#------------------------------------------------------------------------------
#$Date: 2016-02-18 14:25:00 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176728 $
#$URL: svn://www.crystallography.net/cod/cif/8/10/30/8103031.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_8103031
loop_
_publ_author_name
'Kazumasa Sugiyama'
'Makoto Kimiyama'
_publ_section_title
;
 Crystal structure of ammonium tetrairon trisphosphate(V),
 [NH4][Fe4(PO4)3]
;
_journal_issue                   3
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              369
_journal_volume                  224
_journal_year                    2009
_chemical_formula_moiety         'Fe4 O12 P3, H4 N'
_chemical_formula_sum            'Fe4 H4 N O12 P3'
_chemical_formula_weight         526.35
_chemical_name_systematic
;
 Ammonium Tetrairon Tris(phosphate(V))
;
_space_group_IT_number           58
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2 2n'
_symmetry_space_group_name_H-M   'P n n m'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.8002(6)
_cell_length_b                   16.6223(9)
_cell_length_c                   6.3008(4)
_cell_measurement_reflns_used    10021
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      30.49
_cell_measurement_theta_min      3.21
_cell_volume                     1026.41(11)
_computing_cell_refinement       'PROCESS AUTO (Rigaku Corp., 1998)'
_computing_data_collection       'PROCESS AUTO (Rigaku Corp., 1998)'
_computing_data_reduction        'PROCESS AUTO (Rigaku Corp., 1998)'
_computing_molecular_graphics    'ATOMS Ver.6.2 (Dowty, 2005)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'MacKay, Wardojo and Hwu, 1996'
_diffrn_ambient_temperature      294(2)
_diffrn_detector_area_resol_mean 100
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID image-plate'
_diffrn_measurement_method       oscillation
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0514
_diffrn_reflns_av_sigmaI/netI    0.0349
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            9509
_diffrn_reflns_theta_full        30.49
_diffrn_reflns_theta_max         30.49
_diffrn_reflns_theta_min         3.21
_exptl_absorpt_coefficient_mu    6.080
_exptl_absorpt_correction_T_max  0.647
_exptl_absorpt_correction_T_min  0.538
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NNMABS (Higashi, 1998)'
_exptl_crystal_colour            'pale green'
_exptl_crystal_density_diffrn    3.406
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prizm
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.888
_refine_diff_density_min         -0.693
_refine_diff_density_rms         0.129
_refine_ls_extinction_coef       0.0024(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     110
_refine_ls_number_reflns         1688
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0301
_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)+(0.0319P)²+0.0173P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0577
_refine_ls_wR_factor_ref         0.0609
_reflns_number_gt                1354
_reflns_number_total             1688
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            710018.cff
_cod_data_source_block           k0696
_cod_original_cell_volume        1026.41(10)
_cod_original_sg_symbol_H-M      P_n_n_m
_cod_database_code               8103031
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x+1/2, -y+1/2, -z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'-x-1/2, y-1/2, z-1/2'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.53745(5) 0.09413(3) 0.0000 0.00851(12) Uani 1 2 d S . .
Fe2 Fe 0.98136(6) 0.13877(3) 0.0000 0.00940(12) Uani 1 2 d S . .
Fe3 Fe 0.25034(4) 0.20466(2) 0.25112(6) 0.01045(10) Uani 1 1 d . . .
P1 P 0.04105(10) 0.33370(5) 0.0000 0.00759(18) Uani 1 2 d S . .
P2 P 0.45825(9) 0.28350(5) 0.0000 0.00738(18) Uani 1 2 d S . .
P3 P 0.21193(10) 0.03791(5) 0.0000 0.00861(18) Uani 1 2 d S . .
O1 O 0.1156(3) 0.68099(15) 0.0000 0.0121(5) Uani 1 2 d S . .
O2 O 0.6145(3) 0.27663(15) 0.0000 0.0114(5) Uani 1 2 d S . .
O3 O 0.0840(2) 0.37855(11) 0.1989(3) 0.0130(4) Uani 1 1 d . . .
O4 O 0.3959(3) 0.19647(14) 0.0000 0.0102(5) Uani 1 2 d S . .
O5 O 0.1139(3) 0.24859(14) 0.0000 0.0108(5) Uani 1 2 d S . .
O6 O 0.8593(3) 0.04278(14) 0.0000 0.0180(6) Uani 1 2 d S . .
