Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name _publ_author_address 'Costes, Jean-Pierre' ; Laboratoire de Chimie de Coordination du CNRS 205 Route de Narbonne 31077 Toulouse Cedex France ; 'Clemente-Juan, Juan Modesto' ; Instituto de Ciencia Molecular Universidad de Valencia Dr. Moliner 50 46100 Burjassot Spain ; 'Dahan, Francoise' ; Laboratoire de Chimie de Coordination du CNRS 205 Route de Narbonne 31077 Toulouse Cedex France ; 'Nicodeme, Franck' ; Laboratoire de Chimie de Coordination du CNRS 205 Route de Narbonne 31077 Toulouse Cedex France ; _publ_contact_author_address ; Labo Chimie de Coordination CNRS 205, route de Narbonne Toulouse 31077 FRANCE ; _publ_contact_author_email costes@lcc-toulouse.fr _publ_contact_author_fax '(33) 0561553003' _publ_contact_author_phone '(33) 0561333152' _publ_contact_author_name 'Dr Jean-Pierre Costes' _publ_requested_journal 'J.C.S. Dalton Transactions' data_jp21 _database_code_CSD 199304 _publ_section_title ; Ferromagnetic interaction in a polynuclear gadolinium complex: Structure and Magnetic studies ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H17 Gd O10' _chemical_formula_weight 586.60 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/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 13.5709(13) _cell_length_b 6.7141(9) _cell_length_c 22.7232(17) _cell_angle_alpha 90.00 _cell_angle_beta 99.705(14) _cell_angle_gamma 90.00 _cell_volume 2040.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12.0 _cell_measurement_theta_max 18.5 _exptl_crystal_description Plate _exptl_crystal_colour Light-Pink _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.909 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1148 _exptl_absorpt_coefficient_mu 3.308 _exptl_absorpt_correction_type Psi-Scans _exptl_absorpt_correction_T_min 0.6610 _exptl_absorpt_correction_T_max 0.9994 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius CAD4' _diffrn_measurement_method \w-2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% -1.1 _diffrn_reflns_number 4643 _diffrn_reflns_av_R_equivalents 0.0304 _diffrn_reflns_av_sigmaI/netI 0.0355 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 26.98 _reflns_number_total 4454 _reflns_number_gt 3113 _reflns_threshold_expression >2sigma(I) _computing_data_collection CAD4-EXPRESS _computing_cell_refinement CAD4-EXPRESS _computing_data_reduction 'MolEN (Fair, 1990)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ZORTEP (Zolnai, 1996)' _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 