 
data_shelx
 
_audit_creation_method            'SHELXL-2018/1'
_shelx_SHELXL_version_number      '2018/1'
_chemical_name_mineral            'coquimbite'
_chemical_compound_source         'Monte Arsiccio mine, Apuan Alps, Italy'
_chemical_formula_analytical
;      
Al0.96 Fe3.11 H36 O42 S5.97
; 
_chemical_formula_sum
 'Al0.95 Fe3.05 H36 O42 S6' 
_chemical_formula_weight          1096.74

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'
 'Fe'  'Fe'   0.3463   0.8444
 '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'
 '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'
 
_space_group_crystal_system       trigonal
_space_group_IT_number            163
_space_group_name_H-M_alt         'P -3 1 c'
_space_group_name_Hall            '-P 3 2c'
 
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-y, x-y, z'
 '-y, -x, -z+1/2'
 '-x+y, -x, z'
 'x, x-y, -z+1/2'
 '-x+y, y, -z+1/2'
 '-x, -y, -z'
 'y, -x+y, -z'
 'y, x, z-1/2'
 'x-y, x, -z'
 '-x, -x+y, z-1/2'
 'x-y, -y, z-1/2'
 
_cell_length_a                    10.9318(12)
_cell_length_b                    10.9318(12)
_cell_length_c                    17.069(2)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 120
_cell_volume                      1766.6(4)
_cell_formula_units_Z             2
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     9971
_cell_measurement_theta_min       2.386
_cell_measurement_theta_max       32.835
 
_exptl_crystal_description        'anhedral'
_exptl_crystal_colour             'violet'
_exptl_crystal_density_meas       'not measured'
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     2.062         
_exptl_crystal_F_000              1119.4
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.15
_exptl_crystal_size_mid           0.12
_exptl_crystal_size_min           0.10
_exptl_absorpt_coefficient_mu     1.750
_shelx_estimated_absorpt_T_min    ?
_shelx_estimated_absorpt_T_max    ?
_exptl_absorpt_correction_type    'multi-scan'
_exptl_absorpt_correction_T_min   0.904
_exptl_absorpt_correction_T_max   0.932
_exptl_absorpt_process_details    'SADABS (Sheldrick, 1996)'
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       293(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 Smart Breeze'
_diffrn_reflns_number             16979
_diffrn_reflns_av_unetI/netI      0.0092
_diffrn_reflns_av_R_equivalents   0.0185
_diffrn_reflns_limit_h_min        -14
_diffrn_reflns_limit_h_max        14
_diffrn_reflns_limit_k_min        -14
_diffrn_reflns_limit_k_max        13
_diffrn_reflns_limit_l_min        -22
_diffrn_reflns_limit_l_max        21
_diffrn_reflns_theta_min          4.179
_diffrn_reflns_theta_max          27.498
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   0.983
_diffrn_measured_fraction_theta_full  0.979
_diffrn_reflns_Laue_measured_fraction_max    0.983
_diffrn_reflns_Laue_measured_fraction_full   0.979
_diffrn_reflns_point_group_measured_fraction_max   0.983
_diffrn_reflns_point_group_measured_fraction_full  0.979
_reflns_number_total              1341
_reflns_number_gt                 1307
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection      'Apex3 (Bruker AXS Inc., 2016)'
_computing_cell_refinement      'Apex3 (Bruker AXS Inc., 2016)'
_computing_data_reduction       'Apex3 (Bruker AXS Inc., 2016)'
_computing_structure_refinement 'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
_refine_special_details           ?
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0293P)²+2.3592P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    difmap
_refine_ls_hydrogen_treatment     refall
_refine_ls_extinction_method      'SHELXL-2018/1 (Sheldrick 2018)'
_refine_ls_extinction_coef        0.0075(14)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_number_reflns          1341
_refine_ls_number_parameters      110
_refine_ls_number_restraints      7
_refine_ls_R_factor_all           0.0224
_refine_ls_R_factor_gt            0.0219
_refine_ls_wR_factor_ref          0.0664
_refine_ls_wR_factor_gt           0.0661
_refine_ls_goodness_of_fit_ref    1.083
_refine_ls_restrained_S_all       1.089
_refine_ls_shift/su_max           0.019
_refine_ls_shift/su_mean          0.001
 
