Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Zheming Wang' _publ_contact_author_address ; College of Chemistry & Molecular Engineering Peking University Beijing 100871 CHINA ; _publ_contact_author_email ZMW@PKU.EDU.CN _publ_section_title ; A 3D Porous Lanthanide-Fumarate Framework with Water Hexamer Occupied Cavities, Exhibiting Reversible Dehydration and Rehydration Procedure ; loop_ _publ_author_name 'Zheming Wang' 'Song Gao' 'Wen-Hua Zhu' data_CCDC287283 _database_code_depnum_ccdc_archive 'CCDC 287283' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H20 O19 Sm2' _chemical_formula_weight 768.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 2(1)/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.5178(2) _cell_length_b 14.6999(3) _cell_length_c 14.8740(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.2425(9) _cell_angle_gamma 90.00 _cell_volume 2080.54(7) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 21328 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.455 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1472 _exptl_absorpt_coefficient_mu 5.685 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.414 _exptl_absorpt_correction_T_max 0.517 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995, 1997) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(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 'NONIUS KappaCCD Diffractometer' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 0.76 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% None _diffrn_reflns_number 36935 _diffrn_reflns_av_R_equivalents 0.0994 _diffrn_reflns_av_sigmaI/netI 0.0646 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.50 _diffrn_reflns_theta_max 27.49 _reflns_number_total 4765 _reflns_number_gt 3420 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KappaCCD (Nonius B. V., 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL Denzo (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL V5.1 (Sheldrick, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _publ_section_references ; collect: "Collect" data collection software, Nonius B.V., Delft, The Netherlands, 1998. HKL Scalepack & HKL Denzo: Z. Otwinowski and W. Minor, " Processing of X-ray Diffraction Data Collected in Oscillation Mode ", Methods in Enzymology, Volume 276: Macromolecular Crystallography, part A, p.307-326, 1997,C.W. Carter, Jr. & R.M. Sweet, Eds., Academic Press, London. absorption correction: R.H. Blessing (1995) Acta Cryst. A51, 33-37. R.H. Blessing (1997) J.Appl. Cryst. 