#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/17/4111760.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_4111760
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 Rb Se2'
_chemical_formula_weight         640.99
_chemical_name_systematic
'rubidium 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                   7.4022(16)
_cell_length_b                   7.4022(16)
_cell_length_c                   17.816(5)
_cell_measurement_reflns_used    2946
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.37
_cell_measurement_theta_min      3.38
_cell_volume                     845.4(4)
_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      100(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  0.0323
_diffrn_reflns_av_sigmaI/netI    0.0132
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            5356
_diffrn_reflns_theta_full        28.47
_diffrn_reflns_theta_max         28.47
_diffrn_reflns_theta_min         3.38
_exptl_absorpt_coefficient_mu    4.879
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.777
_exptl_crystal_density_meas      0
_exptl_crystal_description       block
_exptl_crystal_F_000             301
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.617
_refine_diff_density_min         -0.812
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     29
_refine_ls_number_reflns         293
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0162
_refine_ls_R_factor_gt           0.0156
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0242P)²+4.2964P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0433
_refine_ls_wR_factor_ref         0.0436
_reflns_number_gt                285
_reflns_number_total             293
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja050205dsi20050421_111540_5.cif
_cod_data_source_block           RbFeSe
_cod_original_sg_symbol_H-M      'R -3 m'
_cod_original_formula_sum        'H6 Fe3 O14 Rb Se2'
_cod_database_code               4111760
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
Fe1 Fe 0.3333 0.1667 0.1667 0.00523(16) Uani 1 4 d S
Rb1 Rb 0.0000 0.0000 0.0000 0.00795(18) Uani 1 12 d S
Se1 Se 0.0000 0.0000 0.30926(3) 0.00483(15) Uani 1 6 d S
O1 O 0.0000 0.0000 0.40024(19) 0.0076(7) Uani 1 6 d S
O2 O 0.2409(3) 0.12043(16) 0.27744(11) 0.0080(4) Uani 1 2 d S
O3 O 0.12636(16) 0.2527(3) 0.14075(11) 0.0100(6) Uani 1 2 d SPD
H1 H 0.1959(14) 0.392(3) 0.121(2) 0.019(10) Uiso 1 2 d SD
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'
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'
Rb Rb -0.9393 2.9676 '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
O3 Fe1 O3 180.0 25 .
O3 Fe1 O3 90.07(12) 25 3
O3 Fe1 O3 89.93(12) . 3
O3 Fe1 O3 89.93(12) 25 27
O3 Fe1 O3 90.07(12) . 27
O3 Fe1 O3 180.0 3 27
O3 Fe1 O2 91.75(7) 25 25
O3 Fe1 O2 88.25(7) . 25
O3 Fe1 O2 88.25(7) 3 25
O3 Fe1 O2 91.75(7) 27 25
O3 Fe1 O2 88.25(7) 25 .
O3 Fe1 O2 91.75(7) . .
O3 Fe1 O2 91.75(7) 3 .
O3 Fe1 O2 88.25(7) 27 .
O2 Fe1 O2 180.0 25 .
O3 Fe1 Rb1 125.39(6) 25 .
O3 Fe1 Rb1 54.61(6) . .
O3 Fe1 Rb1 54.61(6) 3 .
O3 Fe1 Rb1 125.39(6) 27 .
O2 Fe1 Rb1 52.46(6) 25 .
O2 Fe1 Rb1 127.54(6) . .
O3 Fe1 Rb1 54.61(6) 25 7
O3 Fe1 Rb1 125.39(6) . 7
O3 Fe1 Rb1 125.39(6) 3 7
O3 Fe1 Rb1 54.61(6) 27 7
O2 Fe1 Rb1 127.54(6) 25 7
O2 Fe1 Rb1 52.46(6) . 7
Rb1 Fe1 Rb1 180.0 . 7
O2 Rb1 O2 180.00(9) 25 13_444
O2 Rb1 O2 108.89(4) 25 27_445
O2 Rb1 O2 71.11(4) 13_444 27_445
O2 Rb1 O2 71.11(4) 25 15_554
O2 Rb1 O2 108.89(4) 13_444 15_554
O2 Rb1 O2 180.00(7) 27_445 15_554
O2 Rb1 O2 108.89(4) 25 26_455
O2 Rb1 O2 71.11(4) 13_444 26_455
O2 Rb1 O2 108.89(4) 27_445 26_455
O2 Rb1 O2 71.11(4) 15_554 26_455
O2 Rb1 O2 71.11(4) 25 14_544
O2 Rb1 O2 108.89(4) 13_444 14_544
O2 Rb1 O2 71.11(4) 27_445 14_544
O2 Rb1 O2 108.89(4) 15_554 14_544
O2 Rb1 O2 180.00(8) 26_455 14_544
O2 Rb1 O3 122.87(3) 25 19
O2 Rb1 O3 57.13(3) 13_444 19
O2 Rb1 O3 77.18(5) 27_445 19
O2 Rb1 O3 102.82(5) 15_554 19
O2 Rb1 O3 122.87(3) 26_455 19
O2 Rb1 O3 57.13(3) 14_544 19
O2 Rb1 O3 57.13(3) 25 .