w=1/[\s^2^(Fo^2^)+(0.0398P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4454 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0442 _refine_ls_R_factor_gt 0.0291 _refine_ls_wR_factor_ref 0.0680 _refine_ls_wR_factor_gt 0.0656 _refine_ls_goodness_of_fit_ref 0.866 _refine_ls_restrained_S_all 0.866 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd Gd 0.329182(15) 0.16314(3) 0.228658(9) 0.02119(6) Uani 1 d . . . O1 O 0.2366(2) -0.0024(4) 0.30522(12) 0.0230(6) Uani 1 d . . . O2 O 0.1935(2) 0.3037(4) 0.28161(13) 0.0250(7) Uani 1 d . . . O3 O 0.1087(2) 0.5227(5) 0.35564(15) 0.0377(8) Uani 1 d . . . O4 O 0.4719(2) 0.3581(5) 0.20600(14) 0.0332(7) Uani 1 d . . . O5 O 0.5342(3) 0.2229(6) 0.13081(18) 0.0504(11) Uani 1 d . . . H5A H 0.5134 0.1181 0.1426 0.055 Uiso 1 calc R . . O6 O 0.5534(3) 0.6665(6) 0.2568(2) 0.0505(10) Uani 1 d . . . H6A H 0.5274 0.5567 0.2579 0.056 Uiso 1 calc R . . O7 O 0.1799(2) 0.1231(5) 0.16143(14) 0.0317(7) Uani 1 d . . . O8 O 0.1004(2) -0.1471(5) 0.18406(14) 0.0351(7) Uani 1 d . . . O9 O 0.0748(3) 0.3979(6) 0.0975(2) 0.0558(11) Uani 1 d . . . H9A H 0.1272 0.3528 0.1159 0.061 Uiso 1 calc R . . O10 O 0.4713(2) 0.0065(6) 0.28546(16) 0.0416(8) Uani 1 d . . . H10A H 0.476(3) 0.030(6) 0.3280(11) 0.046 Uiso 1 d . . . H10B H 0.506(4) -0.118(5) 0.290(2) 0.046 Uiso 1 d . . . C1 C 0.1983(3) 0.1617(7) 0.31813(18) 0.0262(8) Uani 1 d . . . C2 C 0.1641(3) 0.1862(7) 0.37656(18) 0.0249(9) Uani 1 d . . . C3 C 0.1196(3) 0.3617(7) 0.3909(2) 0.0287(10) Uani 1 d . . . C4 C 0.0844(4) 0.3693(8) 0.4458(2) 0.0437(13) Uani 1 d . . . H4 H 0.0546 0.4851 0.4568 0.048 Uiso 1 calc R . . C5 C 0.0938(4) 0.2081(8) 0.4833(2) 0.0475(15) Uani 1 d . . . H5 H 0.0695 0.2159 0.5191 0.052 Uiso 1 calc R . . C6 C 0.1388(4) 0.0332(9) 0.4688(2) 0.0452(13) Uani 1 d . . . H6 H 0.1457 -0.0756 0.4945 0.050 Uiso 1 calc R . . C7 C 0.1724(3) 0.0261(7) 0.4159(2) 0.0308(10) Uani 1 d . . . H7 H 0.2022 -0.0906 0.4055 0.034 Uiso 1 calc R . . C8 C 0.5345(3) 0.3554(7) 0.1702(2) 0.0306(10) Uani 1 d . . . C9 C 0.6121(4) 0.5118(8) 0.1755(2) 0.0386(11) Uani 1 d . . . C10 C 0.6156(4) 0.6637(9) 0.2170(2) 0.0424(12) Uani 1 d . . . C11 C 0.6838(5) 0.8123(10) 0.2171(3) 0.0619(18) Uani 1 d . . . H11 H 0.6845 0.9194 0.2431 0.068 Uiso 1 calc R . . C12 C 0.7526(5) 0.8032(12) 0.1781(3) 0.070(2) Uani 1 d . . . H12 H 0.7994 0.9047 0.1790 0.078 Uiso 1 calc R . . C13 C 0.7537(5) 0.6512(12) 0.1388(3) 0.072(2) Uani 1 d . . . H13 H 0.8015 0.6463 0.1139 0.079 Uiso 1 calc R . . C14 C 0.6806(5) 0.5012(12) 0.1367(3) 