#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/87/2018707.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2018707
loop_
_publ_author_name
'Dal Bo, Fabrice'
'Hatert, Frédéric'
_publ_section_title
;
 Fe~6.67~(PO₄)~5.35~(HPO₄)~0.65~ and
 Fe~6.23~(PO₄)~4.45~(HPO₄)~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^~2.67~Fe^III^~4~(PO~4~)6
_chemical_formula_iupac          'Fe6.67 (P O4)5.35 (H P O4)0.65'
_chemical_formula_moiety         'Fe6.67 H0.65 O24 P6'
_chemical_formula_sum            'Fe6.67 H0.65 O24 P6'
_chemical_formula_weight         942.93
_chemical_name_common            'Iron Phosphate'
_chemical_name_systematic
;
Heptairon pentaphosphate 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_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                105.278(14)
_cell_angle_beta                 108.055(14)
_cell_angle_gamma                101.993(14)
_cell_formula_units_Z            1
_cell_length_a                   6.3609(10)
_cell_length_b                   7.9750(13)
_cell_length_c                   9.3220(15)
_cell_measurement_reflns_used    7440
_cell_measurement_temperature    293.0
_cell_measurement_theta_max      30.4120
_cell_measurement_theta_min      2.4507
_cell_volume                     411.55(14)
_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 et al., 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 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Agilent Xcalibur Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_limit_h_max       8
_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            21890
_diffrn_reflns_theta_full        30.48
_diffrn_reflns_theta_max         30.48
_diffrn_reflns_theta_min         2.46
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    6.437
_exptl_absorpt_correction_T_max  0.64000
_exptl_absorpt_correction_T_min  0.54272
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Agilent, 2012)
;
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    3.804
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Isometric crystal'
_exptl_crystal_F_000             456.07
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.622
_refine_diff_density_min         -0.501
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_matrix_type           full
_refine_ls_number_parameters     170
_refine_ls_number_reflns         2404
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0306
_refine_ls_R_factor_gt           0.0239
_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/[σ²(Fo²)+(0.0224P)²+0.4764P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0550
_refine_ls_wR_factor_ref         0.0571
_reflns_number_gt                2084
_reflns_number_total             2404
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            fn3113.cif
_cod_data_source_block           H339
_cod_original_cell_volume        411.55(12)
_cod_database_code               2018707
_cod_database_fobs_code          2018707
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
Fe Fe1 0.11782(6) 0.04568(5) 0.38554(4) 0.01338(8) Uani d . 1 1
Fe Fe2 0.45486(6) -0.22200(5) -0.02741(4) 0.01292(9) Uani d . 1 1
Fe Fe3 0.5000 0.5000 0.5000 0.01590(11) Uani d S 1 2
Fe Fe4 0.21811(7) -0.31143(6) 0.21270(5) 0.01511(14) Uani d P 0.8369(18) 1
P P1 0.40324(10) -0.09557(8) 0.66575(7) 0.01167(12) Uani d . 1 1
P P2 -0.27138(10) -0.34924(8) 0.26723(7) 0.01186(12) Uani d . 1 1
P P3 -0.09965(11) -0.26775(9) -0.12952(7) 0.01258(12) Uani d . 1 1
O O1 0.1896(3) -0.0383(2) 0.5847(2) 0.0139(3) Uani d . 1 1
