data_natropl _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H11 As3 Ba0.10 Fe4 K0.13 Na0.68 O19.50' _chemical_formula_weight 805.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source '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' 'Na' 'Na' 0.0362 0.0249 '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' 'As' 'As' 0.0499 2.0058 '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' 'K' 'K' 0.2009 0.2494 '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' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-y, -z, x' 'y, x, z' '-y, -x, z' 'y, -x, -z' '-y, x, -z' 'x, z, y' '-x, z, -y' '-x, -z, y' 'x, -z, -y' 'z, y, x' 'z, -y, -x' '-z, y, -x' '-z, -y, x' _cell_length_a 7.928(9) _cell_length_b 7.928(9) _cell_length_c 7.928(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 498.3(9) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.685 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 386 _exptl_absorpt_coefficient_mu 8.115 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2312 _diffrn_reflns_av_R_equivalents 0.1501 _diffrn_reflns_av_sigmaI/netI 0.1268 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 32.92 _reflns_number_total 385 _reflns_number_gt 226 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.1233P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.13(13) _refine_ls_number_reflns 385 _refine_ls_number_parameters 23 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1401 _refine_ls_R_factor_gt 0.0683 _refine_ls_wR_factor_ref 0.1963 _refine_ls_wR_factor_gt 0.1643 _refine_ls_goodness_of_fit_ref 0.945 _refine_ls_restrained_S_all 0.944 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group As1 As 0.5000 0.0000 0.0000 0.0201(7) Uani 1 8 d S . . Fe1 Fe 0.1429(3) 0.1429(3) 0.1429(3) 0.0229(8) Uani 1 6 d S . . O1 O 0.1261(9) 0.1261(9) 0.3826(12) 0.026(3) Uani 1 2 d S . . O2 O 0.8861(12) 0.8861(12) 0.8861(12) 0.018(4) Uani 1 6 d SD . . H2 H 0.8283(19) 0.8283(19) 0.8283(19) 0.021 Uiso 1 6 d SD . . Na Na 0.050(13) 0.5000 0.5000 0.023(17) Uiso 0.11 4 d SP . . Ba Ba 0.0000 0.5000 0.5000 0.029(13) Uiso 0.03 8 d SP . . K K 0.0000 0.5000 0.5000 0.029(13) Uiso 0.04 8 d SP . . O4 O 0.692(3) 0.692(3) 0.692(3) 0.041(9) Uiso 0.50 6 d SP . . O3 O 0.130(9) 0.5000 0.5000 0.037(14) Uiso 0.25 4 d SP . . 