#------------------------------------------------------------------------------
#$Date: 2016-02-19 23:18:51 +0100 (vie 19 de feb de 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/30/2013012.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_2013012
loop_
_publ_author_name
'Lajmi, Besma'
'Hidouri, Mourad'
'Ben Amara, Mongi'
_publ_section_title
;
 The iron phosphate K₃Fe₅(PO₄)₆
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              i156
_journal_page_last               i158
_journal_paper_doi               10.1107/S0108270102015251
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          'K3 Fe5 (P O4)6'
_chemical_formula_structural     'K3 Fe5 (P O4)6'
_chemical_formula_sum            'Fe5 K3 O24 P6'
_chemical_formula_weight         966.37
_chemical_name_systematic        ?
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.22(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.460(4)
_cell_length_b                   30.997(7)
_cell_length_c                   10.665(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12
_cell_measurement_theta_min      7
_cell_volume                     2135.6(15)
_computing_cell_refinement       'CAD-4 EXPRESS'
_computing_data_collection       'CAD-4 EXPRESS (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'ATOMS (Dowty, 1994)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1993)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4'
_diffrn_measurement_method       ω/2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56087
_diffrn_reflns_av_R_equivalents  0.0303
_diffrn_reflns_av_sigmaI/netI    0.0279
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7763
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.54
_diffrn_standards_decay_%        2
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    2.298
_exptl_absorpt_correction_T_max  0.7104
_exptl_absorpt_correction_T_min  0.6302
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   '(Katayama, 1986)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    3.006
_exptl_crystal_density_meas      3.05(5)
_exptl_crystal_density_method    pycnometry
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1876
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.755
_refine_diff_density_min         -0.793
_refine_ls_extinction_coef       0.00198(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         3823
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0254
_refine_ls_R_factor_gt           0.0186
_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/[σ²(Fo²)+(0.0214P)²+4.5065P] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0487
_refine_ls_wR_factor_ref         0.0505
_reflns_number_gt                3354
_reflns_number_total             3823
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            br1386.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2013012
_cod_database_fobs_code          2013012
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_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_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Fe1 0.2500 0.2500 0.5000 0.00582(6) Uani d S 1 . . Fe
Fe2 0.0000 0.189384(10) 0.2500 0.00677(6) Uani d S 1 . . Fe
Fe3 0.0000 0.193115(10) 0.7500 0.00679(6) Uani d S 1 . . Fe
Fe4 0.24698(3) 0.049909(7) 0.57712(2) 0.00737(5) Uani d . 1 . . Fe
P1 0.0000 0.278396(17) 0.2500 0.00575(9) Uani d S 1 . . P
O11 0.18853(17) 0.30583(4) 0.22474(11) 0.00946(19) Uani d . 1 . . O
O12 0.03724(17) 0.24513(3) 0.35948(10) 0.00758(18) Uani d . 1 . . O
P2 0.0000 0.281775(17) 0.7500 0.00594(9) Uani d S 1 . . P
O21 0.03802(17) 0.24838(4) 0.64090(10) 0.00749(18) Uani d . 1 . . O
O22 0.18915(17) 0.30916(4) 0.77764(11) 0.00936(19) Uani d . 1 . . O
P3 0.14632(6) 0.148952(12) 0.50261(3) 0.00607(7) Uani d . 1 . . P
O31 0.01426(18) 0.14707(4) 0.38235(11) 0.0108(2) Uani d . 1 . . O
O32 0.00308(18) 0.15329(4) 0.61488(11) 0.0116(2) Uani d . 1 . . O
O33 0.27196(18) 0.10763(4) 0.51169(12) 0.0123(2) Uani d . 1 . . O
O34 0.29346(17) 0.18761(3) 0.49822(10) 0.00887(19) Uani d . 1 . . O
P4 0.24699(6) 0.030414(12) 0.87738(4) 0.00673(7) Uani d . 1 . . P
O41 0.22854(19) 0.02291(4) 0.73522(11) 0.0145(2) Uani d . 1 . . O
O42 0.44496(18) 0.05457(4) 0.91038(13) 0.0164(2) Uani d . 1 . . O
O43 0.06373(19) 0.05619(4) 0.92864(13) 0.0161(2) Uani d . 1 . . O
O44 0.2465(2) -0.01530(4) 0.93308(12) 0.0180(2) Uani d . 1 . . O
K1 0.64766(6) 0.138114(15) 0.51135(4) 0.02211(9) Uani d . 1 . . K
K2 0.0000 0.93923(3) 0.7500 0.0477(2) Uani d S 1 . . K
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.0667 0.0580 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.1399 0.1562 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.2886 0.5448 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
2 -4 3
-2 -4 -3
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
_geom_angle_publ_flag
O34 Fe1 O34 7_556 . 180.0 ?
