Crystal structure of K~0.75~[Fe^II^~3.75~Fe^III^~1.25~(HPO~3~)~6~]·0.5H~2~O, an open-framework iron phosphite with mixed-valent Fe^II^/Fe^III^ ions
Larrea, Edurne S.; Mesa, José Luis; Legarra, Estibaliz; Aguayo, Andrés Tomás; Arriortua, Maria Isabel; Acta Crystallographica Section E 72 (2016) 63–65; doi:10.1107/S2056989015024007

data_2241434
_publ_section_title
;
 Crystal structure of
 K~0.75~[Fe^II^~3.75~Fe^III^~1.25~(HPO~3~)~6~]&#x00B7;0.5H~2~O, an
 open-framework iron phosphite with mixed-valent Fe^II^/Fe^III^ 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
;
<i>OLEX2</i> (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       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova'
_diffrn_measurement_method       '\w 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
;
(<i>CrysAlis Pro</i>; 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/[\s^2^(Fo^2^)+(0.0254P)^2^+2.2546P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0607
_reflns_number_gt                618
_reflns_number_total             647
_reflns_threshold_expression     >2\s(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