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 As1 0.0163(12) 0.0220(9) 0.0220(9) 0.000 0.000 0.000 Fe1 0.0229(8) 0.0229(8) 0.0229(8) -0.0001(9) -0.0001(9) -0.0001(9) O1 0.029(3) 0.029(3) 0.019(5) 0.002(3) 0.002(3) -0.010(4) O2 0.018(4) 0.018(4) 0.018(4) 0.001(3) 0.001(3) 0.001(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 As1 O1 1.692(11) 6 ? As1 O1 1.692(11) 5 ? As1 O1 1.692(11) 8_655 ? As1 O1 1.692(11) 7_655 ? As1 K 3.964(4) 9 ? As1 K 3.964(4) 5_554 ? As1 K 3.964(4) 5 ? As1 K 3.964(4) 9_545 ? Fe1 O1 1.910(10) 9 ? Fe1 O1 1.910(10) . ? Fe1 O1 1.910(10) 5 ? Fe1 O2 2.061(8) 4_466 ? Fe1 O2 2.061(8) 2_664 ? Fe1 O2 2.061(8) 3_646 ? O1 As1 1.692(11) 9 ? O1 Na 3.17(2) . ? O1 Ba 3.264(6) . ? O1 Ba 3.264(6) 5 ? O1 K 3.264(6) 5 ? O2 Fe1 2.061(8) 3_666 ? O2 Fe1 2.061(8) 2_666 ? O2 Fe1 2.061(8) 4_666 ? O2 O4 2.67(4) . ? O2 H2 0.79(2) . ? Na O3 0.64(10) . ? Na Na 0.8(2) 2_565 ? Na O3 1.43(15) 2_565 ? Na O4 2.97(7) 2_665 ? Na O4 2.97(7) 3_656 ? Na O4 5.52(10) 4_566 ? Na O2 7.92(9) ? ? Ba Na 0.40(10) 2_565 ? Ba O3 1.03(7) . ? Ba O3 1.03(7) 2_565 ? Ba O4 3.255(6) 4_466 ? Ba O4 3.255(6) 3_656 ? Ba O4 3.255(6) 2_665 ? Ba O4 3.255(6) 1_455 ? Ba O1 3.264(6) 4_566 ? Ba O1 3.264(6) 11_566 ? Ba O1 3.264(6) 3_556 ? Ba O1 3.264(6) 12_565 ? O4 Na 2.97(7) 10_656 ? O4 Na 2.97(7) 6_566 ? O4 Na 2.97(7) 2_665 ? O4 O1 3.191(11) 2_665 ? O4 Ba 3.255(6) 1_655 ? O4 Ba 3.255(6) 9_556 ? O4 K 3.255(6) 1_655 ? O4 K 3.255(6) 5_565 ? O4 K 3.255(6) 9_556 ? O4 Ba 3.255(6) 5_565 ? O4 O3 4.94(7) . ? O3 Na 1.43(15) 2_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 O1 As1 O1 113.3(6) 6 5 ? O1 As1 O1 107.6(3) 6 8_655 ? O1 As1 O1 107.6(3) 5 8_655 ? O1 As1 O1 107.6(3) 6 7_655 ? O1 As1 O1 107.6(3) 5 7_655 ? O1 As1 O1 113.3(6) 8_655 7_655 ? O1 As1 K 126.19(15) 6 9 ? O1 As1 K 53.81(15) 5 9 ? O1 As1 K 53.81(15) 8_655 9 ? O1 As1 K 126.19(15) 7_655 9 ? O1 As1 K 53.81(15) 6 5_554 ? O1 As1 K 126.19(15) 5 5_554 ? O1 As1 K 53.81(15) 8_655 5_554 ? O1 As1 K 126.19(15) 7_655 5_554 ? K As1 K 90.0 9 5_554 ? O1 As1 K 126.19(15) 6 5 ? O1 As1 K 53.81(15) 5 5 ? O1 As1 K 126.19(15) 8_655 5 ? O1 As1 K 53.81(15) 7_655 5 ? K As1 K 90.0 9 5 ? K As1 K 180.0 5_554 5 ? O1 As1 K 53.81(15) 6 9_545 ? O1 As1 K 126.19(15) 5 9_545 ? O1 As1 K 126.19(15) 8_655 9_545 ? O1 As1 K 53.81(15) 7_655 9_545 ? K As1 K 180.0 9 9_545 ? K As1 K 90.0 5_554 9_545 ? K As1 K 90.0 5 9_545 ? O1 Fe1 O1 97.7(4) 9 . ? O1 Fe1 O1 97.7(4) 9 5 ? O1 Fe1 O1 97.7(4) . 