#------------------------------------------------------------------------------
#$Date: 2016-02-21 11:56:54 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176809 $
#$URL: svn://www.crystallography.net/cod/cif/2/24/00/2240052.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_2240052
loop_
_publ_author_name
'Berrocal, Teresa'
'Mesa, Jose Luis'
'Larrea, Edurne'
'Arrieta, Juan Manuel'
_publ_section_title
;
 Crystal structure of (NH₄)₂[FeII₅(HPO₃)₆], a new
 open-framework phosphite
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              309
_journal_page_last               311
_journal_paper_doi               10.1107/S1600536814021783
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          '(N H4)2 [Fe5 (H P O3)6]'
_chemical_formula_moiety         '2(N1 H4 +), Fe5 H6 O18 P6 2-'
_chemical_formula_sum            'Fe5 H14 N2 O18 P6'
_chemical_formula_weight         795.20
_chemical_name_systematic
;
Diammonium hexaphosphitopentaferrate(II)
;
_space_group_crystal_system      trigonal
_space_group_IT_number           165
_space_group_name_Hall           '-P 3 2"c'
_space_group_name_H-M_alt        'P -3 c 1'
_symmetry_space_group_name_Hall  '-P 3 2"c'
_symmetry_space_group_name_H-M   'P -3 c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method
;
Olex2 1.2
(compiled 2014.05.21 svn.r2940 for OlexSys, GUI svn.r4846)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   10.3862(15)
_cell_length_b                   10.3862(15)
_cell_length_c                   9.2089(14)
_cell_measurement_reflns_used    2414
_cell_measurement_temperature    100.0(10)
_cell_measurement_theta_max      28.2900
_cell_measurement_theta_min      2.2530
_cell_volume                     860.3(2)
_computing_cell_refinement
;
CrysAlis PRO (Agilent, 2014)
;
_computing_data_collection
;
CrysAlis PRO (Agilent, 2014)
;
_computing_data_reduction
;
CrysAlis PRO (Agilent, 2014)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2010)
;
_computing_publication_material
;
OLEX2 (Dolomanov et al.,  2009)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2008)
;
_computing_structure_solution
;
SUPERFLIP (Palatinus & Chapuis, 2007)
;
_diffrn_ambient_temperature      100.0(10)
_diffrn_detector_area_resol_mean 16.2439
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'four-circle κ-geometry diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova (single source at offset)'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0727
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            6343
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         2.212
_exptl_absorpt_coefficient_mu    4.776
_exptl_absorpt_correction_T_max  0.893
_exptl_absorpt_correction_T_min  0.566
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
(CrysAlis PRO; Agilent, 2014)
;
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    3.070
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       acicular
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.176
_exptl_crystal_size_mid          0.046
_exptl_crystal_size_min          0.024
_refine_diff_density_max         0.527
_refine_diff_density_min         -0.763
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.168
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     68
_refine_ls_number_reflns         659
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.156
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0332
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0126P)²+2.2823P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0632
_refine_ls_wR_factor_ref         0.0651
_reflns_number_gt                618
_reflns_number_total             659
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            wm5036sup1.cf
_cod_data_source_block           I
_cod_original_cell_volume        860.3(3)
_cod_database_code               2240052
_cod_database_fobs_code          2240052
#BEGIN Tags that were not found in dictionaries:
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelxl_version_number           2.014
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, 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_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe Fe1 0.61330(9) 0.0000 0.2500 0.0209(2) Uani d 1 . .
Fe Fe2 0.6667 0.3333 0.33453(10) 0.0202(3) Uani d 1 . .
P P1 0.88002(13) 0.29352(13) 0.09044(10) 0.0224(3) Uani d 1 . .
H H1P 1.020(5) 0.343(3) 0.091(2) 0.027 Uiso d 1 . .
O O2 0.8512(3) 0.3935(3) 0.1927(3) 0.0234(7) Uani d 1 . .
O O3 0.8404(3) 0.3102(4) -0.0665(3) 0.0243(7) Uani d 1 . .
O O1 0.8063(4) 0.1345(4) 0.1440(3) 0.0284(8) Uani d 1 . .
