#------------------------------------------------------------------------------
#$Date: 2016-02-17 16:11:22 +0200 (Wed, 17 Feb 2016) $
#$Revision: 176648 $
#$URL: svn://www.crystallography.net/cod/cif/2/24/14/2241434.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2241434
loop_
_publ_author_name
'Larrea, Edurne S.'
'Mesa, José Luis'
'Legarra, Estibaliz'
'Aguayo, Andrés Tomás'
'Arriortua, Maria Isabel'
_publ_section_title
;
 Crystal structure of
 K~0.75~[FeII~3.75~FeIII~1.25~(HPO₃)₆]·0.5H₂O, an
 open-framework iron phosphite with mixed-valent FeII/FeIII ions
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              63
_journal_page_last               65
_journal_paper_doi               10.1107/S2056989015024007
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac
'K0.75 [FeII3.75FeIII1.25 (H P O3)6] , 0.5H2 O'
_chemical_formula_moiety         '0.5(Fe10 H12 K1.5 O36 P12), 0.5(H2 O)'
_chemical_formula_sum            'Fe5 H7 K0.75 O18.5 P6'
_chemical_formula_weight         797.45
_chemical_name_systematic
;
Potassium hexaphosphitopentaferrate(II,III) hemihydrate
;
_space_group_IT_number           165
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3 2"c'
_symmetry_space_group_name_H-M   'P -3 c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   10.1567(5)
_cell_length_b                   10.1567(5)
_cell_length_c                   9.2774(6)
_cell_measurement_reflns_used    3002
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.961
_cell_measurement_theta_min      2.301
_cell_volume                     828.82(8)
_computing_cell_refinement
;
CrysAlis Pro (Agilent, 2014)
;
_computing_data_collection
;
CrysAlis Pro (Agilent, 2014)
;
_computing_data_reduction
;
CrysAlis Pro (Agilent, 2014)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2001)
;
_computing_publication_material
;
WinGX (Farrugia, 2012)
;
_computing_structure_refinement
;
SHELXL-2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
OLEX2 (Dolomanov, 2009)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.2439
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.94
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  'Multilayer optics'
_diffrn_radiation_source         'Nova (Mo) X-ray micro-source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0255
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5132
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         28.17
_diffrn_reflns_theta_min         2.32
_exptl_absorpt_coefficient_mu    5.141
_exptl_absorpt_correction_T_max  0.845
_exptl_absorpt_correction_T_min  0.423
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
(CrysAlis Pro; Agilent, 2014)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    3.195
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             779
_exptl_crystal_size_max          0.287
_exptl_crystal_size_mid          0.048
_exptl_crystal_size_min          0.036
_refine_diff_density_max         0.8
_refine_diff_density_min         -0.499
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.187
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     54
_refine_ls_number_reflns         647
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.187
_refine_ls_R_factor_all          0.0271
_refine_ls_R_factor_gt           0.0256
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0254P)²+2.2546P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0607
_reflns_number_gt                618
_reflns_number_total             647
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            wm5216sup1.cif
_cod_data_source_block           I
_cod_depositor_comments
;Adding full bibliography for 2241434.cif.

 Adding full bibliography for 2241434.cif.
;
_cod_original_formula_sum        'Fe5 H7 K0.75 O18.50 P6'
_cod_database_code               2241434
_cod_database_fobs_code          2241434
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'y, x, -z+1/2'
'-x+y, -x, z'
'-x, -x+y, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'-y, -x, z-1/2'
'x-y, x, -z'
'x, x-y, z-1/2'
'-x+y, y, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_group
Fe Fe1 0.62108(5) 0 0.25 0.00709(16) Uani d S 1 .
Fe Fe2 0.6667 0.3333 0.33159(7) 0.00659(18) Uani d S 1 .
P P1 0.70307(8) 0.11196(8) 0.58780(7) 0.00748(18) Uani d . 1 .
O O3 0.6916(2) 0.1569(2) 0.4316(2) 0.0110(4) Uani d . 1 .