30, 421-426. maXus: S.Mackay, C.J.Gilmore, C.Edwards, M. Tremayne, N. Stuart, K.Shankland maXus: a computer program for the solution and refinement of crystal structures from diffraction data", University of Glasgow, Scotland, UK, Nonius BV, Delft, The Netherlands and MacScience Co. Ltd., Yokohama, Japan (1998). Sheldrick, G. M. (1998). SHELXTL Version 5.1. Bruker Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. Sheldrick, G. M. (1997). SHELX-97. PC Version. University of Goettingen, Germany. ; _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. Treatment on H: H atoms of fumarate ligand were added geometrically and refined by riding model. H atoms of water O13, O14, O15, O16 and O17 were added from difference Fourier map, and refinded by DFIX instructions in which O-H distances were set 0.96(3) and H-H distances 1.52(3) Angstroms according to the ideal molecular geometry of water, and with one common isotropic thermal parameter. H atoms of water O18 and O19 could not be located from difference Fourier map thus not involved in the structure refinement. ; _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^)+(0.0222P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'difmap and geom' _refine_ls_hydrogen_treatment constrained _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00156(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4765 _refine_ls_number_parameters 330 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0547 _refine_ls_R_factor_gt 0.0284 _refine_ls_wR_factor_ref 0.0568 _refine_ls_wR_factor_gt 0.0526 _refine_ls_goodness_of_fit_ref 0.934 _refine_ls_restrained_S_all 0.934 _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 Sm1 Sm -0.18894(2) 0.346122(16) 0.905591(14) 0.01192(8) Uani 1 1 d . . . Sm2 Sm 0.02774(2) 0.163770(16) 0.745159(14) 0.01208(8) Uani 1 1 d . . . C1 C 0.1149(4) 0.3548(3) 0.8731(3) 0.0131(10) Uani 1 1 d . . . C2 C 0.2694(4) 0.3539(3) 0.8658(3) 0.0176(10) Uani 1 1 d . . . H2 H 0.3082 0.3724 0.8104 0.021 Uiso 1 1 calc R . . C3 C 0.3570(4) 0.3290(3) 0.9310(3) 0.0191(11) Uani 1 1 d . . . H3 H 0.3208 0.3113 0.9874 0.023 Uiso 1 1 calc R . . C4 C 0.5116(4) 0.3281(3) 0.9180(3) 0.0144(10) Uani 1 1 d . . . C5 C -0.2799(4) 0.1844(3) 0.7338(3) 0.0143(10) Uani 1 1 d . . . C6 C -0.4354(5) 0.1849(3) 0.7283(3) 0.0192(11) Uani 1 1 d . . . H6 