data_04src0949_90
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          'Fe3 H6 O14 S2, 12(O0.08)'
_chemical_formula_sum
 'Fe3 H6 O15 S2'
_chemical_formula_weight          477.72
 
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'
 
_symmetry_cell_setting            Trigonal
_symmetry_space_group_name_H-M    R-3m
_symmetry_space_group_name_hall   '-R 3 2"' 
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-y, x-y, z'
 '-x+y, -x, z'
 'y, x, -z'
 '-x, -x+y, -z'
 'x-y, -y, -z'
 '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+1/3'
 '-x+2/3, -x+y+1/3, -z+1/3'
 'x-y+2/3, -y+1/3, -z+1/3'
 '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+2/3'
 '-x+1/3, -x+y+2/3, -z+2/3'
 'x-y+1/3, -y+2/3, -z+2/3'
 '-x, -y, -z'
 'y, -x+y, -z'
 'x-y, x, -z'
 '-y, -x, z'
 'x, x-y, z'
 '-x+y, y, z'
 '-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+1/3'
 'x+2/3, x-y+1/3, z+1/3'
 '-x+y+2/3, y+1/3, z+1/3'
 '-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+2/3'
 'x+1/3, x-y+2/3, z+2/3'
 '-x+y+1/3, y+2/3, z+2/3'
 
_cell_length_a                    7.3218(10)
_cell_length_b                    7.3218(10)
_cell_length_c                    16.881(3)
_cell_angle_alpha                 90.00
_cell_angle_beta                  90.00
_cell_angle_gamma                 120.00
_cell_volume                      783.7(2)
_cell_formula_units_Z             3
_cell_measurement_temperature     90(2)
_cell_measurement_reflns_used     2891
_cell_measurement_theta_min       2.91
_cell_measurement_theta_max       27.48
 
_exptl_crystal_description        cube
_exptl_crystal_colour             orange
_exptl_crystal_size_max           0.08
_exptl_crystal_size_mid           0.08
_exptl_crystal_size_min           0.08
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     3.037
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              708
_exptl_absorpt_coefficient_mu     4.603
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.7096
_exptl_absorpt_correction_T_max   0.7096
_exptl_absorpt_process_details    'SADABS V2.10 (Sheldrick, G.M., 2003)'
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       90(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device_type   'Bruker-Nonius KappaCCD Area Detector'
_diffrn_measurement_method        'φ and ω scans'
_diffrn_detector_area_resol_mean  9.091
_diffrn_standards_number          none
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         negligible
_diffrn_reflns_number             3462
_diffrn_reflns_av_R_equivalents   0.0246
_diffrn_reflns_av_sigmaI/netI     0.0174
_diffrn_reflns_limit_h_min        -9
_diffrn_reflns_limit_h_max        9
_diffrn_reflns_limit_k_min        -9
_diffrn_reflns_limit_k_max        9
_diffrn_reflns_limit_l_min        -21
_diffrn_reflns_limit_l_max        19
_diffrn_reflns_theta_min          3.43
_diffrn_reflns_theta_max          27.47
_reflns_number_total              252
_reflns_number_gt                 249
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        ?
_computing_cell_refinement        'DENZO, COLLECT'
_computing_data_reduction         'DENZO, COLLECT'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     'PLATON (Spek, 1990)'
_computing_publication_material   ?
 
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² 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/[σ²(Fo²)+(0.0214P)²+3.8223P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      SHELXL
_refine_ls_extinction_coef        0.0049(7)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_number_reflns          252
_refine_ls_number_parameters      27
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0201
_refine_ls_R_factor_gt            0.0197
_refine_ls_wR_factor_ref          0.0524
_refine_ls_wR_factor_gt           0.0516
_refine_ls_goodness_of_fit_ref    1.218
_refine_ls_restrained_S_all       1.218
_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
Fe1 Fe 0.3333 0.1667 0.1667 0.0062(3) Uani 1 4 d S . .
S1 S 0.6667 0.3333 0.02475(6) 0.0042(3) Uani 1 6 d S . .
O1 O 0.4471(3) 0.22355(15) 0.05420(10) 0.0073(4) Uani 1 2 d S . .
O2 O 0.12751(15) -0.12751(15) 0.13522(12) 0.0095(4) Uani 1 2 d S . .
H2O H 0.1748 -0.1749 0.1163 0.004(9) Uiso 1 2 d SR . .
O3 O 0.6667 0.3333 -0.06137(18) 0.0080(7) Uani 1 6 d S . .
O4 O 0.0000 0.0000 0.0000 0.0234(13) Uani 1 12 d S . .
 
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
Fe1 0.0054(3) 0.0072(3) 0.0055(3) 0.00065(9) 0.00130(17) 0.00271(17)
S1 0.0054(4) 0.0054(4) 0.0018(5) 0.000 0.000 0.00268(18)
O1 0.0050(9) 0.0102(7) 0.0050(8) 0.0002(3) 0.0005(6) 0.0025(5)
O2 0.0048(7) 0.0048(7) 0.0189(10) -0.0036(4) 0.0036(4) 0.0023(7)
O3 0.0116(10) 0.0116(10) 0.0008(13) 0.000 0.000 0.0058(5)
O4 0.0259(19) 0.0259(19) 0.018(3) 0.000 0.000 0.0130(10)
 
_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 O2 1.9865(8) 26 ?
Fe1 O2 1.9865(8) 2 ?
Fe1 O2 1.9865(8) . ?
Fe1 O2 1.9865(8) 25 ?
Fe1 O1 2.0311(17) . ?
Fe1 O1 2.0311(17) 25 ?
S1 O3 1.454(3) . ?
S1 O1 1.4783(18) 2_655 ?
S1 O1 1.4783(18) 3_665 ?
S1 O1 1.4783(18) . ?
O2 Fe1 1.9865(8) 3 ?
 
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
O2 Fe1 O2 180.0 26 2 ?
O2 Fe1 O2 90.35(11) 26 . ?
O2 Fe1 O2 89.65(11) 2 . ?
O2 Fe1 O2 89.65(11) 26 25 ?
O2 Fe1 O2 90.35(11) 2 25 ?
O2 Fe1 O2 180.0 . 25 ?
O2 Fe1 O1 90.95(6) 26 . ?
O2 Fe1 O1 89.06(6) 2 . ?
O2 Fe1 O1 89.06(6) . . ?
O2 Fe1 O1 90.95(6) 25 . ?
O2 Fe1 O1 89.06(6) 26 25 ?
O2 Fe1 O1 90.94(6) 2 25 ?
O2 Fe1 O1 90.94(6) . 25 ?
O2 Fe1 O1 89.05(6) 25 25 ?
O1 Fe1 O1 180.0 . 25 ?
O3 S1 O1 109.65(7) . 2_655 ?
O3 S1 O1 109.65(7) . 3_665 ?
O1 S1 O1 109.29(8) 2_655 3_665 ?
O3 S1 O1 109.65(7) . . ?
O1 S1 O1 109.29(8) 2_655 . ?
O1 S1 O1 109.29(8) 3_665 . ?
S1 O1 Fe1 130.45(11) . . ?
Fe1 O2 Fe1 134.27(10) 3 . ?
 
_diffrn_measured_fraction_theta_max    1.000
_diffrn_reflns_theta_full              27.47
_diffrn_measured_fraction_theta_full   1.000
_refine_diff_density_max    0.510
_refine_diff_density_min   -0.499
_refine_diff_density_rms    0.106
