data_vauxite _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H14 Al2 F0.10 Fe O16 P2' _chemical_formula_weight 443.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source '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' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Al' 'Al' 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.1276(2) _cell_length_b 11.5836(3) _cell_length_c 6.15960(10) _cell_angle_alpha 98.3152(10) _cell_angle_beta 92.0139(10) _cell_angle_gamma 108.1695(9) _cell_volume 610.05(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.416 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 450 _exptl_absorpt_coefficient_mu 1.738 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.7805 _exptl_absorpt_correction_T_max 0.9181 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21764 _diffrn_reflns_av_R_equivalents 0.0171 _diffrn_reflns_av_sigmaI/netI 0.0137 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 36.33 _reflns_number_total 5904 _reflns_number_gt 5705 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^)+(0.0312P)^2^+0.2366P] 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 5904 _refine_ls_number_parameters 252 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0208 _refine_ls_R_factor_gt 0.0200 _refine_ls_wR_factor_ref 0.0602 _refine_ls_wR_factor_gt 0.0597 _refine_ls_goodness_of_fit_ref 1.138 _refine_ls_restrained_S_all 1.145 _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 Fe1 Fe 0.0000 0.0000 0.0000 0.01307(4) Uani 1 2 d S . . Fe2 Fe 0.0000 0.5000 0.0000 0.00812(3) Uani 1 2 d S . . Al1 Al 0.66684(3) 0.29066(2) 0.18660(4) 0.00623(4) Uani 1 1 d . . . Al2 Al 0.0000 0.5000 0.5000 0.00588(6) Uani 1 2 d S . . Al3 Al 0.5000 0.5000 0.0000 0.00733(6) Uani 1 2 d S . . P1 P 0.99043(2) 0.263763(19) 0.21546(3) 0.00756(4) Uani 1 1 d . . . P2 P 0.31018(2) 0.638669(18) 0.29177(3) 0.00557(4) Uani 1 1 d . . . O1 O 0.81155(7) 0.20641(6) 0.20208(10) 0.00945(9) Uani 1 1 d . . . O2 O 0.03516(8) 0.32915(6) 0.01385(11) 0.01120(10) Uani 1 1 d . . . O3 O 0.04736(7) 0.35452(6) 0.42968(10) 0.00964(10) Uani 1 1 d . . . O4 O 0.06203(8) 0.15995(6) 0.21072(12) 0.01308(11) Uani 1 1 d . . . O5 O 0.13584(7) 0.57142(6) 0.29633(10) 0.00859(9) Uani 1 1 d . . . O6 O 0.62393(7) 0.28520(6) 0.48268(10) 0.00910(9) Uani 1 1 d . . . O7 O 0.32751(7) 0.72489(6) 0.12120(10) 0.00873(9) Uani 1 1 d . . . O8 O 0.39427(8) 0.54577(6) 