O7 O 0.1675(2) 0.09035(10) 0.1926(3) 0.0164(4) Uani 1 1 d . . .
O8 O 0.4037(2) 0.32270(11) 0.2027(3) 0.0140(4) Uani 1 1 d . . .
O9 O 0.3660(3) 0.02170(14) 0.0000 0.0146(5) Uani 1 2 d S . .
N N 0.3003(5) 0.4698(2) 0.0000 0.0243(8) Uani 1 2 d S . .
H1 H 0.2176 0.4682 0.0000 0.029 Uiso 1 2 d S . .
H2 H 0.3176 0.5191 0.0000 0.029 Uiso 1 2 d S . .
H3 H 0.3207 0.4421 0.1197 0.029 Uiso 1 1 d . . .
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'
N N 0.0061 0.0033 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Fe1 O3 142.51(12) 3 8_665 ?
O3 Fe1 O9 108.50(6) 3 . ?
O3 Fe1 O9 108.50(6) 8_665 . ?
O3 Fe1 O9 95.91(6) 3 5_655 ?
O3 Fe1 O9 95.91(6) 8_665 5_655 ?
O9 Fe1 O9 80.53(12) . 5_655 ?
O3 Fe1 O4 88.19(6) 3 . ?
O3 Fe1 O4 88.19(6) 8_665 . ?
O9 Fe1 O4 86.43(10) . . ?
O9 Fe1 O4 166.96(10) 5_655 . ?
O6 Fe2 O8 91.50(6) . 8_665 ?
O6 Fe2 O8 91.50(6) . 3 ?
O8 Fe2 O8 124.06(11) 8_665 3 ?
O6 Fe2 O5 178.56(11) . 1_655 ?
O8 Fe2 O5 87.82(6) 8_665 1_655 ?
O8 Fe2 O5 87.82(6) 3 1_655 ?
O6 Fe2 O7 101.13(8) . 1_655 ?
O8 Fe2 O7 147.55(8) 8_665 1_655 ?
O8 Fe2 O7 85.72(7) 3 1_655 ?
O5 Fe2 O7 80.10(7) 1_655 1_655 ?
O6 Fe2 O7 101.13(8) . 6_655 ?
O8 Fe2 O7 85.72(7) 8_665 6_655 ?
O8 Fe2 O7 147.55(8) 3 6_655 ?
O5 Fe2 O7 80.10(7) 1_655 6_655 ?
O7 Fe2 O7 62.65(9) 1_655 6_655 ?
O2 Fe3 O1 82.21(8) 3_455 7_656 ?
O2 Fe3 O7 91.16(9) 3_455 . ?
O1 Fe3 O7 101.85(9) 7_656 . ?
O2 Fe3 O4 174.78(9) 3_455 . ?
O1 Fe3 O4 97.14(8) 7_656 . ?
O7 Fe3 O4 94.05(8) . . ?
O2 Fe3 O5 95.95(8) 3_455 . ?
O1 Fe3 O5 171.47(9) 7_656 . ?
O7 Fe3 O5 86.48(8) . . ?
O4 Fe3 O5 83.93(8) . . ?
O2 Fe3 O8 111.15(8) 3_455 . ?
O1 Fe3 O8 81.98(8) 7_656 . ?
O7 Fe3 O8 157.70(7) . . ?
O4 Fe3 O8 63.65(7) . . ?
O5 Fe3 O8 90.99(8) . . ?
O3 P1 O3 111.31(15) . 6 ?
O3 P1 O1 110.57(10) . 5_565 ?
O3 P1 O1 110.57(10) 6 5_565 ?
O3 P1 O5 108.27(10) . . ?
O3 P1 O5 108.27(10) 6 . ?
O1 P1 O5 107.73(15) 5_565 . ?
O8 P2 O8 113.14(15) . 6 ?
O8 P2 O2 112.35(9) . . ?
O8 P2 O2 112.35(9) 6 . ?
O8 P2 O4 104.85(9) . . ?
O8 P2 O4 104.85(9) 6 . ?
O2 P2 O4 108.64(14) . . ?
O6 P3 O9 107.37(15) 5_655 . ?
O6 P3 O7 111.57(10) 5_655 . ?
O9 P3 O7 111.97(10) . . ?
O6 P3 O7 111.57(10) 5_655 6 ?
O9 P3 O7 111.97(10) . 6 ?
O7 P3 O7 102.45(15) . 6 ?
