Crystal structure of (NH~4~)~2~[Fe^II^~5~(HPO~3~)~6~], a new open-framework phosphite
Berrocal, Teresa; Mesa, Jose Luis; Larrea, Edurne; Arrieta, Juan Manuel; Acta Crystallographica Section E 70 (2014) 309–311; doi:10.1107/S1600536814021783

data_2240052
_publ_section_title
;
 Crystal structure of (NH~4~)~2~[Fe^II^~5~(HPO~3~)~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 <i>et al.</i>,  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 \k-geometry diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova (single source at offset)'
_diffrn_measurement_method       '\w 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
;
(<i>CrysAlis PRO</i>; 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/[\s^2^(Fo^2^)+(0.0126P)^2^+2.2823P] where P=(Fo^2^+2Fc^2^)/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>2\s(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
_shelx_hkl_checksum              35156
_shelx_res_checksum              45228
_shelxl_version_number           2.014