#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/76/2227651.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_2227651
loop_
_publ_author_name
'Wöhlert, Susanne'
'Wriedt, Mario'
'Jess, Inke'
'Näther, Christian'
_publ_section_title
;
 catena-Poly[(E)-4,4'-(ethene-1,2-diyl)dipyridinium
 [[bis(thiocyanato-κN)ferrate(II)]-di-μ-thiocyanato-κ²N:S;κ²S:N]]
;
_journal_coeditor_code           IM2228
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1256
_journal_paper_doi               10.1107/S160053681003624X
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '(C12 H12 N2) [Fe (N C S)4]'
_chemical_formula_moiety         'C12 H12 N2 2+, C4 Fe N4 S4 2-'
_chemical_formula_sum            'C16 H12 Fe N6 S4'
_chemical_formula_weight         472.41
_chemical_name_systematic
;
catena-Poly[(E)-4,4'-(ethene-1,2-diyl)dipyridinium
[[bis(thiocyanato-κN)ferrate(II)]-di-μ-thiocyanato-
κ²N:S;κ²S:N]]
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.562(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   5.7360(2)
_cell_length_b                   11.5093(4)
_cell_length_c                   15.0971(6)
_cell_measurement_reflns_used    16607
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2
_cell_volume                     990.14(6)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2008)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2008)'
_computing_data_reduction        'X-AREA (Stoe & Cie, 2008)'
_computing_molecular_graphics
'XP in SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'XCIF in SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Stoe IPDS-2'
_diffrn_measurement_method       ω
_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  0.0286
_diffrn_reflns_av_sigmaI/netI    0.0143
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16607
_diffrn_reflns_theta_full        27.97
_diffrn_reflns_theta_max         27.97
_diffrn_reflns_theta_min         2.23
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.197
_exptl_absorpt_correction_T_max  0.895
_exptl_absorpt_correction_T_min  0.826
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(X-SHAPE and X-RED32; Stoe & Cie, 2008)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.585
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             480
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.570
_refine_diff_density_min         -0.207
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     124
_refine_ls_number_reflns         2379
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0334
_refine_ls_R_factor_gt           0.0287
_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)+(0.0291P)²+0.4228P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0658
_refine_ls_wR_factor_ref         0.0676
_reflns_number_gt                2173
_reflns_number_total             2379
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            im2228.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2227651
_cod_database_fobs_code          2227651
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Fe Fe1 1.0000 0.0000 0.5000 0.03128(10) Uani d S 1 . .
N N2 0.3720(3) 0.38242(17) 0.30355(13) 0.0541(4) Uani d . 1 . .
H H2 0.2544 0.3548 0.2697 0.065 Uiso calc R 1 . .
S S1 0.26743(7) 0.16763(4) 0.57486(3) 0.03779(11) Uani d . 1 . .
C C1 0.5284(3) 0.12116(14) 0.55629(11) 0.0334(3) Uani d . 1 . .
N N1 0.7106(3) 0.08926(14) 0.54301(11) 0.0430(4) Uani d . 1 . .
S S11 1.12064(9) -0.23939(5) 0.76873(3) 0.04587(13) Uani d . 1 . .
C C11 1.0730(3) -0.15568(16) 0.68107(12) 0.0371(4) Uani d . 1 . .
N N11 1.0414(3) -0.09600(16) 0.61976(11) 0.0490(4) Uani d . 1 . .
C C21 0.6655(4) 0.52070(17) 0.32949(15) 0.0522(5) Uani d . 1 . .
H H21 0.7402 0.5868 0.3113 0.063 Uiso calc R 1 . .
C C22 0.7421(3) 0.46922(17) 0.41067(13) 0.0425(4) Uani d . 1 . .
C C23 0.6230(4) 0.3727(2) 0.43548(15) 0.0571(6) Uani d . 1 . .
H H23 0.6699 0.3361 0.4895 0.069 Uiso calc R 1 . .
C C24 0.4368(4) 0.3310(2) 0.38090(17) 0.0620(6) Uani d . 1 . .