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_site_symmetry_order  
 _atom_site_calc_flag
 _atom_site_refinement_flags_posn
 _atom_site_refinement_flags_adp
 _atom_site_refinement_flags_occupancy
 _atom_site_disorder_assembly
 _atom_site_disorder_group
Fe1 Fe 0.333333 0.666667 0.250000 0.01170(16) Uani 1 6 d S T P . .
Fe2 Fe 0.666667 0.333333 0.00259(3) 0.01726(15) Uani 1 3 d S T P . .
S1 S 0.24467(4) 0.41495(4) 0.12299(2) 0.01426(15) Uani 1 1 d . . . . .
Al Al 0.000000 0.000000 0.000000 0.0132(4) Uani 0.946(7) 6 d S T P . .
Fe Fe 0.000000 0.000000 0.000000 0.0132(4) Uani 0.054(7) 6 d S T P . .
O1 O 0.31822(14) 0.34515(14) 0.09097(9) 0.0239(3) Uani 1 1 d . . . . .
O2 O 0.10817(15) 0.31079(14) 0.15501(8) 0.0226(3) Uani 1 1 d . . . . .
O3 O 0.21965(15) 0.49421(14) 0.05998(8) 0.0218(3) Uani 1 1 d . . . . .
O4 O 0.33578(13) 0.51613(13) 0.18445(7) 0.0176(3) Uani 1 1 d . . . . .
OW1 O 0.16495(15) 0.07034(14) 0.06168(9) 0.0224(3) Uani 1 1 d D . . . .
OW2 O 0.44914(18) 0.11626(18) 0.20991(10) 0.0320(4) Uani 1 1 d D . . . .
OW3 O 0.57193(18) 0.16215(17) 0.07119(9) 0.0298(3) Uani 1 1 d D . . . .
H11 H 0.187(4) 0.015(4) 0.0899(19) 0.070(11) Uiso 1 1 d D . . . .
H12 H 0.224(3) 0.165(2) 0.073(2) 0.058(10) Uiso 1 1 d D . . . .
H21 H 0.366(2) 0.033(2) 0.2069(19) 0.044(8) Uiso 1 1 d D . . . .
H22 H 0.510(6) 0.104(7) 0.242(4) 0.057(15) Uiso 0.47(4) 1 d D . P . .
H23 H 0.443(6) 0.191(5) 0.230(4) 0.057(15) Uiso 0.53(4) 1 d D . P . .
H31 H 0.599(4) 0.096(3) 0.074(2) 0.061(10) Uiso 1 1 d D . . . .
H32 H 0.529(4) 0.155(4) 0.1190(14) 0.069(11) Uiso 1 1 d D . . . .
 
 
_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
Fe1 O4 2.0011(13) 5_565 ?
Fe1 O4 2.0011(13) 4_565 ?
Fe1 O4 2.0011(13) 6 ?
Fe1 O4 2.0011(13) 2_665 ?
Fe1 O4 2.0011(13) 3_665 ?
Fe1 O4 2.0012(12) . ?
Fe2 O3 1.9739(14) 8 ?
Fe2 O3 1.9739(14) 7_665 ?
Fe2 O3 1.9740(14) 10_655 ?
Fe2 OW3 2.0019(15) 2_655 ?
Fe2 OW3 2.0019(15) . ?
Fe2 OW3 2.0019(15) 4_665 ?
S1 O2 1.4571(14) . ?
S1 O1 1.4632(14) . ?
S1 O4 1.4881(13) . ?
S1 O3 1.4898(14) . ?
Al OW1 1.8880(13) 7 ?
Al OW1 1.8880(13) 8 ?
Al OW1 1.8880(13) 2 ?
Al OW1 1.8880(13) 10 ?
Al OW1 1.8880(13) 4 ?
Al OW1 1.8880(13) . ?
OW1 H11 0.898(19) . ?
OW1 H12 0.926(18) . ?
OW2 H21 0.911(18) . ?
OW2 H22 0.93(2) . ?
OW2 H23 0.92(2) . ?
OW3 H31 0.909(18) . ?
OW3 H32 0.926(18) . ?
 