O34 Fe1 O12 7_556 7_556 90.92(5) yes
O34 Fe1 O12 . 7_556 89.08(5) yes
O34 Fe1 O12 7_556 . 89.08(5) ?
O34 Fe1 O12 . . 90.92(5) ?
O12 Fe1 O12 7_556 . 180.0 ?
O34 Fe1 O21 7_556 . 85.42(5) yes
O34 Fe1 O21 . . 94.58(5) yes
O12 Fe1 O21 7_556 . 84.99(6) yes
O12 Fe1 O21 . . 95.01(6) yes
O34 Fe1 O21 7_556 7_556 94.58(5) ?
O34 Fe1 O21 . 7_556 85.42(5) ?
O12 Fe1 O21 7_556 7_556 95.01(6) ?
O12 Fe1 O21 . 7_556 84.99(6) ?
O21 Fe1 O21 . 7_556 180.0 ?
O31 Fe2 O31 . 2 94.31(7) yes
O31 Fe2 O22 . 8_455 87.33(6) yes
O31 Fe2 O22 2 8_455 94.41(6) yes
O31 Fe2 O22 . 7_556 94.41(6) ?
O31 Fe2 O22 2 7_556 87.33(6) ?
O22 Fe2 O22 8_455 7_556 177.45(6) yes
O31 Fe2 O12 . 2 166.43(5) yes
O31 Fe2 O12 2 2 98.49(5) yes
O22 Fe2 O12 8_455 2 87.20(5) yes
O22 Fe2 O12 7_556 2 90.70(5) yes
O31 Fe2 O12 . . 98.49(5) ?
O31 Fe2 O12 2 . 166.43(5) ?
O22 Fe2 O12 8_455 . 90.70(5) ?
O22 Fe2 O12 7_556 . 87.20(5) ?
O12 Fe2 O12 2 . 69.17(6) yes
O32 Fe3 O32 . 2_556 98.84(8) yes
O32 Fe3 O11 . 8_456 85.58(6) yes
O32 Fe3 O11 2_556 8_456 95.63(6) yes
O32 Fe3 O11 . 7_556 95.63(6) ?
O32 Fe3 O11 2_556 7_556 85.58(6) ?
O11 Fe3 O11 8_456 7_556 178.15(7) yes
O32 Fe3 O21 . 2_556 163.62(5) yes
O32 Fe3 O21 2_556 2_556 96.26(5) yes
O11 Fe3 O21 8_456 2_556 86.68(5) yes
O11 Fe3 O21 7_556 2_556 91.81(5) yes
O32 Fe3 O21 . . 96.26(5) ?
O32 Fe3 O21 2_556 . 163.62(5) ?
O11 Fe3 O21 8_456 . 91.81(5) ?
O11 Fe3 O21 7_556 . 86.68(5) ?
O21 Fe3 O21 2_556 . 69.57(6) yes
O44 Fe4 O41 6 . 118.61(6) yes
O44 Fe4 O33 6 . 103.56(6) yes
O41 Fe4 O33 . . 137.82(6) yes
O44 Fe4 O42 6 2_656 95.42(7) yes
O41 Fe4 O42 . 2_656 92.22(6) yes
O33 Fe4 O42 . 2_656 82.67(5) yes
O44 Fe4 O43 6 2_556 91.83(7) yes
O41 Fe4 O43 . 2_556 90.22(7) yes
O33 Fe4 O43 . 2_556 89.08(5) yes
O42 Fe4 O43 2_656 2_556 170.10(6) yes
O11 P1 O11 . 2 111.48(10) yes
O11 P1 O12 . . 112.32(7) yes
O11 P1 O12 2 . 110.93(7) yes
O11 P1 O12 . 2 110.93(7) ?
O11 P1 O12 2 2 112.32(7) ?
