#------------------------------------------------------------------------------
#$Date: 2017-03-08 08:58:45 +0200 (Wed, 08 Mar 2017) $
#$Revision: 194089 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/07/2020739.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_2020739
loop_
_publ_author_name
'Jochim, Aleksej'
'Jess, Inke'
'Näther, Christian'
_publ_section_title
;
 Crystal structure of
 diaquabis(4-cyanopyridine-\kN)bis(thiocyanato-\kN)iron(II)
 4-cyanopyridine disolvate
;
_journal_coeditor_code           WM5371
_journal_issue                   4
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_page_first              463
_journal_paper_doi               10.1107/S205698901700322X
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac
'[Fe (N C S)2 (C6 H4 N2)2 (H2 O)2], 2C6 H4 N2'
_chemical_formula_moiety         'C14 H12 Fe N6 O2 S2, 2(C6 H4 N2)'
_chemical_formula_sum            'C26 H20 Fe N10 O2 S2'
_chemical_formula_weight         624.49
_chemical_name_systematic
;
Diaquabis(4-cyanopyridine-κN)bis(thiocyanato-κN)iron(II)
4-cyanopyridine disolvate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 96.195(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.5376(4)
_cell_length_b                   15.2200(10)
_cell_length_c                   12.1214(6)
_cell_measurement_reflns_used    18864
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      56.3
_cell_measurement_theta_min      3.8
_cell_volume                     1565.88(15)
_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 (Sheldrick, 2008) and DIAMOND (Brandenburg, 2014)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Stoe IPDS-1'
_diffrn_measurement_method       'Phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0467
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            18486
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.092
_diffrn_reflns_theta_min         2.677
_exptl_absorpt_coefficient_mu    0.655
_exptl_absorpt_correction_T_max  0.9533
_exptl_absorpt_correction_T_min  0.8835
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
(X-RED and X-SHAPE; Stoe & Cie, 2008)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_description       block
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.1247
_exptl_crystal_size_mid          0.0980
_exptl_crystal_size_min          0.0599
_refine_diff_density_max         0.261
_refine_diff_density_min         -0.459
_refine_ls_extinction_coef       0.019(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2014 (Sheldrick, 2015)
;
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     188
_refine_ls_number_reflns         3743
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0373
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0581P)²+0.1102P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0880
_refine_ls_wR_factor_ref         0.0936
_reflns_number_gt                2960
_reflns_number_total             3743
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            wm5371sup1.cif
_cod_data_source_block           I
_cod_database_code               2020739
_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.
;
_shelxl_version_number           2.014
loop_
_space_group_symop_operation_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_occupancy
Fe Fe1 0.5000 0.5000 1.0000 0.02513(11) Uani d 1
N N1 0.58788(18) 0.62971(9) 0.99472(12) 0.0358(3) Uani d 1
C C1 0.62673(19) 0.69914(10) 0.96961(13) 0.0305(3) Uani d 1
S S1 0.68128(7) 0.79604(3) 0.93149(5) 0.05165(16) Uani d 1
N N11 0.42359(17) 0.50738(9) 0.81712(11) 0.0317(3) Uani d 1
C C11 0.2830(2) 0.47429(11) 0.77885(14) 0.0351(4) Uani d 1
H H11 0.2267 0.4414 0.8283 0.042 Uiso calc 1
C C12 0.2158(2) 0.48550(11) 0.67119(15) 0.0390(4) Uani d 1