0.22796(10) 0.01080(10) Uani 1 1 d . . . O9 O 0.53156(7) 0.38301(6) 0.16413(10) 0.01037(16) Uani 0.97(4) 1 d PD . . F9 F 0.53156(7) 0.38301(6) 0.16413(10) 0.01037(16) Uani 0.05(3) 1 d P . . O10 O 0.83752(7) 0.44742(5) 0.25926(10) 0.00736(9) Uani 1 1 d D . . O11 O 0.76719(9) 0.96152(7) 0.14152(14) 0.01833(13) Uani 1 1 d D . . O12 O 0.05817(12) 0.90647(10) 0.27609(17) 0.02875(18) Uani 1 1 d D . . O13 O 0.50170(8) 0.13696(6) 0.12240(11) 0.01405(11) Uani 1 1 d D . . O14 O 0.69389(8) 0.61897(6) 0.14391(11) 0.01263(11) Uani 1 1 d D . . O15 O 0.38023(11) 0.95715(8) 0.33703(15) 0.02292(15) Uani 1 1 d D . . O16 O 0.70670(10) 0.80824(8) 0.46621(13) 0.02047(14) Uani 1 1 d D . . H91 H 0.482(2) 0.3909(19) 0.292(2) 0.033(7) Uiso 0.97(4) 1 d PD . . H101 H 0.788(2) 0.5061(15) 0.278(3) 0.029(5) Uiso 1 1 d D . . H111 H 0.774(3) 1.0441(10) 0.179(4) 0.036(5) Uiso 1 1 d D . . H112 H 0.757(3) 0.924(2) 0.268(3) 0.042(6) Uiso 1 1 d D . . H121 H 0.022(3) 0.8195(9) 0.241(4) 0.055(7) Uiso 1 1 d D . . H122 H 0.1623(16) 0.930(3) 0.337(5) 0.066 Uiso 1 1 d D . . H131 H 0.477(3) 0.0756(17) 0.205(3) 0.049(7) Uiso 1 1 d D . . H132 H 0.4210(19) 0.123(2) 0.018(3) 0.038(6) Uiso 1 1 d D . . H141 H 0.702(3) 0.6858(18) 0.254(4) 0.061(8) Uiso 1 1 d D . . H142 H 0.7814(18) 0.645(2) 0.070(4) 0.043(6) Uiso 1 1 d D . . H151 H 0.372(3) 0.8790(11) 0.264(3) 0.033(5) Uiso 1 1 d D . . H152 H 0.459(2) 0.966(2) 0.440(3) 0.040 Uiso 1 1 d D . . H161 H 0.767(2) 0.809(2) 0.593(3) 0.046(6) Uiso 1 1 d D . . H162 H 0.6081(16) 0.786(3) 0.513(4) 0.059(8) 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 Fe1 0.01421(8) 0.00954(7) 0.01458(8) -0.00318(6) -0.00147(6) 0.00514(6) Fe2 0.00827(7) 0.00953(7) 0.00611(6) 0.00148(5) 0.00024(5) 0.00218(5) Al1 0.00659(9) 0.00679(10) 0.00548(9) 0.00121(7) 0.00060(7) 0.00231(7) Al2 0.00607(13) 0.00609(13) 0.00526(12) 0.00045(10) 0.00080(10) 0.00179(10) Al3 0.00741(13) 0.00873(14) 0.00742(13) 0.00190(10) 0.00131(10) 0.00450(11) P1 0.00773(8) 0.00690(8) 0.00834(8) 0.00002(6) 0.00042(6) 0.00334(6) P2 0.00550(7) 0.00667(7) 0.00468(7) 0.00105(5) 0.00079(5) 0.00208(6) O1 0.0078(2) 0.0084(2) 0.0127(2) 0.00170(18) 0.00044(18) 0.00329(18) O2 0.0120(2) 0.0123(2) 0.0100(2) 0.00246(19) 0.00308(19) 0.0044(2) O3 0.0121(2) 0.0085(2) 0.0085(2) -0.00109(17) -0.00110(18) 0.00490(19) O4 0.0129(3) 0.0096(2) 0.0174(3) -0.0022(2) -0.0028(2) 0.0070(2) O5 0.0061(2) 0.0113(2) 0.0071(2) 