#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/17/4111759.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_4111759
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 K O14 Se2'
_chemical_formula_weight         594.62
_chemical_name_systematic
'potassium triiron(iii)bis(selenate)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                   7.3902(9)
_cell_length_b                   7.3902(9)
_cell_length_c                   17.498(3)
_cell_measurement_temperature    183(2)
_cell_volume                     827.6(2)
_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  0.0706
_diffrn_reflns_av_sigmaI/netI    0.0310
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            1130
_diffrn_reflns_theta_full        23.27
_diffrn_reflns_theta_max         23.27
_diffrn_reflns_theta_min         3.39
_exptl_absorpt_coefficient_mu    10.947
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            tan
_exptl_crystal_density_diffrn    3.579
_exptl_crystal_density_meas      0
_exptl_crystal_description       block
_exptl_crystal_F_000             849
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.913
_refine_diff_density_min         -0.690
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.245
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     29
_refine_ls_number_reflns         171
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.241
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0367
_refine_ls_shift/su_max          0.023
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0000P)²+42.7254P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0781
_refine_ls_wR_factor_ref         0.0786
_reflns_number_gt                169
_reflns_number_total             171
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja050205dsi20050421_111540_4.cif
_cod_data_source_block           KFeSe
_cod_original_sg_symbol_H-M      'R -3 m'
_cod_original_formula_sum        'H6 Fe3 K O14 Se2'
_cod_database_code               4111759
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
K1 K 0.0000 0.0000 0.0000 0.0131(14) Uani 1 12 d S
Se1 Se 0.0000 0.0000 0.31151(9) 0.0053(5) Uani 1 6 d S
Fe1 Fe 0.3333 0.1667 0.1667 0.0074(6) Uani 1 4 d S
O1 O 0.0000 0.0000 0.4036(7) 0.011(3) Uani 1 6 d S
O2 O 0.2410(11) 0.1205(6) 0.2792(3) 0.0103(17) Uani 1 2 d S
O3 O 0.1258(6) 0.2516(12) 0.1387(4) 0.0088(16) Uani 1 2 d SD
H1 H 0.193(4) 0.386(8) 0.113(5) 0.04(5) Uiso 1 2 d SPD
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'
K K 0.2009 0.2494 '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'
Se Se -0.0929 2.2259 '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
O2 K1 O2 180.0(3) 25 13_444
O2 K1 O2 109.77(12) 25 27_445
O2 K1 O2 70.23(12) 13_444 27_445
O2 K1 O2 70.23(12) 25 15_554
O2 K1 O2 109.77(12) 13_444 15_554
O2 K1 O2 180.0(2) 27_445 15_554
O2 K1 O2 70.23(12) 25 14_544
