data_vulc1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'coquimbite vulcano' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Al0.17 Fe0.50 H6 O7 S' _chemical_formula_weight 182.53 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' 'Al' 'Al' 0.0645 0.0514 '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' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M P-31c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-y, -x, -z+1/2' 'x, x-y, -z+1/2' '-x+y, y, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'y, x, z-1/2' '-x, -x+y, z-1/2' 'x-y, -y, z-1/2' _cell_length_a 10.9100(7) _cell_length_b 10.9100(7) _cell_length_c 17.0625(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1758.8(2) _cell_formula_units_Z 12 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 6120 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 31.61 _exptl_crystal_description 'flattened prism' _exptl_crystal_colour violet _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.068 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1118 _exptl_absorpt_coefficient_mu 1.737 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.880 _exptl_absorpt_correction_T_max 1.000 _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 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 18097 _diffrn_reflns_av_R_equivalents 0.0414 _diffrn_reflns_av_sigmaI/netI 0.0250 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 31.76 _reflns_number_total 1939 _reflns_number_gt 1567 _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^)+(0.0532P)^2^+0.5490P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1939 _refine_ls_number_parameters 108 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0472 _refine_ls_R_factor_gt 0.0351 _refine_ls_wR_factor_ref 0.0924 _refine_ls_wR_factor_gt 0.0882 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.010 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 Al1 Al 0.0000 0.0000 0.0000 0.01276(13) Uani 1 6 d S . . Fe2 Fe 0.3333 0.6667 0.2500 0.01068(6) Uani 1 6 d S . . Fe3 Fe 0.6667 0.3333 0.002502(13) 0.01723(5) Uani 1 3 d S . . S1 S 0.244618(19) 0.414813(19) 0.122883(12) 0.01328(5) Uani 1 1 d . . . O1 O 0.31831(6) 0.34528(6) 0.09069(4) 0.02288(17) Uani 1 1 d . . . O2 O 0.10784(6) 0.31042(7) 0.15472(4) 0.02127(17) Uani 1 1 d . . . O3 O 0.21952(6) 0.49428(6) 0.06010(4) 0.02057(17) Uani 1 1 d . . . O4 O 0.33561(6) 0.51557(6) 0.18440(4) 0.01649(15) Uani 1 1 d . . . OW1 O 0.16433(6) 0.06986(6) 0.06158(4) 0.02104(16) Uani 1 1 d D . . OW2 O 0.44934(7) 0.11625(7) 0.20976(5) 0.0307(2) Uani 1 1 d D . . OW3 O 0.57197(7) 0.16249(7) 0.07096(4) 0.02909(19) Uani 1 1 d D . . H11 H 0.1828(7) 0.0143(5) 0.0866(5) 0.063(5) Uiso 1 1 d D . . H12 H 0.2182(13) 0.1551(5) 0.0749(7) 0.058(5) Uiso 1 1 d D . . H21 H 0.3721(7) 0.0379(7) 0.2081(8) 0.042(4) Uiso 1 1 d D . . H22A H 0.5170(5) 0.1125(9) 0.2319(7) 0.041(8) Uiso 0.50 1 d PD . . H22B H 0.4203(6) 0.1621(6) 0.2362(6) 0.090(14) Uiso 0.50 1 d PD . . H31 H 0.5964(5) 0.1003(5) 0.0732(8) 0.052(4) Uiso 1 1 d D . . H32 H 0.5298(9) 0.1448(16) 0.1145(3) 0.067(5) 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 