O12 P1 O12 . 2 98.24(9) yes
O22 P2 O22 2_556 . 111.89(10) yes
O22 P2 O21 2_556 . 110.59(6) yes
O22 P2 O21 . . 112.54(7) yes
O22 P2 O21 2_556 2_556 112.54(7) ?
O22 P2 O21 . 2_556 110.59(6) ?
O21 P2 O21 . 2_556 97.97(9) yes
O33 P3 O32 . . 110.52(7) yes
O33 P3 O34 . . 109.29(7) yes
O32 P3 O34 . . 109.54(7) yes
O33 P3 O31 . . 108.39(7) yes
O32 P3 O31 . . 108.80(8) yes
O34 P3 O31 . . 110.28(7) yes
O42 P4 O43 . . 108.11(8) yes
O42 P4 O44 . . 111.53(8) yes
O43 P4 O44 . . 109.92(8) yes
O42 P4 O41 . . 111.36(8) yes
O43 P4 O41 . . 111.95(8) yes
O44 P4 O41 . . 103.96(7) yes
O32 K1 O33 1_655 . 152.98(5) ?
O32 K1 O31 1_655 1_655 55.39(5) ?
O33 K1 O31 . 1_655 147.07(5) ?
O32 K1 O34 1_655 . 130.94(5) ?
O33 K1 O34 . . 55.18(5) ?
O31 K1 O34 1_655 . 129.25(5) ?
O32 K1 O42 1_655 2_656 103.44(4) ?
O33 K1 O42 . 2_656 57.40(4) ?
O31 K1 O42 1_655 2_656 115.39(4) ?
O34 K1 O42 . 2_656 110.68(5) ?
O32 K1 O11 1_655 8_556 58.23(4) ?
O33 K1 O11 . 8_556 107.51(5) ?
O31 K1 O11 1_655 8_556 104.93(4) ?
O34 K1 O11 . 8_556 77.15(5) ?
O42 K1 O11 2_656 8_556 110.10(4) ?
O32 K1 O22 1_655 8 100.02(5) ?
O33 K1 O22 . 8 106.60(5) ?
O31 K1 O22 1_655 8 56.62(4) ?
O34 K1 O22 . 8 74.39(5) ?
O42 K1 O22 2_656 8 140.97(4) ?
O11 K1 O22 8_556 8 108.72(4) ?
O32 K1 O43 1_655 2_656 62.96(4) ?
O33 K1 O43 . 2_656 104.65(5) ?
O31 K1 O43 1_655 2_656 71.34(4) ?
O34 K1 O43 . 2_656 158.49(4) ?
O42 K1 O43 2_656 2_656 48.01(4) ?
O11 K1 O43 8_556 2_656 105.57(4) ?
O22 K1 O43 8 2_656 122.93(4) ?
O44 K2 O44 1_565 2_566 121.47(6) ?
O44 K2 O41 1_565 1_565 48.68(4) ?
O44 K2 O41 2_566 1_565 79.15(5) ?
O44 K2 O41 1_565 2_566 79.15(5) ?
O44 K2 O41 2_566 2_566 48.68(4) ?
O41 K2 O41 1_565 2_566 59.59(6) ?
O44 K2 O31 1_565 5_566 139.81(4) ?
O44 K2 O31 2_566 5_566 95.77(4) ?
O41 K2 O31 1_565 5_566 139.18(4) ?
O41 K2 O31 2_566 5_566 141.04(4) ?
O44 K2 O31 1_565 6_566 95.77(4) ?
O44 K2 O31 2_566 6_566 139.81(4) ?
O41 K2 O31 1_565 6_566 141.04(4) ?
O41 K2 O31 2_566 6_566 139.18(4) ?
O31 K2 O31 5_566 6_566 55.73(5) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Fe1 O34 7_556 1.9544(12) yes
Fe1 O34 . 1.9544(12) ?
Fe1 O12 7_556 2.0351(14) yes
Fe1 O12 . 2.0351(14) ?
Fe1 O21 . 2.0376(14) yes
Fe1 O21 7_556 2.0376(14) ?
Fe2 O31 . 1.9289(12) yes
Fe2 O31 2 1.9289(12) ?
Fe2 O22 8_455 2.0312(16) yes
Fe2 O22 7_556 2.0312(16) ?
