Mixed-valence phosphato?hydrogenphosphato?iron network compounds 1?{[C4N2H11.6]1.5[FeIIFeIII(PO4)(H0.8PO4)2]�H2O} and 3?[FeII5FeIII2(PO4)2(H0.5PO4)4]: structure elucidation with the help of M�ssbauer spectroscopy and a caveat on X-ray diffraction
Abu-Shandi, Khalid; Winkler, Heiner; Gerdan, Michael; Emmerling, Franziska; Wu, Biao; Janiak, Christoph; Dalton Transactions  (2003) 2815–; doi:10.1039/b301610b

data_7012817
_publ_section_title
;
 Mixed-valence phosphato?hydrogenphosphato?iron network compounds
 1?{[C4N2H11.6]1.5[FeIIFeIII(PO4)(H0.8PO4)2]&#xFFFD;H2O} and
 3?[FeII5FeIII2(PO4)2(H0.5PO4)4]: structure elucidation with the help
 of M&#xFFFD;ssbauer spectroscopy and a caveat on X-ray diffraction
;
_journal_issue                   14
_journal_name_full               'Dalton Transactions'
_journal_page_first              2815
_journal_paper_doi               10.1039/b301610b
_journal_year                    2003
_chemical_formula_moiety         'Fe7, (H0.5PO4)4, (PO4)2'
_chemical_formula_sum            'Fe3.5 H O12 P3'
_chemical_formula_weight         481.39
_chemical_name_common
;
Bis(mu6,7-hydrogenphosphato)-tetrakis(mu7-phosphato)-di-
iron(iii)-penta-iron(ii)
;
_chemical_name_systematic
;
Bis(mu6,7-hydrogenphosphato)-tetrakis(mu7-phosphato)-
di-iron(III)-penta-iron(II)
;
_space_group_IT_number           2
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                103.874(6)
_cell_angle_beta                 109.286(6)
_cell_angle_gamma                101.577(6)
_cell_formula_units_Z            2
_cell_length_a                   6.562(3)
_cell_length_b                   7.980(4)
_cell_length_c                   9.536(4)
_cell_measurement_temperature    293(2)
_cell_volume                     435.7(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.909
_diffrn_measured_fraction_theta_max 0.909
_diffrn_measurement_device_type  'Bruker AXS CCD'
_diffrn_measurement_method       '\w scan'
_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  0.0185
_diffrn_reflns_av_sigmaI/netI    0.0311
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3935
_diffrn_reflns_theta_full        28.64
_diffrn_reflns_theta_max         28.64
_diffrn_reflns_theta_min         2.40
_exptl_absorpt_coefficient_mu    6.351
_exptl_absorpt_correction_T_max  0.5418
_exptl_absorpt_correction_T_min  0.1401
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black-green
_exptl_crystal_density_diffrn    3.669
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       isometric
_exptl_crystal_F_000             466
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.620
_refine_diff_density_min         -0.729
_refine_diff_density_rms         0.189
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         2030
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0283
_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^)+(0.0410P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0699
_refine_ls_wR_factor_ref         0.0712
_reflns_number_gt                1773
_reflns_number_total             2030
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b301610b.txt
_cod_data_source_block           k9
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Multi-scan' changed
to 'multi-scan' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'H Fe3.50 O12 P3'
_cod_database_code               7012817