5 ? O1 Fe1 O2 92.0(4) 9 4_466 ? O1 Fe1 O2 92.0(4) . 4_466 ? O1 Fe1 O2 165.3(5) 5 4_466 ? O1 Fe1 O2 92.0(4) 9 2_664 ? O1 Fe1 O2 165.3(5) . 2_664 ? O1 Fe1 O2 92.0(4) 5 2_664 ? O2 Fe1 O2 76.6(6) 4_466 2_664 ? O1 Fe1 O2 165.3(5) 9 3_646 ? O1 Fe1 O2 92.0(4) . 3_646 ? O1 Fe1 O2 92.0(4) 5 3_646 ? O2 Fe1 O2 76.6(6) 4_466 3_646 ? O2 Fe1 O2 76.6(6) 2_664 3_646 ? As1 O1 Fe1 129.0(6) 9 . ? As1 O1 Na 106.2(13) 9 . ? Fe1 O1 Na 103.9(3) . . ? As1 O1 Ba 101.5(2) 9 . ? Fe1 O1 Ba 104.0(2) . . ? Na O1 Ba 6.8(18) . . ? As1 O1 Ba 101.5(2) 9 5 ? Fe1 O1 Ba 104.0(2) . 5 ? Na O1 Ba 112.1(17) . 5 ? Ba O1 Ba 118.3(3) . 5 ? As1 O1 K 101.5(2) 9 5 ? Fe1 O1 K 104.0(2) . 5 ? Na O1 K 112.1(17) . 5 ? Ba O1 K 118.3(3) . 5 ? Ba O1 K 0.0 5 5 ? Fe1 O2 Fe1 102.0(5) 3_666 2_666 ? Fe1 O2 Fe1 102.0(5) 3_666 4_666 ? Fe1 O2 Fe1 102.0(5) 2_666 4_666 ? Fe1 O2 O4 116.2(4) 3_666 . ? Fe1 O2 O4 116.2(4) 2_666 . ? Fe1 O2 O4 116.2(4) 4_666 . ? Fe1 O2 H2 116.2(4) 3_666 . ? Fe1 O2 H2 116.2(4) 2_666 . ? Fe1 O2 H2 116.2(4) 4_666 . ? O4 O2 H2 0.0(10) . . ? O3 Na Na 180.00(3) . 2_565 ? O3 Na O3 180.000(5) . 2_565 ? Na Na O3 0.000(12) 2_565 2_565 ? O3 Na O4 46.3(16) . 2_665 ? Na Na O4 133.7(16) 2_565 2_665 ? O3 Na O4 133.7(16) 2_565 2_665 ? O3 Na O4 46.3(16) . 3_656 ? Na Na O4 133.7(16) 2_565 3_656 ? O3 Na O4 133.7(16) 2_565 3_656 ? O4 Na O4 93(3) 2_665 3_656 ? O3 Na O1 79.0(18) . . ? Na Na O1 101.0(19) 2_565 . ? O3 Na O1 101.0(18) 2_565 . ? O4 Na O1 62.6(10) 2_665 . ? O4 Na O1 101(2) 3_656 . ? O3 Na O4 22.9(5) . 4_566 ? Na Na O4 157.1(5) 2_565 4_566 ? O3 Na O4 157.1(5) 2_565 4_566 ? O4 Na O4 50.5(16) 2_665 4_566 ? O4 Na O4 50.5(16) 3_656 4_566 ? O1 Na O4 59.1(15) . 4_566 ? O3 Na O2 33.1(4) . ? ? Na Na O2 146.9(4) 2_565 ? ? O3 Na O2 146.9(4) 2_565 ? ? O4 Na O2 13.2(13) 2_665 ? ? O4 Na O2 79(2) 3_656 ? ? O1 Na O2 65.9(14) . ? ? O4 Na O2 39.5(5) 4_566 ? ? Na Ba O3 180.00(3) 2_565 . ? Na Ba O3 0.00(2) 2_565 2_565 ? O3 Ba O3 180.000(7) . 