#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/85/2238537.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_2238537
loop_
_publ_author_name
'Wöhlert, Susanne'
'Jess, Inke'
'Näther, Christian'
_publ_section_title
;
 catena-Poly[[bis(thiocyanato-κN)iron(II)]-bis(μ-dipyrazin-2-yl
 disulfide-κ²N⁴:N^4'^)]
;
_journal_coeditor_code           NR2047
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m487
_journal_paper_doi               10.1107/S1600536813021958
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '[Fe (N C S)2 (C8 H6 N4 S2)2]'
_chemical_formula_moiety         'C18 H12 Fe N10 S6'
_chemical_formula_sum            'C18 H12 Fe N10 S6'
_chemical_formula_weight         616.59
_chemical_name_systematic
'catena-Poly[[bis(thiocyanato-κN)iron(II)]-bis(μ-dipyrazin-2-yl disulfide-κ²N⁴:N^4'^)]'
_space_group_IT_number           64
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2ac 2'
_symmetry_space_group_name_H-M   'C m c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.0530(10)
_cell_length_b                   8.0559(5)
_cell_length_c                   16.1952(9)
_cell_measurement_reflns_used    7765
_cell_measurement_temperature    293
_cell_measurement_theta_max      25.99
_cell_measurement_theta_min      3.02
_cell_volume                     2485.8(2)
_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, 2012)'
_computing_publication_material  'XCIF in SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Stoe IPDS-2'
_diffrn_measurement_method       'ω scan'
_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  0.0349
_diffrn_reflns_av_sigmaI/netI    0.0168
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            7765
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         3.02
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.141
_exptl_absorpt_correction_T_max  0.9016
_exptl_absorpt_correction_T_min  0.7816
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(X-SHAPE and X-RED32; Stoe & Cie, 2008)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.648
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.105
_exptl_crystal_size_mid          0.081
_exptl_crystal_size_min          0.046
_refine_diff_density_max         0.690
_refine_diff_density_min         -0.338
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.152
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     86
_refine_ls_number_reflns         1242
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.152
_refine_ls_R_factor_all          0.0607
_refine_ls_R_factor_gt           0.0505
_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)+(0.0413P)²+5.3642P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1079
_refine_ls_wR_factor_ref         0.1127
_reflns_number_gt                1077
_reflns_number_total             1242
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            nr2047.cif
_cod_data_source_block           I
_cod_original_sg_symbol_Hall     '-C 2bc 2'
_cod_database_code               2238537
_cod_database_fobs_code          2238537
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'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1, z+1/2'
'x+1/2, -y+1/2, -z'
'-x+1/2, y+1, -z+1/2'
'-x, -y, -z'
'x, y-1/2, -z-1/2'
'-x, y, z'
'x, -y-1/2, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, y, -z-1/2'
'-x+1/2, y+1/2, z'
'x+1/2, -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_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
Fe Fe1 0.5000 0.0000 0.5000 0.0384(3) Uani d S 1 4
N N1 0.5000 0.1936(5) 0.5832(3) 0.0507(10) Uani d S 1 2
C C1 0.5000 0.3240(5) 0.6134(3) 0.0397(10) Uani d S 1 2
S S1 0.5000 0.50646(16) 0.65366(9) 0.0640(4) Uani d S 1 2
N N10 0.41517(13) 0.1291(3) 0.42501(17) 0.0428(6) Uani d . 1 1
C C10 0.37695(15) 0.2524(4) 0.4557(2) 0.0445(7) Uani d . 1 1
H H10 0.3819 0.2818 0.5109 0.053 Uiso calc R 1 1
C C11 0.32962(17) 0.3380(4) 0.4062(2) 0.0490(8) Uani d . 1 1
C C12 0.3600(2) 0.1830(6) 0.2972(2) 0.0713(11) Uani d . 1 1
H H12 0.3561 0.1563 0.2415 0.086 Uiso calc R 1 1
C C13 0.4057(2) 0.0943(5) 0.3454(2) 0.0579(9) Uani d . 1 1
H H13 0.4309 0.0073 0.3219 0.070 Uiso calc R 1 1
N N11 0.32128(18) 0.3053(4) 0.3271(2) 0.0649(9) Uani d . 1 1
S S11 0.27348(5) 0.50102(12) 0.43778(8) 0.0687(3) Uani d . 1 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'
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'
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
N1 Fe1 N1 9_656 . 180.00(18) y
N1 Fe1 N10 9_656 . 89.81(11) y
N1 Fe1 N10 . . 90.19(11) y
N1 Fe1 N10 9_656 11_655 89.81(11) ?
N1 Fe1 N10 . 11_655 90.19(11) ?
N10 Fe1 N10 . 11_655 90.62(13) y
N1 Fe1 N10 9_656 3_556 90.19(11) ?
N1 Fe1 N10 . 3_556 89.81(11) ?
N10 Fe1 N10 . 3_556 89.38(13) y
N10 Fe1 N10 11_655 3_556 180.0 ?
N1 Fe1 N10 9_656 9_656 90.19(11) ?
N1 Fe1 N10 . 9_656 89.81(11) ?
N10 Fe1 N10 . 9_656 180.00(11) ?
N10 Fe1 N10 11_655 9_656 89.38(13) ?
N10 Fe1 N10 3_556 9_656 90.62(13) ?
C1 N1 Fe1 . . 164.1(4) ?
N1 C1 S1 . . 179.0(4) ?
C10 N10 C13 . . 116.5(3) ?
C10 N10 Fe1 . . 122.1(2) ?
C13 N10 Fe1 . . 121.1(2) ?
N10 C10 C11 . . 120.7(3) ?
N10 C10 H10 . . 119.6 ?
C11 C10 H10 . . 119.6 ?
N11 C11 C10 . . 122.7(3) ?
N11 C11 S11 . . 110.9(3) ?
C10 C11 S11 . . 126.4(3) ?
N11 C12 C13 . . 122.3(4) ?
N11 C12 H12 . . 118.9 ?
C13 C12 H12 . . 118.9 ?
N10 C13 C12 . . 121.8(4) ?
N10 C13 H13 . . 119.1 ?
C12 C13 H13 . . 119.1 ?
C11 N11 C12 . . 116.0(3) ?
C11 S11 S11 . 3_566 106.45(13) ?
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 N1 9_656 2.061(4) ?
Fe1 N1 . 2.061(4) y
Fe1 N10 . 2.273(3) y
Fe1 N10 11_655 2.273(3) ?
Fe1 N10 3_556 2.273(3) ?
Fe1 N10 9_656 2.273(3) ?
N1 C1 . 1.158(6) ?
C1 S1 . 1.608(5) ?
N10 C10 . 1.328(4) ?
N10 C13 . 1.332(5) ?
C10 C11 . 1.390(4) ?
C10 H10 . 0.9300 ?
C11 N11 . 1.318(5) ?
C11 S11 . 1.769(3) ?
C12 N11 . 1.323(5) ?
C12 C13 . 1.371(5) ?
C12 H12 . 0.9300 ?
C13 H13 . 0.9300 ?
S11 S11 3_566 2.015(2) ?
