#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/86/2228654.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_2228654
loop_
_publ_author_name
'Hidouri, Mourad'
'Ben Amara, Mongi'
_publ_section_title
;
 K~0.53~Mn~2.37~Fe~1.24~(PO₄)₃
;
_journal_coeditor_code           BR2150
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              i1
_journal_paper_doi               10.1107/S1600536810051238
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'K0.53 Mn2.37 Fe1.24 (P O4)3'
_chemical_formula_structural     'K0.53 Mn2.37 Fe1.24 P3 O12'
_chemical_formula_sum            'Fe1.24 K0.53 Mn2.37 O12 P3'
_chemical_formula_weight         505.28
_chemical_name_systematic
;
Potassium dimanganese iron triphosphate
;
_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                 114.87(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.272(2)
_cell_length_b                   12.606(2)
_cell_length_c                   6.416(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14.38
_cell_measurement_theta_min      9.78
_cell_volume                     900.5(6)
_computing_cell_refinement       'CAD-4 EXPRESS (Enraf--Nonius, 1994)'
_computing_data_collection       'CAD-4 EXPRESS (Enraf--Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare et al., 1993)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf--Nonius TurboCAD-4'
_diffrn_measurement_method       'non-profiled omega/2theta'
_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  0.0421
_diffrn_reflns_av_sigmaI/netI    0.0450
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1754
_diffrn_reflns_theta_full        29.97
_diffrn_reflns_theta_max         29.97
_diffrn_reflns_theta_min         2.44
_diffrn_standards_decay_%        1
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    6.072
_exptl_absorpt_correction_T_max  0.81
_exptl_absorpt_correction_T_min  0.42
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
(Parkin et al., 1995)
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    3.727
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             957
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.781
_refine_diff_density_min         -0.675
_refine_ls_extinction_coef       0.0009(4)
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_matrix_type           full
_refine_ls_number_parameters     102
_refine_ls_number_reflns         1308
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0536
_refine_ls_R_factor_gt           0.0367
_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)+(0.0451P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0826
_refine_ls_wR_factor_ref         0.0890
_reflns_number_gt                1047
_reflns_number_total             1308
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            br2150.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2228654
_cod_database_fobs_code          2228654
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_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_disorder_assembly
_atom_site_disorder_group
K K 0.0000 -0.0116(2) 0.2500 0.0229(7) Uani d SP 0.531(5) . .
Mn Mn1 0.0000 0.26376(7) 0.2500 0.0156(2) Uani d S 1 . .
Fe Fe2 0.22489(4) 0.15521(4) 0.13977(8) 0.01004(16) Uani d P 0.6217(6) . .
Mn Mn2 0.22489(4) 0.15521(4) 0.13977(8) 0.01004(16) Uani d P 0.3783(7) . .
Mn Mn3 -0.02360(17) 0.49774(17) 0.0393(4) 0.0209(5) Uani d P 0.3064(12) . .
P P1 0.0000 0.28642(11) -0.2500 0.0096(3) Uani d S 1 . .
O O11 0.0479(2) 0.2160(2) -0.0331(4) 0.0138(5) Uani d . 1 . .
O O12 -0.0942(3) 0.3615(2) -0.2314(6) 0.0251(7) Uani d . 1 . .
P P2 0.24436(8) 0.10810(7) 0.63905(15) 0.0093(2) Uani d . 1 . .
O O21 0.2272(2) 0.1782(2) 0.8220(4) 0.0156(6) Uani d . 1 . .
O O22 0.1735(3) 0.1629(2) 0.4048(4) 0.0169(6) Uani d . 1 . .
O O23 0.3783(2) 0.1019(2) 0.6976(6) 0.0255(7) Uani d . 1 . .
O O24 0.1930(2) -0.0019(2) 0.6349(5) 0.0178(6) Uani d . 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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 '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'
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
3 -5 0
3 3 2
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
O24 K O24 . 2 174.63(16) ?
O24 K O24 . 6 73.24(8) ?
O24 K O24 2 6 106.42(8) ?
O24 K O24 . 5_556 106.42(8) ?
O24 K O24 2 5_556 73.24(8) ?
O24 K O24 6 5_556 172.95(16) ?
O24 K O11 . 5 114.87(10) ?
O24 K O11 2 5 70.34(8) ?
O24 K O11 6 5 87.10(9) ?
O24 K O11 5_556 5 99.26(10) ?
O24 K O11 . 6_556 70.34(8) ?
O24 K O11 2 6_556 114.87(10) ?
O24 K O11 6 6_556 99.26(10) ?
O24 K O11 5_556 6_556 87.10(9) ?
O11 K O11 5 6_556 52.22(11) ?
O24 K O22 . . 53.32(8) ?
O24 K O22 2 . 121.80(11) ?
O24 K O22 6 . 57.49(9) ?
O24 K O22 5_556 . 116.43(11) ?
O11 K O22 5 . 144.11(8) ?
O11 K O22 6_556 . 122.58(8) ?
O24 K O22 . 2 121.80(11) ?
O24 K O22 2 2 53.32(8) ?
O24 K O22 6 2 116.43(11) ?