H -0.4874 0.1983 0.7805 0.023 Uiso 1 1 calc R . . C7 C -0.5025(4) 0.1670(3) 0.6522(3) 0.0166(10) Uani 1 1 d . . . H7 H -0.4479 0.1583 0.6002 0.020 Uiso 1 1 calc R . . C8 C -0.6587(4) 0.1594(3) 0.6416(3) 0.0142(10) Uani 1 1 d . . . C9 C 0.0132(4) 0.1628(3) 0.9729(3) 0.0154(10) Uani 1 1 d . . . C10 C 0.0397(5) 0.1017(3) 1.0509(3) 0.0172(10) Uani 1 1 d . . . H10 H 0.1266 0.0700 1.0547 0.021 Uiso 1 1 calc R . . C11 C -0.0518(5) 0.0893(3) 1.1151(3) 0.0217(11) Uani 1 1 d . . . H11 H -0.1290 0.1300 1.1188 0.026 Uiso 1 1 calc R . . C12 C -0.0393(5) 0.0153(3) 1.1813(3) 0.0190(10) Uani 1 1 d . . . O1 O 0.0394(3) 0.3169(2) 0.81365(19) 0.0146(7) Uani 1 1 d . . . O2 O 0.0594(3) 0.3950(2) 0.9388(2) 0.0198(7) Uani 1 1 d . . . O3 O 0.5864(3) 0.2692(2) 0.9578(2) 0.0176(7) Uani 1 1 d . . . O4 O 0.5655(3) 0.3871(2) 0.8672(2) 0.0191(7) Uani 1 1 d . . . O5 O -0.2162(3) 0.2212(2) 0.8011(2) 0.0184(7) Uani 1 1 d . . . O6 O -0.2107(3) 0.1471(2) 0.6735(2) 0.0167(7) Uani 1 1 d . . . O7 O -0.7045(3) 0.1272(2) 0.5677(2) 0.0170(7) Uani 1 1 d . . . O8 O -0.7334(3) 0.1803(2) 0.7062(2) 0.0184(7) Uani 1 1 d . . . O9 O -0.0892(3) 0.2179(2) 0.9768(2) 0.0229(8) Uani 1 1 d . . . O10 O 0.0919(3) 0.1545(2) 0.9065(2) 0.0190(7) Uani 1 1 d . . . O11 O -0.1487(3) -0.0137(2) 1.2180(2) 0.0201(7) Uani 1 1 d . . . O12 O 0.0796(3) -0.0237(2) 1.1954(2) 0.0204(7) Uani 1 1 d . . . O13 O -0.1895(3) 0.4268(2) 0.7615(2) 0.0248(8) Uani 1 1 d D . . O14 O -0.2146(3) 0.5052(2) 0.9399(2) 0.0219(8) Uani 1 1 d D . . O15 O 0.0175(3) 0.2799(2) 0.6289(2) 0.0234(8) Uani 1 1 d D . . O16 O 0.0335(3) 0.0722(2) 0.6061(2) 0.0178(7) Uani 1 1 d D . . O17 O 0.0670(4) 0.4631(3) 0.6683(3) 0.0379(10) Uani 1 1 d D . . O18 O -0.1475(7) 0.5671(5) 0.5678(4) 0.117(2) Uani 1 1 d . . . O19 O 0.1261(7) 0.5951(5) 0.5452(5) 0.137(3) Uani 1 1 d . . . H131 H -0.250(4) 0.470(3) 0.736(4) 0.065(7) Uiso 1 1 d D . . H132 H -0.102(3) 0.436(4) 0.734(4) 0.065(7) Uiso 1 1 d D . . H141 H -0.158(5) 0.537(3) 0.981(3) 0.065(7) Uiso 1 1 d D . . H142 H -0.242(5) 0.550(3) 0.897(3) 0.065(7) Uiso 1 1 d D . . H151 H 0.035(6) 0.269(4) 0.566(2) 0.065(7) Uiso 1 1 d D . . H152 H 0.032(6) 0.3451(19) 0.633(4) 0.065(7) Uiso 1 1 d D . . H161 H 0.123(4) 0.080(4) 0.583(4) 0.065(7) Uiso 1 1 d D . . H162 H 0.008(5) 0.013(2) 0.608(4) 0.065(7) Uiso 1 1 d D . . H171 H 0.157(4) 0.482(4) 0.690(3) 0.065(7) Uiso 1 1 d D . . H172 H 0.041(5) 0.499(4) 0.622(3) 0.065(7) Uiso 1 1 d 