0.065(2) Uani 1 d . . . H14 H 0.6783 0.3967 0.1096 0.071 Uiso 1 calc R . . C15 C 0.1065(3) 0.0052(7) 0.15349(17) 0.0262(9) Uani 1 d . . . C16 C 0.0227(4) 0.0540(7) 0.1046(2) 0.0311(10) Uani 1 d . . . C17 C 0.0104(4) 0.2458(8) 0.0794(2) 0.0334(11) Uani 1 d . . . C18 C -0.0710(4) 0.2848(10) 0.0361(2) 0.0514(16) Uani 1 d . . . H18 H -0.0801 0.4133 0.0209 0.057 Uiso 1 calc R . . C19 C -0.1383(4) 0.1425(11) 0.0149(2) 0.0582(18) Uani 1 d . . . H19 H -0.1920 0.1722 -0.0150 0.064 Uiso 1 calc R . . C20 C -0.1259(4) -0.0489(11) 0.0385(3) 0.065(2) Uani 1 d . . . H20 H -0.1712 -0.1486 0.0243 0.071 Uiso 1 calc R . . C21 C -0.0468(4) -0.0904(9) 0.0828(3) 0.0498(15) Uani 1 d . . . H21 H -0.0397 -0.2184 0.0986 0.055 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd 0.02269(10) 0.01500(10) 0.02759(10) -0.00177(11) 0.00917(7) -0.00139(11) O1 0.0255(14) 0.0138(14) 0.0301(15) -0.0017(13) 0.0060(12) 0.0003(13) O2 0.0352(17) 0.0130(15) 0.0305(16) -0.0004(12) 0.0155(13) 0.0047(12) O3 0.0436(19) 0.0268(18) 0.0492(19) 0.0038(16) 0.0266(16) 0.0163(16) O4 0.0286(16) 0.038(2) 0.0359(17) 0.0021(16) 0.0131(13) -0.0068(16) O5 0.050(2) 0.045(2) 0.064(2) -0.015(2) 0.034(2) -0.0256(19) O6 0.046(2) 0.0236(18) 0.088(3) -0.019(2) 0.029(2) -0.0012(19) O7 0.0332(17) 0.0233(19) 0.0361(17) -0.0010(14) -0.0016(13) -0.0093(14) O8 0.0309(16) 0.0348(19) 0.0390(17) 0.0094(17) 0.0045(13) -0.0045(16) O9 0.058(3) 0.033(2) 0.069(3) 0.0156(19) -0.011(2) 0.0043(19) O10 0.0374(19) 0.033(2) 0.050(2) -0.0106(18) -0.0041(16) 0.0107(17) C1 0.035(2) 0.020(2) 0.026(2) -0.004(2) 0.0116(17) -0.002(2) C2 0.027(2) 0.021(2) 0.028(2) 0.0004(19) 0.0071(16) 0.0014(19) C3 0.033(2) 0.023(2) 0.033(2) 0.008(2) 0.0112(18) 0.005(2) C4 0.055(3) 0.041(3) 0.040(3) 0.004(2) 0.025(2) 0.019(3) C5 0.068(4) 0.051(4) 0.029(2) 0.005(3) 0.025(3) 0.016(3) C6 0.055(3) 0.045(3) 0.038(3) 0.013(3) 0.016(2) 0.010(3) C7 0.030(2) 0.025(2) 0.038(2) 0.010(2) 0.0084(19) 0.007(2) C8 0.030(2) 0.027(2) 0.038(2) 0.003(2) 0.0138(18) -0.004(2) C9 0.038(3) 0.034(3) 0.045(3) -0.005(2) 0.010(2) -0.010(2) C10 0.034(2) 0.045(3) 0.048(3) 0.005(3) 0.005(2) -0.009(3) C11 0.056(4) 0.054(4) 0.072(4) -0.022(4) 0.002(3) -0.021(3) C12 0.069(4) 0.080(5) 0.063(4) -0.006(4) 0.014(3) -0.051(4) C13 0.069(4) 0.098(6) 0.054(3) -0.017(4) 0.025(3) -0.048(5) C14 0.065(4) 0.087(5) 0.050(3) -0.014(4) 0.031(3) -0.045(4) C15 0.028(2) 0.029(2) 0.024(2) 0.0010(19) 0.0083(17) 0.003(2) C16 0.039(3) 0.024(2) 0.034(2) 0.011(2) 0.015(2) 0.002(2) C17 0.037(3) 0.033(3) 0.030(2) 0.001(2) 0.005(2) 