Fe~6.67~(PO~4~)~5.35~(HPO~4~)~0.65~ and Fe~6.23~(PO~4~)~4.45~(HPO~4~)~1.55~: two new mixed-valence iron phosphates
Dal Bo, Fabrice; Hatert, Frédéric; Acta Crystallographica Section C 68 (2012) i83–i85; doi:10.1107/S0108270112043016

data_2018708
_publ_section_title
;
 Fe~6.67~(PO~4~)~5.35~(HPO~4~)~0.65~ and
 Fe~6.23~(PO~4~)~4.45~(HPO~4~)~1.55~: two new mixed-valence iron
 phosphates
;
_journal_coeditor_code           FN3113
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              i83
_journal_page_last               i85
_journal_paper_doi               10.1107/S0108270112043016
_journal_volume                  68
_journal_year                    2012
_chemical_formula_analytical     Fe^II^~2.228~Fe^III^~4~(PO~4~)6
_chemical_formula_iupac          'Fe6.23 (P O4)4.45 (H P O4)1.55'
_chemical_formula_moiety         'Fe6.23 H1.55 O24 P6'
_chemical_formula_sum            'Fe6.23 H1.55 O24 P6'
_chemical_formula_weight         919.26
_chemical_name_common            'Iron Phosphate'
_chemical_name_systematic
;
Heptairon tetraphosphate bis(hydrogen phosphate)
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                105.303(3)
_cell_angle_beta                 108.176(3)
_cell_angle_gamma                101.700(3)
_cell_formula_units_Z            1
_cell_length_a                   6.3445(2)
_cell_length_b                   7.9353(3)
_cell_length_c                   9.2829(3)
_cell_measurement_reflns_used    11179
_cell_measurement_temperature    293.0
_cell_measurement_theta_max      30.4031
_cell_measurement_theta_min      2.4619
_cell_volume                     407.03(3)
_computing_cell_refinement
;
CrysAlis PRO (Agilent, 2012)
;
_computing_data_collection
;
CrysAlis PRO (Agilent, 2012)
;
_computing_data_reduction
;
CrysAlis PRO (Agilent, 2012)
;
_computing_molecular_graphics
;
ATOMS (Dowty, 1993)
;
_computing_publication_material
;
OLEX2 (Dolomanov <i>et al.</i>, 2009)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293
_diffrn_detector_area_resol_mean 16.0087
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Agilent Xcalibur Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0310
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            21571
_diffrn_reflns_theta_full        30.47
_diffrn_reflns_theta_max         30.47
_diffrn_reflns_theta_min         2.47
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    6.131
_exptl_absorpt_correction_T_max  0.786
_exptl_absorpt_correction_T_min  0.573
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
[CrysAlis PRO (Agilent, 2012), based on expressions derived by
Clark & Reid (1995)]
;
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    3.750
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Isometric crystal'
_exptl_crystal_F_000             445.53
_exptl_crystal_size_max          0.1519
_exptl_crystal_size_mid          0.1035
_exptl_crystal_size_min          0.0577
_refine_diff_density_max         0.956
_refine_diff_density_min         -0.677
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.138
_refine_ls_matrix_type           full
_refine_ls_number_parameters     170
_refine_ls_number_reflns         2378
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.138
_refine_ls_R_factor_all          0.0309
_refine_ls_R_factor_gt           0.0267
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0503P)^2^+0.6294P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0831
_refine_ls_wR_factor_ref         0.0854
_reflns_number_gt                2167
_reflns_number_total             2378
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            fn3113.cif
_cod_data_source_block           H347
_cod_original_cell_volume        407.03(2)
_cod_database_code               2018708
_cod_database_fobs_code          2018708