#------------------------------------------------------------------------------
#$Date: 2023-12-07 13:47:44 +0200 (Thu, 07 Dec 2023) $
#$Revision: 288128 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/29/2022930.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_2022930
loop_
_publ_author_name
'Näther, Christian'
'Müller-Meinhard, Asmus'
'Jess, Inke'
_publ_section_title
;
 Synthesis, crystal structure and properties of
 tetra-kis-(pyridine-3-carbo-nitrile)-dithio-cyanatoiron(II) and of
 diaqua-bis-(pyridine-3-carbo-nitrile)-di-thio-cyanatoiron(II)
 pyridine-3-carbo-nitrile monosolvate.
;
_journal_issue                   'Pt 11'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first              1093
_journal_page_last               1099
_journal_paper_doi               10.1107/S205698902300909X
_journal_volume                  79
_journal_year                    2023
_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(pyridine-3-carbonitrile)dithiocyanatoiron(II) pyridine-3-carbonitrile
monosolvate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_cell_angle_alpha                84.7650(10)
_cell_angle_beta                 77.7870(10)
_cell_angle_gamma                70.8260(10)
_cell_formula_units_Z            1
_cell_length_a                   8.10650(10)
_cell_length_b                   8.28800(10)
_cell_length_c                   11.4347(2)
_cell_measurement_reflns_used    25131
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      79.6570
_cell_measurement_theta_min      3.9450
_cell_volume                     709.021(18)
_computing_cell_refinement
;
CrysAlisPro 1.171.42.100a (Rigaku OD, 2023)
;
_computing_data_collection
;
CrysAlisPro 1.171.42.100a (Rigaku OD, 2023)
;
_computing_data_reduction
;
CrysAlisPro 1.171.42.100a (Rigaku OD, 2023)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg & Putz, 1999)
;
_computing_publication_material
;
Publcif (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2016/6 (Sheldrick, 2015a)
;
_computing_structure_solution
;
SHELXT2014/5 (Sheldrick, 2015b)
;
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0219
_diffrn_reflns_av_unetI/netI     0.0089
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            29397
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.346
_diffrn_reflns_theta_min         3.957
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    6.012
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72660
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysalisPro; Rigaku OD, 2023)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_description       block
_exptl_crystal_F_000             320
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.287
_refine_diff_density_min         -0.245
_refine_ls_extinction_coef       0.0036(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method
;
SHELXL-2016/6 (Sheldrick 2016)
;
_refine_ls_goodness_of_fit_ref   1.146
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         2999
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.146
_refine_ls_R_factor_all          0.0215
_refine_ls_R_factor_gt           0.0215
_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)+(0.0302P)²+0.2457P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0600
_refine_ls_wR_factor_ref         0.0600
_reflns_number_gt                2999
_reflns_number_total             2999
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            hb8079sup1.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 2022929--2022930.cif.'
_cod_database_code               2022930
_cod_database_fobs_code          2022930
_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'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe Fe1 0.500000 0.500000 0.500000 0.01216(8) Uani d 1 . .
N N1 0.23749(14) 0.50517(14) 0.58058(10) 0.0175(2) Uani d 1 . .
C C1 0.10930(16) 0.48617(15) 0.64015(11) 0.0145(2) Uani d 1 . .
S S1 -0.06651(4) 0.45890(4) 0.72985(3) 0.01772(9) Uani d 1 . .
O O1 0.58744(12) 0.38660(11) 0.65983(8) 0.01684(18) Uani d 1 . .
N N11 0.55002(13) 0.24567(12) 0.42347(9) 0.0137(2) Uani d 1 . .
C C11 0.41230(15) 0.20838(15) 0.39913(10) 0.0144(2) Uani d 1 . .
H H11 0.295430 0.284514 0.423936 0.017 Uiso calc 1 . .
C C12 0.43436(16) 0.06162(15) 0.33861(11) 0.0151(2) Uani d 1 . .
C C13 0.60473(17) -0.05288(15) 0.30294(11) 0.0179(2) Uani d 1 . .
H H13 0.622799 -0.154127 0.262362 0.022 Uiso calc 1 . .
C C14 0.74656(16) -0.01402(16) 0.32865(12) 0.0183(2) Uani d 1 . .
H H14 0.864668 -0.088837 0.306060 0.022 Uiso calc 1 . .
C C15 0.71430(16) 0.13553(15) 0.38781(11) 0.0163(2) Uani d 1 . .
H H15 0.812998 0.161414 0.403931 0.020 Uiso calc 1 . .
C C16 0.27896(17) 0.03358(16) 0.31361(12) 0.0195(3) Uani d 1 . .
N N12 0.15470(16) 0.01357(16) 0.29369(12) 0.0292(3) Uani d 1 . .
N N21 0.40361(14) 0.59653(13) 0.85071(9) 0.0177(2) Uani d 1 . .
C C21 0.22852(17) 0.62145(16) 0.88138(11) 0.0176(2) Uani d 1 . .
H H21 0.176535 0.564393 0.838477 0.021 Uiso calc 1 . .
C C22 0.11976(16) 0.72784(15) 0.97378(11) 0.0160(2) Uani d 1 . .
C C23 0.19423(17) 0.81232(16) 1.03776(11) 0.0177(2) Uani d 1 . .
H H23 0.122870 0.885180 1.101462 0.021 Uiso calc 1 . .
C C24 0.37532(17) 0.78663(16) 1.00549(12) 0.0190(3) Uani d 1 . .
H H24 0.430907 0.842236 1.046636 0.023 Uiso calc 1 . .