N N2 0.970(5) -0.047(3) 0.059(2) 0.045(9) Uani d 0.1667 A -2
N N1 1.024(5) -0.015(6) 0.2033(17) 0.020(7) Uani d 0.1667 B -1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 -1 0.0880
0 -4 0 0.0058
3 -2 0 0.0403
-2 1 0 0.0044
0 4 0 0.0186
0 0 1 0.0880
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
O2 Fe1 O2 4_545 3_665 87.23(17)
O2 Fe1 O3 3_665 9_545 102.21(11)
O2 Fe1 O3 3_665 10_666 76.48(10)
O2 Fe1 O3 4_545 9_545 76.48(10)
O2 Fe1 O3 4_545 10_666 102.21(11)
O3 Fe1 O3 9_545 10_666 178.24(17)
O1 Fe1 O2 5 3_665 165.86(10)
O1 Fe1 O2 5 4_545 87.80(12)
O1 Fe1 O2 . 3_665 87.80(12)
O1 Fe1 O2 . 4_545 165.86(10)
O1 Fe1 O3 5 9_545 89.46(11)
O1 Fe1 O3 . 10_666 89.46(11)
O1 Fe1 O3 . 9_545 91.67(11)
O1 Fe1 O3 5 10_666 91.67(11)
O1 Fe1 O1 5 . 99.93(18)
O2 Fe2 O2 3_665 2_655 86.57(11)
O2 Fe2 O2 . 2_655 86.57(11)
O2 Fe2 O2 . 3_665 86.57(11)
O2 Fe2 O3 . 10_666 92.54(11)
O2 Fe2 O3 2_655 12_556 92.54(11)
O2 Fe2 O3 3_665 11_656 92.54(11)
O2 Fe2 O3 2_655 10_666 163.65(12)
O2 Fe2 O3 . 11_656 163.65(11)
O2 Fe2 O3 . 12_556 77.08(11)
O2 Fe2 O3 2_655 11_656 77.08(11)
O2 Fe2 O3 3_665 12_556 163.65(11)
O2 Fe2 O3 3_665 10_666 77.08(11)
O3 Fe2 O3 10_666 11_656 103.18(9)
O3 Fe2 O3 10_666 12_556 103.18(9)
O3 Fe2 O3 12_556 11_656 103.18(9)
O3 P1 O2 . . 110.28(17)
O1 P1 O2 . . 111.96(17)
O1 P1 O3 . . 114.29(17)
Fe1 O2 Fe2 2_655 . 103.34(12)
P1 O2 Fe1 . 2_655 127.30(17)
P1 O2 Fe2 . . 128.71(18)
Fe2 O3 Fe1 10_665 8_665 99.01(10)
P1 O3 Fe1 . 8_665 124.27(18)
P1 O3 Fe2 . 10_665 134.56(18)
P1 O1 Fe1 . . 133.9(2)
O1 P1 H1P . . 106.9(14)
O2 P1 H1P . . 107.0(12)
O3 P1 H1P . . 105.9(12)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Fe1 O2 4_545 2.086(3)
Fe1 O2 3_665 2.086(3)
Fe1 O3 10_666 2.217(3)
Fe1 O3 9_545 2.217(3)
Fe1 O1 . 2.030(3)
Fe1 O1 5 2.030(3)
Fe2 O2 . 2.138(3)
Fe2 O2 3_665 2.138(3)
Fe2 O2 2_655 2.138(3)
Fe2 O3 10_666 2.140(3)
Fe2 O3 11_656 2.140(3)
Fe2 O3 12_556 2.140(3)
P1 O2 . 1.538(3)
P1 O3 . 1.536(3)
P1 O1 . 1.514(3)
O2 Fe1 2_655 2.086(3)
O3 Fe1 8_665 2.217(3)
O3 Fe2 10_665 2.140(3)
P1 H1P . 1.28(5)
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_4
_geom_torsion
O2 P1 O3 Fe1 8_665 120.4(2)
O2 P1 O3 Fe2 10_665 -39.2(3)
O2 P1 O1 Fe1 . 34.8(3)
O3 P1 O2 Fe1 2_655 -89.9(2)
O3 P1 O2 Fe2 . 101.0(2)
O3 P1 O1 Fe1 . -91.5(3)
O1 P1 O2 Fe1 2_655 141.7(2)
O1 P1 O2 Fe2 . -27.5(3)
O1 P1 O3 Fe1 8_665 -112.4(2)
O1 P1 O3 Fe2 10_665 88.0(3)
