#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/87/2018708.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_2018708
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^~2.228~Fe^III^~4~(PO~4~)6
_chemical_formula_iupac          'Fe6.23 (P O4)4.45 (H P O4)1.55'
_chemical_formula_moiety         'Fe6.23 H1.55 O24 P6'
_chemical_formula_sum            'Fe6.23 H1.55 O24 P6'
_chemical_formula_weight         919.26
_chemical_name_common            'Iron Phosphate'
_chemical_name_systematic
;
Heptairon tetraphosphate bis(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_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                105.303(3)
_cell_angle_beta                 108.176(3)
_cell_angle_gamma                101.700(3)
_cell_formula_units_Z            1
_cell_length_a                   6.3445(2)
_cell_length_b                   7.9353(3)
_cell_length_c                   9.2829(3)
_cell_measurement_reflns_used    11179
_cell_measurement_temperature    293.0
_cell_measurement_theta_max      30.4031
_cell_measurement_theta_min      2.4619
_cell_volume                     407.03(3)
_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 0.963
_diffrn_measured_fraction_theta_max 0.963
_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  0.0310
_diffrn_reflns_limit_h_max       9
_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            21571
_diffrn_reflns_theta_full        30.47
_diffrn_reflns_theta_max         30.47
_diffrn_reflns_theta_min         2.47
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    6.131
_exptl_absorpt_correction_T_max  0.786
_exptl_absorpt_correction_T_min  0.573
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
[CrysAlis PRO (Agilent, 2012), based on expressions derived by
Clark & Reid (1995)]
;
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    3.750
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Isometric crystal'
_exptl_crystal_F_000             445.53
_exptl_crystal_size_max          0.1519
_exptl_crystal_size_mid          0.1035
_exptl_crystal_size_min          0.0577
_refine_diff_density_max         0.956
_refine_diff_density_min         -0.677
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.138
_refine_ls_matrix_type           full
_refine_ls_number_parameters     170
_refine_ls_number_reflns         2378
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.138
_refine_ls_R_factor_all          0.0309
_refine_ls_R_factor_gt           0.0267
_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)+(0.0503P)²+0.6294P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0831
_refine_ls_wR_factor_ref         0.0854
_reflns_number_gt                2167
_reflns_number_total             2378
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            fn3113.cif
_cod_data_source_block           H347
_cod_original_cell_volume        407.03(2)
_cod_database_code               2018708
_cod_database_fobs_code          2018708
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 -0.61697(6) 0.45850(5) 0.11678(4) 0.00709(11) Uani d . 1 1
Fe Fe2 -0.04932(6) 0.27698(5) 0.47371(5) 0.00698(11) Uani d . 1 1
Fe Fe3 1.0000 1.0000 0.0000 0.00897(13) Uani d S 1 2
Fe Fe4 0.28654(11) 0.81443(9) 0.28898(8) 0.0096(2) Uani d P 0.614(2) 1
P P1 -0.09424(11) 0.40554(9) 0.16637(8) 0.00517(14) Uani d . 1 1
P P2 0.77367(11) 0.84989(9) 0.23196(8) 0.00504(13) Uani d . 1 1
P P3 -0.60279(11) 0.23246(9) 0.36786(8) 0.00614(14) Uani d . 1 1
O O1 -0.3109(3) 0.4594(3) 0.0836(2) 0.0071(4) Uani d . 1 1
O O2 0.1212(3) 0.5322(3) 0.1611(2) 0.0084(4) Uani d . 1 1
O O3 0.5450(3) 0.7327(3) 0.2271(2) 0.0081(3) Uani d . 1 1
