#------------------------------------------------------------------------------
#$Date: 2008-01-13 22:15:36 +0000 (Sun, 13 Jan 2008) $
#$Revision: 14 $
#$URL: svn://www.crystallography.net/cod/cif/4/4000413.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_4000413
_journal_name_full 'Chemistry of Materials'
_journal_year    2004
_chemical_formula_moiety         'F30 Fe10, 0.58(K0.50), 0.569(K0.50), 4(K), 0.6
_chemical_formula_structural      'F240 Fe80 K42'
_chemical_formula_sum             'F30 Fe10 K5.24'
_chemical_formula_weight          1333.52
_symmetry_cell_setting            orthorhombic
_symmetry_space_group_name_H-M    'Bbm2'
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
 1 x,y,z
 2 -x,-y,z
 3 -x,y+1/2,z
 4 x,-y+1/2,z
 5 x+1/2,y,z+1/2
 6 -x+1/2,-y,z+1/2
 7 -x+1/2,y+1/2,z+1/2
 8 x+1/2,-y+1/2,z+1/2
_cell_length_a                    35.730(3)
_cell_length_b                    17.872(1)
_cell_length_c                    7.9030(6)
_cell_angle_alpha                 90.00
_cell_angle_beta                  90.00
_cell_angle_gamma                 90.00
_cell_volume                      5046.6(7)
_cell_formula_units_Z             8
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     807
_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     3.510
_exptl_crystal_density_method     ?
_exptl_crystal_F_000              5037
_exptl_absorpt_coefficient_mu     6.650
_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_%         ?
_diffrn_reflns_number             14349
_diffrn_reflns_av_R_equivalents   0.0259
_diffrn_reflns_av_sigmaI/netI     0.0311
_diffrn_reflns_limit_h_min        -44
_diffrn_reflns_limit_h_max        46
_diffrn_reflns_limit_k_min        -15
_diffrn_reflns_limit_k_max        22
_diffrn_reflns_limit_l_min        -9
_diffrn_reflns_limit_l_max        10
_diffrn_reflns_theta_min          1.61
_diffrn_reflns_theta_max          27.49
_reflns_number_total              5333
_reflns_number_observed           1826
_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^)+(0.0311P)^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        0.000061(6)
_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    0.45(2)
_refine_ls_number_reflns          4281
_refine_ls_number_parameters      445
_refine_ls_number_restraints      1
_refine_ls_R_factor_all           0.0939
_refine_ls_R_factor_obs           0.0225
_refine_ls_wR_factor_all          0.0758
_refine_ls_wR_factor_obs          0.0506
_refine_ls_goodness_of_fit_all    0.746
_refine_ls_goodness_of_fit_obs    1.035
_refine_ls_restrained_S_all       0.826
_refine_ls_restrained_S_obs       1.035
_refine_ls_shift/esd_max          0.985
_refine_ls_shift/esd_mean         0.168
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 0.42827(5) 0.06898(10) 0.2917(3) 0.0132(4) Uani 1 d . .
Fe2 Fe 0.17835(5) -0.06873(10) 0.2920(3) 0.0124(4) Uani 1 d . .
Fe3 Fe 0.32149(5) 0.06874(10) 0.2924(3) 0.0108(4) Uani 1 d . .
Fe4 Fe 0.07141(5) -0.06898(10) 0.2918(3) 0.0110(4) Uani 1 d . .
Fe5 Fe 0.21552(5) 0.14289(10) 0.2904(2) 0.0097(4) Uani 1 d . .
Fe6 Fe 0.03458(5) 0.14335(10) 0.2927(2) 0.0134(4) Uani 1 d . .
Fe7 Fe 0.46550(5) -0.14310(10) 0.2912(2) 0.0121(4) Uani 1 d . .
Fe8 Fe 0.28429(5) -0.14294(11) 0.2916(2) 0.0122(4) Uani 1 d . .
Fe9 Fe 0.12471(8) -0.2500 0.2919(4) 0.0114(5) Uani 1 d S .
Fe10 Fe 0.37497(8) 0.2500 0.2916(4) 0.0120(5) Uani 1 d S .
Fe11 Fe 0.37475(8) -0.2500 0.2931(4) 0.0113(5) Uani 1 d S .
Fe12 Fe 0.12528(8) 0.2500 0.2926(4) 0.0124(5) Uani 1 d S .
K1 K 0.0000 0.0000 0.0410(12) 0.0131(13) Uani 0.580(7) d SP .
K2 K 0.5000 0.0000 0.0412(13) 0.0124(13) Uani 0.569(7) d SP .
K3 K 0.28759(8) 0.2500 0.0388(9) 0.0339(9) Uani 1 d S .
K4 K 0.29009(8) 0.2500 0.5406(10) 0.0440(10) Uani 1 d S .
K5 K 0.53869(9) -0.2500 0.5394(10) 0.0395(9) Uani 1 d S .
K6 K -0.03852(9) 0.2500 0.5417(10) 0.0419(9) Uani 1 d S .
K7 K 0.24999(5) 0.00007(11) 0.0414(11) 0.0221(11) Uani 0.669(6) d P .