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 Sm1 0.00939(12) 0.01530(14) 0.01103(13) -0.00065(10) -0.00075(9) 0.00049(9) Sm2 0.01030(12) 0.01499(14) 0.01094(13) -0.00063(10) 0.00009(9) -0.00008(9) C1 0.017(2) 0.010(2) 0.012(2) 0.0007(19) -0.0028(19) -0.0019(18) C2 0.015(2) 0.021(3) 0.017(2) -0.002(2) 0.0027(19) -0.0038(19) C3 0.013(2) 0.028(3) 0.016(2) 0.001(2) 0.002(2) 0.000(2) C4 0.016(2) 0.017(3) 0.011(2) -0.004(2) -0.0015(19) 0.0010(19) C5 0.016(2) 0.011(2) 0.016(2) 0.0003(19) 0.0006(19) -0.0015(18) C6 0.015(2) 0.030(3) 0.013(2) -0.004(2) 0.002(2) -0.001(2) C7 0.010(2) 0.020(3) 0.019(3) 0.000(2) 0.0028(19) 0.0010(19) C8 0.014(2) 0.016(3) 0.013(2) 0.004(2) -0.0005(18) 0.0029(19) C9 0.019(2) 0.012(2) 0.014(2) -0.002(2) -0.0062(19) -0.002(2) C10 0.019(2) 0.013(3) 0.019(3) -0.001(2) -0.003(2) 0.0011(19) C11 0.021(2) 0.021(3) 0.023(3) -0.001(2) -0.001(2) 0.004(2) C12 0.029(3) 0.016(3) 0.012(2) -0.003(2) -0.005(2) -0.002(2) O1 0.0165(16) 0.0157(18) 0.0116(16) -0.0032(13) -0.0013(13) -0.0002(13) O2 0.0139(16) 0.029(2) 0.0168(18) -0.0091(15) 0.0030(14) -0.0022(14) O3 0.0140(15) 0.024(2) 0.0151(17) 0.0039(14) -0.0025(13) 0.0038(14) O4 0.0110(15) 0.025(2) 0.0217(18) 0.0066(15) -0.0012(13) -0.0007(13) O5 0.0134(16) 0.0216(19) 0.0202(18) -0.0053(15) -0.0021(14) 0.0018(13) O6 0.0117(15) 0.0231(19) 0.0151(16) -0.0026(14) 0.0000(13) 0.0023(13) O7 0.0134(15) 0.027(2) 0.0107(17) -0.0025(14) -0.0019(13) -0.0049(13) O8 0.0119(15) 0.027(2) 0.0160(17) -0.0042(14) 0.0011(13) -0.0016(13) O9 0.0205(17) 0.027(2) 0.0207(18) 0.0064(15) 0.0007(14) 0.0045(15) O10 0.0256(17) 0.0200(19) 0.0115(16) -0.0006(14) -0.0001(14) 0.0019(14) O11 0.0195(16) 0.0234(19) 0.0175(17) 0.0004(14) 0.0034(13) 0.0018(14) O12 0.0182(16) 0.0193(19) 0.0233(18) 0.0054(15) -0.0049(14) -0.0007(14) O13 0.0188(17) 0.034(2) 0.0214(19) 0.0073(16) 0.0040(15) 0.0079(15) O14 0.0277(18) 0.016(2) 0.0220(19) -0.0036(14) -0.0110(15) 0.0000(14) O15 0.0335(19) 0.023(2) 0.0138(18) -0.0005(15) -0.0004(15) -0.0019(16) O16 0.0139(15) 0.0189(19) 0.0208(18) -0.0033(15) 0.0031(14) -0.0015(14) O17 0.034(2) 0.032(2) 0.047(3) 0.0062(19) -0.0062(19) -0.0059(18) O18 0.139(6) 0.092(5) 0.118(5) -0.001(4) -0.011(4) 0.019(4) O19 0.125(6) 0.141(7) 0.146(7) 0.018(5) 0.012(5) -0.011(5) _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 Sm1 O9 2.352(3) . ? Sm1 O14 2.407(3) . ? Sm1 O5 2.416(3) . ? Sm1 O13 2.450(3) . ? Sm1 O7 2.450(3) 4_666 ? Sm1 O4 2.468(3) 1_455 ? Sm1 O2 