0.00169(17) 0.00090(16) 0.00070(18) O6 0.0098(2) 0.0107(2) 0.0050(2) 0.00054(17) 0.00018(17) 0.00121(19) O7 0.0124(2) 0.0088(2) 0.0056(2) 0.00234(17) 0.00134(17) 0.00356(19) O8 0.0131(2) 0.0125(2) 0.0105(2) 0.00346(19) 0.00475(19) 0.0083(2) O9 0.0115(3) 0.0130(3) 0.0100(3) 0.00439(19) 0.00316(18) 0.0074(2) F9 0.0115(3) 0.0130(3) 0.0100(3) 0.00439(19) 0.00316(18) 0.0074(2) O10 0.0068(2) 0.0073(2) 0.0081(2) 0.00089(16) -0.00009(16) 0.00262(17) O11 0.0171(3) 0.0145(3) 0.0220(3) 0.0007(2) -0.0009(2) 0.0043(2) O12 0.0286(4) 0.0282(4) 0.0297(4) 0.0006(3) -0.0049(3) 0.0122(4) O13 0.0137(3) 0.0113(3) 0.0127(3) 0.0039(2) -0.0029(2) -0.0027(2) O14 0.0092(2) 0.0129(3) 0.0137(3) -0.0009(2) 0.00140(19) 0.0020(2) O15 0.0317(4) 0.0125(3) 0.0240(4) 0.0041(3) 0.0025(3) 0.0058(3) O16 0.0187(3) 0.0259(4) 0.0168(3) 0.0007(3) 0.0004(2) 0.0084(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 Fe1 O4 2.0091(6) 2 ? Fe1 O4 2.0091(6) . ? Fe1 O11 2.2641(8) 1_445 ? Fe1 O11 2.2641(8) 2_665 ? Fe1 O12 2.2751(10) 2_565 ? Fe1 O12 2.2751(10) 1_545 ? Fe2 O5 2.0779(6) . ? Fe2 O5 2.0779(6) 2_565 ? Fe2 O2 2.1142(7) . ? Fe2 O2 2.1142(7) 2_565 ? Fe2 O10 2.2372(6) 2_665 ? Fe2 O10 2.2372(6) 1_455 ? Al1 O1 1.8784(6) . ? Al1 O9 1.8823(6) . ? Al1 O7 1.8825(6) 2_665 ? Al1 O6 1.8845(6) . ? Al1 O13 1.9181(7) . ? Al1 O10 1.9688(6) . ? Al2 O3 1.8629(6) . ? Al2 O3 1.8630(6) 2_566 ? Al2 O5 1.8882(6) 2_566 ? Al2 O5 1.8882(6) . ? Al2 O10 1.9468(6) 2_666 ? Al2 O10 1.9468(6) 1_455 ? Al3 O8 1.8393(6) . ? Al3 O8 1.8393(6) 2_665 ? Al3 O9 1.8870(6) . ? Al3 F9 1.8870(6) 2_665 ? Al3 O9 1.8870(6) 2_665 ? Al3 O14 1.9576(7) 2_665 ? Al3 O14 1.9576(7) . ? P1 O3 1.5252(6) 1_655 ? P1 O4 1.5347(7) 1_655 ? P1 O2 1.5484(7) 1_655 ? P1 O1 1.5531(6) . ? P2 O8 1.5217(6) . ? P2 O6 1.5250(6) 2_666 ? P2 O7 1.5307(6) . ? P2 O5 1.5415(6) . ? O2 P1 1.5484(7) 1_455 ? O3 P1 1.5252(6) 1_455 ? O4 P1 1.5347(7) 1_455 ? O6 P2 1.5250(6) 2_666 ? O7 Al1 1.8825(6) 2_665 ? O9 H91 0.928(9) . ? O10 Al2 1.9468(6) 1_655 ? O10 Fe2 2.2372(6) 1_655 ? O10 H101 0.922(9) . ? O11 Fe1 2.2641(8) 1_665 ? O11 H111 0.932(9) . ? O11 H112 0.935(9) . ? O12 Fe1 2.2751(10) 1_565 ? O12 H121 0.946(10) . ? O12 H122 0.950(10) . ? O13 H131 0.911(10) . ? O13 H132 0.917(9) . ? O14 H141 0.935(10) . ? O14 H142 0.922(10) . ? O15 H151 0.932(9) . ? O15 H152 0.913(9) . ? O16 H161 0.933(10) . ? O16 H162 0.924(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Fe1 O4 180.00(4) 2 . ? O4 Fe1 O11 94.27(3) 2 1_445 ? O4 Fe1 O11 85.73(3) . 