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
O4 Fe1 O4 89.18(8) 5_565 4_565 ?
O4 Fe1 O4 91.78(5) 5_565 6 ?
O4 Fe1 O4 87.27(7) 4_565 6 ?
O4 Fe1 O4 87.27(7) 5_565 2_665 ?
O4 Fe1 O4 91.78(5) 4_565 2_665 ?
O4 Fe1 O4 178.67(7) 6 2_665 ?
O4 Fe1 O4 91.78(5) 5_565 3_665 ?
O4 Fe1 O4 178.67(7) 4_565 3_665 ?
O4 Fe1 O4 91.78(5) 6 3_665 ?
O4 Fe1 O4 89.18(8) 2_665 3_665 ?
O4 Fe1 O4 178.67(7) 5_565 . ?
O4 Fe1 O4 91.78(5) 4_565 . ?
O4 Fe1 O4 89.18(8) 6 . ?
O4 Fe1 O4 91.78(5) 2_665 . ?
O4 Fe1 O4 87.27(7) 3_665 . ?
O3 Fe2 O3 93.49(6) 8 7_665 ?
O3 Fe2 O3 93.49(6) 8 10_655 ?
O3 Fe2 O3 93.49(6) 7_665 10_655 ?
O3 Fe2 OW3 173.55(6) 8 2_655 ?
O3 Fe2 OW3 84.66(6) 7_665 2_655 ?
O3 Fe2 OW3 92.79(7) 10_655 2_655 ?
O3 Fe2 OW3 92.79(7) 8 . ?
O3 Fe2 OW3 173.55(6) 7_665 . ?
O3 Fe2 OW3 84.66(6) 10_655 . ?
OW3 Fe2 OW3 89.25(7) 2_655 . ?
O3 Fe2 OW3 84.67(6) 8 4_665 ?
O3 Fe2 OW3 92.79(7) 7_665 4_665 ?
O3 Fe2 OW3 173.55(6) 10_655 4_665 ?
OW3 Fe2 OW3 89.25(7) 2_655 4_665 ?
OW3 Fe2 OW3 89.25(7) . 4_665 ?
O2 S1 O1 110.35(8) . . ?
O2 S1 O4 111.08(8) . . ?
O1 S1 O4 108.23(8) . . ?
O2 S1 O3 108.13(8) . . ?
O1 S1 O3 110.01(9) . . ?
O4 S1 O3 109.03(8) . . ?
OW1 Al OW1 91.92(6) 7 8 ?
OW1 Al OW1 88.08(6) 7 2 ?
OW1 Al OW1 180.00(9) 8 2 ?
OW1 Al OW1 91.92(6) 7 10 ?
OW1 Al OW1 91.92(6) 8 10 ?
OW1 Al OW1 88.08(6) 2 10 ?
OW1 Al OW1 88.08(6) 7 4 ?
OW1 Al OW1 88.08(6) 8 4 ?
OW1 Al OW1 91.92(6) 2 4 ?
OW1 Al OW1 180.00(10) 10 4 ?
OW1 Al OW1 180.0 7 . ?
OW1 Al OW1 88.08(6) 8 . ?
OW1 Al OW1 91.92(6) 2 . ?
OW1 Al OW1 88.08(6) 10 . ?
OW1 Al OW1 91.92(6) 4 . ?
S1 O3 Fe2 137.31(9) . 7_665 ?
S1 O4 Fe1 136.57(8) . . ?
Al OW1 H11 123(3) . . ?
Al OW1 H12 124(2) . . ?
H11 OW1 H12 111(3) . . ?
H21 OW2 H22 109(4) . . ?
H21 OW2 H23 115(4) . . ?
H22 OW2 H23 107(6) . . ?
Fe2 OW3 H31 123(2) . . ?
Fe2 OW3 H32 127(2) . . ?
H31 OW3 H32 104(3) . . ?
 
_refine_diff_density_max    0.820
_refine_diff_density_min   -0.333
_refine_diff_density_rms    0.073



