Tetrahedrally Coordinated Iron(II) Incorporation in the Super-Sodalite Aluminophosphate Fe~3~Al~6~(PO~4~)~12~·4tren·17H~2~O (MIL-74)
Beitone, Lionel; Loiseau, Thierry; Millange, Franck; Huguenard, Clarisse; Fink, Gerhard; Taulelle, Francis; Grenèche, Jean-Marc; Férey, Gérard; Chemistry of Materials 15 (2003) 4590–4597; doi:10.1021/cm034535d

data_1101170
_publ_section_title
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 Tetrahedrally Coordinated Iron(II) Incorporation in the Super-Sodalite
 Aluminophosphate Fe~3~Al~6~(PO~4~)~12~&#x00B7;4tren&#x00B7;17H~2~O (MIL-74)
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_journal_coden_ASTM              CMATEX
_journal_issue                   24
_journal_name_full               'Chemistry of Materials'
_journal_page_first              4590
_journal_page_last               4597
_journal_paper_doi               10.1021/cm034535d
_journal_volume                  15
_journal_year                    2003
_chemical_formula_sum            'C24 H118 Al6 Fe3 N16 O65 P12'
_chemical_formula_weight         2372.41
_space_group_IT_number           217
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  'I -4 2 3'
_symmetry_space_group_name_H-M   'I -4 3 m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.77050(10)
_cell_length_b                   16.77050(10)
_cell_length_c                   16.77050(10)
_cell_measurement_temperature    293(2)
_cell_volume                     4716.70(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_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  0.0183
_diffrn_reflns_av_sigmaI/netI    0.0092
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            16616
_diffrn_reflns_theta_full        29.80
_diffrn_reflns_theta_max         29.80
_diffrn_reflns_theta_min         2.43
_exptl_absorpt_coefficient_mu    0.829
_exptl_crystal_density_diffrn    1.670
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2460
_refine_diff_density_max         0.635
_refine_diff_density_min         -0.433
_refine_diff_density_rms         0.089
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.05(4)
_refine_ls_extinction_coef       0.0009(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.252
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     66
_refine_ls_number_reflns         1245
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.252
_refine_ls_R_factor_all          0.0328
_refine_ls_R_factor_gt           0.0327
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0640P)^2^+2.3364P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0991
_refine_ls_wR_factor_ref         0.0993
_reflns_number_gt                1238
_reflns_number_total             1245
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             4000328
_cod_data_source_file            cm034535dsi20030625_053928.cif
_cod_data_source_block           lb1491
_cod_database_code               1101170