#------------------------------------------------------------------------------
#$Date: 2017-01-21 04:00:49 +0200 (Sat, 21 Jan 2017) $
#$Revision: 190795 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/20/2242026.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_2242026
loop_
_publ_author_name
'Tanaka, Rikako'
'Matsushita, Nobuyuki'
_publ_section_title
;
 Crystal structure of bis(1-ethylpyridinium) dioxonium
 hexacyanidoferrate(II)
;
_journal_coeditor_code           WM5355
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              219
_journal_page_last               222
_journal_paper_doi               10.1107/S2056989017000810
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          '(C7 H10 N1)2 (H3 O)2 [Fe (C N)6]'
_chemical_formula_moiety         '2(C7 H10 N1 +), 2(H3 O +), C6 Fe N6 4-'
_chemical_formula_sum            'C20 H26 Fe N8 O2'
_chemical_formula_weight         466.34
_chemical_name_systematic
;
Bis(1-ethylpyridinium) dioxonium hexacyanidoferrate(II)
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           58
_space_group_name_Hall           '-P 2 2n'
_space_group_name_H-M_alt        'P n n m'
_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
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.8807(4)
_cell_length_b                   12.1279(7)
_cell_length_c                   8.3962(2)
_cell_measurement_reflns_used    8639
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      32.01
_cell_measurement_theta_min      3.36
_cell_volume                     1209.79(9)
_computing_cell_refinement
;
RAPID-AUTO (Rigaku, 2006)
;
_computing_data_collection
;
RAPID-AUTO (Rigaku, 2006)
;
_computing_data_reduction
;
RAPID-AUTO (Rigaku, 2006)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2016)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2014 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID imaging-plate'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0342
_diffrn_reflns_av_sigmaI/netI    0.0168
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            25575
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.021
_diffrn_reflns_theta_min         3.360
_exptl_absorpt_coefficient_mu    0.654
_exptl_absorpt_correction_T_max  0.952
_exptl_absorpt_correction_T_min  0.907
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(ABSCOR; Higashi, 1995)
;
_exptl_crystal_colour            pale-yellow
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             488
_exptl_crystal_size_max          0.275
_exptl_crystal_size_mid          0.125
_exptl_crystal_size_min          0.075
_refine_diff_density_max         0.500
_refine_diff_density_min         -0.697
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     88
_refine_ls_number_reflns         2213
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0455
_refine_ls_R_factor_gt           0.0360
_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)+(0.0356P)²+0.6061P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0852
_refine_ls_wR_factor_ref         0.0927
_reflns_number_gt                1840
_reflns_number_total             2216
