data_Chile
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             'coquimbite Chile'
_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                    10.9370(4)
_cell_length_b                    10.9370(4)
_cell_length_c                    17.0813(7)
_cell_angle_alpha                 90.00
_cell_angle_beta                  90.00
_cell_angle_gamma                 120.00
_cell_volume                      1769.49(12)
_cell_formula_units_Z             12
_cell_measurement_temperature     294(2)
_cell_measurement_reflns_used     9823
_cell_measurement_theta_min       2.38
_cell_measurement_theta_max       31.20
_exptl_crystal_description        'flattened prism'
_exptl_crystal_colour             'pale violet'
_exptl_crystal_size_max           0.25
_exptl_crystal_size_mid           0.20
_exptl_crystal_size_min           0.18
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     2.055
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1118
_exptl_absorpt_coefficient_mu     1.727
_exptl_absorpt_correction_type    empirical
_exptl_absorpt_correction_T_min   0.785
_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             17829
_diffrn_reflns_av_R_equivalents   0.0307
_diffrn_reflns_av_sigmaI/netI     0.0152
_diffrn_reflns_limit_h_min        -15
_diffrn_reflns_limit_h_max        15
_diffrn_reflns_limit_k_min        -15
_diffrn_reflns_limit_k_max        15
_diffrn_reflns_limit_l_min        -24
_diffrn_reflns_limit_l_max        24
_diffrn_reflns_theta_min          2.15
_diffrn_reflns_theta_max          31.48
_reflns_number_total              1917
_reflns_number_gt                 1717
_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^)+(0.0439P)^2^+0.6146P] 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          1917
_refine_ls_number_parameters      109
_refine_ls_number_restraints      7
_refine_ls_R_factor_all           0.0252
_refine_ls_R_factor_gt            0.0220
_refine_ls_wR_factor_ref          0.0746
_refine_ls_wR_factor_gt           0.0734
_refine_ls_goodness_of_fit_ref    1.081
_refine_ls_restrained_S_all       1.081
_refine_ls_shift/su_max           0.029
_refine_ls_shift/su_mean          0.015
 
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 0.01350(7) Uani 0.7608(13) 6 d SP . .
Fe1 Fe 0.0000 0.0000 0.0000 0.01350(7) Uani 0.2392(13) 6 d SP . .
Fe2 Fe 0.3333 0.6667 0.2500 0.01147(4) Uani 1 6 d S . .
Fe3 Fe 0.6667 0.3333 0.002498(9) 0.01703(3) Uani 1 3 d S . .
S1 S 0.244809(13) 0.415175(13) 0.123067(8) 0.01412(3) Uani 1 1 d . . .
O1 O 0.31847(5) 0.34563(4) 0.09110(3) 0.02376(12) Uani 1 1 d . . .
O2 O 0.10858(5) 0.31136(5) 0.15507(3) 0.02223(12) Uani 1 1 d . . .
O3 O 0.21976(4) 0.49418(4) 0.06020(3) 0.02146(11) Uani 1 1 d . . .
O4 O 0.33579(4) 0.51624(4) 0.18451(3) 0.01732(10) Uani 1 1 d . . .
OW1 O 0.16668(4) 0.07066(4) 0.06225(3) 0.02367(12) Uani 1 1 d D . .
OW2 O 0.44922(5) 0.11635(5) 0.20994(3) 0.03175(15) Uani 1 1 d D . .
OW3 O 0.57200(5) 0.16221(5) 0.07123(3) 0.02949(13) Uani 1 1 d D . .
H11 H 0.1851(7) 0.0205(6) 0.0924(5) 0.085(5) Uiso 1 1 d D . .
H12 H 0.2264(11) 0.1545(6) 0.0760(6) 0.073(4) Uiso 1 1 d D . .
H21 H 0.3722(6) 0.0384(6) 0.2091(7) 0.040(3) Uiso 1 1 d D . .
H22A H 0.5068(5) 0.1020(8) 0.2363(6) 0.044(6) Uiso 0.50 1 d PD . .
H22B H 0.4342(7) 0.1729(5) 0.2362(5) 0.034(5) Uiso 0.50 1 d PD . .
H31 H 0.5930(5) 0.0987(4) 0.0751(7) 0.060(4) Uiso 1 1 d D . .
H32 H 0.5317(7) 0.1528(10) 0.1142(3) 0.041(3) 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 0.01171(9) 0.01171(9) 0.01707(15) 0.000 0.000 0.00586(4)
Fe1 0.01171(9) 0.01171(9) 0.01707(15) 0.000 0.000 0.00586(4)
Fe2 0.01087(5) 0.01087(5) 0.01265(8) 0.000 0.000 0.00544(2)
Fe3 0.01800(4) 0.01800(4) 0.01508(6) 0.000 0.000 0.00900(2)
S1 0.01402(4) 0.01139(4) 0.01586(6) -0.00226(4) -0.00059(4) 0.00554(3)
O1 0.02056(15) 0.01930(15) 0.0325(2) -0.00920(16) 0.00008(17) 0.01076(11)
O2 0.01748(16) 0.01813(16) 0.0239(2) 0.00037(16) 0.00309(16) 0.00352(12)
O3 0.02232(16) 0.01950(16) 0.01972(19) 0.00171(15) -0.00414(15) 0.00832(12)
O4 0.01841(14) 0.01524(14) 0.01858(19) -0.00573(13) -0.00413(14) 0.00861(10)
OW1 0.02285(16) 0.01619(15) 0.0306(2) -0.00207(15) -0.00893(16) 0.00870(12)
OW2 0.0313(2) 0.0268(2) 0.0314(2) -0.00226(19) 0.00318(19) 0.01032(16)
OW3 0.03932(19) 0.02753(17) 0.0273(2) 0.01067(16) 0.01408(18) 0.02098(13)
 