Al1 0.01039(15) 0.01039(15) 0.0175(3) 0.000 0.000 0.00520(8) Fe2 0.00999(7) 0.00999(7) 0.01206(11) 0.000 0.000 0.00500(3) Fe3 0.01792(6) 0.01792(6) 0.01584(9) 0.000 0.000 0.00896(3) S1 0.01313(6) 0.01027(6) 0.01524(8) -0.00241(6) -0.00073(6) 0.00495(5) O1 0.0198(2) 0.0181(2) 0.0321(3) -0.0099(2) -0.0001(2) 0.01051(17) O2 0.0165(2) 0.0175(2) 0.0230(3) -0.0003(2) 0.0032(2) 0.00328(18) O3 0.0212(2) 0.0194(2) 0.0183(3) 0.0012(2) -0.0044(2) 0.00812(18) O4 0.0180(2) 0.0146(2) 0.0179(3) -0.0055(2) -0.0040(2) 0.00896(15) OW1 0.0198(2) 0.0141(2) 0.0280(3) -0.0016(2) -0.0084(2) 0.00756(16) OW2 0.0292(3) 0.0263(3) 0.0308(3) -0.0022(3) 0.0034(3) 0.0095(2) OW3 0.0386(3) 0.0275(2) 0.0276(3) 0.0100(2) 0.0136(3) 0.02129(19) _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 Al1 OW1 1.8796(6) . ? Al1 OW1 1.8796(6) 8 ? Al1 OW1 1.8796(6) 7 ? Al1 OW1 1.8796(6) 2 ? Al1 OW1 1.8796(6) 9 ? Al1 OW1 1.8796(6) 3 ? Fe2 O4 2.0029(7) 3_565 ? Fe2 O4 2.0029(7) 5_565 ? Fe2 O4 2.0029(7) 6 ? Fe2 O4 2.0029(7) 2_665 ? Fe2 O4 2.0029(7) . ? Fe2 O4 2.0029(7) 4_665 ? Fe3 O3 1.9710(6) 9_655 ? Fe3 O3 1.9710(6) 7_665 ? Fe3 O3 1.9710(6) 8 ? Fe3 OW3 1.9950(7) 2_655 ? Fe3 OW3 1.9950(7) . ? Fe3 OW3 1.9950(7) 3_665 ? S1 O2 1.4558(6) . ? S1 O1 1.4607(8) . ? S1 O4 1.4847(6) . ? S1 O3 1.4870(7) . ? O3 Fe3 1.9710(6) 7_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 OW1 Al1 OW1 88.21(3) . 8 ? OW1 Al1 OW1 180.00(4) . 7 ? OW1 Al1 OW1 91.79(3) 8 7 ? OW1 Al1 OW1 91.79(3) . 2 ? OW1 Al1 OW1 180.00(4) 8 2 ? OW1 Al1 OW1 88.21(3) 7 2 ? OW1 Al1 OW1 88.21(3) . 9 ? OW1 Al1 OW1 91.79(3) 8 9 ? OW1 Al1 OW1 91.79(3) 7 9 ? OW1 Al1 OW1 88.21(3) 2 9 ? OW1 Al1 OW1 91.79(3) . 3 ? OW1 Al1 OW1 88.21(3) 8 3 ? OW1 Al1 OW1 88.21(3) 7 3 ? OW1 Al1 OW1 91.79(3) 2 3 ? OW1 Al1 OW1 180.00(5) 9 3 ? O4 Fe2 O4 89.08(3) 3_565 5_565 ? O4 Fe2 O4 87.31(4) 3_565 6 ? O4 Fe2 O4 91.81(3) 5_565 6 ? O4 Fe2 O4 91.81(3) 3_565 2_665 ? O4 Fe2 O4 87.31(4) 5_565 2_665 ? O4 Fe2 O4 178.77(3) 6 2_665 ? O4 Fe2 O4 91.81(3) 3_565 . ? O4 Fe2 O4 178.77(3) 5_565 . ? O4 Fe2 O4 89.08(3) 6 . ? O4 Fe2 O4 91.81(3) 2_665 . ? O4 Fe2 O4 178.77(3) 3_565 4_665 ? O4 Fe2 O4 91.81(3) 5_565 4_665 ? O4 Fe2 O4 91.81(3) 6 4_665 ? O4 Fe2 O4 89.08(3) 2_665 4_665 ? O4 Fe2 O4 87.31(4) . 4_665 ? O3 Fe3 O3 93.41(3) 9_655 7_665 ? O3 Fe3 O3 93.41(3) 9_655 8 ? O3 Fe3 O3 93.41(3) 7_665 8 ? O3 Fe3 OW3 92.86(3) 9_655 2_655 ? O3 Fe3 OW3 84.74(3) 7_665 2_655 ? O3 Fe3 OW3 173.56(3) 8 2_655 ? O3 Fe3 OW3 84.74(3) 9_655 . ? O3 Fe3 OW3 173.56(3) 7_665 . ? O3 Fe3 OW3 92.86(3) 8 . ? OW3 Fe3 OW3 89.19(3) 2_655 . ? O3 Fe3 OW3 173.56(3) 9_655 3_665 ? O3 Fe3 OW3 92.86(3) 7_665 3_665 ? O3 Fe3 OW3 84.74(3) 8 3_665 ? OW3 Fe3 OW3 89.19(3) 2_655 3_665 ? OW3 Fe3 OW3 89.19(3) . 3_665 ? O2 S1 O1 110.43(4) . . ? O2 S1 O4 111.08(4) . . ? O1 S1 O4 108.21(4) . . ? O2 S1 O3 108.02(4) . . ? O1 S1 O3 109.97(4) . . ? O4 S1 O3 109.12(4) . . ? S1 O3 Fe3 137.30(4) . 7_665 ? S1 O4 Fe2 136.52(4) . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 31.76 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 0.698 _refine_diff_density_min -0.781 _refine_diff_density_rms 0.100