#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/75/2237599.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_2237599
loop_
_publ_author_name
'Wöhlert, Susanne'
'Jess, Inke'
'Näther, Christian'
_publ_section_title
;
 Diaquabis[bis(pyrazin-2-yl)
 sulfide-κN⁴]bis(thiocyanato-κN)iron(II) monohydrate
;
_journal_coeditor_code           BT6895
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m196
_journal_paper_doi               10.1107/S1600536813006314
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '[Fe (N C S)2 (C8 H6 N4 S)2 (H2 O)2], H2 O'
_chemical_formula_moiety         'C18 H16 Fe N10 O2 S4, H2 O'
_chemical_formula_sum            'C18 H18 Fe N10 O3 S4'
_chemical_formula_weight         606.51
_chemical_name_systematic
;
Diaquabis[bis(pyrazin-2-yl)
sulfide-κN⁴]bis(thiocyanato-κN)iron(II) monohydrate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 109.770(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.5110(8)
_cell_length_b                   15.8583(9)
_cell_length_c                   14.8025(12)
_cell_measurement_reflns_used    10774
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      2.34
_cell_volume                     2542.9(3)
_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, 2011)
;
_computing_publication_material
;
XCIF in SHELXTL (Sheldrick, 2008) and publCIF (Westrip, 2010)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Stoe IPDS-1'
_diffrn_measurement_method       'phi 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  0.0443
_diffrn_reflns_av_sigmaI/netI    0.0302
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10774
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.34
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.964
_exptl_absorpt_correction_T_max  0.8587
_exptl_absorpt_correction_T_min  0.6895
_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    1.584
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.2510
_exptl_crystal_size_mid          0.1464
_exptl_crystal_size_min          0.0893
_refine_diff_density_max         0.520
_refine_diff_density_min         -0.490
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     165
_refine_ls_number_reflns         2496
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0376
_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)+(0.0412P)²+5.1033P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0839
_refine_ls_wR_factor_ref         0.0901
_reflns_number_gt                2012
_reflns_number_total             2496
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            bt6895.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2237599
_cod_database_fobs_code          2237599
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'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_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
Fe Fe1 0.7500 0.7500 0.0000 0.01850(14) Uani d S 1 2
N N1 0.6524(2) 0.83973(14) 0.05049(17) 0.0283(5) Uani d . 1 1
C C1 0.5978(2) 0.88512(16) 0.08281(19) 0.0250(6) Uani d . 1 1
S S1 0.51942(8) 0.94785(6) 0.12789(7) 0.0495(3) Uani d . 1 1
N N10 0.68155(19) 0.64769(13) 0.07296(16) 0.0217(4) Uani d . 1 1
C C10 0.5612(2) 0.63655(16) 0.05785(19) 0.0231(5) Uani d . 1 1
H H10 0.5030 0.6753 0.0184 0.028 Uiso calc R 1 1
C C11 0.5199(2) 0.56900(16) 0.09904(19) 0.0221(5) Uani d . 1 1
C C12 0.7178(3) 0.52477(18) 0.1702(2) 0.0309(6) Uani d . 1 1