2.509(3) . ? Sm1 O3 2.554(3) 1_455 ? Sm1 O1 2.628(3) . ? Sm1 C4 2.872(4) 1_455 ? Sm1 C1 2.945(4) . ? Sm2 O8 2.370(3) 1_655 ? Sm2 O15 2.430(3) . ? Sm2 O10 2.467(3) . ? Sm2 O16 2.470(3) . ? Sm2 O12 2.470(3) 3_557 ? Sm2 O1 2.472(3) . ? Sm2 O6 2.499(3) . ? Sm2 O11 2.543(3) 3_557 ? Sm2 O5 2.623(3) . ? Sm2 C12 2.851(5) 3_557 ? Sm2 C5 2.945(4) . ? C1 O1 1.258(5) . ? C1 O2 1.266(5) . ? C1 C2 1.477(6) . ? C2 C3 1.317(6) . ? C2 H2 0.9500 . ? C3 C4 1.489(6) . ? C3 H3 0.9500 . ? C4 O3 1.260(5) . ? C4 O4 1.266(5) . ? C4 Sm1 2.872(4) 1_655 ? C5 O6 1.252(5) . ? C5 O5 1.279(5) . ? C5 C6 1.481(6) . ? C6 C7 1.314(6) . ? C6 H6 0.9500 . ? C7 C8 1.496(6) . ? C7 H7 0.9500 . ? C8 O8 1.247(5) . ? C8 O7 1.265(5) . ? C9 O10 1.258(5) . ? C9 O9 1.270(5) . ? C9 C10 1.485(6) . ? C10 C11 1.319(6) . ? C10 H10 0.9500 . ? C11 C12 1.470(6) . ? C11 H11 0.9500 . ? C12 O11 1.261(5) . ? C12 O12 1.281(5) . ? C12 Sm2 2.851(5) 3_557 ? O3 Sm1 2.554(3) 1_655 ? O4 Sm1 2.468(3) 1_655 ? O7 Sm1 2.450(3) 4_565 ? O8 Sm2 2.370(3) 1_455 ? O11 Sm2 2.543(3) 3_557 ? O12 Sm2 2.470(3) 3_557 ? O13 H131 0.93(3) . ? O13 H132 0.95(3) . ? O14 H141 0.93(3) . ? O14 H142 0.95(3) . ? O15 H151 0.96(3) . ? O15 H152 0.97(3) . ? O16 H161 0.93(3) . ? O16 H162 0.90(3) . ? O17 H171 0.94(3) . ? O17 H172 0.90(3) . ? 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 Sm1 O14 136.45(11) . . ? O9 Sm1 O5 73.58(11) . . ? O14 Sm1 O5 149.87(11) . . ? O9 Sm1 O13 140.85(10) . . ? O14 Sm1 O13 73.53(11) . . ? O5 Sm1 O13 78.89(11) . . ? O9 Sm1 O7 73.59(10) . 4_666 ? O14 Sm1 O7 68.11(11) . 4_666 ? O5 Sm1 O7 138.30(11) . 4_666 ? O13 Sm1 O7 141.65(11) . 4_666 ? O9 Sm1 O4 132.11(10) . 1_455 ? O14 Sm1 O4 73.27(11) . 1_455 ? O5 Sm1 O4 87.07(10) . 1_455 ? O13 Sm1 O4 72.26(10) . 1_455 ? O7 Sm1 O4 96.39(9) 4_666 1_455 ? O9 Sm1 O2 76.78(11) . . ? O14 Sm1 O2 77.28(11) . . ? O5 Sm1 O2 115.56(9) . . ? O13 Sm1 O2 91.01(11) . . ? O7 Sm1 O2 80.65(9) 4_666 . ? O4 Sm1 O2 149.20(11) 1_455 . ? O9 Sm1 O3 80.85(10) . 1_455 ? O14 Sm1 O3 106.02(10) . 1_455 ? O5 Sm1 O3 77.31(10) . 1_455 ? O13 Sm1 O3 119.61(10) . 1_455 ? O7 Sm1 O3 72.73(10) 4_666 1_455 ? O4 Sm1 O3 51.93(10) 1_455 1_455 ? O2 Sm1 O3 149.12(10) . 1_455 ? O9 Sm1 O1 76.89(10) . . ? O14 Sm1 O1 110.97(10) . . ? O5 Sm1 O1 67.63(9) . . ? O13 Sm1 O1 67.05(10) . . ? O7 Sm1 O1 127.34(9) 4_666 . ? O4 Sm1 O1 135.16(9) 1_455 . ? O2 Sm1 O1 50.43(9) . . ? O3 Sm1 O1 142.47(9) 1_455 . ? O9 Sm1 C4 106.77(12) . 1_455 ? O14 Sm1 C4 88.32(12) . 