1_445 ? O4 Fe1 O11 85.73(3) 2 2_665 ? O4 Fe1 O11 94.27(3) . 2_665 ? O11 Fe1 O11 180.00(5) 1_445 2_665 ? O4 Fe1 O12 89.06(3) 2 2_565 ? O4 Fe1 O12 90.94(3) . 2_565 ? O11 Fe1 O12 96.13(3) 1_445 2_565 ? O11 Fe1 O12 83.87(3) 2_665 2_565 ? O4 Fe1 O12 90.94(3) 2 1_545 ? O4 Fe1 O12 89.06(3) . 1_545 ? O11 Fe1 O12 83.87(3) 1_445 1_545 ? O11 Fe1 O12 96.13(3) 2_665 1_545 ? O12 Fe1 O12 180.00(4) 2_565 1_545 ? O5 Fe2 O5 180.0 . 2_565 ? O5 Fe2 O2 88.87(2) . . ? O5 Fe2 O2 91.13(2) 2_565 . ? O5 Fe2 O2 91.13(2) . 2_565 ? O5 Fe2 O2 88.87(2) 2_565 2_565 ? O2 Fe2 O2 180.0 . 2_565 ? O5 Fe2 O10 104.78(2) . 2_665 ? O5 Fe2 O10 75.22(2) 2_565 2_665 ? O2 Fe2 O10 95.61(2) . 2_665 ? O2 Fe2 O10 84.39(2) 2_565 2_665 ? O5 Fe2 O10 75.22(2) . 1_455 ? O5 Fe2 O10 104.78(2) 2_565 1_455 ? O2 Fe2 O10 84.39(2) . 1_455 ? O2 Fe2 O10 95.61(2) 2_565 1_455 ? O10 Fe2 O10 180.0 2_665 1_455 ? O1 Al1 O9 176.33(3) . . ? O1 Al1 O7 90.39(3) . 2_665 ? O9 Al1 O7 87.94(3) . 2_665 ? O1 Al1 O6 93.24(3) . . ? O9 Al1 O6 88.97(3) . . ? O7 Al1 O6 169.38(3) 2_665 . ? O1 Al1 O13 90.39(3) . . ? O9 Al1 O13 92.70(3) . . ? O7 Al1 O13 84.62(3) 2_665 . ? O6 Al1 O13 85.37(3) . . ? O1 Al1 O10 88.97(3) . . ? O9 Al1 O10 87.98(3) . . ? O7 Al1 O10 96.57(3) 2_665 . ? O6 Al1 O10 93.47(3) . . ? O13 Al1 O10 178.65(3) . . ? O3 Al2 O3 180.00(4) . 2_566 ? O3 Al2 O5 90.15(3) . 2_566 ? O3 Al2 O5 89.85(3) 2_566 2_566 ? O3 Al2 O5 89.85(3) . . ? O3 Al2 O5 90.15(3) 2_566 . ? O5 Al2 O5 180.0 2_566 . ? O3 Al2 O10 88.91(3) . 2_666 ? O3 Al2 O10 91.09(3) 2_566 2_666 ? O5 Al2 O10 86.85(3) 2_566 2_666 ? O5 Al2 O10 93.15(3) . 2_666 ? O3 Al2 O10 91.09(3) . 1_455 ? O3 Al2 O10 88.91(3) 2_566 1_455 ? O5 Al2 O10 93.15(3) 2_566 1_455 ? O5 Al2 O10 86.85(3) . 1_455 ? O10 Al2 O10 180.000(1) 2_666 1_455 ? O8 Al3 O8 180.0 . 2_665 ? O8 Al3 O9 86.94(3) . . ? O8 Al3 O9 93.06(3) 2_665 . ? O8 Al3 F9 93.06(3) . 2_665 ? O8 Al3 F9 86.94(3) 2_665 2_665 ? O9 Al3 F9 180.0 . 2_665 ? O8 Al3 O9 93.06(3) . 2_665 ? O8 Al3 O9 86.94(3) 2_665 2_665 ? O9 Al3 O9 180.0 . 2_665 ? F9 Al3 O9 0.00(4) 2_665 2_665 ? O8 Al3 O14 89.75(3) . 2_665 ? O8 Al3 O14 90.25(3) 2_665 2_665 ? O9 Al3 O14 90.98(3) . 