H H12 0.7760 0.4863 0.2100 0.037 Uiso calc R 1 1
C C13 0.7596(2) 0.59152(17) 0.1297(2) 0.0275(6) Uani d . 1 1
H H13 0.8458 0.5978 0.1424 0.033 Uiso calc R 1 1
N N11 0.5975(2) 0.51276(14) 0.15487(16) 0.0265(5) Uani d . 1 1
S S2 0.36039(6) 0.54851(4) 0.07358(6) 0.03024(18) Uani d . 1 1
N N20 0.1422(2) 0.71530(17) 0.13551(19) 0.0365(6) Uani d . 1 1
C C20 0.1863(2) 0.64829(19) 0.1039(2) 0.0323(6) Uani d . 1 1
H H20 0.1322 0.6031 0.0752 0.039 Uiso calc R 1 1
C C21 0.3091(2) 0.64298(17) 0.1120(2) 0.0264(6) Uani d . 1 1
C C22 0.3399(4) 0.7716(3) 0.1788(6) 0.129(3) Uani d . 1 1
H H22 0.3930 0.8179 0.2049 0.155 Uiso calc R 1 1
C C23 0.2211(3) 0.7764(2) 0.1745(3) 0.0604(12) Uani d . 1 1
H H23 0.1938 0.8244 0.2000 0.072 Uiso calc R 1 1
N N21 0.3859(3) 0.7044(2) 0.1476(4) 0.0998(19) Uani d . 1 1
O O1 0.90576(16) 0.76058(11) 0.12427(13) 0.0264(4) Uani d . 1 1
H H1O1 0.9775 0.7416 0.1362 0.040 Uiso d R 1 1
H H2O1 0.9184 0.8036 0.1593 0.040 Uiso d R 1 1
O O2 0.5000 0.39109(15) 0.2500 0.0247(5) Uani d S 1 2
H H1O2 0.5302 0.4227 0.2182 0.037 Uiso d R 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'
Cl Cl 0.1484 0.1585 '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'
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
O1 Fe1 O1 7_665 . 180.0
O1 Fe1 N1 7_665 . 87.98(8)
O1 Fe1 N1 . . 92.02(8)
O1 Fe1 N1 7_665 7_665 92.02(8)
O1 Fe1 N1 . 7_665 87.98(8)
N1 Fe1 N1 . 7_665 180.00(12)
O1 Fe1 N10 7_665 . 91.68(8)
O1 Fe1 N10 . . 88.32(8)
N1 Fe1 N10 . . 90.08(8)
N1 Fe1 N10 7_665 . 89.92(8)
O1 Fe1 N10 7_665 7_665 88.32(8)
O1 Fe1 N10 . 7_665 91.68(8)
N1 Fe1 N10 . 7_665 89.92(8)
N1 Fe1 N10 7_665 7_665 90.08(8)
N10 Fe1 N10 . 7_665 180.00(9)
C1 N1 Fe1 . . 175.3(2)
N1 C1 S1 . . 179.1(2)
C10 N10 C13 . . 117.0(2)
C10 N10 Fe1 . . 121.96(17)
C13 N10 Fe1 . . 120.93(17)
N10 C10 C11 . . 121.0(2)
N10 C10 H10 . . 119.5
C11 C10 H10 . . 119.5
N11 C11 C10 . . 122.0(2)
N11 C11 S2 . . 115.92(19)
C10 C11 S2 . . 121.9(2)
N11 C12 C13 . . 121.9(2)
N11 C12 H12 . . 119.1
C13 C12 H12 . . 119.1
N10 C13 C12 . . 121.5(2)
N10 C13 H13 . . 119.2
C12 C13 H13 . . 119.2
C11 N11 C12 . . 116.6(2)
C21 S2 C11 . . 102.11(12)
C23 N20 C20 . . 116.9(3)
N20 C20 C21 . . 121.3(3)
N20 C20 H20 . . 119.3
C21 C20 H20 . . 119.3
N21 C21 C20 . . 121.6(3)
N21 C21 S2 . . 120.6(2)
C20 C21 S2 . . 117.8(2)
N21 C22 C23 . . 122.7(3)
N21 C22 H22 . . 118.6
C23 C22 H22 . . 118.6
N20 C23 C22 . . 121.1(3)
N20 C23 H23 . . 119.5
C22 C23 H23 . . 119.5
C21 N21 C22 . . 116.2(3)
Fe1 O1 H1O1 . . 130.1
Fe1 O1 H2O1 . . 121.7
H1O1 O1 H2O1 . . 102.0
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 O1 7_665 2.0965(17) ?
Fe1 O1 . 2.0965(17) y
Fe1 N1 . 2.101(2) y
Fe1 N1 7_665 2.101(2) ?
Fe1 N10 . 2.235(2) y
Fe1 N10 7_665 2.235(2) ?
N1 C1 . 1.160(3) ?
C1 S1 . 1.630(3) ?
N10 C10 . 1.339(3) ?
N10 C13 . 1.340(3) ?
C10 C11 . 1.393(4) ?
C10 H10 . 0.9500 ?
C11 N11 . 1.333(3) ?
C11 S2 . 1.775(3) ?
C12 N11 . 1.339(4) ?
C12 C13 . 1.381(4) ?
C12 H12 . 0.9500 ?
C13 H13 . 0.9500 ?
S2 C21 . 1.773(3) ?
N20 C23 . 1.319(4) ?
N20 C20 . 1.329(4) ?
C20 C21 . 1.381(4) ?
C20 H20 . 0.9500 ?
C21 N21 . 1.302(4) ?
C22 N21 . 1.340(5) ?
C22 C23 . 1.349(5) ?
C22 H22 . 0.9500 ?
C23 H23 . 0.9500 ?
O1 H1O1 . 0.8400 ?
O1 H2O1 . 0.8400 ?
O2 H1O2 . 0.8400 ?
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
O2 H1O2 N11 . 0.84 2.00 2.834(3) 171.0
O1 H1O1 N20 1_655 0.84 1.94 2.765(3) 165.3
O1 H2O1 O2 3 0.84 1.94 2.749(3) 162.1