H H24 0.3550 0.2664 0.3979 0.074 Uiso calc R 1 . .
C C25 0.4812(4) 0.47453(19) 0.27648(15) 0.0555(6) Uani d . 1 . .
H H25 0.4323 0.5077 0.2213 0.067 Uiso calc R 1 . .
C C26 0.9479(4) 0.52118(18) 0.46271(14) 0.0494(5) Uani d . 1 . .
H H26 1.0085 0.5891 0.4410 0.059 Uiso calc R 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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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'
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N11 Fe1 N11 . 3_756 180.0 ?
N11 Fe1 N1 . . 90.39(7) ?
N11 Fe1 N1 3_756 . 89.61(7) y
N11 Fe1 N1 . 3_756 89.61(7) ?
N11 Fe1 N1 3_756 3_756 90.39(7) y
N1 Fe1 N1 . 3_756 180.0(9) ?
N11 Fe1 S1 . 3_656 89.26(5) ?
N11 Fe1 S1 3_756 3_656 90.74(5) y
N1 Fe1 S1 . 3_656 92.77(4) ?
N1 Fe1 S1 3_756 3_656 87.23(4) y
N11 Fe1 S1 . 1_655 90.74(5) ?
N11 Fe1 S1 3_756 1_655 89.26(5) y
N1 Fe1 S1 . 1_655 87.23(4) ?
N1 Fe1 S1 3_756 1_655 92.77(4) y
S1 Fe1 S1 3_656 1_655 180.0 ?
C25 N2 C24 . . 122.48(18) ?
C25 N2 H2 . . 118.8 ?
C24 N2 H2 . . 118.8 ?
C1 S1 Fe1 . 1_455 100.68(6) ?
N1 C1 S1 . . 179.60(19) ?
C1 N1 Fe1 . . 166.29(15) ?
N11 C11 S11 . . 179.25(19) ?
C11 N11 Fe1 . . 174.08(17) ?
C25 C21 C22 . . 120.0(2) ?
C25 C21 H21 . . 120.0 ?
C22 C21 H21 . . 120.0 ?
C23 C22 C21 . . 117.88(18) ?
C23 C22 C26 . . 125.17(19) ?
C21 C22 C26 . . 116.93(19) ?
C24 C23 C22 . . 120.0(2) ?
C24 C23 H23 . . 120.0 ?
C22 C23 H23 . . 120.0 ?
N2 C24 C23 . . 119.9(2) ?
N2 C24 H24 . . 120.1 ?
C23 C24 H24 . . 120.1 ?
N2 C25 C21 . . 119.8(2) ?
N2 C25 H25 . . 120.1 ?
C21 C25 H25 . . 120.1 ?
C26 C26 C22 3_766 . 124.7(3) ?
C26 C26 H26 3_766 . 117.6 ?
C22 C26 H26 . . 117.6 ?
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
Fe1 N11 . 2.1090(16) y
Fe1 N11 3_756 2.1090(16) ?
Fe1 N1 . 2.1165(15) y
Fe1 N1 3_756 2.1165(15) ?
Fe1 S1 3_656 2.6375(5) y
Fe1 S1 1_655 2.6375(5) ?
N2 C25 . 1.320(3) ?
N2 C24 . 1.324(3) ?
N2 H2 . 0.8600 ?
S1 C1 . 1.6437(17) ?
S1 Fe1 1_455 2.6375(5) y
C1 N1 . 1.147(2) ?
S11 C11 . 1.6345(19) ?
C11 N11 . 1.150(2) ?
C21 C25 . 1.359(3) ?
C21 C22 . 1.387(3) ?
C21 H21 . 0.9300 ?
C22 C23 . 1.378(3) ?
C22 C26 . 1.469(3) ?
C23 C24 . 1.360(3) ?
C23 H23 . 0.9300 ?
C24 H24 . 0.9300 ?
C25 H25 . 0.9300 ?
C26 C26 3_766 1.307(4) ?
C26 H26 . 0.9300 ?
