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_7012816
_publ_section_title
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 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         '2Fe, 1.5(C4N2H11.6), H2O, 2(H0.8PO4), PO4'
_chemical_formula_sum            'C6 H21 Fe2 N3 O13 P3'
_chemical_formula_weight         547.87
_chemical_name_common
;
piperazinedium-(bis(mu-hydrogenphosphato) (mu4-
phosphato)diferrate(II,III))-hydrate
;
_chemical_name_systematic
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piperazinedium-[bis(mu-hydrogenphosphato)
(mu4-phosphato)diferrate(II,III)]-hydrate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 93.950(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.3704(15)
_cell_length_b                   8.5616(15)
_cell_length_c                   23.865(4)
_cell_measurement_temperature    213(2)
_cell_volume                     1706.2(5)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker 1997)'
_computing_data_reduction        'SAINT (Bruker 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.922
_diffrn_measured_fraction_theta_max 0.922
_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  0.0186
_diffrn_reflns_av_sigmaI/netI    0.0206
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            14884
_diffrn_reflns_theta_full        28.89
_diffrn_reflns_theta_max         28.89
_diffrn_reflns_theta_min         2.44
_exptl_absorpt_coefficient_mu    2.057
_exptl_absorpt_correction_T_max  0.7904
_exptl_absorpt_correction_T_min  0.5869
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'deep blue'
_exptl_crystal_density_diffrn    2.133
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             1116
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.451
_refine_diff_density_min         -0.577
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         4137
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0295
_refine_ls_R_factor_gt           0.0240
_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^)+(0.0405P)^2^+0.2957P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0637
_refine_ls_wR_factor_ref         0.0659
_reflns_number_gt                3487
_reflns_number_total             4137
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b301610b.txt
_cod_data_source_block           k4
_cod_depositor_comments
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The following automatic conversions were performed:
'_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 
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_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7012816