O O2 -0.0426(3) -0.2318(2) 0.2725(2) 0.0141(3) Uani d . 1 1
O O3 0.5193(3) -0.3106(2) 0.1581(2) 0.0146(3) Uani d . 1 1
O O4 0.1344(3) -0.2605(2) -0.0070(2) 0.0156(3) Uani d . 1 1
O O5 0.3790(3) -0.0296(2) 0.3387(2) 0.0152(3) Uani d . 1 1
O O6 0.4322(3) -0.0519(2) -0.1545(2) 0.0137(3) Uani d . 1 1
O O7 -0.2224(3) -0.4589(2) -0.2611(2) 0.0183(4) Uani d . 1 1
O O8 0.3704(3) -0.2918(2) 0.5788(2) 0.0196(4) Uani d . 1 1
O O9 0.7502(3) -0.2188(3) -0.0368(2) 0.0192(4) Uani d . 1 1
O O10 -0.2888(3) -0.5483(2) 0.2046(2) 0.0172(4) Uani d . 1 1
O O11 0.0503(3) 0.1327(3) 0.2131(2) 0.0191(4) Uani d . 1 1
O O12 0.2714(3) 0.3008(2) 0.5591(2) 0.0150(3) Uani d . 1 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
O1 Fe1 O1 2_556 . 82.49(7)
O1 Fe1 O2 2_556 . 82.94(7)
O2 Fe1 O1 . . 79.79(7)
O5 Fe1 O1 . . 90.53(7)
O5 Fe1 O1 . 2_556 162.52(7)
O5 Fe1 O2 . . 80.05(7)
O5 Fe1 O12 . . 105.50(7)
O11 Fe1 O1 . . 176.80(8)
O11 Fe1 O1 . 2_556 95.73(8)
O11 Fe1 O2 . . 102.68(8)
O11 Fe1 O5 . . 91.90(8)
O11 Fe1 O12 . . 94.46(8)
O12 Fe1 O1 . . 82.88(7)
O12 Fe1 O1 . 2_556 89.59(7)
O12 Fe1 O2 . . 161.87(7)
O3 Fe2 O4 . . 80.51(7)
O3 Fe2 O6 . 2_655 85.77(7)
O3 Fe2 O6 . . 160.98(7)
O4 Fe2 O6 . 2_655 87.28(7)
O6 Fe2 O4 . . 99.45(7)
O6 Fe2 O6 . 2_655 75.25(7)
O9 Fe2 O3 . . 92.25(8)
O9 Fe2 O4 . . 171.18(8)
O9 Fe2 O6 . 2_655 97.27(8)
O9 Fe2 O6 . . 89.04(8)
O9 Fe2 O10 . 2_545 94.14(8)
O10 Fe2 O3 2_545 . 100.35(8)
O10 Fe2 O4 2_545 . 82.31(8)
O10 Fe2 O6 2_545 . 98.48(8)
O10 Fe2 O6 2_545 2_655 166.84(7)
O12 Fe3 O12 . 2_666 180.0
O12 Fe3 O7 . 2 94.64(7)
O12 Fe3 O7 2_666 2 85.36(7)
O12 Fe3 O7 2_666 1_666 94.64(7)
O12 Fe3 O7 . 1_666 85.36(7)
O7 Fe3 O7 2 1_666 180.00(9)
O8 Fe3 O12 2_656 2_666 93.32(7)
O8 Fe3 O12 1_565 . 93.32(7)
O8 Fe3 O12 2_656 . 86.68(7)
O8 Fe3 O12 1_565 2_666 86.68(7)
O8 Fe3 O7 1_565 2 81.40(7)
O8 Fe3 O7 2_656 2 98.60(7)
O8 Fe3 O7 1_565 1_666 98.60(7)
O8 Fe3 O7 2_656 1_666 81.40(7)
O8 Fe3 O8 2_656 1_565 179.9990(10)
O2 Fe4 O3 . . 163.02(7)
O2 Fe4 O4 . . 96.12(7)
O2 Fe4 O5 . . 77.69(7)
O4 Fe4 O3 . . 76.48(7)
O5 Fe4 O3 . . 86.85(7)
O5 Fe4 O4 . . 89.29(7)
O7 Fe4 O2 2_545 . 106.40(7)
O7 Fe4 O3 2_545 . 89.61(7)
O7 Fe4 O4 2_545 . 131.85(7)
O7 Fe4 O5 2_545 . 136.39(7)
O1 P1 O6 . 1_556 105.76(10)
O5 P1 O1 2_656 . 107.68(10)
O5 P1 O6 2_656 1_556 108.29(10)
O8 P1 O1 . . 111.23(11)
O8 P1 O6 . 1_556 113.87(10)
O8 P1 O5 . 2_656 109.75(11)
O2 P2 O3 . 1_455 109.81(10)
O2 P2 O12 . 2_556 109.72(10)
O3 P2 O12 1_455 2_556 108.83(10)
O10 P2 O2 . . 108.78(10)
O10 P2 O3 . 1_455 110.94(10)
O10 P2 O12 . 2_556 108.74(10)
O9 P3 O4 1_455 . 107.65(10)
O9 P3 O11 1_455 2 111.43(11)
O9 P3 O7 1_455 . 110.85(11)
O11 P3 O4 2 . 108.84(11)
O11 P3 O7 2 . 107.18(11)
O7 P3 O4 . . 110.91(10)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Fe1 O1 . 2.0877(17)
Fe1 O1 2_556 2.0501(17)
Fe1 O2 . 2.0529(18)
Fe1 O5 . 2.0092(18)
Fe1 O11 . 1.8802(18)
Fe1 O12 . 2.0423(18)
Fe2 O3 . 1.9955(18)
Fe2 O4 . 2.0727(18)
Fe2 O6 . 2.0215(17)
Fe2 O6 2_655 2.1921(18)
Fe2 O9 . 1.9028(18)
Fe2 O10 2_545 1.9290(19)
Fe3 O12 . 2.2222(17)
Fe3 O12 2_666 2.2222(17)
Fe3 O7 2 2.2635(18)
Fe3 O7 1_666 2.2635(18)
Fe3 O8 2_656 2.0688(18)
Fe3 O8 1_565 2.0688(18)
Fe4 O2 . 2.0712(18)
Fe4 O3 . 2.1284(18)
Fe4 O4 . 2.1198(18)
Fe4 O5 . 2.0941(19)
Fe4 O7 2_545 2.0017(19)
P1 O1 . 1.5588(18)
P1 O6 1_556 1.5611(18)
P1 O5 2_656 1.5493(18)
P1 O8 . 1.4963(19)
P2 O2 . 1.5368(18)
P2 O3 1_455 1.5490(18)
P2 O12 2_556 1.5627(18)
P2 O10 . 1.5070(19)
P3 O4 . 1.5495(18)
P3 O9 1_455 1.5170(19)
P3 O11 2 1.5225(19)
P3 O7 . 1.5377(19)