2_565 ? Na Ba O4 41.3(8) 2_565 4_466 ? O3 Ba O4 138.7(7) . 4_466 ? O3 Ba O4 41.3(8) 2_565 4_466 ? Na Ba O4 138.7(8) 2_565 3_656 ? O3 Ba O4 41.3(8) . 3_656 ? O3 Ba O4 138.7(7) 2_565 3_656 ? O4 Ba O4 124.4(9) 4_466 3_656 ? Na Ba O4 138.7(8) 2_565 2_665 ? O3 Ba O4 41.3(7) . 2_665 ? O3 Ba O4 138.7(8) 2_565 2_665 ? O4 Ba O4 124.4(9) 4_466 2_665 ? O4 Ba O4 82.6(15) 3_656 2_665 ? Na Ba O4 41.3(8) 2_565 1_455 ? O3 Ba O4 138.7(8) . 1_455 ? O3 Ba O4 41.3(7) 2_565 1_455 ? O4 Ba O4 82.6(15) 4_466 1_455 ? O4 Ba O4 124.4(9) 3_656 1_455 ? O4 Ba O4 124.4(9) 2_665 1_455 ? Na Ba O1 107.83(16) 2_565 4_566 ? O3 Ba O1 72.17(16) . 4_566 ? O3 Ba O1 107.83(16) 2_565 4_566 ? O4 Ba O1 141.9(6) 4_466 4_566 ? O4 Ba O1 58.6(2) 3_656 4_566 ? O4 Ba O1 93.5(4) 2_665 4_566 ? O4 Ba O1 70.9(6) 1_455 4_566 ? Na Ba O1 107.83(16) 2_565 11_566 ? O3 Ba O1 72.17(16) . 11_566 ? O3 Ba O1 107.83(16) 2_565 11_566 ? O4 Ba O1 141.9(6) 4_466 11_566 ? O4 Ba O1 93.5(4) 3_656 11_566 ? O4 Ba O1 58.6(2) 2_665 11_566 ? O4 Ba O1 70.9(6) 1_455 11_566 ? O1 Ba O1 52.3(3) 4_566 11_566 ? Na Ba O1 72.17(17) 2_565 3_556 ? O3 Ba O1 107.83(16) . 3_556 ? O3 Ba O1 72.17(16) 2_565 3_556 ? O4 Ba O1 58.6(2) 4_466 3_556 ? O4 Ba O1 141.9(6) 3_656 3_556 ? O4 Ba O1 70.9(6) 2_665 3_556 ? O4 Ba O1 93.5(4) 1_455 3_556 ? O1 Ba O1 146.9(3) 4_566 3_556 ? O1 Ba O1 95.38(9) 11_566 3_556 ? Na Ba O1 72.17(16) 2_565 12_565 ? O3 Ba O1 107.83(16) . 12_565 ? O3 Ba O1 72.17(16) 2_565 12_565 ? O4 Ba O1 58.6(2) 4_466 12_565 ? O4 Ba O1 70.9(6) 3_656 12_565 ? O4 Ba O1 141.9(6) 2_665 12_565 ? O4 Ba O1 93.5(4) 1_455 12_565 ? O1 Ba O1 95.38(9) 4_566 12_565 ? O1 Ba O1 146.9(3) 11_566 12_565 ? O1 Ba O1 115.1(3) 3_556 12_565 ? Na Ba O1 107.83(17) 2_565 . ? O3 Ba O1 72.17(16) . . ? O3 Ba O1 107.83(16) 2_565 . ? O4 Ba O1 70.9(6) 4_466 . ? O4 Ba O1 93.5(4) 3_656 . ? O4 Ba O1 58.6(2) 2_665 . ? O4 Ba O1 141.9(6) 1_455 . ? O1 Ba O1 144.3(3) 4_566 . ? O1 Ba O1 115.1(3) 11_566 . ? O1 Ba O1 49.5(4) 3_556 . ? O1 Ba O1 95.38(9) 12_565 . ? O2 O4 Na 101.1(16) . 10_656 ? O2 O4 Na 101.1(16) . 6_566 ? Na O4 Na 116.4(10) 10_656 6_566 ? O2 O4 Na 101.1(16) . 2_665 ? Na O4 Na 116.4(10) 10_656 2_665 ? Na O4 Na 116.4(10) 6_566 2_665 ? O2 O4 O1 85.4(8) . 