P1 O1 Fe3 130.74(6) 5_565 4 ?
P1 O1 Fe3 130.74(6) 5_565 7_665 ?
Fe3 O1 Fe3 97.64(11) 4 7_665 ?
P2 O2 Fe3 128.83(7) . 3 ?
P2 O2 Fe3 128.83(7) . 8_665 ?
Fe3 O2 Fe3 97.85(11) 3 8_665 ?
P1 O3 Fe1 146.09(13) . 3_455 ?
P2 O4 Fe3 101.61(9) . 6 ?
P2 O4 Fe3 101.61(9) . . ?
Fe3 O4 Fe3 95.67(11) 6 . ?
P2 O4 Fe1 117.90(15) . . ?
Fe3 O4 Fe1 118.15(7) 6 . ?
Fe3 O4 Fe1 118.15(7) . . ?
P1 O5 Fe3 124.82(8) . 6 ?
P1 O5 Fe3 124.82(8) . . ?
Fe3 O5 Fe3 92.16(10) 6 . ?
P1 O5 Fe2 117.81(15) . 1_455 ?
Fe3 O5 Fe2 94.71(8) 6 1_455 ?
Fe3 O5 Fe2 94.71(8) . 1_455 ?
P3 O6 Fe2 170.61(19) 5_655 . ?
P3 O7 Fe3 122.39(11) . . ?
P3 O7 Fe2 90.39(9) . 1_455 ?
Fe3 O7 Fe2 94.68(7) . 1_455 ?
P2 O8 Fe2 137.75(13) . 3_455 ?
P3 O9 Fe1 134.26(15) . . ?
P3 O9 Fe1 126.27(15) . 5_655 ?
Fe1 O9 Fe1 99.47(12) . 5_655 ?
H1 N H2 104.00 . . ?
H1 N H3 102.00 . . ?
H2 N H3 117.00 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 O3 2.0036(17) 3 ?
Fe1 O3 2.0036(17) 8_665 ?
Fe1 O9 2.067(3) . ?
Fe1 O9 2.145(3) 5_655 ?
Fe1 O4 2.195(2) . ?
Fe2 O6 1.995(3) . ?
Fe2 O8 2.1212(18) 8_665 ?
Fe2 O8 2.1212(18) 3 ?
Fe2 O5 2.240(3) 1_655 ?
Fe2 O7 2.334(2) 1_655 ?
Fe2 O7 2.334(2) 6_655 ?
Fe3 O2 2.0802(18) 3_455 ?
Fe3 O1 2.0834(18) 7_656 ?
Fe3 O7 2.0992(18) . ?
Fe3 O4 2.1347(18) . ?
Fe3 O5 2.1967(19) . ?
Fe3 O8 2.490(2) . ?
P1 O3 1.5177(18) . ?
P1 O3 1.5177(18) 6 ?
P1 O1 1.554(3) 5_565 ?
P1 O5 1.585(3) . ?
P2 O8 1.5302(18) . ?
P2 O8 1.5302(18) 6 ?
P2 O2 1.536(3) . ?
P2 O4 1.570(2) . ?
P3 O6 1.512(3) 5_655 ?
P3 O9 1.534(3) . ?
P3 O7 1.5563(18) . ?
P3 O7 1.5563(18) 6 ?
O1 P1 1.554(3) 5_565 ?
O1 Fe3 2.0834(18) 4 ?
O1 Fe3 2.0834(18) 7_665 ?
O2 Fe3 2.0802(18) 3 ?
O2 Fe3 2.0802(18) 8_665 ?
O3 Fe1 2.0036(17) 3_455 ?
O4 Fe3 2.1347(18) 6 ?
O5 Fe3 2.1967(19) 6 ?
O5 Fe2 2.240(3) 1_455 ?
O6 P3 1.512(3) 5_655 ?
O7 Fe2 2.334(2) 1_455 ?
O8 Fe2 2.1212(18) 3_455 ?
O9 Fe1 2.145(3) 5_655 ?
N O7 2.805(3) 4 ?
N O7 2.805(3) 7_665 ?
N O3 2.892(4) 6 ?
N O8 2.939(4) 6 ?
N O6 3.2098(10) 3_455 ?
N O6 3.2098(10) 3_454 ?
N P3 3.3497(12) 7_666 ?
N P3 3.3497(12) 7_665 ?
N H1 0.81 . ?
N H2 0.84 . ?
N H3 0.91 . ?