K8 K 0.37762(8) -0.07686(7) 0.5407(7) 0.0376(4) Uani 1 d . .
K9 K 0.12842(9) 0.07939(8) 0.5408(7) 0.0393(4) Uani 1 d . .
F1 F 0.0148(3) 0.2500 0.2775(17) 0.030(3) Uani 1 d S .
F2 F 0.2360(3) 0.2500 0.2984(16) 0.027(3) Uani 1 d S .
F3 F 0.2665(3) -0.2500 0.2758(16) 0.021(3) Uani 1 d S .
F4 F 0.4835(3) -0.2500 0.2977(16) 0.017(2) Uani 1 d S .
F5 F 0.1970(2) 0.0361(4) 0.2733(12) 0.032(2) Uani 1 d . .
F6 F 0.0534(2) 0.0360(5) 0.3024(13) 0.034(2) Uani 1 d . .
F7 F 0.2677(2) 0.1061(4) 0.2969(12) 0.026(2) Uani 1 d . .
F8 F 0.4460(2) -0.0369(4) 0.2739(12) 0.027(2) Uani 1 d . .
F9 F 0.4809(2) 0.1074(5) 0.3041(12) 0.030(2) Uani 1 d . .
F10 F 0.0188(2) -0.1065(5) 0.2729(12) 0.029(2) Uani 1 d . .
F11 F 0.3023(2) -0.0366(4) 0.2960(12) 0.030(2) Uani 1 d . .
F12 F 0.2327(2) -0.1075(5) 0.2709(12) 0.034(2) Uani 1 d . .
F13 F 0.1254(2) -0.0301(3) 0.2979(13) 0.023(2) Uani 1 d . .
F14 F 0.3752(2) 0.0313(4) 0.2791(12) 0.024(2) Uani 1 d . .
F15 F 0.0891(2) 0.1664(5) 0.3076(12) 0.031(2) Uani 1 d . .
F16 F 0.3382(2) -0.1712(5) 0.3099(13) 0.031(2) Uani 1 d . .
F17 F 0.1624(2) 0.1697(5) 0.2728(13) 0.031(2) Uani 1 d . .
F18 F 0.4119(2) -0.1695(4) 0.2698(12) 0.032(2) Uani 1 d . .
F19 F 0.4158(2) 0.1771(4) 0.3005(11) 0.024(2) Uani 1 d . .
F20 F 0.1658(2) -0.1760(5) 0.3000(14) 0.039(2) Uani 1 d . .
F21 F 0.3348(2) 0.1750(4) 0.2707(13) 0.032(2) Uani 1 d . .
F22 F 0.0855(2) -0.1759(5) 0.2721(12) 0.038(3) Uani 1 d . .
F23 F 0.47223(12) -0.1479(2) 0.0387(14) 0.0257(12) Uani 1 d . .
F24 F 0.22177(13) 0.1453(3) 0.0350(15) 0.0316(13) Uani 1 d . .
F25 F 0.31905(13) 0.0612(3) 0.0373(15) 0.0318(14) Uani 1 d . .
F26 F 0.43098(13) 0.0774(3) 0.0372(15) 0.0319(13) Uani 1 d . .
F27 F 0.3795(2) 0.2500 0.0374(22) 0.043(2) Uani 1 d S .
F28 F 0.1201(2) 0.2500 0.0320(22) 0.045(2) Uani 1 d S .
F29 F 0.32484(14) 0.0697(3) 0.5347(15) 0.037(2) Uani 1 d . .
F30 F 0.42701(13) 0.0576(3) 0.5341(15) 0.0281(13) Uani 1 d . .
F31 F 0.21149(13) 0.1375(2) 0.5369(14) 0.0288(13) Uani 1 d . .
F32 F 0.46147(14) -0.1395(3) 0.5307(16) 0.0349(15) Uani 1 d . .
F33 F 0.3692(2) 0.2500 0.5429(21) 0.034(2) Uani 1 d S .