Fe2 O12 2 2.0987(12) yes
Fe2 O12 . 2.0988(12) ?
Fe2 P1 . 2.7591(9) ?
Fe2 K1 1_455 3.9400(15) ?
Fe2 K1 2_655 3.9400(15) ?
Fe2 K2 5_566 3.9865(12) ?
Fe3 O32 . 1.8977(12) yes
Fe3 O32 2_556 1.8977(12) ?
Fe3 O11 8_456 2.0293(16) yes
Fe3 O11 7_556 2.0293(17) ?
Fe3 O21 2_556 2.0859(12) yes
Fe3 O21 . 2.0859(12) ?
Fe3 P2 . 2.7482(9) ?
Fe3 K1 1_455 3.8107(15) ?
Fe3 K1 2_656 3.8107(15) ?
Fe4 O44 6 1.8736(13) yes
Fe4 O41 . 1.8867(12) yes
Fe4 O33 . 1.9273(12) yes
Fe4 O42 2_656 1.9992(17) yes
Fe4 O43 2_556 2.0173(17) yes
Fe4 K1 . 3.8316(13) ?
Fe4 K2 5_566 3.8454(13) ?
P1 O11 . 1.5105(13) yes
P1 O11 2 1.5105(13) ?
P1 O12 . 1.5756(11) yes
P1 O12 2 1.5756(11) ?
P1 K1 7_556 3.7556(9) ?
P1 K1 8_455 3.7556(9) ?
O11 Fe3 7_556 2.0293(16) ?
O11 K1 8_455 2.8746(13) ?
P2 O22 2_556 1.5158(13) yes
P2 O22 . 1.5158(13) ?
P2 O21 . 1.5772(11) yes
P2 O21 2_556 1.5772(12) ?
P2 K1 8_456 3.8503(9) ?
P2 K1 7_556 3.8503(9) ?
O22 Fe2 7_556 2.0312(16) ?
O22 K1 8_456 2.9934(13) ?
P3 O33 . 1.5193(12) yes
P3 O32 . 1.5220(13) yes
P3 O34 . 1.5302(12) yes
P3 O31 . 1.5387(13) yes
P3 K1 1_455 3.241(2) ?
P3 K1 . 3.257(2) ?
O31 K1 1_455 2.757(2) ?
O31 K2 5_566 3.0257(15) ?
O32 K1 1_455 2.5870(19) ?
O33 K1 . 2.6045(18) ?
O34 K1 . 2.7579(17) ?
P4 O42 . 1.5220(14) yes
P4 O43 . 1.5310(14) yes
P4 O44 . 1.5366(13) yes
P4 O41 . 1.5380(13) yes
P4 K2 1_545 3.5163(11) ?
P4 K1 2_656 3.6070(9) ?
O41 K2 1_545 2.9890(16) ?
O42 Fe4 2_656 1.9992(17) ?
O42 K1 2_656 2.7867(15) ?
O43 Fe4 2_556 2.0173(17) ?
O43 K1 2_656 3.2132(16) ?
O44 Fe4 6_556 1.8736(13) ?
O44 K2 1_545 2.8830(18) ?
K1 O32 1_655 2.5870(19) yes
K1 O33 . 2.6045(18) yes
K1 O31 1_655 2.757(2) yes
K1 O34 . 2.7579(17) yes
K1 O42 2_656 2.7867(15) yes
K1 O11 8_556 2.8746(13) yes
K1 O22 8 2.9934(13) yes
K1 O43 2_656 3.2132(16) yes
K1 P3 1_655 3.241(2) ?
K1 P4 2_656 3.6070(9) ?
K1 P1 7_556 3.7556(9) ?
K2 O44 1_565 2.8830(18) yes
K2 O44 2_566 2.8830(18) ?
K2 O41 1_565 2.9890(16) yes
K2 O41 2_566 2.9890(16) ?
K2 O31 5_566 3.0257(15) yes
K2 O31 6_566 3.0257(15) ?
K2 P4 1_565 3.5163(11) ?
K2 P4 2_566 3.5163(11) ?
K2 Fe4 6_566 3.8454(13) ?
K2 Fe4 5_566 3.8454(13) ?
K2 Fe2 5_566 3.9865(13) ?
K2 K1 6_466 4.3296(15) ?
