K~6~[Fe~8.27~(HPO~3~)~12~]: a new mixed-valence iron phosphite
Hamchaoui, Farida; Alonzo, Véronique; Rebbah, Houria; Le Fur, Eric; Acta Crystallographica Section C 70 (2014) 351–354; doi:10.1107/S2053229614004021

data_2019443
_publ_section_title
;
 K~6~[Fe~8.27~(HPO~3~)~12~]: a new mixed-valence iron phosphite
;
_journal_coeditor_code           FN3162
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              351
_journal_page_last               354
_journal_paper_doi               10.1107/S2053229614004021
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          'K6 [Fe8.27 (H P O3)12]'
_chemical_formula_moiety         'Fe8.27 H12 O36 P12, K(6)'
_chemical_formula_sum            'Fe8.27 H12 K6 O36 P12'
_chemical_formula_weight         1656.18
_chemical_name_systematic
;
Hexapotassium octairon(II,III) dodecaphosphonate
;
_space_group_IT_number           166
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3 2"'
_symmetry_space_group_name_H-M   'R -3 m :H'
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            1
_cell_length_a                   5.38220(10)
_cell_length_b                   5.38220(10)
_cell_length_c                   34.6521(8)
_cell_measurement_reflns_used    1362
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      42.106
_cell_measurement_theta_min      2.91
_cell_volume                     869.32(3)
_computing_cell_refinement       'DIRAX/LSQ (Duisenberg <i>et al.</i>, 2000)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'EVALCCD (Duisenberg <i>et al.</i>, 2003)'
_computing_molecular_graphics    'SHELXL97 (Sheldrick, 2008)'
_computing_publication_material  'WinGX (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>, 1999)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD area-detector'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0322
_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       58
_diffrn_reflns_limit_l_min       -62
_diffrn_reflns_number            6203
_diffrn_reflns_theta_full        39.96
_diffrn_reflns_theta_max         39.96
_diffrn_reflns_theta_min         3.53
_exptl_absorpt_coefficient_mu    4.750
_exptl_absorpt_correction_T_max  0.789
_exptl_absorpt_correction_T_min  0.684
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2002)'
_exptl_crystal_colour            'dark grey'
_exptl_crystal_density_diffrn    3.164
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             809
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.692
_refine_diff_density_min         -1.066
_refine_ls_extinction_coef       0.0017(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     33
_refine_ls_number_reflns         748
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_gt           0.0266
_refine_ls_shift/su_max          0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0469P)^2^+0.4877P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0699
_reflns_number_gt                633
_reflns_number_total             748
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fn3162sup1.cf
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'R -3 m'
_cod_original_formula_sum        'Fe8.27 H12 O36 P12 K6'
_cod_database_code               2019443
_cod_database_fobs_code          2019443