2_665 ? Na O4 O1 174(2) 10_656 2_665 ? Na O4 O1 61.7(3) 6_566 2_665 ? Na O4 O1 61.7(3) 2_665 2_665 ? O2 O4 Ba 96.0(7) . 1_655 ? Na O4 Ba 117.9(5) 10_656 1_655 ? Na O4 Ba 117.9(5) 6_566 1_655 ? Na O4 Ba 5.0(14) 2_665 1_655 ? O1 O4 Ba 60.84(4) 2_665 1_655 ? O2 O4 Ba 96.0(7) . 9_556 ? Na O4 Ba 5.0(14) 10_656 9_556 ? Na O4 Ba 117.9(5) 6_566 9_556 ? Na O4 Ba 117.9(5) 2_665 9_556 ? O1 O4 Ba 178.6(16) 2_665 9_556 ? Ba O4 Ba 118.9(3) 1_655 9_556 ? O2 O4 K 96.0(7) . 1_655 ? Na O4 K 117.9(5) 10_656 1_655 ? Na O4 K 117.9(5) 6_566 1_655 ? Na O4 K 5.0(14) 2_665 1_655 ? O1 O4 K 60.84(4) 2_665 1_655 ? Ba O4 K 0.0 1_655 1_655 ? Ba O4 K 118.9(3) 9_556 1_655 ? O2 O4 K 96.0(7) . 5_565 ? Na O4 K 117.9(5) 10_656 5_565 ? Na O4 K 5.0(14) 6_566 5_565 ? Na O4 K 117.9(5) 2_665 5_565 ? O1 O4 K 60.84(4) 2_665 5_565 ? Ba O4 K 118.9(3) 1_655 5_565 ? Ba O4 K 118.9(3) 9_556 5_565 ? K O4 K 118.9(3) 1_655 5_565 ? O2 O4 K 96.0(7) . 9_556 ? Na O4 K 5.0(14) 10_656 9_556 ? Na O4 K 117.9(5) 6_566 9_556 ? Na O4 K 117.9(5) 2_665 9_556 ? O1 O4 K 178.6(16) 2_665 9_556 ? Ba O4 K 118.9(3) 1_655 9_556 ? Ba O4 K 0.0 9_556 9_556 ? K O4 K 118.9(3) 1_655 9_556 ? K O4 K 118.9(3) 5_565 9_556 ? O2 O4 Ba 96.0(7) . 5_565 ? Na O4 Ba 117.9(5) 10_656 5_565 ? Na O4 Ba 5.0(14) 6_566 5_565 ? Na O4 Ba 117.9(5) 2_665 5_565 ? O1 O4 Ba 60.84(4) 2_665 5_565 ? Ba O4 Ba 118.9(3) 1_655 5_565 ? Ba O4 Ba 118.9(3) 9_556 5_565 ? K O4 Ba 118.9(3) 1_655 5_565 ? K O4 Ba 0.0 5_565 5_565 ? K O4 Ba 118.9(3) 9_556 5_565 ? O2 O4 O3 151.0(4) . . ? Na O4 O3 66.1(14) 10_656 . ? Na O4 O3 66.1(14) 6_566 . ? Na O4 O3 107.9(19) 2_665 . ? O1 O4 O3 108.2(8) 2_665 . ? Ba O4 O3 113.0(11) 1_655 . ? Ba O4 O3 70.6(6) 9_556 . ? K O4 O3 113.0(11) 1_655 . ? K O4 O3 70.6(6) 5_565 . ? K O4 O3 70.6(6) 9_556 . ? Ba O4 O3 70.6(6) 5_565 . ? Na O3 Ba 0.000(16) . . ? Na O3 Na 0.00(2) . 2_565 ? Ba O3 Na 0.000(3) . 2_565 ? Na O3 O4 154.2(4) . . ? Ba O3 O4 154.2(4) . . ? Na O3 O4 154.2(4) 2_565 . ? 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 O2 H2 O4 0.79(2) 1.88(5) 2.67(4) 180(4) . _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 32.92 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 1.562 _refine_diff_density_min -0.813 _refine_diff_density_rms 0.322