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            wm5355sup1.cif
_cod_data_source_block           I
_cod_database_code               2242026
_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.
;
loop_
_space_group_symop_operation_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_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
Fe Fe1 0.0000 0.0000 0.0000 0.02095(10) Uani d 1
C C1 -0.05743(16) 0.14661(15) 0.0000 0.0257(3) Uani d 1
C C2 0.10536(11) 0.04026(10) 0.16115(15) 0.0255(2) Uani d 1
N N1 -0.09019(17) 0.23642(15) 0.0000 0.0371(4) Uani d 1
N N2 0.16963(11) 0.06441(11) 0.25910(15) 0.0352(3) Uani d 1
N N3 0.00181(15) 0.25836(14) 0.5000 0.0333(3) Uani d 1
C C3 0.1469(2) 0.4327(2) 0.5000 0.0485(6) Uani d 1
H H3 0.1978 0.4930 0.5000 0.073 Uiso calc 1
C C4 0.10987(15) 0.38888(16) 0.3591(2) 0.0498(4) Uani d 1
H H4 0.1344 0.4192 0.2607 0.075 Uiso calc 1
C C5 0.03717(15) 0.30083(14) 0.3608(2) 0.0431(4) Uani d 1
H H5 0.0118 0.2698 0.2633 0.065 Uiso calc 1
C C6 -0.0794(2) 0.16567(19) 0.5000 0.0485(6) Uani d 1
H H6A -0.0670 0.1193 0.5954 0.073 Uiso d 1
C C7 -0.1981(2) 0.2077(2) 0.5000 0.0570(7) Uani d 1
H H7A -0.2503 0.1452 0.5000 0.086 Uiso d 1
H H7B -0.2108 0.2527 0.5953 0.086 Uiso d 1
O O1 0.30049(12) 0.08078(12) 0.5000 0.0279(3) Uani d 1
H H1A 0.342(2) 0.143(2) 0.5000 0.042 Uiso d 1
H H1B 0.2513(15) 0.0800(15) 0.414(2) 0.042 Uiso d 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
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'
O O 0.0106 0.0060 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
C1 Fe1 C1 5 . 180.0
C1 Fe1 C2 5 5 89.78(5)
C1 Fe1 C2 . 5 90.22(5)
C1 Fe1 C2 5 6 90.22(5)
C1 Fe1 C2 . 6 89.78(5)
C2 Fe1 C2 5 6 89.60(7)
C1 Fe1 C2 5 2 89.78(5)
C1 Fe1 C2 . 2 90.22(5)
C2 Fe1 C2 5 2 90.40(7)
C2 Fe1 C2 6 2 180.00(11)
C1 Fe1 C2 5 . 90.22(5)
C1 Fe1 C2 . . 89.78(5)
C2 Fe1 C2 5 . 180.0
C2 Fe1 C2 6 . 90.40(7)
C2 Fe1 C2 2 . 89.60(7)
N1 C1 Fe1 . . 178.67(18)
N2 C2 Fe1 . . 179.77(13)
C5 N3 C5 6_556 . 120.8(2)
C5 N3 C6 6_556 . 119.61(10)
C5 N3 C6 . . 119.61(10)
C4 C3 C4 . 6_556 119.5(2)
C4 C3 H3 . . 120.2
C4 C3 H3 6_556 . 120.2
C3 C4 C5 . . 119.65(17)
C3 C4 H4 . . 120.2
C5 C4 H4 . . 120.2
N3 C5 C4 . . 120.20(16)
N3 C5 H5 . . 119.9
C4 C5 H5 . . 119.9
N3 C6 C7 . . 110.77(19)
N3 C6 H6A . . 109.5
C7 C6 H6A . . 109.5
C6 C7 H7A . . 109.4
C6 C7 H7B . . 109.5
H7A C7 H7B . . 109.5
H1A O1 H1B . . 110.5(14)
H1A O1 H1B . 6_556 110.5(14)
H1B O1 H1B . 6_556 102(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Fe1 C1 5 1.9045(18)
Fe1 C1 . 1.9045(18)
Fe1 C2 5 1.9068(13)
Fe1 C2 6 1.9068(13)
Fe1 C2 2 1.9068(13)
Fe1 C2 . 1.9069(13)
C1 N1 . 1.157(2)
C2 N2 . 1.1598(17)
N3 C5 6_556 1.3447(19)
N3 C5 . 1.3447(19)
N3 C6 . 1.482(3)
C3 C4 . 1.369(2)
C3 C4 6_556 1.369(2)
C3 H3 . 0.9500
C4 C5 . 1.373(2)
C4 H4 . 0.9500
C5 H5 . 0.9500
C6 C7 . 1.499(4)
C6 H6A . 0.9900
C7 H7A . 0.9800
C7 H7B . 0.9800
O1 H1A . 0.90(3)
O1 H1B . 0.931(18)
O1 H1B 6_556 0.931(18)
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O1 H1A N1 4 0.90(3) 1.67(3) 2.569(2) 176(3)
O1 H1B N2 . 0.931(18) 1.632(19) 2.5589(15) 173.6(18)

_cod_database_fobs_code 2242026