1_455 ? O5 Sm1 C4 83.02(11) . 1_455 ? O13 Sm1 C4 96.75(12) . 1_455 ? O7 Sm1 C4 82.54(11) 4_666 1_455 ? O4 Sm1 C4 26.04(11) 1_455 1_455 ? O2 Sm1 C4 161.02(11) . 1_455 ? O3 Sm1 C4 26.00(11) 1_455 1_455 ? O1 Sm1 C4 148.35(11) . 1_455 ? O9 Sm1 C1 73.75(11) . . ? O14 Sm1 C1 95.58(11) . . ? O5 Sm1 C1 91.12(11) . . ? O13 Sm1 C1 79.59(11) . . ? O7 Sm1 C1 103.58(11) 4_666 . ? O4 Sm1 C1 151.62(11) 1_455 . ? O2 Sm1 C1 25.25(10) . . ? O3 Sm1 C1 154.22(11) 1_455 . ? O1 Sm1 C1 25.27(10) . . ? C4 Sm1 C1 173.62(12) 1_455 . ? O8 Sm2 O15 77.19(11) 1_655 . ? O8 Sm2 O10 91.41(10) 1_655 . ? O15 Sm2 O10 137.40(11) . . ? O8 Sm2 O16 79.20(10) 1_655 . ? O15 Sm2 O16 77.76(11) . . ? O10 Sm2 O16 140.83(10) . . ? O8 Sm2 O12 125.36(10) 1_655 3_557 ? O15 Sm2 O12 146.05(11) . 3_557 ? O10 Sm2 O12 72.64(10) . 3_557 ? O16 Sm2 O12 82.08(10) . 3_557 ? O8 Sm2 O1 88.44(10) 1_655 . ? O15 Sm2 O1 69.80(10) . . ? O10 Sm2 O1 68.98(10) . . ? O16 Sm2 O1 147.13(10) . . ? O12 Sm2 O1 128.80(10) 3_557 . ? O8 Sm2 O6 140.61(10) 1_655 . ? O15 Sm2 O6 75.11(10) . . ? O10 Sm2 O6 127.82(9) . . ? O16 Sm2 O6 67.99(9) . . ? O12 Sm2 O6 72.08(10) 3_557 . ? O1 Sm2 O6 107.30(9) . . ? O8 Sm2 O11 73.10(10) 1_655 3_557 ? O15 Sm2 O11 140.67(10) . 3_557 ? O10 Sm2 O11 68.99(10) . 3_557 ? O16 Sm2 O11 71.89(10) . 3_557 ? O12 Sm2 O11 52.30(9) 3_557 3_557 ? O1 Sm2 O11 133.26(10) . 3_557 ? O6 Sm2 O11 114.18(10) . 3_557 ? O8 Sm2 O5 154.79(10) 1_655 . ? O15 Sm2 O5 88.73(10) . . ? O10 Sm2 O5 84.90(10) . . ? O16 Sm2 O5 118.49(10) . . ? O12 Sm2 O5 77.23(10) 3_557 . ? O1 Sm2 O5 66.94(9) . . ? O6 Sm2 O5 50.58(9) . . ? O11 Sm2 O5 127.63(9) 3_557 . ? O8 Sm2 C12 99.15(12) 1_655 3_557 ? O15 Sm2 C12 157.20(12) . 3_557 ? O10 Sm2 C12 64.49(11) . 3_557 ? O16 Sm2 C12 79.45(11) . 3_557 ? O12 Sm2 C12 26.64(11) 3_557 3_557 ? O1 Sm2 C12 132.94(11) . 3_557 ? O6 Sm2 C12 95.76(12) . 3_557 ? O11 Sm2 C12 26.24(10) 3_557 3_557 ? O5 Sm2 C12 101.67(11) . 3_557 ? O8 Sm2 C5 158.92(12) 1_655 . ? O15 Sm2 C5 82.09(11) . . ? O10 Sm2 C5 106.63(11) . . ? O16 Sm2 C5 92.76(11) . . ? O12 Sm2 C5 71.83(11) 3_557 . ? O1 Sm2 C5 88.02(11) . . ? O6 Sm2 C5 24.89(10) . . ? O11 Sm2 C5 123.14(11) 3_557 . ? O5 Sm2 C5 25.73(10) . . ? C12 Sm2 C5 98.46(13) 3_557 . ? O1 C1 O2 120.5(4) . . ? O1 C1 C2 119.9(4) . . ? O2 C1 C2 119.6(4) . . ? O1 C1 Sm1 63.1(2) . . ? O2 C1 Sm1 57.7(2) . . ? C2 C1 Sm1 174.0(3) . . ? C3 C2 C1 124.2(4) . . ? C3 C2 H2 117.9 . . ? C1 C2 H2 117.9 . . ? C2 C3 C4 121.2(4) . . ? C2 C3 H3 119.4 . . ? C4 C3 H3 119.4 . . ? O3 C4 O4 121.2(4) . . ? O3 C4 C3 119.7(4) . . ? O4 C4 C3 119.1(4) . . ? O3 C4 Sm1 62.8(2) . 