 O4 98.49(7) . 1_556 ? O2 Ba1 O4 142.43(5) 8_565 1_556 ? O2 Ba1 O4 142.43(5) . 1_556 ? O1 Ba1 O4 98.32(5) 8_565 1_556 ? O1 Ba1 O4 98.32(5) . 1_556 ? O3 Ba1 C1 79.11(6) 5_565 8_565 ? O2 Ba1 C1 147.55(7) 1_556 8_565 ? O2 Ba1 C1 84.58(7) 8_566 8_565 ? O4 Ba1 C1 72.12(6) . 8_565 ? O2 Ba1 C1 22.79(7) 8_565 8_565 ? O2 Ba1 C1 88.53(7) . 8_565 ? O1 Ba1 C1 22.80(7) 8_565 8_565 ? O1 Ba1 C1 130.18(8) . 8_565 ? O4 Ba1 C1 121.12(6) 1_556 8_565 ? O3 Ba1 Ba1 85.49(5) 5_565 1_554 ? O2 Ba1 Ba1 139.87(5) 1_556 1_554 ? O2 Ba1 Ba1 139.87(5) 8_566 1_554 ? O4 Ba1 Ba1 42.27(5) . 1_554 ? O2 Ba1 Ba1 38.00(4) 8_565 1_554 ? O2 Ba1 Ba1 38.00(4) . 1_554 ? O1 Ba1 Ba1 73.47(5) 8_565 1_554 ? O1 Ba1 Ba1 73.47(5) . 1_554 ? O4 Ba1 Ba1 140.76(4) 1_556 1_554 ? C1 Ba1 Ba1 56.79(6) 8_565 1_554 ? C1 O1 Ba1 91.39(19) . . ? C2 C3 C4 121.2(3) . . ? C2 C3 H3 119.4 . . ? C4 C3 H3 119.4 . . ? O3 C4 C3 122.97(19) . . ? O3 C4 C3 122.97(19) . 8_575 ? C3 C4 C3 114.0(4) . 8_575 ? C3 C2 O5 122.8(3) . . ? C3 C2 C1 124.2(3) . . ? O5 C2 C1 113.0(3) . . ? C2 O5 C2 117.9(3) . 8_575 ? C1 O2 Ba1 135.5(2) . 1_554 ? C1 O2 Ba1 94.90(19) . . ? Ba1 O2 Ba1 101.87(7) 1_554 . ? O1 C1 O2 125.3(3) . . ? O1 C1 C2 119.0(3) . . ? O2 C1 C2 115.7(3) . . ? Ba1 O4 Ba1 98.49(7) . 1_554 ? Ba1 O4 H4A 106.4 . . ? Ba1 O4 H4A 103.3 1_554 . ? Ba1 O4 H4B 122.3 . . ? Ba1 O4 H4B 116.9 1_554 . ? H4A O4 H4B 107.4 . . ? C4 O3 Ba1 141.5(2) . 5_565 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 24.96 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.272 _refine_diff_density_min -0.440 _refine_diff_density_rms 0.086