O2 K1 O2 109.77(12) 13_444 14_544
O2 K1 O2 70.23(12) 27_445 14_544
O2 K1 O2 109.77(12) 15_554 14_544
O2 K1 O2 109.77(12) 25 26_455
O2 K1 O2 70.23(12) 13_444 26_455
O2 K1 O2 109.77(12) 27_445 26_455
O2 K1 O2 70.23(12) 15_554 26_455
O2 K1 O2 180.0(2) 14_544 26_455
O2 K1 O3 122.33(10) 25 19
O2 K1 O3 57.67(10) 13_444 19
O2 K1 O3 75.61(19) 27_445 19
O2 K1 O3 104.39(19) 15_554 19
O2 K1 O3 57.67(10) 14_544 19
O2 K1 O3 122.33(10) 26_455 19
O2 K1 O3 57.67(10) 25 3
O2 K1 O3 122.33(10) 13_444 3
O2 K1 O3 57.67(10) 27_445 3
O2 K1 O3 122.33(10) 15_554 3
O2 K1 O3 75.61(19) 14_544 3
O2 K1 O3 104.39(19) 26_455 3
O3 K1 O3 122.8(2) 19 3
O2 K1 O3 122.33(10) 25 21
O2 K1 O3 57.67(10) 13_444 21
O2 K1 O3 122.33(10) 27_445 21
O2 K1 O3 57.67(10) 15_554 21
O2 K1 O3 104.39(19) 14_544 21
O2 K1 O3 75.61(19) 26_455 21
O3 K1 O3 57.2(2) 19 21
O3 K1 O3 180.00(14) 3 21
O2 K1 O3 75.61(19) 25 20
O2 K1 O3 104.39(19) 13_444 20
O2 K1 O3 122.33(10) 27_445 20
O2 K1 O3 57.67(10) 15_554 20
O2 K1 O3 57.67(10) 14_544 20
O2 K1 O3 122.33(10) 26_455 20
O3 K1 O3 57.2(2) 19 20
O3 K1 O3 122.8(2) 3 20
O3 K1 O3 57.2(2) 21 20
O2 K1 O3 104.39(19) 25 2
O2 K1 O3 75.61(19) 13_444 2
O2 K1 O3 57.67(10) 27_445 2
O2 K1 O3 122.33(10) 15_554 2
O2 K1 O3 122.33(10) 14_544 2
O2 K1 O3 57.67(10) 26_455 2
O3 K1 O3 122.8(2) 19 2
O3 K1 O3 57.2(2) 3 2
O3 K1 O3 122.8(2) 21 2
O3 K1 O3 180.0(5) 20 2
O2 K1 Fe1 90.79(10) 25 2
O2 K1 Fe1 89.21(10) 13_444 2
O2 K1 Fe1 90.79(10) 27_445 2
O2 K1 Fe1 89.21(10) 15_554 2
O2 K1 Fe1 145.36(12) 14_544 2
O2 K1 Fe1 34.64(12) 26_455 2
O3 K1 Fe1 146.70(5) 19 2
O3 K1 Fe1 69.75(14) 3 2
O3 K1 Fe1 110.25(14) 21 2
O3 K1 Fe1 146.69(5) 20 2
O3 K1 Fe1 33.31(5) 2 2
O1 Se1 O2 110.1(2) . 3
O1 Se1 O2 110.1(2) . 2
O2 Se1 O2 108.8(2) 3 2
O1 Se1 O2 110.1(2) . .
O2 Se1 O2 108.8(2) 3 .
O2 Se1 O2 108.8(2) 2 .
O3 Fe1 O3 90.8(4) 25 3
O3 Fe1 O3 179.999(1) 25 .
O3 Fe1 O3 89.2(4) 3 .
O3 Fe1 O3 89.2(4) 25 27
O3 Fe1 O3 179.999(1) 3 27
O3 Fe1 O3 90.8(4) . 27
O3 Fe1 O2 92.5(2) 25 25
O3 Fe1 O2 87.5(2) 3 25
O3 Fe1 O2 87.5(2) . 25
O3 Fe1 O2 92.5(2) 27 25
O3 Fe1 O2 87.5(2) 25 .
O3 Fe1 O2 92.5(2) 3 .
O3 Fe1 O2 92.5(2) . .
O3 Fe1 O2 87.5(2) 27 .
O2 Fe1 O2 179.999(1) 25 .
O3 Fe1 K1 53.6(2) 25 7
O3 Fe1 K1 126.4(2) 3 7
O3 Fe1 K1 126.4(2) . 7
O3 Fe1 K1 53.6(2) 27 7
O2 Fe1 K1 127.1(2) 25 7
O2 Fe1 K1 52.9(2) . 7
Se1 O2 Fe1 126.8(4) . .
Se1 O2 K1 140.7(3) . 7
Fe1 O2 K1 92.5(2) . 7
Fe1 O3 Fe1 136.8(4) 2 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
K1 O2 2.884(7) 25
K1 O2 2.884(7) 13_444
K1 O2 2.884(7) 27_445
K1 O2 2.884(7) 15_554
K1 O2 2.884(7) 14_544
K1 O2 2.884(7) 26_455
K1 O3 2.913(7) 19
K1 O3 2.913(7) 3
K1 O3 2.913(7) 21
K1 O3 2.913(7) 20
K1 O3 2.913(7) 2
K1 Fe1 3.6134(4) 2
Se1 O1 1.611(11) .
Se1 O2 1.643(7) 3
Se1 O2 1.643(7) 2
Se1 O2 1.643(7) .
Fe1 O3 1.987(3) 25
Fe1 O3 1.987(3) 3
Fe1 O3 1.987(3) .
Fe1 O3 1.987(3) 27
Fe1 O2 2.056(6) 25
Fe1 O2 2.056(6) .
Fe1 K1 3.6134(4) 7
O2 K1 2.884(7) 7
O3 Fe1 1.987(3) 2
