#------------------------------------------------------------------------------
#$Date: 2008-01-13 22:15:36 +0000 (Sun, 13 Jan 2008) $
#$Revision: 14 $
#$URL: svn://www.crystallography.net/cod/cif/4/4000412.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_4000412
_journal_name_full 'Chemistry of Materials'
_journal_year    2004
_publ_section_title
;
Charge order and tilt modulation in multiferroic K~x~M^2+~x~M^3+~1-x~F~3~
(0.4<x<0.6) transition metal fluorides with tetragonal tungsten bronze structure
;
loop_
    _publ_author_name
    'Fabbrici, Simone'
    'Montanari, Erica'
    'Righi, Lara'
    'Calestani, Gianluca'
    'Migliori, Andrea'
_chemical_formula_moiety          '2(F15 Fe5), 4(K), 5(K0.25)'
_chemical_formula_structural      'F30 Fe10 K5.25'
_chemical_formula_sum             'F30 Fe10 K5.25'
_chemical_formula_weight          1333.78
_symmetry_cell_setting            tetragonal
_symmetry_space_group_name_H-M    'P4bm'
loop_
    _symmetry_equiv_pos_site_id
    _symmetry_equiv_pos_as_xyz
    1 x,y,z
    2 -x,-y,z
    3 -y,x,z
    4 y,-x,z
    5 -x+1/2,y+1/2,z
    6 x+1/2,-y+1/2,z
    7 y+1/2,x+1/2,z
    8 -y+1/2,-x+1/2,z
_cell_length_a                    12.6340(10)
_cell_length_b                    12.6340(10)
_cell_length_c                    3.9515(3)
_cell_angle_alpha                 90.00
_cell_angle_beta                  90.00
_cell_angle_gamma                 90.00
_cell_volume                      630.73(9)
_cell_formula_units_Z             1
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     330
_cell_measurement_theta_min       5.1
_cell_measurement_theta_max       27.5
_exptl_crystal_description        'prism'
_exptl_crystal_colour             'brown'
_exptl_crystal_size_max           .113
_exptl_crystal_size_mid           .064
_exptl_crystal_size_min           .048
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     3.5112
_exptl_crystal_density_method     ?
_exptl_crystal_F_000              629.8
_exptl_absorpt_coefficient_mu     6.652
_exptl_absorpt_correction_type    empirical
_exptl_absorpt_correction_T_min   0.606
_exptl_absorpt_correction_T_max   0.727
_diffrn_ambient_temperature       293(2)
_diffrn_radiation_wavelength      0.71069
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'fine-focus sealed tube'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device        'Bruker AXS 100 CCD'
_diffrn_measurement_method        '/f and /w scans'
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         0
_diffrn_reflns_number             5162
_diffrn_reflns_av_R_equivalents   0.0373
_diffrn_reflns_av_sigmaI/netI     0.0216
_diffrn_reflns_limit_h_min        -15
_diffrn_reflns_limit_h_max        15
_diffrn_reflns_limit_k_min        -15
_diffrn_reflns_limit_k_max        15
_diffrn_reflns_limit_l_min        -5
_diffrn_reflns_limit_l_max        5
_diffrn_reflns_theta_min          2.28
_diffrn_reflns_theta_max          27.50
_reflns_number_total              753
_reflns_number_observed           642
_reflns_observed_criterion        'I>2sigma(I)'
'SMART Program Package (Bruker AXS Inc., 1998)'
'SMART Program Package (Bruker AXS Inc., 1998)'
'SAINT Program Package (Bruker AXS Inc., 1998)'
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme
 'calc w=1/[\s^2^(Fo^2^)+(0.0315P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    ?
_refine_ls_hydrogen_treatment     ?
_refine_ls_extinction_method      SHELXL
_refine_ls_extinction_coef        0.0022(5)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^'
_refine_ls_abs_structure_details
 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack    0.52(5)
_refine_ls_number_reflns          747
_refine_ls_number_parameters      63
_refine_ls_number_restraints      1
_refine_ls_R_factor_all           0.0272
_refine_ls_R_factor_obs           0.0215
_refine_ls_wR_factor_all          0.0515
_refine_ls_wR_factor_obs          0.0497
_refine_ls_goodness_of_fit_all    1.000
_refine_ls_goodness_of_fit_obs    1.050
_refine_ls_restrained_S_all       0.996
_refine_ls_restrained_S_obs       1.049
_refine_ls_shift/esd_max          1.795
_refine_ls_shift/esd_mean         0.353
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_thermal_displace_type
 _atom_site_occupancy
 _atom_site_calc_flag
 _atom_site_refinement_flags
 _atom_site_disorder_group
Fe1 Fe 0.5000 0.0000 0.4988(10) 0.0118(2) Uani 1 d S .
Fe2 Fe 0.21199(3) 0.07421(2) 0.50003(2) 0.01193(14) Uani 1 d . .
K1 K 0.17231(5) 0.32769(5) -0.0007(18) 0.0413(3) Uani 1 d S .
K2 K 0.0000 0.0000 0.0036(29) 0.0173(5) Uani 0.625(4) d SP .
F1 F 0.14322(14) -0.07018(12) 0.4883(29) 0.0339(5) Uani 1 d . .
F2 F 0.28080(12) 0.21920(12) 0.4942(39) 0.0251(6) Uani 1 d S .
F3 F 0.34563(13) -0.00673(15) 0.4887(27) 0.0380(7) Uani 1 d . .
F4 F 0.5000 0.0000 -0.0175(73) 0.0523(12) Uani 1 d S .
F5 F 0.2090(2) 0.0766(2) -0.0165(44) 0.0423(9) Uani 1 d . .
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 0.0114(2) 0.0114(2) 0.0126(4) 0.000 0.000 -0.0003(3)
Fe2 0.0125(2) 0.0112(2) 0.0121(2) -0.0007(13) 0.000(2) 0.00048(13)
K1 0.0511(4) 0.0511(4) 0.0218(6) -0.002(2) 0.002(2) 0.0262(5)
K2 0.0172(7) 0.0172(7) 0.0175(10) 0.000 0.000 0.000
F1 0.0326(10) 0.0188(8) 0.0503(14) 0.004(4) -0.008(5) -0.0039(7)
F2 0.0215(7) 0.0215(7) 0.032(2) 0.002(4) -0.002(4) -0.0016(9)
F3 0.0149(8) 0.0377(10) 0.061(2) -0.016(4) -0.004(4) 0.0020(8)
F4 0.071(2) 0.071(2) 0.015(3) 0.000 0.000 -0.003(2)
F5 0.0432(11) 0.0748(15) 0.009(2) 0.002(4) -0.003(4) -0.0197(9)