data_pyracmonite _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Al0.11 Fe0.89 H10.44 K0.39 N2.61 O12 S3' _chemical_formula_weight 403.22 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Fe' 'Fe' 0.3463 0.8444 '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' 'S' 'S' 0.1246 0.1234 '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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 '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 trigonal _symmetry_space_group_name_H-M R3c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-y, -x, z+1/2' '-x+y, y, z+1/2' 'x, x-y, z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' '-y+2/3, -x+1/3, z+5/6' '-x+y+2/3, y+1/3, z+5/6' 'x+2/3, x-y+1/3, z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-y+1/3, -x+2/3, z+7/6' '-x+y+1/3, y+2/3, z+7/6' 'x+1/3, x-y+2/3, z+7/6' _cell_length_a 15.2171(14) _cell_length_b 15.2171(14) _cell_length_c 8.9323(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1791.3(3) _cell_formula_units_Z 6 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 2730 _cell_measurement_theta_min 2.68 _cell_measurement_theta_max 28.87 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas 2.22 _exptl_crystal_density_diffrn 2.243 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1227.1 _exptl_absorpt_coefficient_mu 1.871 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.84 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(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 'Bruker APEX II CCD diffractometer' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5148 _diffrn_reflns_av_R_equivalents 0.0290 _diffrn_reflns_av_sigmaI/netI 0.0273 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.68 _diffrn_reflns_theta_max 29.61 _reflns_number_total 1064 _reflns_number_gt 1010 _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^)+(0.0572P)^2^+6.9446P] 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 refall _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 0.06(4) _refine_ls_number_reflns 1064 _refine_ls_number_parameters 76 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0415 _refine_ls_R_factor_gt 0.0394 _refine_ls_wR_factor_ref 0.1010 _refine_ls_wR_factor_gt 0.1001 _refine_ls_goodness_of_fit_ref 1.103 _refine_ls_restrained_S_all 1.102 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.003 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 0.0000 0.0000 0.13800(4) 0.01631(6) Uani 0.89 3 d SP . . Al Al 0.0000 0.0000 0.13800(4) 0.01631(6) Uani 0.11 3 d SP . . S S 0.169129(19) 0.142909(19) 0.38360(3) 0.02027(7) Uani 1 1 d . . . O1 O 0.11980(10) 0.09339(12) 0.52147(11) 0.0585(5) Uani 1 1 d . . . O2 O 0.09084(8) 0.11849(7) 0.26675(11) 0.0299(3) Uani 1 1 d . . . O3 O 0.22180(11) 0.25160(10) 0.40719(19) 0.0693(6) Uani 1 1 d . . . O4 O 0.23838(9) 0.11279(12) 0.33386(19) 0.0730(4) Uani 1 1 d . . . N N 0.07773(6) 0.30174(6) 0.24189(11) 0.0322(2) Uani 0.87 1 d P . . K K 0.07773(6) 0.30174(6) 0.24189(11) 0.0322(2) Uani 0.13 1 d P . . H1 H 0.0312(17) 0.3069(19) 0.264(3) 0.059(7) Uiso 0.87 1 d P . . H2 H 0.1126(14) 0.3421(16) 0.169(3) 0.047(7) Uiso 0.87 1 d P . . H3 H 0.066(2) 0.244(2) 0.207(4) 0.077(9) Uiso 0.87 1 d P . . H4 H 0.1122(19) 0.332(2) 0.323(4) 0.091(10) Uiso 0.87 1 d P . . 