Na~4~Fe^2+^Fe^3+^(PO~4~)~3~, a new synthetic NASICON-type phosphate
Hatert, Frédéric; Acta Crystallographica Section E 65 (2009) i30–; doi:10.1107/S1600536809009210

data_2221444
_publ_section_title
;
 Na~4~Fe^2+^Fe^3+^(PO~4~)~3~, a new synthetic NASICON-type phosphate
;
_journal_coeditor_code           MG2067
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              i30
_journal_paper_doi               10.1107/S1600536809009210
_journal_volume                  65
_journal_year                    2009
_chemical_formula_analytical     Na3.96Fe2.07(PO4)3
_chemical_formula_iupac          'Na3.96 Fe2.07 (P O4)3'
_chemical_formula_moiety         'Na4 (Fe 2+) (Fe 3+) (P O4)3'
_chemical_formula_structural     Na4Fe2(PO4)3
_chemical_formula_sum            'Fe2 Na4 O12 P3'
_chemical_formula_weight         488.57
_chemical_name_common            'Tetrasodium diiron triphosphate'
_chemical_name_systematic
;
Tetrasodium diiron tris(phosphate)
;
_space_group_IT_number           167
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   8.9543(9)
_cell_length_b                   8.9543(9)
_cell_length_c                   21.280(4)
_cell_measurement_reflns_used    35
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.6
_cell_measurement_theta_min      5.9
_cell_volume                     1477.6(3)
_computing_cell_refinement       'XSCANS (Siemens, 1991)'
_computing_data_collection       'XSCANS (Siemens, 1991)'
_computing_data_reduction        'SHELXTL-Plus (Sheldrick, 2008)'
_computing_molecular_graphics    'ATOMS (Dowty, 1993)'
_computing_publication_material  'SHELXTL-Plus (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0214
_diffrn_reflns_av_sigmaI/netI    0.0194
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       1
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            721
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         3.25
_diffrn_standards_decay_%        1.9
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.680
_exptl_absorpt_correction_T_max  0.896
_exptl_absorpt_correction_T_min  0.693
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(XSCANS; Siemens, 1991)'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    3.294
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'isometric crystal'
_exptl_crystal_F_000             1422
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.030
_refine_diff_density_max         1.703
_refine_diff_density_min         -0.970
_refine_ls_extinction_coef       0.0027(6)
_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   1.399
_refine_ls_matrix_type           full
_refine_ls_number_parameters     35
_refine_ls_number_reflns         294
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.399
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0523
_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^)+(0.0415P)^2^+5P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1246
_refine_ls_wR_factor_ref         0.1250
_reflns_number_gt                284
_reflns_number_total             294
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            mg2067.cif
_cod_data_source_block           I
_cod_original_cell_volume        1477.6(4)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               2221444
_cod_database_fobs_code          2221444