0.001(2) C18 0.048(3) 0.062(4) 0.038(3) 0.019(3) -0.009(2) 0.005(3) C19 0.032(3) 0.092(5) 0.043(3) 0.016(4) -0.015(2) -0.011(3) C20 0.040(3) 0.075(5) 0.070(4) 0.021(4) -0.016(3) -0.027(3) C21 0.037(3) 0.052(4) 0.056(3) 0.014(3) -0.003(2) -0.015(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd O7 2.338(3) . ? Gd O10 2.377(3) . ? Gd O3 2.411(3) 4_656 ? Gd O8 2.415(3) 4_666 ? Gd O2 2.439(3) 4_656 ? Gd O4 2.462(3) . ? Gd O1 2.490(3) 4_666 ? Gd O2 2.545(3) . ? Gd O1 2.565(3) . ? O1 C1 1.274(5) . ? O1 Gd 2.490(3) 4_656 ? O2 C1 1.259(5) . ? O2 Gd 2.439(3) 4_666 ? O3 C3 1.339(5) . ? O3 Gd 2.411(3) 4_666 ? O4 C8 1.272(5) . ? O5 C8 1.262(6) . ? O5 H5A 0.8200 . ? O6 C10 1.338(6) . ? O6 H6A 0.8200 . ? O7 C15 1.261(5) . ? O8 C15 1.247(6) . ? O8 Gd 2.415(3) 4_656 ? O9 C17 1.362(6) . ? O9 H9A 0.8200 . ? O10 H10A 0.97(3) . ? O10 H10B 0.96(4) . ? C1 C2 1.487(5) . ? C2 C3 1.388(6) . ? C2 C7 1.391(6) . ? C3 C4 1.410(6) . ? C4 C5 1.369(7) . ? C4 H4 0.9300 . ? C5 C6 1.389(7) . ? C5 H5 0.9300 . ? C6 C7 1.356(6) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C9 1.477(6) . ? C9 C10 1.385(8) . ? C9 C14 1.387(7) . ? C10 C11 1.360(8) . ? C11 C12 1.393(9) . ? C11 H11 0.9300 . ? C12 C13 1.357(10) . ? C12 H12 0.9300 . ? C13 C14 1.409(8) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 C16 1.486(6) . ? C16 C21 1.385(7) . ? C16 C17 1.408(7) . ? C17 C18 1.375(7) . ? C18 C19 1.353(8) . ? C18 H18 0.9300 . ? C19 C20 1.392(9) . ? C19 H19 0.9300 . ? C20 C21 1.370(8) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? 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 Gd O10 146.94(12) . . ? O7 Gd O3 79.43(11) . 4_656 ? O10 Gd O3 84.15(12) . 4_656 ? O7 Gd O8 140.95(11) . 4_666 ? O10 Gd O8 67.36(12) . 4_666 ? O3 Gd O8 135.71(11) 4_656 4_666 ? O7 Gd O2 75.06(11) . 4_656 ? O10 Gd O2 72.06(12) . 4_656 ? O3 Gd O2 65.96(10) 4_656 4_656 ? O8 Gd O2 128.81(11) 4_666 4_656 ? O7 Gd O4 123.35(11) . . ? O10 Gd O4 75.77(12) . . ? O3 Gd O4 69.46(11) 4_656 . ? O8 Gd O4 71.03(11) 4_666 . ? O2 Gd O4 126.66(11) 4_656 . ? O7 Gd O1 71.07(10) . 4_666 ? O10 Gd O1 141.50(11) . 4_666 ? O3 Gd O1 105.20(10) 4_656 4_666 ? O8 Gd O1 81.36(10) 4_666 4_666 ? O2 Gd O1 146.08(10) 4_656 4_666 ? O4 Gd O1 73.12(10) . 4_666 ? O7 Gd O2 74.65(11) . . ? O10 Gd O2 119.52(11) . . ? O3 Gd O2 153.96(11) 4_656 . ? O8 Gd O2 68.51(10) 4_666 . ? O2 Gd O2 108.81(7) 4_656 . ? O4 Gd O2 123.97(10) . . ? O1 Gd O2 63.98(9) 4_666 . ? O7 Gd O1 85.63(10) . . ? O10 Gd O1 83.41(11) . . ? O3 Gd O1 130.27(10) 4_656 . ? O8 Gd O1 80.96(10) 4_666 . ? O2 Gd O1 64.38(9) 4_656 . ? O4 Gd O1 149.83(10) . . ? O1 Gd O1 114.17(6) 4_666 . ? O2 Gd O1 50.49(9) . . ? C1 O1 Gd 135.4(3) . 