F34 F 0.13200(13) 0.2500 0.5378(19) 0.0267(14) Uani 1 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
Fe1 0.0154(9) 0.0101(9) 0.0141(11) 0.0006(11) 0.0034(10) 0.0035(7)
Fe2 0.0142(9) 0.0101(9) 0.0131(10) 0.0010(11) -0.0005(10) 0.0026(7)
Fe3 0.0150(9) 0.0066(9) 0.0107(9) -0.0004(10) 0.0006(10) -0.0001(6)
Fe4 0.0090(8) 0.0111(9) 0.0130(10) -0.0009(11) -0.0024(9) -0.0031(6)
Fe5 0.0118(8) 0.0093(9) 0.0079(10) 0.0021(9) 0.0003(10) -0.0019(7)
Fe6 0.0169(9) 0.0085(9) 0.0147(11) -0.0025(9) -0.0001(11) 0.0006(7)
Fe7 0.0143(9) 0.0076(9) 0.0145(11) 0.0022(9) -0.0001(11) -0.0014(7)
Fe8 0.0086(8) 0.0138(10) 0.0143(11) -0.0029(10) -0.0009(10) -0.0009(7)
Fe9 0.0147(11) 0.0059(11) 0.0136(11) 0.000 0.0035(13) 0.000
Fe10 0.0108(10) 0.0125(11) 0.0127(11) 0.000 -0.0033(13) 0.000
Fe11 0.0142(11) 0.0060(11) 0.0137(11) 0.000 -0.0004(14) 0.000
Fe12 0.0113(10) 0.0127(12) 0.0132(11) 0.000 0.0004(13) 0.000
K1 0.014(2) 0.019(3) 0.007(2) 0.000 0.000 0.003(2)
K2 0.009(2) 0.018(3) 0.010(3) 0.000 0.000 0.000(2)
K3 0.0212(14) 0.057(2) 0.024(2) 0.000 0.003(3) 0.000
K4 0.0178(14) 0.088(3) 0.026(2) 0.000 -0.004(3) 0.000
K5 0.031(2) 0.069(2) 0.018(2) 0.000 -0.001(3) 0.000
K6 0.032(2) 0.071(2) 0.022(2) 0.000 0.005(3) 0.000
K7 0.023(2) 0.011(2) 0.032(3) -0.003(2) -0.008(2) 0.0005(13)
K8 0.0661(11) 0.0227(8) 0.0238(8) 0.000(2) 0.002(3) -0.0133(13)
K9 0.0743(13) 0.0216(8) 0.0221(8) -0.002(2) -0.004(3) -0.0031(12)
F1 0.029(6) 0.031(7) 0.030(8) 0.000 -0.004(6) 0.000
F2 0.023(6) 0.046(7) 0.012(5) 0.000 -0.002(5) 0.000
F3 0.012(5) 0.009(5) 0.043(8) 0.000 -0.002(5) 0.000
F4 0.024(5) 0.001(4) 0.027(6) 0.000 -0.004(6) 0.000
F5 0.031(4) 0.020(4) 0.044(6) 0.002(4) 0.006(4) -0.019(3)
F6 0.042(5) 0.027(5) 0.032(5) -0.006(5) -0.002(5) 0.007(4)
F7 0.022(4) 0.018(4) 0.038(5) 0.003(4) 0.004(4) 0.002(3)
F8 0.019(4) 0.010(4) 0.052(6) 0.004(4) 0.001(5) 0.012(3)
F9 0.031(4) 0.038(5) 0.023(4) -0.001(5) 0.001(5) 0.002(4)
F10 0.006(3) 0.031(5) 0.050(6) 0.006(5) -0.001(4) -0.011(3)
F11 0.035(4) 0.023(5) 0.033(5) -0.007(4) 0.002(4) 0.009(3)
F12 0.030(4) 0.024(5) 0.047(7) -0.001(4) -0.002(4) 0.018(3)
F13 0.037(4) 0.016(3) 0.018(3) -0.002(4) -0.005(4) 0.003(4)
F14 0.012(3) 0.026(4) 0.034(5) -0.006(4) 0.002(4) -0.007(4)
F15 0.032(4) 0.032(4) 0.029(4) 0.020(4) -0.013(4) -0.021(3)
F16 0.029(4) 0.028(4) 0.036(5) 0.001(5) -0.006(5) 0.005(3)
F17 0.020(4) 0.027(5) 0.047(6) 0.000(5) 0.001(5) 0.017(4)
F18 0.024(4) 0.012(4) 0.061(7) -0.001(4) -0.002(5) 0.001(3)
F19 0.033(4) 0.012(4) 0.026(4) 0.001(4) -0.015(4) 0.013(3)
F20 0.029(5) 0.040(5) 0.046(6) 0.011(5) -0.001(5) -0.002(4)
F21 0.022(4) 0.017(4) 0.056(6) -0.002(4) -0.006(5) -0.007(3)
F22 0.034(4) 0.013(4) 0.066(7) -0.013(5) 0.004(5) 0.016(3)
F23 0.042(3) 0.026(3) 0.008(3) -0.008(5) -0.002(5) 0.006(2)
F24 0.052(3) 0.030(3) 0.012(3) -0.001(5) 0.004(6) 0.014(2)
F25 0.033(3) 0.058(3) 0.005(3) -0.007(5) -0.004(5) -0.014(2)
F26 0.038(3) 0.038(3) 0.020(3) 0.018(5) -0.001(5) 0.008(2)
F27 0.051(4) 0.055(4) 0.021(3) 0.000 0.019(8) 0.000
F28 0.077(5) 0.046(3) 0.011(3) 0.000 0.001(8) 0.000
F29 0.040(3) 0.068(4) 0.004(3) -0.014(5) -0.006(5) -0.002(2)
F30 0.026(2) 0.037(3) 0.022(3) -0.013(5) -0.005(5) 0.004(2)
F31 0.048(3) 0.023(3) 0.015(3) -0.008(5) -0.013(5) 0.003(2)
F32 0.055(3) 0.038(3) 0.011(3) -0.007(5) 0.003(5) -0.010(2)
F33 0.039(4) 0.051(3) 0.013(3) 0.000 -0.010(8) 0.000
F34 0.012(3) 0.046(3) 0.021(3) 0.000 0.015(7) 0.000