2_665 ? F9 Al3 O14 89.02(3) 2_665 2_665 ? O9 Al3 O14 89.02(3) 2_665 2_665 ? O8 Al3 O14 90.25(3) . . ? O8 Al3 O14 89.75(3) 2_665 . ? O9 Al3 O14 89.02(3) . . ? F9 Al3 O14 90.98(3) 2_665 . ? O9 Al3 O14 90.98(3) 2_665 . ? O14 Al3 O14 180.0 2_665 . ? O3 P1 O4 109.43(4) 1_655 1_655 ? O3 P1 O2 110.80(4) 1_655 1_655 ? O4 P1 O2 109.49(4) 1_655 1_655 ? O3 P1 O1 109.64(4) 1_655 . ? O4 P1 O1 108.58(4) 1_655 . ? O2 P1 O1 108.87(4) 1_655 . ? O8 P2 O6 110.31(4) . 2_666 ? O8 P2 O7 110.15(3) . . ? O6 P2 O7 109.18(3) 2_666 . ? O8 P2 O5 110.05(4) . . ? O6 P2 O5 109.67(3) 2_666 . ? O7 P2 O5 107.43(3) . . ? P1 O1 Al1 126.43(4) . . ? P1 O2 Fe2 120.26(4) 1_455 . ? P1 O3 Al2 124.56(4) 1_455 . ? P1 O4 Fe1 127.03(4) 1_455 . ? P2 O5 Al2 137.83(4) . . ? P2 O5 Fe2 118.97(3) . . ? Al2 O5 Fe2 101.78(3) . . ? P2 O6 Al1 137.61(4) 2_666 . ? P2 O7 Al1 135.98(4) . 2_665 ? P2 O8 Al3 139.13(4) . . ? Al1 O9 Al3 139.52(4) . . ? Al1 O9 H91 111.5(14) . . ? Al3 O9 H91 106.4(14) . . ? Al2 O10 Al1 128.98(3) 1_655 . ? Al2 O10 Fe2 94.54(2) 1_655 1_655 ? Al1 O10 Fe2 117.15(3) . 1_655 ? Al2 O10 H101 104.6(13) 1_655 . ? Al1 O10 H101 103.9(13) . . ? Fe2 O10 H101 105.4(13) 1_655 . ? Fe1 O11 H111 95.2(14) 1_665 . ? Fe1 O11 H112 116.4(15) 1_665 . ? H111 O11 H112 110(2) . . ? Fe1 O12 H121 112.9(17) 1_565 . ? Fe1 O12 H122 119.3(18) 1_565 . ? H121 O12 H122 107(2) . . ? Al1 O13 H131 127.3(16) . . ? Al1 O13 H132 122.7(14) . . ? H131 O13 H132 108(2) . . ? Al3 O14 H141 125.4(17) . . ? Al3 O14 H142 122.4(15) . . ? H141 O14 H142 105(2) . . ? H151 O15 H152 98.4(19) . . ? H161 O16 H162 102(2) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O9 H91 O6 0.928(9) 2.42(2) 2.6396(9) 93.4(14) . O9 H91 O8 0.928(9) 2.26(2) 2.5638(9) 98.4(15) . O10 H101 O14 0.922(9) 2.023(13) 2.8531(9) 149.0(18) . O11 H112 O16 0.935(9) 1.909(11) 2.8197(12) 164(2) . O14 H141 O16 0.935(10) 1.773(10) 2.7067(11) 177(3) . O15 H151 O7 0.932(9) 1.786(10) 2.7112(10) 172(2) . O13 H132 O11 0.917(9) 1.852(12) 2.7211(10) 157(2) 2_665 O14 H142 O2 0.922(10) 1.718(12) 2.6139(9) 163(2) 2_665 O16 H161 O4 0.933(10) 1.853(12) 2.7495(11) 160(2) 2_666 O16 H162 O6 0.924(10) 2.022(13) 2.9166(10) 163(3) 2_666 O13 H131 O15 0.911(10) 1.713(12) 2.6027(11) 165(2) 1_545 O11 H111 O1 0.932(9) 1.787(10) 2.7050(10) 168(2) 1_565 O15 H152 O15 0.913(9) 1.876(11) 2.7491(19) 159(2) 2_676 O12 H121 O2 0.946(10) 2.072(18) 2.8979(12) 145(2) 2_565 O12 H122 O15 0.950(10) 1.915(15) 2.8124(14) 157(3) . _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 36.33 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.462 _refine_diff_density_min -0.854 _refine_diff_density_rms 0.093