O O2 0.3954(2) -0.1473(2) 0.3120(2) 0.0095(4) Uani d . 1 .
O O1 0.8210(2) 0.1342(2) 0.1437(2) 0.0124(4) Uani d . 1 .
K K1 1 0 0.25 0.0247(5) Uani d SP 0.75 1
O O1W 1 0 0.063(2) 0.033(4) Uani d SP 0.25 2
H H1 0.645(4) -0.033(4) 0.592(4) 0.011(9) Uiso d . 1 .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 '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'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
O1 Fe1 O1 . 6 97.50(12)
O1 Fe1 O2 . . 167.07(8)
O1 Fe1 O2 6 . 89.81(8)
O1 Fe1 O2 . 6 89.81(8)
O1 Fe1 O2 6 6 167.07(8)
O2 Fe1 O2 . 6 85.10(11)
O1 Fe1 O3 . 6 90.97(8)
O1 Fe1 O3 6 6 91.82(8)
O2 Fe1 O3 . 6 78.11(8)
O2 Fe1 O3 6 6 98.73(7)
O1 Fe1 O3 . . 91.82(8)
O1 Fe1 O3 6 . 90.97(8)
O2 Fe1 O3 . . 98.73(7)
O2 Fe1 O3 6 . 78.11(8)
O3 Fe1 O3 6 . 175.77(11)
O1 Fe1 K1 . . 48.75(6)
O1 Fe1 K1 6 . 48.75(6)
O2 Fe1 K1 . . 137.45(6)
O2 Fe1 K1 6 . 137.45(6)
O3 Fe1 K1 6 . 92.11(5)
O3 Fe1 K1 . . 92.11(5)
O2 Fe2 O2 6 3_655 85.13(8)
O2 Fe2 O2 6 5_665 85.13(8)
O2 Fe2 O2 3_655 5_665 85.13(8)
O2 Fe2 O3 6 . 78.10(8)
O2 Fe2 O3 3_655 . 93.44(7)
O2 Fe2 O3 5_665 . 163.22(8)
O2 Fe2 O3 6 2_655 163.23(8)
O2 Fe2 O3 3_655 2_655 78.10(8)
O2 Fe2 O3 5_665 2_655 93.44(7)
O3 Fe2 O3 . 2_655 102.63(7)
O2 Fe2 O3 6 4_665 93.44(7)
O2 Fe2 O3 3_655 4_665 163.22(8)
O2 Fe2 O3 5_665 4_665 78.10(8)
O3 Fe2 O3 . 4_665 102.63(7)
O3 Fe2 O3 2_655 4_665 102.63(7)
O1 P1 O2 9_666 7_656 112.13(11)
O1 P1 O3 9_666 . 114.32(11)
O2 P1 O3 7_656 . 110.24(11)
O1 P1 H1 9_666 . 105.9(16)
O2 P1 H1 7_656 . 105.6(16)
O3 P1 H1 . . 108.1(16)
P1 O3 Fe2 . . 135.47(12)
P1 O3 Fe1 . . 123.82(12)
Fe2 O3 Fe1 . . 98.26(8)
P1 O2 Fe1 7_656 . 127.45(12)
P1 O2 Fe2 7_656 3_545 130.31(12)
Fe1 O2 Fe2 . 3_545 101.19(8)
P1 O1 Fe1 9_665 . 129.84(13)
P1 O1 K1 9_665 . 124.86(11)
Fe1 O1 K1 . . 99.63(7)
O1 K1 O1 2_645 5_765 171.12(8)
O1 K1 O1 2_645 4_765 109.30(4)
O1 K1 O1 5_765 4_765 63.23(8)
O1 K1 O1 2_645 3_645 63.23(8)
O1 K1 O1 5_765 3_645 109.30(4)
O1 K1 O1 4_765 3_645 78.54(8)
O1 K1 O1 2_645 . 109.30(4)