H H12 0.1150 0.4617 0.6472 0.047 Uiso calc 1
C C13 0.2990(2) 0.53234(13) 0.59914(14) 0.0399(4) Uani d 1
C C14 0.4458(2) 0.56588(13) 0.63609(15) 0.0425(4) Uani d 1
H H14 0.5055 0.5976 0.5877 0.051 Uiso calc 1
C C15 0.5029(2) 0.55172(12) 0.74578(14) 0.0381(4) Uani d 1
H H15 0.6036 0.5747 0.7718 0.046 Uiso calc 1
C C16 0.2332(3) 0.54478(18) 0.48511(18) 0.0570(6) Uani d 1
N N12 0.1795(3) 0.5537(2) 0.39540(17) 0.0837(8) Uani d 1
O O1 0.28045(13) 0.55033(7) 1.02877(9) 0.0320(2) Uani d 1
H H1 0.2201 0.5134 1.0535 0.048 Uiso d 1
H H2 0.2728 0.5951 1.0684 0.048 Uiso d 1
N N21 1.2086(2) 0.80713(12) 0.64837(15) 0.0523(4) Uani d 1
C C21 1.0626(3) 0.7796(2) 0.6202(2) 0.0774(9) Uani d 1
H H21 1.0072 0.8031 0.5546 0.093 Uiso calc 1
C C22 0.9863(3) 0.71950(19) 0.67912(19) 0.0685(8) Uani d 1
H H22 0.8813 0.7018 0.6554 0.082 Uiso calc 1
C C23 1.0672(2) 0.68573(11) 0.77413(14) 0.0347(4) Uani d 1
C C24 1.2197(2) 0.71283(11) 0.80597(15) 0.0378(4) Uani d 1
H H24 1.2775 0.6904 0.8713 0.045 Uiso calc 1
C C25 1.2856(2) 0.77362(13) 0.73992(17) 0.0445(4) Uani d 1
H H25 1.3907 0.7923 0.7609 0.053 Uiso calc 1
C C26 0.9913(2) 0.62137(12) 0.83758(14) 0.0361(4) Uani d 1
N N22 0.9307(2) 0.56987(11) 0.88643(14) 0.0460(4) Uani 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'
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'
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 3_667 . 180.0
O1 Fe1 N1 3_667 . 90.55(5)
O1 Fe1 N1 . . 89.45(5)
O1 Fe1 N1 3_667 3_667 89.45(5)
O1 Fe1 N1 . 3_667 90.55(5)
N1 Fe1 N1 . 3_667 180.0
O1 Fe1 N11 3_667 3_667 88.63(5)
O1 Fe1 N11 . 3_667 91.37(5)
N1 Fe1 N11 . 3_667 90.59(5)
N1 Fe1 N11 3_667 3_667 89.41(5)
O1 Fe1 N11 3_667 . 91.37(5)
O1 Fe1 N11 . . 88.63(5)
N1 Fe1 N11 . . 89.41(5)
N1 Fe1 N11 3_667 . 90.59(5)
N11 Fe1 N11 3_667 . 180.0
C1 N1 Fe1 . . 166.44(14)
N1 C1 S1 . . 178.74(15)
C15 N11 C11 . . 117.64(15)
C15 N11 Fe1 . . 123.39(12)
C11 N11 Fe1 . . 118.54(11)
N11 C11 C12 . . 123.23(17)
N11 C11 H11 . . 118.4
C12 C11 H11 . . 118.4
C11 C12 C13 . . 118.18(17)
C11 C12 H12 . . 120.9
C13 C12 H12 . . 120.9
C12 C13 C14 . . 119.72(17)
C12 C13 C16 . . 119.85(19)
C14 C13 C16 . . 120.42(19)
C13 C14 C15 . . 117.86(17)
C13 C14 H14 . . 121.1
C15 C14 H14 . . 121.1
N11 C15 C14 . . 123.35(17)
N11 C15 H15 . . 118.3
C14 C15 H15 . . 118.3
N12 C16 C13 . . 179.0(3)
Fe1 O1 H1 . . 114.2
Fe1 O1 H2 . . 121.3
H1 O1 H2 . . 104.5
C21 N21 C25 . . 117.42(17)
N21 C21 C22 . . 124.4(2)
N21 C21 H21 . . 117.8
C22 C21 H21 . . 117.8
C21 C22 C23 . . 117.5(2)
C21 C22 H22 . . 121.2
C23 C22 H22 . . 121.2
C22 C23 C24 . . 119.69(17)
C22 C23 C26 . . 119.08(17)
C24 C23 C26 . . 121.22(15)
C23 C24 C25 . . 117.94(17)
C23 C24 H24 . . 121.0
C25 C24 H24 . . 121.0
N21 C25 C24 . . 123.03(18)
N21 C25 H25 . . 118.5
C24 C25 H25 . . 118.5
N22 C26 C23 . . 179.1(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Fe1 O1 3_667 2.0888(11)
Fe1 O1 . 2.0888(11)
Fe1 N1 . 2.1153(13)
Fe1 N1 3_667 2.1153(13)
Fe1 N11 3_667 2.2451(14)
Fe1 N11 . 2.2451(14)
N1 C1 . 1.158(2)
C1 S1 . 1.6286(16)
N11 C15 . 1.337(2)
N11 C11 . 1.338(2)
C11 C12 . 1.378(3)
C11 H11 . 0.9500
C12 C13 . 1.382(3)
C12 H12 . 0.9500
C13 C14 . 1.382(3)
C13 C16 . 1.447(3)
C14 C15 . 1.383(3)
C14 H14 . 0.9500
C15 H15 . 0.9500
C16 N12 . 1.141(3)
O1 H1 . 0.8400
O1 H2 . 0.8400
N21 C21 . 1.325(3)
N21 C25 . 1.329(3)
C21 C22 . 1.368(3)
C21 H21 . 0.9500
C22 C23 . 1.377(3)
C22 H22 . 0.9500
C23 C24 . 1.380(3)
C23 C26 . 1.442(2)
C24 C25 . 1.382(3)
C24 H24 . 0.9500
C25 H25 . 0.9500
C26 N22 . 1.140(2)
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
C12 H12 N12 3_566 0.95 2.52 3.437(3) 161.5
C14 H14 S1 4_575 0.95 3.01 3.960(2) 177.2
O1 H1 N22 3_667 0.84 2.00 2.8380(19) 177.2
O1 H2 N21 4_476 0.84 1.89 2.7159(19) 167.7

_cod_database_fobs_code 2020739