1_655 ? O4 C4 Sm1 58.8(2) . 1_655 ? C3 C4 Sm1 173.1(3) . 1_655 ? O6 C5 O5 119.9(4) . . ? O6 C5 C6 120.2(4) . . ? O5 C5 C6 119.9(4) . . ? O6 C5 Sm2 57.2(2) . . ? O5 C5 Sm2 62.9(2) . . ? C6 C5 Sm2 174.4(3) . . ? C7 C6 C5 120.9(4) . . ? C7 C6 H6 119.5 . . ? C5 C6 H6 119.5 . . ? C6 C7 C8 124.7(4) . . ? C6 C7 H7 117.6 . . ? C8 C7 H7 117.6 . . ? O8 C8 O7 124.8(4) . . ? O8 C8 C7 118.8(4) . . ? O7 C8 C7 116.3(4) . . ? O10 C9 O9 124.7(4) . . ? O10 C9 C10 117.5(4) . . ? O9 C9 C10 117.8(4) . . ? C11 C10 C9 123.1(4) . . ? C11 C10 H10 118.4 . . ? C9 C10 H10 118.4 . . ? C10 C11 C12 122.8(4) . . ? C10 C11 H11 118.6 . . ? C12 C11 H11 118.6 . . ? O11 C12 O12 120.8(4) . . ? O11 C12 C11 119.0(4) . . ? O12 C12 C11 120.0(4) . . ? O11 C12 Sm2 63.1(2) . 3_557 ? O12 C12 Sm2 59.9(2) . 3_557 ? C11 C12 Sm2 160.4(3) . 3_557 ? C1 O1 Sm2 135.5(3) . . ? C1 O1 Sm1 91.6(2) . . ? Sm2 O1 Sm1 109.45(10) . . ? C1 O2 Sm1 97.0(3) . . ? C4 O3 Sm1 91.2(3) . 1_655 ? C4 O4 Sm1 95.1(3) . 1_655 ? C5 O5 Sm1 150.1(3) . . ? C5 O5 Sm2 91.4(2) . . ? Sm1 O5 Sm2 111.43(11) . . ? C5 O6 Sm2 97.9(3) . . ? C8 O7 Sm1 140.1(3) . 4_565 ? C8 O8 Sm2 136.8(3) . 1_455 ? C9 O9 Sm1 142.5(3) . . ? C9 O10 Sm2 128.3(3) . . ? C12 O11 Sm2 90.7(3) . 3_557 ? C12 O12 Sm2 93.5(3) . 3_557 ? Sm1 O13 H131 132(3) . . ? Sm1 O13 H132 117(3) . . ? H131 O13 H132 106(3) . . ? Sm1 O14 H141 125(3) . . ? Sm1 O14 H142 123(3) . . ? H141 O14 H142 104(3) . . ? Sm2 O15 H151 125(3) . . ? Sm2 O15 H152 130(3) . . ? H151 O15 H152 101(3) . . ? Sm2 O16 H161 107(3) . . ? Sm2 O16 H162 119(4) . . ? H161 O16 H162 112(4) . . ? H171 O17 H172 109(4) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O13 H131 O12 0.93(3) 1.89(3) 2.780(4) 159(5) 4_565 O13 H132 O17 0.95(3) 1.94(3) 2.884(5) 174(5) . O14 H141 O2 0.93(3) 1.81(3) 2.735(4) 176(5) 3_567 O14 H142 O6 0.95(3) 1.82(3) 2.765(4) 172(5) 2_456 O15 H151 O3 0.96(3) 1.79(3) 2.739(4) 169(5) 4_565 O15 H152 O17 0.97(3) 1.84(3) 2.795(5) 167(5) . O16 H161 O7 0.93(3) 1.80(3) 2.695(4) 159(5) 1_655 O16 H162 O4 0.90(3) 2.01(3) 2.910(4) 170(5) 2_546 O17 H171 O11 0.94(3) 1.95(3) 2.887(5) 172(5) 4_665 O17 H172 O18 0.90(3) 2.19(4) 2.934(8) 140(5) . O17 H172 O19 0.90(3) 2.00(4) 2.734(8) 138(4) . _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.276 _refine_diff_density_min -1.224 _refine_diff_density_rms 0.175