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 0.01909(7) 0.01909(7) 0.01075(10) 0.000 0.000 0.00954(4) Al 0.01909(7) 0.01909(7) 0.01075(10) 0.000 0.000 0.00954(4) S 0.01528(9) 0.02044(10) 0.01894(11) -0.00215(11) 0.00059(10) 0.00431(7) O1 0.0390(6) 0.0803(8) 0.0184(5) 0.0180(5) 0.0043(5) 0.0013(6) O2 0.0384(4) 0.0252(4) 0.0216(4) -0.0034(3) -0.0095(4) 0.0126(3) O3 0.0732(9) 0.0238(5) 0.0685(8) -0.0016(6) -0.0324(8) -0.0075(6) O4 0.0513(4) 0.1238(7) 0.0721(8) -0.0514(6) -0.0266(5) 0.0650(3) N 0.0315(3) 0.0324(3) 0.0330(4) 0.0048(3) -0.0011(3) 0.0163(2) K 0.0315(3) 0.0324(3) 0.0330(4) 0.0048(3) -0.0011(3) 0.0163(2) _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 1.9585(12) 4_554 ? Fe O1 1.9585(12) 5_554 ? Fe O1 1.9585(12) 6_554 ? Fe O2 1.9980(9) . ? Fe O2 1.9980(9) 2 ? Fe O2 1.9980(9) 3 ? S O4 1.4145(18) . ? S O1 1.4430(11) . ? S O3 1.4480(13) . ? S O2 1.4846(11) . ? S K 3.6865(9) 8 ? S K 3.7809(10) 10_554 ? O1 Al 1.9585(12) 4 ? O1 Fe 1.9585(12) 4 ? O1 K 3.3787(17) 5 ? O3 K 2.8938(16) 18_554 ? O3 K 3.082(2) 5 ? O4 K 2.9088(19) 8 ? O4 K 2.914(2) 3 ? O4 K 3.0957(18) 10_554 ? 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 94.38(4) 4_554 5_554 ? O1 Fe O1 94.38(4) 4_554 6_554 ? O1 Fe O1 94.38(4) 5_554 6_554 ? O1 Fe O2 176.90(5) 4_554 . ? O1 Fe O2 87.22(6) 5_554 . ? O1 Fe O2 88.15(6) 6_554 . ? O1 Fe O2 87.22(6) 4_554 2 ? O1 Fe O2 88.15(6) 5_554 2 ? O1 Fe O2 176.90(5) 6_554 2 ? O2 Fe O2 90.17(4) . 2 ? O1 Fe O2 88.15(6) 4_554 3 ? O1 Fe O2 176.90(5) 5_554 3 ? O1 Fe O2 87.22(6) 6_554 3 ? O2 Fe O2 90.17(4) . 3 ? O2 Fe O2 90.17(4) 2 3 ? O4 S O1 112.10(11) . . ? O4 S O3 109.83(9) . . ? O1 S O3 108.58(9) . . ? O4 S O2 109.43(8) . . ? O1 S O2 109.05(7) . . ? O3 S O2 107.74(8) . . ? O4 S K 46.87(7) . 8 ? O1 S K 77.10(7) . 8 ? O3 S K 93.82(8) . 8 ? O2 S K 153.48(5) . 8 ? O4 S K 51.12(7) . 10_554 ? O1 S K 160.87(8) . 10_554 ? O3 S K 74.18(7) . 10_554 ? O2 S K 87.31(4) . 10_554 ? K S K 83.85(2) 8 10_554 ? S O1 Al 152.24(8) . 4 ? S O1 Fe 152.24(8) . 4 ? Al O1 Fe 0.0 4 4 ? S O1 K 97.46(7) . 5 ? Al O1 K 101.60(5) 4 5 ? Fe O1 K 101.60(5) 4 5 ? S O2 Fe 137.47(8) . . ? S O3 K 148.49(11) . 18_554 ? S O3 K 110.81(8) . 5 ? K O3 K 82.24(4) 18_554 5 ? S O4 K 112.35(9) . 8 ? S O4 K 135.51(7) . 3 ? K O4 K 84.95(6) 8 3 ? S O4 K 108.04(9) . 10_554 ? K O4 K 112.38(5) 8 10_554 ? K O4 K 101.47(6) 3 10_554 ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 29.61 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 1.019 _refine_diff_density_min -0.607 _refine_diff_density_rms 0.109