Crystal Structure of Pharmacosiderite (Buerger) data_pharm _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common pharmacosiderite _chemical_melting_point ? _chemical_formula_moiety '(H3O)Fe4(AsO4)3(OH)4.4H2O' _chemical_formula_sum 'H15 As3 Fe4 O21' _chemical_formula_weight 799.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Fe' 'Fe' -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'As' 'As' -0.9300 1.0051 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 '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 Cubic _symmetry_space_group_name_H-M P-43m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'z, x, y' 'y, z, x' 'x, z, y' 'y, x, z' 'z, y, x' 'x, -y, -z' 'z, -x, -y' 'y, -z, -x' 'x, -z, -y' 'y, -x, -z' 'z, -y, -x' '-x, y, -z' '-z, x, -y' '-y, z, -x' '-x, z, -y' '-y, x, -z' '-z, y, -x' '-x, -y, z' '-z, -x, y' '-y, -z, x' '-x, -z, y' '-y, -x, z' '-z, -y, x' _cell_length_a 7.980(10) _cell_length_b 7.980(10) _cell_length_c 7.980(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 508.2(11) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description cubic _exptl_crystal_colour pale green _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.612 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 386 _exptl_absorpt_coefficient_mu 28.782 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'equi-inclination diffractometer' _diffrn_measurement_method 'equi-inclination' _diffrn_detector_area_resol_mean 'proportional counter (Ar)' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 128 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0004 _diffrn_reflns_limit_h_min 1 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_theta_min 7.85 _diffrn_reflns_theta_max 69.49 _reflns_number_total 128 _reflns_number_gt 128 _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^)+(0.0710P)^2^+7.5426P] 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 SHELXL _refine_ls_extinction_coef 0.004(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(5) _refine_ls_number_reflns 128 _refine_ls_number_parameters 16 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0539 _refine_ls_R_factor_gt 0.0539 _refine_ls_wR_factor_ref 0.1482 _refine_ls_wR_factor_gt 0.1482 _refine_ls_goodness_of_fit_ref 1.307 _refine_ls_restrained_S_all 1.307 _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 Fe Fe 0.1429(3) 0.1429(3) 0.1429(3) 0.0150(14) Uani 1 6 d S . . As As 0.5000 0.0000 0.0000 0.0233(13) Uani 1 8 d S . . O1 O 0.1230(12) 0.1230(12) 0.3829(16) 0.025(3) Uiso 1 2 d S . . O2 O 0.8868(14) 0.8868(14) 0.8868(14) 0.013(4) Uiso 1 6 d S . . O3 O 0.5000 0.069(6) 0.5000 0.057(12) Uiso 0.50 4 d SP . . O4 O 0.694(4) 0.694(4) 0.694(4) 0.048(14) Uiso 0.50 6 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 Fe 0.0150(14) 0.0150(14) 0.0150(14) -0.0017(10) -0.0017(10) -0.0017(10) As 0.0124(19) 0.0287(16) 0.0287(16) 0.000 0.000 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 Fe O1 1.928(14) 3 ? Fe O1 1.928(14) 2 ? Fe O1 1.928(14) . ? Fe O2 2.071(9) 19_664 ? Fe O2 2.071(9) 7_466 ? Fe O2 2.071(9) 13_646 ? As O1 1.673(14) 8 ? As O1 1.673(14) 20_655 ? As O1 1.673(14) 14_655 ? As O1 1.673(14) 2 ? O1 As 1.673(14) 3 ? O1 O3 3.180(11) . ? O2 Fe 2.071(9) 7_666 ? O2 Fe 2.071(9) 19_666 ? O2 Fe 2.071(9) 13_666 ? O2 O4 2.67(6) . ? O3 O3 1.10(9) 7_556 ? O4 O3 2.89(3) 8_566 ? O4 O1 3.230(15) 19_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 Fe O1 99.0(5) 3 2 ? O1 Fe O1 99.0(5) 3 . ? O1 Fe O1 99.0(5) 2 . ? O1 Fe O2 91.3(5) 3 19_664 ? O1 Fe O2 91.3(5) 2 19_664 ? O1 Fe O2 164.0(6) . 19_664 ? O1 Fe O2 91.3(5) 3 7_466 ? O1 Fe O2 164.0(6) 2 7_466 ? O1 Fe O2 91.3(5) . 7_466 ? O2 Fe O2 76.2(7) 19_664 7_466 ? O1 Fe O2 164.0(6) 3 13_646 ? O1 Fe O2 91.3(5) 2 13_646 ? O1 Fe O2 91.3(5) . 13_646 ? O2 Fe O2 76.2(7) 19_664 13_646 ? O2 Fe O2 76.2(7) 7_466 13_646 ? O1 As O1 108.2(4) 8 20_655 ? O1 As O1 108.2(4) 8 14_655 ? O1 As O1 112.1(9) 20_655 14_655 ? O1 As O1 112.1(9) 8 2 ? O1 As O1 108.2(4) 20_655 2 ? O1 As O1 108.2(4) 14_655 2 ? As O1 Fe 130.6(8) 3 . ? As O1 O3 108.1(7) 3 . ? Fe O1 O3 103.0(4) . . ? Fe O2 Fe 102.3(6) 7_666 19_666 ? Fe O2 Fe 102.3(6) 7_666 13_666 ? Fe O2 Fe 102.3(6) 19_666 13_666 ? Fe O2 O4 116.0(5) 7_666 . ? Fe O2 O4 116.0(5) 19_666 . ? Fe O2 O4 116.0(5) 13_666 . ? O3 O3 O1 97.8(9) 7_556 . ? O2 O4 O3 103.8(14) . 8_566 ? O2 O4 O1 85.5(11) . 19_665 ? O3 O4 O1 171(2) 8_566 19_665 ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 69.49 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 1.337 _refine_diff_density_min -0.691 _refine_diff_density_rms 0.223