_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 1.9084(5) 7 ?
Al1 OW1 1.9084(5) . ?
Al1 OW1 1.9084(5) 8 ?
Al1 OW1 1.9084(5) 9 ?
Al1 OW1 1.9084(5) 3 ?
Al1 OW1 1.9084(5) 2 ?
Fe2 O4 2.0008(5) 3_565 ?
Fe2 O4 2.0008(5) 5_565 ?
Fe2 O4 2.0008(5) 6 ?
Fe2 O4 2.0008(5) 2_665 ?
Fe2 O4 2.0008(5) 4_665 ?
Fe2 O4 2.0008(5) . ?
Fe3 O3 1.9763(4) 9_655 ?
Fe3 O3 1.9763(4) 8 ?
Fe3 O3 1.9763(4) 7_665 ?
Fe3 OW3 2.0038(5) 2_655 ?
Fe3 OW3 2.0038(5) . ?
Fe3 OW3 2.0038(5) 3_665 ?
S1 O2 1.4547(4) . ?
S1 O1 1.4623(6) . ?
S1 O3 1.4871(5) . ?
S1 O4 1.4878(4) . ?
O3 Fe3 1.9763(4) 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 180.00(3) 7 . ?
OW1 Al1 OW1 91.97(2) 7 8 ?
OW1 Al1 OW1 88.03(2) . 8 ?
OW1 Al1 OW1 91.97(2) 7 9 ?
OW1 Al1 OW1 88.03(2) . 9 ?
OW1 Al1 OW1 91.97(2) 8 9 ?
OW1 Al1 OW1 88.03(2) 7 3 ?
OW1 Al1 OW1 91.97(2) . 3 ?
OW1 Al1 OW1 88.03(2) 8 3 ?
OW1 Al1 OW1 180.00(3) 9 3 ?
OW1 Al1 OW1 88.03(2) 7 2 ?
OW1 Al1 OW1 91.97(2) . 2 ?
OW1 Al1 OW1 180.00(3) 8 2 ?
OW1 Al1 OW1 88.03(2) 9 2 ?
OW1 Al1 OW1 91.97(2) 3 2 ?
O4 Fe2 O4 89.18(2) 3_565 5_565 ?
O4 Fe2 O4 87.26(3) 3_565 6 ?
O4 Fe2 O4 91.784(18) 5_565 6 ?
O4 Fe2 O4 91.784(18) 3_565 2_665 ?
O4 Fe2 O4 87.26(3) 5_565 2_665 ?
O4 Fe2 O4 178.66(2) 6 2_665 ?
O4 Fe2 O4 178.66(2) 3_565 4_665 ?
O4 Fe2 O4 91.784(18) 5_565 4_665 ?
O4 Fe2 O4 91.784(18) 6 4_665 ?
O4 Fe2 O4 89.18(2) 2_665 4_665 ?
O4 Fe2 O4 91.784(18) 3_565 . ?
O4 Fe2 O4 178.66(2) 5_565 . ?
O4 Fe2 O4 89.18(2) 6 . ?
O4 Fe2 O4 91.784(18) 2_665 . ?
O4 Fe2 O4 87.26(3) 4_665 . ?
O3 Fe3 O3 93.408(18) 9_655 8 ?
O3 Fe3 O3 93.408(18) 9_655 7_665 ?
O3 Fe3 O3 93.408(18) 8 7_665 ?
O3 Fe3 OW3 92.85(2) 9_655 2_655 ?
O3 Fe3 OW3 173.57(2) 8 2_655 ?
O3 Fe3 OW3 84.78(2) 7_665 2_655 ?
O3 Fe3 OW3 84.78(2) 9_655 . ?
O3 Fe3 OW3 92.85(2) 8 . ?
O3 Fe3 OW3 173.57(2) 7_665 . ?
OW3 Fe3 OW3 89.15(2) 2_655 . ?
O3 Fe3 OW3 173.57(2) 9_655 3_665 ?
O3 Fe3 OW3 84.78(2) 8 3_665 ?
O3 Fe3 OW3 92.85(2) 7_665 3_665 ?
OW3 Fe3 OW3 89.15(2) 2_655 3_665 ?
OW3 Fe3 OW3 89.15(2) . 3_665 ?
O2 S1 O1 110.48(3) . . ?
O2 S1 O3 108.09(3) . . ?
O1 S1 O3 110.00(3) . . ?
O2 S1 O4 111.00(3) . . ?
O1 S1 O4 108.18(3) . . ?
O3 S1 O4 109.08(3) . . ?
S1 O3 Fe3 137.35(3) . 7_665 ?
S1 O4 Fe2 136.58(3) . . ?
 
_diffrn_measured_fraction_theta_max    0.971
_diffrn_reflns_theta_full              31.48
_diffrn_measured_fraction_theta_full   0.971
_refine_diff_density_max    0.812
_refine_diff_density_min   -0.365
_refine_diff_density_rms    0.071