#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/17/4111758.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4111758
loop_
_publ_author_name
'Bart M. Bartlett'
'Daniel G. Nocera'
_publ_contact_author             'Daniel G. Nocera'
_publ_contact_author_email       nocera@mit.edu
_publ_section_title
;
 Long-Range Magnetic Ordering in Iron Jarosites Prepared by Redox-Based
 Hydrothermal Methods
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8985
_journal_page_last               8993
_journal_paper_doi               10.1021/ja050205d
_journal_volume                  127
_journal_year                    2005
_chemical_formula_sum            'Fe3 H6 O14 S2 Tl'
_chemical_formula_weight         666.09
_chemical_name_common            'thallium jarosite '
_chemical_name_systematic
'thallium triiron(iii)bis(sulfate)hexahyrdoxide'
_space_group_IT_number           166
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-R 3 2"'
_symmetry_space_group_name_H-M   'R -3 m :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   7.3226(7)
_cell_length_b                   7.3226(7)
_cell_length_c                   17.610(2)
_cell_measurement_temperature    183(2)
_cell_volume                     817.75(14)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0589
_diffrn_reflns_av_sigmaI/netI    0.0281
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            1080
_diffrn_reflns_theta_full        23.22
_diffrn_reflns_theta_max         23.22
_diffrn_reflns_theta_min         3.41
_exptl_absorpt_coefficient_mu    19.111
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            tan
_exptl_crystal_density_diffrn    4.058
_exptl_crystal_description       block
_exptl_crystal_F_000             927
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.754
_refine_diff_density_min         -0.649
_refine_diff_density_rms         0.166
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.292
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     29
_refine_ls_number_reflns         169
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.287
_refine_ls_R_factor_all          0.0207
_refine_ls_R_factor_gt           0.0207
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0092P)²+25.9698P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0546
_refine_ls_wR_factor_ref         0.0546
_reflns_number_gt                169
_reflns_number_total             169
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja050205dsi20050421_111540_3.cif
_cod_data_source_block           TlFeS
_cod_original_cell_volume        817.74(15)
_cod_original_sg_symbol_H-M      'R -3 m'
_cod_original_formula_sum        'H6 Fe3 O14 S2 Tl'
_cod_database_code               4111758
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+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-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+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-y+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z'
'-x+y, y, z'
'x, x-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+y+2/3, y+1/3, z+1/3'
'x+2/3, x-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+y+1/3, y+2/3, z+2/3'
'x+1/3, x-y+2/3, z+2/3'
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
Tl1 Tl 0.0000 0.0000 0.0000 0.0123(4) Uani 1 12 d S
S1 S 0.0000 0.0000 0.3050(2) 0.0055(9) Uani 1 6 d S
Fe1 Fe 0.3333 0.1667 0.1667 0.0054(5) Uani 1 4 d S
O1 O 0.0000 0.0000 0.3873(6) 0.009(2) Uani 1 6 d S
O2 O 0.2202(10) 0.1101(5) 0.2762(3) 0.0090(14) Uani 1 2 d S
O3 O 0.1283(5) 0.2565(10) 0.1374(3) 0.012(2) Uani 1 2 d SPD
H1 H 0.13(3) 0.27(5) 0.0824(15) 0.23(16) Uiso 1 2 d SD
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
Tl1 0.0130(4) 0.0130(4) 0.0108(5) 0.000 0.000 0.0065(2)
S1 0.0050(12) 0.0050(12) 0.0066(19) 0.000 0.000 0.0025(6)
Fe1 0.0029(10) 0.0039(8) 0.0091(10) 0.0001(3) 0.0002(7) 0.0015(5)
O1 0.011(4) 0.011(4) 0.005(5) 0.000 0.000 0.0055(18)
O2 0.006(3) 0.011(2) 0.009(3) 0.0016(13) 0.003(3) 0.0030(17)
O3 0.009(3) 0.010(4) 0.016(4) -0.002(3) -0.0011(14) 0.0051(19)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 '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'
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'
Tl Tl -2.8358 9.6688 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
O1 S1 O2 109.9(3) . 3
O1 S1 O2 109.9(3) . .
O2 S1 O2 109.0(3) 3 .
O1 S1 O2 109.9(3) . 2
O2 S1 O2 109.0(3) 3 2
O2 S1 O2 109.0(3) . 2
O3 Fe1 O3 89.6(4) 25 3
O3 Fe1 O3 179.999(1) 25 .
O3 Fe1 O3 90.4(4) 3 .
O3 Fe1 O3 90.4(4) 25 27
O3 Fe1 O3 179.999(1) 3 27
O3 Fe1 O3 89.6(4) . 27
O3 Fe1 O2 90.9(2) 25 25
O3 Fe1 O2 89.1(2) 3 25
O3 Fe1 O2 89.1(2) . 25
O3 Fe1 O2 90.9(2) 27 25
O3 Fe1 O2 89.1(2) 25 .
O3 Fe1 O2 90.9(2) 3 .
O3 Fe1 O2 90.9(2) . .
O3 Fe1 O2 89.1(2) 27 .
O2 Fe1 O2 179.999(1) 25 .
S1 O2 Fe1 130.3(4) . .
Fe1 O3 Fe1 134.5(3) 2 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
S1 O1 1.450(11) .
S1 O2 1.486(6) 3
S1 O2 1.486(6) .
S1 O2 1.486(6) 2
Fe1 O3 1.985(3) 25
Fe1 O3 1.985(3) 3
Fe1 O3 1.985(3) .
Fe1 O3 1.985(3) 27
Fe1 O2 2.058(6) 25
Fe1 O2 2.058(6) .
O3 Fe1 1.985(3) 2