O24 K O22 5_556 2 57.49(9) ?
O11 K O22 5 2 122.58(8) ?
O11 K O22 6_556 2 144.11(8) ?
O22 K O22 . 2 82.66(13) ?
O23 Mn3 O23 7_556 8_455 75.91(14) ?
O23 Mn3 O12 7_556 5_565 84.68(13) ?
O23 Mn3 O12 8_455 5_565 121.62(16) ?
Mn1 Mn3 O12 5_565 . 76.0(3) ?
O23 Mn3 O12 7_556 . 94.38(14) ?
O23 Mn3 O12 8_455 . 79.85(14) ?
O12 Mn3 O12 5_565 . 157.20(11) ?
Mn1 Mn3 O23 5_565 3_454 69.7(3) ?
O23 Mn3 O23 7_556 3_454 157.58(11) ?
O23 Mn3 O23 8_455 3_454 123.93(15) ?
O12 Mn3 O23 5_565 3_454 91.62(14) ?
O12 Mn3 O23 . 3_454 80.58(13) ?
O23 Mn1 O23 7_556 8_455 78.61(15) ?
O23 Mn1 O11 7_556 . 86.39(11) ?
O23 Mn1 O11 8_455 . 118.95(12) ?
O23 Mn1 O11 7_556 2 118.95(12) ?
O23 Mn1 O11 8_455 2 86.39(11) ?
O11 Mn1 O11 . 2 148.43(15) ?
O23 Mn1 O22 7_556 2 159.42(10) ?
O23 Mn1 O22 8_455 2 85.06(10) ?
O11 Mn1 O22 . 2 90.70(10) ?
O11 Mn1 O22 2 2 71.87(10) ?
O23 Mn1 O22 7_556 . 85.06(10) ?
O23 Mn1 O22 8_455 . 159.42(10) ?
O11 Mn1 O22 . . 71.87(10) ?
O11 Mn1 O22 2 . 90.70(10) ?
O22 Mn1 O22 2 . 113.36(14) ?
O24 Fe2 O12 6 8_556 94.65(12) ?
O24 Fe2 O22 6 . 86.05(12) ?
O12 Fe2 O22 8_556 . 109.44(13) ?
O24 Fe2 O21 6 1_554 101.92(12) ?
O12 Fe2 O21 8_556 1_554 87.13(12) ?
O22 Fe2 O21 . 1_554 161.16(11) ?
O24 Fe2 O11 6 . 101.11(11) ?
O12 Fe2 O11 8_556 . 162.62(11) ?
O22 Fe2 O11 . . 79.18(11) ?
O21 Fe2 O11 1_554 . 82.52(11) ?
O24 Fe2 O21 6 7_556 174.59(11) ?
O12 Fe2 O21 8_556 7_556 81.71(11) ?
O22 Fe2 O21 . 7_556 91.37(11) ?
O21 Fe2 O21 1_554 7_556 81.97(11) ?
O11 Fe2 O21 . 7_556 83.04(10) ?
O12 P1 O12 2_554 . 104.0(3) ?
O12 P1 O11 2_554 2_554 107.33(17) ?
O12 P1 O11 . 2_554 114.23(15) ?
O12 P1 O11 2_554 . 114.23(15) ?
O12 P1 O11 . . 107.33(17) ?
O11 P1 O11 2_554 . 109.7(2) ?
O24 P2 O23 . . 110.71(16) ?
O24 P2 O22 . . 109.32(15) ?
O23 P2 O22 . . 111.67(18) ?
O24 P2 O21 . . 110.22(17) ?
O23 P2 O21 . . 108.50(16) ?
O22 P2 O21 . . 106.32(16) ?
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
K O24 . 2.608(3) ?
K O24 2 2.608(3) ?
K O24 6 2.767(3) ?
K O24 5_556 2.767(3) ?
K O11 5 2.869(4) ?
K O11 6_556 2.869(4) ?
K O22 . 2.929(3) ?
K O22 2 2.929(3) ?
Mn3 O23 7_556 2.253(4) ?
Mn3 O23 8_455 2.256(4) ?
Mn3 O12 5_565 2.294(4) ?
Mn3 O12 . 2.335(4) ?
Mn3 O23 3_454 2.400(4) ?
Mn1 O23 7_556 2.189(3) ?
Mn1 O23 8_455 2.189(3) ?
Mn1 O11 . 2.215(3) ?
Mn1 O11 2 2.215(3) ?
Mn1 O22 2 2.315(3) ?
Mn1 O22 . 2.315(3) ?
Fe2 O24 6 1.970(3) ?
Fe2 O12 8_556 2.027(3) ?
Fe2 O22 . 2.049(3) ?
Fe2 O21 1_554 2.071(3) ?
Fe2 O11 . 2.123(3) ?
Fe2 O21 7_556 2.167(3) ?
P1 O12 2_554 1.537(3) ?
P1 O12 . 1.537(3) ?
P1 O11 2_554 1.544(3) ?
P1 O11 . 1.544(3) ?
P2 O24 . 1.519(3) ?
P2 O23 . 1.526(3) ?
P2 O22 . 1.547(3) ?
P2 O21 . 1.553(3) ?