O2 Rb1 O3 122.87(3) 13_444 .
O2 Rb1 O3 102.82(5) 27_445 .
O2 Rb1 O3 77.18(5) 15_554 .
O2 Rb1 O3 57.13(3) 26_455 .
O2 Rb1 O3 122.87(3) 14_544 .
O3 Rb1 O3 180.00(6) 19 .
O2 Rb1 O3 57.13(3) 25 3
O2 Rb1 O3 122.87(3) 13_444 3
O2 Rb1 O3 57.13(3) 27_445 3
O2 Rb1 O3 122.87(3) 15_554 3
O2 Rb1 O3 102.82(5) 26_455 3
O2 Rb1 O3 77.18(5) 14_544 3
O3 Rb1 O3 123.94(7) 19 3
O3 Rb1 O3 56.06(7) . 3
O2 Rb1 O3 122.87(3) 25 21
O2 Rb1 O3 57.13(3) 13_444 21
O2 Rb1 O3 122.87(3) 27_445 21
O2 Rb1 O3 57.13(3) 15_554 21
O2 Rb1 O3 77.18(5) 26_455 21
O2 Rb1 O3 102.82(5) 14_544 21
O3 Rb1 O3 56.06(7) 19 21
O3 Rb1 O3 123.94(7) . 21
O3 Rb1 O3 180.00(4) 3 21
O2 Rb1 O3 77.18(5) 25 20
O2 Rb1 O3 102.82(5) 13_444 20
O2 Rb1 O3 122.87(3) 27_445 20
O2 Rb1 O3 57.13(3) 15_554 20
O2 Rb1 O3 122.87(3) 26_455 20
O2 Rb1 O3 57.13(3) 14_544 20
O3 Rb1 O3 56.06(7) 19 20
O3 Rb1 O3 123.94(7) . 20
O3 Rb1 O3 123.94(7) 3 20
O3 Rb1 O3 56.06(7) 21 20
O2 Rb1 O3 102.82(5) 25 2
O2 Rb1 O3 77.18(5) 13_444 2
O2 Rb1 O3 57.13(3) 27_445 2
O2 Rb1 O3 122.87(3) 15_554 2
O2 Rb1 O3 57.13(3) 26_455 2
O2 Rb1 O3 122.87(3) 14_544 2
O3 Rb1 O3 123.94(7) 19 2
O3 Rb1 O3 56.06(7) . 2
O3 Rb1 O3 56.06(7) 3 2
O3 Rb1 O3 123.94(7) 21 2
O3 Rb1 O3 180.00(6) 20 2
O1 Se1 O2 110.16(7) . 3
O1 Se1 O2 110.16(7) . .
O2 Se1 O2 108.77(7) 3 .
O1 Se1 O2 110.16(7) . 2
O2 Se1 O2 108.77(7) 3 2
O2 Se1 O2 108.77(7) . 2
Se1 O2 Fe1 126.88(11) . .
Se1 O2 Rb1 139.79(10) . 7
Fe1 O2 Rb1 93.33(7) . 7
Fe1 O3 Fe1 137.51(11) . 2
Fe1 O3 Rb1 92.55(6) . .
Fe1 O3 Rb1 92.55(6) 2 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 O3 1.9855(8) 25
Fe1 O3 1.9855(8) .
Fe1 O3 1.9855(8) 3
Fe1 O3 1.9855(8) 27
Fe1 O2 2.061(2) 25
Fe1 O2 2.061(2) .
Fe1 Rb1 3.6583(8) .
Fe1 Rb1 3.6583(8) 7
Rb1 O2 2.906(2) 25
Rb1 O2 2.906(2) 13_444
Rb1 O2 2.906(2) 27_445
Rb1 O2 2.906(2) 15_554
Rb1 O2 2.906(2) 26_455
Rb1 O2 2.906(2) 14_544
Rb1 O3 2.985(2) 19
Rb1 O3 2.985(2) .
Rb1 O3 2.985(2) 3
Rb1 O3 2.985(2) 21
Rb1 O3 2.985(2) 20
Rb1 O3 2.985(2) 2
Se1 O1 1.621(3) .
Se1 O2 1.645(2) 3
Se1 O2 1.645(2) .
Se1 O2 1.645(2) 2
O2 Rb1 2.906(2) 7
O3 Fe1 1.9855(8) 2