O O4 -0.0673(3) 0.4494(3) 0.3459(2) 0.0072(3) Uani d . 1 1
O O5 0.7909(3) 1.0499(3) 0.2929(2) 0.0104(4) Uani d . 1 1
O O6 0.9837(3) 0.8120(3) 0.3417(2) 0.0085(4) Uani d . 1 1
O O7 0.7306(4) 0.9574(3) -0.2321(3) 0.0145(4) Uani d . 1 1
O O8 -0.5490(4) 0.3726(3) 0.2886(2) 0.0123(4) Uani d . 1 1
O O9 -0.3711(3) 0.2344(3) 0.4892(2) 0.0103(4) Uani d . 1 1
O O10 0.2474(3) 0.2797(3) 0.4626(2) 0.0118(4) Uani d . 1 1
O O11 0.7749(3) 0.8007(3) 0.0575(2) 0.0081(4) Uani d . 1 1
O O12 0.8785(4) 1.2081(3) 0.0811(3) 0.0139(4) 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'
Fe Fe 0.3463 0.8444 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-8 1 9 0.0383
0 6 7 0.0279
5 -7 -7 0.0327
3 -5 -10 0.0312
6 1 -12 0.0269
3 -1 -12 0.0228
-3 -2 13 0.0305
-1 7 -12 0.0286
9 -3 -5 0.0191
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_465 82.31(8)
O1 Fe1 O11 . 2_565 89.06(8)
O3 Fe1 O1 1_455 2_465 79.82(8)
O3 Fe1 O1 1_455 . 83.24(8)
O3 Fe1 O11 1_455 2_565 161.92(8)
O2 Fe1 O1 1_455 . 164.01(8)
O2 Fe1 O1 1_455 2_465 90.55(8)
O2 Fe1 O3 1_455 1_455 81.42(8)
O2 Fe1 O11 1_455 2_565 104.31(8)
O11 Fe1 O1 2_565 2_465 82.96(8)
O8 Fe1 O1 . 2_465 176.45(9)
O8 Fe1 O1 . . 95.60(8)
O8 Fe1 O3 . 1_455 102.83(8)
O8 Fe1 O2 . 1_455 92.18(9)
O8 Fe1 O11 . 2_565 94.16(9)
O4 Fe2 O4 . 2_566 74.85(8)
O4 Fe2 O9 . . 100.32(8)
O5 Fe2 O4 1_445 2_566 167.77(8)
O5 Fe2 O4 1_445 . 97.53(8)
O5 Fe2 O6 1_445 2_666 101.47(8)
O5 Fe2 O9 1_445 . 82.49(9)
O6 Fe2 O4 2_666 2_566 86.23(8)
O6 Fe2 O4 2_666 . 160.96(8)
O6 Fe2 O9 2_666 . 81.21(8)
O9 Fe2 O4 . 2_566 89.40(8)
O10 Fe2 O4 . 2_566 96.57(8)
O10 Fe2 O4 . . 87.76(8)
O10 Fe2 O5 . 1_445 92.61(9)
O10 Fe2 O6 . 2_666 92.45(8)
O10 Fe2 O9 . . 171.01(9)
O11 Fe3 O11 2_775 . 180.0
O12 Fe3 O11 2_775 2_775 94.28(8)
O12 Fe3 O11 . 2_775 85.72(8)
O12 Fe3 O11 2_775 . 85.72(8)
O12 Fe3 O11 . . 94.28(8)
O12 Fe3 O12 2_775 . 180.00(10)
O12 Fe3 O7 2_775 . 97.10(8)
O12 Fe3 O7 . 2_775 97.10(8)
O12 Fe3 O7 . . 82.90(8)
O12 Fe3 O7 2_775 2_775 82.90(8)
O7 Fe3 O11 2_775 . 85.84(7)
O7 Fe3 O11 . . 94.16(7)
O7 Fe3 O11 . 2_775 85.84(7)
O7 Fe3 O11 2_775 2_775 94.16(7)
O7 Fe3 O7 2_775 . 180.0
O3 Fe4 O6 . 1_455 162.47(8)
O3 Fe4 O2 . . 78.04(8)
O3 Fe4 O9 . 2_566 96.77(8)
O2 Fe4 O6 . 1_455 85.71(8)
O2 Fe4 O9 . 2_566 90.12(8)
O9 Fe4 O6 2_566 1_455 76.56(7)
O7 Fe4 O3 2_675 . 107.08(9)
O7 Fe4 O6 2_675 1_455 88.87(8)
O7 Fe4 O2 2_675 . 133.66(9)
O7 Fe4 O9 2_675 2_566 132.99(9)
O3 P2 O6 . . 110.00(11)
O3 P2 O11 . . 110.02(11)
O5 P2 O3 . . 109.10(11)
O5 P2 O6 . . 110.91(11)
O5 P2 O11 . . 108.23(11)
O6 P2 O11 . . 108.56(11)
O1 P1 O4 . . 105.52(11)
O2 P1 O1 . . 107.80(11)
O2 P1 O4 . . 108.80(11)
O12 P1 O1 1_445 . 111.44(12)
O12 P1 O4 1_445 . 113.52(11)
O12 P1 O2 1_445 . 109.54(12)
O9 P3 O7 . 2_565 111.39(12)
O10 P3 O9 1_455 . 107.21(11)
O10 P3 O8 1_455 . 111.87(12)
O10 P3 O7 1_455 2_565 110.15(12)
O8 P3 O9 . . 108.64(11)
O8 P3 O7 . 2_565 107.60(12)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Fe1 O1 2_465 2.0792(19)
Fe1 O1 . 2.0576(18)
Fe1 O3 1_455 2.025(2)
Fe1 O2 1_455 1.9910(19)
Fe1 O11 2_565 2.0614(19)
Fe1 O8 . 1.8597(19)
Fe2 O4 . 2.0314(18)
Fe2 O4 2_566 2.1731(19)
Fe2 O5 1_445 1.922(2)
Fe2 O6 2_666 1.9805(19)
Fe2 O9 . 2.0573(19)
Fe2 O10 . 1.914(2)
Fe3 O11 2_775 2.1979(19)
Fe3 O11 . 2.1979(19)
Fe3 O12 . 2.027(2)
Fe3 O12 2_775 2.027(2)
Fe3 O7 2_775 2.182(2)
Fe3 O7 . 2.182(2)
Fe4 O3 . 2.064(2)
Fe4 O6 1_455 2.123(2)
Fe4 O2 . 2.096(2)
Fe4 O9 2_566 2.120(2)
Fe4 O7 2_675 2.029(2)
P2 O3 . 1.537(2)
P2 O5 . 1.506(2)
P2 O6 . 1.5427(19)
P2 O11 . 1.5652(19)
P1 O1 . 1.5542(19)
P1 O4 . 1.5559(19)
P1 O2 . 1.5462(19)
P1 O12 1_445 1.504(2)
P3 O9 . 1.542(2)
P3 O10 1_455 1.519(2)
P3 O8 . 1.526(2)
P3 O7 2_565 1.543(2)