O1 K1 O1 5_765 . 78.54(8)
O1 K1 O1 4_765 . 109.30(4)
O1 K1 O1 3_645 . 171.12(8)
O1 K1 O1 2_645 6 78.54(8)
O1 K1 O1 5_765 6 109.30(4)
O1 K1 O1 4_765 6 171.12(8)
O1 K1 O1 3_645 6 109.30(4)
O1 K1 O1 . 6 63.23(8)
O1 K1 Fe1 2_645 4_765 140.73(4)
O1 K1 Fe1 5_765 4_765 31.62(4)
O1 K1 Fe1 4_765 4_765 31.62(4)
O1 K1 Fe1 3_645 4_765 94.44(4)
O1 K1 Fe1 . 4_765 94.44(4)
O1 K1 Fe1 6 4_765 140.73(4)
O1 K1 Fe1 2_645 2_645 31.62(4)
O1 K1 Fe1 5_765 2_645 140.73(4)
O1 K1 Fe1 4_765 2_645 94.44(4)
O1 K1 Fe1 3_645 2_645 31.62(4)
O1 K1 Fe1 . 2_645 140.73(4)
O1 K1 Fe1 6 2_645 94.44(4)
Fe1 K1 Fe1 4_765 2_645 120
O1 K1 Fe1 2_645 . 94.44(4)
O1 K1 Fe1 5_765 . 94.44(4)
O1 K1 Fe1 4_765 . 140.73(4)
O1 K1 Fe1 3_645 . 140.73(4)
O1 K1 Fe1 . . 31.62(4)
O1 K1 Fe1 6 . 31.62(4)
Fe1 K1 Fe1 4_765 . 120
Fe1 K1 Fe1 2_645 . 120
O1 K1 K1 2_645 7_756 109.64(4)
O1 K1 K1 5_765 7_756 70.36(4)
O1 K1 K1 4_765 7_756 109.64(4)
O1 K1 K1 3_645 7_756 70.36(4)
O1 K1 K1 . 7_756 109.64(4)
O1 K1 K1 6 7_756 70.36(4)
Fe1 K1 K1 4_765 7_756 90
Fe1 K1 K1 2_645 7_756 90
Fe1 K1 K1 . 7_756 90
O1 K1 K1 2_645 7_755 70.36(4)
O1 K1 K1 5_765 7_755 109.64(4)
O1 K1 K1 4_765 7_755 70.36(4)
O1 K1 K1 3_645 7_755 109.64(4)
O1 K1 K1 . 7_755 70.36(4)
O1 K1 K1 6 7_755 109.64(4)
Fe1 K1 K1 4_765 7_755 90
Fe1 K1 K1 2_645 7_755 90
Fe1 K1 K1 . 7_755 90
K1 K1 K1 7_756 7_755 180
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Fe1 O1 . 2.046(2)
Fe1 O1 6 2.046(2)
Fe1 O2 . 2.096(2)
Fe1 O2 6 2.096(2)
Fe1 O3 6 2.179(2)
Fe1 O3 . 2.179(2)
Fe1 K1 . 3.8486(6)
Fe2 O2 6 2.134(2)
Fe2 O2 3_655 2.134(2)
Fe2 O2 5_665 2.134(2)
Fe2 O3 . 2.143(2)
Fe2 O3 2_655 2.143(2)
Fe2 O3 4_665 2.143(2)
P1 O1 9_666 1.529(2)
P1 O2 7_656 1.534(2)
P1 O3 . 1.541(2)
P1 H1 . 1.29(4)
O2 P1 7_656 1.534(2)
O2 Fe2 3_545 2.134(2)
O1 P1 9_665 1.529(2)
O1 K1 . 2.935(2)
K1 O1 2_645 2.935(2)
K1 O1 5_765 2.935(2)
K1 O1 4_765 2.935(2)
K1 O1 3_645 2.935(2)
K1 O1 6 2.935(2)
K1 Fe1 4_765 3.8486(6)
K1 Fe1 2_645 3.8486(6)
K1 K1 7_756 4.6387(3)
K1 K1 7_755 4.6387(3)
O1W O1W 7_755 1.17(4)
