 
data_2004src0948_rt
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          'Fe3 O9 S2, 3(H2 O)'
_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
 'Fe'  'Fe'   0.3463   0.8444
 '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'
 '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'
 'y, x, -z'
 '-x+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'
 'y+2/3, x+1/3, -z+1/3'
 '-x+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'
 'y+1/3, x+2/3, -z+2/3'
 '-x+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'
 '-y, -x, z'
 'x-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'
 '-y+2/3, -x+1/3, z+1/3'
 'x-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'
 '-y+1/3, -x+2/3, z+2/3'
 'x-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                    7.342(2)
_cell_length_b                    7.342(2)
_cell_length_c                    17.007(5)
_cell_angle_alpha                 90.00
_cell_angle_beta                  90.00
_cell_angle_gamma                 120.00
_cell_volume                      793.9(4)
_cell_formula_units_Z             3
_cell_measurement_temperature     291(2)
_cell_measurement_reflns_used     ?
_cell_measurement_theta_min       ?
_cell_measurement_theta_max       ?
 
_exptl_crystal_description        fleck
_exptl_crystal_colour             yellow
_exptl_crystal_size_max           0.01
_exptl_crystal_size_mid           0.01
_exptl_crystal_size_min           0.01
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     2.997
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              708
_exptl_absorpt_coefficient_mu     4.544
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.9560
_exptl_absorpt_correction_T_max   0.9560
_exptl_absorpt_process_details    'SORTAV (R.H.Blessing, 1995, 1997)'
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       291(2)
_diffrn_radiation_wavelength      0.69020
_diffrn_radiation_type            synchrotron
_diffrn_radiation_source          'Enraf Nonius FR591 rotating anode'
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'Enraf Nonius KappaCCD area detector'
_diffrn_measurement_method        'ω and φ scans to fill Ewald sphere'
_diffrn_detector_area_resol_mean  '9.091 pixels/mm'
_diffrn_standards_number          'n/a'
_diffrn_standards_interval_count  'n/a'
_diffrn_standards_interval_time   'n/a'
_diffrn_standards_decay_%         'n/a'

_diffrn_reflns_number             2412
_diffrn_reflns_av_R_equivalents   0.0248
_diffrn_reflns_av_sigmaI/netI     0.0248
_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        -22
_diffrn_reflns_limit_l_max        22
_diffrn_reflns_theta_min          3.32
_diffrn_reflns_theta_max          27.48
_reflns_number_total              252
_reflns_number_gt                 252
_reflns_threshold_expression      >2σ(I)
 
_computing_data_collection        
;
'DENZO (Otwinowski and Minor, 1997) & COLLECT (Hooft, 1998) '
;
_computing_cell_refinement        'DENZO and COLLECT'
_computing_data_reduction         'DENZO and COLLECT'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 2008)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 2008)' 
_computing_molecular_graphics     'PLATON (Watkin, Pearce 1995)'
_computing_publication_material   SHELXL-97
 
_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 > 2σ(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)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          252
_refine_ls_number_parameters      29
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0572
_refine_ls_R_factor_gt            0.0217
_refine_ls_wR_factor_ref          0.0585
_refine_ls_wR_factor_gt           0.0244
_refine_ls_goodness_of_fit_ref    1.086
_refine_ls_restrained_S_all       1.086
_refine_ls_shift/su_max           0
_refine_ls_shift/su_mean          0
 
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
O4 O 1.3333 0.6667 0.1667 0.028 Uani 1 12 d S . .
S1 S 0.6667 0.3333 0.1413 0.009 Uani 1 6 d S . .
Fe1 Fe 1.0000 0.5000 0.0000 0.011 Uani 1 4 d S . .
O2 O 0.8856 0.4428 0.1119 0.014 Uani 1 2 d S . .
O1 O 1.2063 0.7937 0.0316 0.017 Uani 1 2 d S . .
O3 O 0.6667 0.3333 0.2270 0.015 Uani 1 6 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
O4 0.033 0.033 0.019 0.000 0.000 0.016
S1 0.010 0.010 0.007 0.000 0.000 0.005
Fe1 0.009 0.011 0.012 0.001 0.002 0.005
O2 0.009 0.018 0.012 0.001 0.002 0.005
O1 0.010 0.010 0.029 -0.005 0.005 0.004
O3 0.019 0.019 0.007 0.000 0.000 0.010
 
_geom_special_details
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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
S1 O3 1.4575 . ?
S1 O2 1.4791 21_665 ?
S1 O2 1.4791 . ?
S1 O2 1.4791 2_655 ?
Fe1 O1 1.9917 19_765 ?
Fe1 O1 1.9917 . ?
Fe1 O1 1.9917 2_755 ?
Fe1 O1 1.9917 20_565 ?
Fe1 O2 2.0374 . ?
Fe1 O2 2.0374 19_765 ?
O1 Fe1 1.9917 3_655 ?
 
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
O3 S1 O2 109.8 . 21_665 ?
O3 S1 O2 109.8 . . ?
O2 S1 O2 109.2 21_665 . ?
O3 S1 O2 109.8 . 2_655 ?
O2 S1 O2 109.2 21_665 2_655 ?
O2 S1 O2 109.2 . 2_655 ?
O1 Fe1 O1 180.0 19_765 . ?
O1 Fe1 O1 90.8 19_765 2_755 ?
O1 Fe1 O1 89.2 . 2_755 ?
O1 Fe1 O1 89.2 19_765 20_565 ?
O1 Fe1 O1 90.8 . 20_565 ?
O1 Fe1 O1 180.0 2_755 20_565 ?
O1 Fe1 O2 91.0 19_765 . ?
O1 Fe1 O2 89.0 . . ?
O1 Fe1 O2 89.0 2_755 . ?
O1 Fe1 O2 91.0 20_565 . ?
O1 Fe1 O2 89.0 19_765 19_765 ?
O1 Fe1 O2 91.0 . 19_765 ?
O1 Fe1 O2 91.0 2_755 19_765 ?
O1 Fe1 O2 89.0 20_565 19_765 ?
O2 Fe1 O2 180.0 . 19_765 ?
S1 O2 Fe1 130.7 . . ?
Fe1 O1 Fe1 134.3 . 3_655 ?
 
_diffrn_measured_fraction_theta_max    0.913
_diffrn_reflns_theta_full              27.48
_diffrn_measured_fraction_theta_full   0.913
_refine_diff_density_max    0.569
_refine_diff_density_min   -0.421
_refine_diff_density_rms    0