4_656 ? C1 O1 Gd 92.7(2) . . ? Gd O1 Gd 111.85(10) 4_656 . ? C1 O2 Gd 143.5(3) . 4_666 ? C1 O2 Gd 94.0(2) . . ? Gd O2 Gd 114.31(11) 4_666 . ? C3 O3 Gd 140.6(3) . 4_666 ? C8 O4 Gd 139.5(3) . . ? C8 O5 H5A 109.5 . . ? C10 O6 H6A 109.5 . . ? C15 O7 Gd 137.9(3) . . ? C15 O8 Gd 146.7(3) . 4_656 ? C17 O9 H9A 109.5 . . ? Gd O10 H10A 113(3) . . ? Gd O10 H10B 142(3) . . ? H10A O10 H10B 95(4) . . ? O2 C1 O1 118.8(3) . . ? O2 C1 C2 121.1(4) . . ? O1 C1 C2 120.1(4) . . ? C3 C2 C7 119.8(4) . . ? C3 C2 C1 121.2(4) . . ? C7 C2 C1 119.0(4) . . ? O3 C3 C2 123.6(4) . . ? O3 C3 C4 118.7(4) . . ? C2 C3 C4 117.7(4) . . ? C5 C4 C3 120.8(5) . . ? C5 C4 H4 119.6 . . ? C3 C4 H4 119.6 . . ? C4 C5 C6 121.3(4) . . ? C4 C5 H5 119.4 . . ? C6 C5 H5 119.4 . . ? C7 C6 C5 117.9(5) . . ? C7 C6 H6 121.1 . . ? C5 C6 H6 121.1 . . ? C6 C7 C2 122.6(5) . . ? C6 C7 H7 118.7 . . ? C2 C7 H7 118.7 . . ? O5 C8 O4 122.7(4) . . ? O5 C8 C9 118.4(4) . . ? O4 C8 C9 118.8(4) . . ? C10 C9 C14 121.4(5) . . ? C10 C9 C8 121.4(4) . . ? C14 C9 C8 117.2(5) . . ? O6 C10 C11 119.7(6) . . ? O6 C10 C9 121.2(5) . . ? C11 C10 C9 119.2(5) . . ? C10 C11 C12 119.7(6) . . ? C10 C11 H11 120.2 . . ? C12 C11 H11 120.2 . . ? C13 C12 C11 122.3(6) . . ? C13 C12 H12 118.8 . . ? C11 C12 H12 118.8 . . ? C12 C13 C14 118.3(6) . . ? C12 C13 H13 120.8 . . ? C14 C13 H13 120.8 . . ? C9 C14 C13 119.0(6) . . ? C9 C14 H14 120.5 . . ? C13 C14 H14 120.5 . . ? O8 C15 O7 124.1(4) . . ? O8 C15 C16 118.9(4) . . ? O7 C15 C16 117.1(4) . . ? C21 C16 C17 117.9(5) . . ? C21 C16 C15 120.2(4) . . ? C17 C16 C15 121.9(4) . . ? O9 C17 C18 118.0(5) . . ? O9 C17 C16 122.5(4) . . ? C18 C17 C16 119.4(5) . . ? C19 C18 C17 122.2(6) . . ? C19 C18 H18 118.9 . . ? C17 C18 H18 118.9 . . ? C18 C19 C20 118.9(5) . . ? C18 C19 H19 120.5 . . ? C20 C19 H19 120.5 . . ? C21 C20 C19 120.0(6) . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C20 C21 C16 121.5(6) . . ? C20 C21 H21 119.3 . . ? C16 C21 H21 119.3 . . ? 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 O5 H5A O3 0.82 1.78 2.421(4) 133.4 4_656 O6 H6A O4 0.82 1.85 2.533(5) 139.3 . O9 H9A O7 0.82 1.93 2.617(5) 141.4 . O10 H10A O9 0.97(3) 2.13(4) 2.925(6) 138(3) 4_656 O10 H10B O6 0.96(4) 1.80(4) 2.669(5) 150(4) 1_545 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.98 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.016 _refine_diff_density_min -1.296 _refine_diff_density_rms 0.120 #===END