C C25 0.47433(16) 0.67873(16) 0.91238(11) 0.0177(2) Uani d 1 . .
H H25 0.598501 0.661992 0.891042 0.021 Uiso calc 1 . .
C C26 -0.06797(17) 0.74885(16) 1.00254(11) 0.0191(3) Uani d 1 . .
N N22 -0.21762(15) 0.76797(16) 1.02557(11) 0.0256(3) Uani d 1 . .
H H1A 0.531(3) 0.450(3) 0.724(2) 0.045(6) Uiso d 1 . .
H H1B 0.693(3) 0.369(3) 0.6554(18) 0.042(6) 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 0.0181 0.0091 '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 -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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 2_666 . 180.0 n
N1 Fe1 O1 . . 89.42(4) y
N1 Fe1 O1 2_666 . 90.58(4) y
N1 Fe1 O1 . 2_666 90.58(4) ?
N1 Fe1 O1 2_666 2_666 89.42(4) ?
N1 Fe1 N11 . . 89.86(4) y
N1 Fe1 N11 2_666 . 90.14(4) y
N1 Fe1 N11 2_666 2_666 89.86(4) ?
N1 Fe1 N11 . 2_666 90.14(4) ?
O1 Fe1 O1 2_666 . 180.0 n
O1 Fe1 N11 2_666 . 87.62(3) y
O1 Fe1 N11 2_666 2_666 92.38(3) ?
O1 Fe1 N11 . . 92.38(3) y
O1 Fe1 N11 . 2_666 87.62(3) ?
N11 Fe1 N11 . 2_666 180.0 n
Fe1 N1 C1 . . 167.09(10) y
N1 C1 S1 . . 177.12(11) ?
Fe1 O1 H1A . . 113.2(14) ?
Fe1 O1 H1B . . 112.3(14) ?
H1A O1 H1B . . 106.9(19) ?
C11 N11 Fe1 . . 118.64(8) ?
C11 N11 C15 . . 117.74(10) ?
C15 N11 Fe1 . . 123.18(8) ?
N11 C11 H11 . . 118.8 ?
N11 C11 C12 . . 122.34(11) ?
C12 C11 H11 . . 118.8 ?
C11 C12 C16 . . 118.64(11) ?
C13 C12 C11 . . 119.66(11) ?
C13 C12 C16 . . 121.70(11) ?
C12 C13 H13 . . 121.1 ?
C14 C13 C12 . . 117.77(11) ?
C14 C13 H13 . . 121.1 ?
C13 C14 H14 . . 120.4 ?
C13 C14 C15 . . 119.26(11) ?
C15 C14 H14 . . 120.4 ?
N11 C15 C14 . . 123.23(11) ?
N11 C15 H15 . . 118.4 ?
C14 C15 H15 . . 118.4 ?
N12 C16 C12 . . 179.12(14) ?
C21 N21 C25 . . 117.81(11) ?
N21 C21 H21 . . 118.8 ?
N21 C21 C22 . . 122.43(11) ?
C22 C21 H21 . . 118.8 ?
C21 C22 C23 . . 119.45(11) ?
C21 C22 C26 . . 119.67(11) ?
C23 C22 C26 . . 120.87(11) ?
C22 C23 H23 . . 121.0 ?
C24 C23 C22 . . 117.93(12) ?
C24 C23 H23 . . 121.0 ?
C23 C24 H24 . . 120.5 ?
C23 C24 C25 . . 119.07(11) ?
C25 C24 H24 . . 120.5 ?
N21 C25 C24 . . 123.30(11) ?
N21 C25 H25 . . 118.3 ?
C24 C25 H25 . . 118.3 ?
N22 C26 C22 . . 179.03(14) ?
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 2_666 2.1207(10) ?
Fe1 N1 . 2.1207(10) y
Fe1 O1 2_666 2.1267(9) ?
Fe1 O1 . 2.1267(9) y
Fe1 N11 . 2.2358(10) y
Fe1 N11 2_666 2.2358(10) ?
N1 C1 . 1.1649(17) ?
C1 S1 . 1.6387(12) ?
O1 H1A . 0.89(2) ?
O1 H1B . 0.81(2) ?
N11 C11 . 1.3390(15) ?
N11 C15 . 1.3463(15) ?
C11 H11 . 0.9500 ?
C11 C12 . 1.3960(16) ?
C12 C13 . 1.3949(17) ?
C12 C16 . 1.4421(17) ?
C13 H13 . 0.9500 ?
C13 C14 . 1.3841(17) ?
C14 H14 . 0.9500 ?
C14 C15 . 1.3883(17) ?
C15 H15 . 0.9500 ?
C16 N12 . 1.1435(18) ?
N21 C21 . 1.3380(16) ?
N21 C25 . 1.3436(16) ?
C21 H21 . 0.9500 ?
C21 C22 . 1.3916(18) ?
C22 C23 . 1.3956(17) ?
C22 C26 . 1.4419(17) ?
C23 H23 . 0.9500 ?
C23 C24 . 1.3844(17) ?
C24 H24 . 0.9500 ?
C24 C25 . 1.3850(18) ?
C25 H25 . 0.9500 ?
C26 N22 . 1.1456(17) ?
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 N21 . 0.89(2) 1.88(2) 2.7615(14) 175(2)
O1 H1B S1 1_655 0.81(2) 2.62(2) 3.3184(9) 145.7(18)
C11 H11 N1 . 0.95 2.54 3.1243(16) 120
C11 H11 S1 2_566 0.95 3.03 3.6833(12) 128
C14 H14 S1 2_656 0.95 2.98 3.7688(13) 141
C15 H15 N1 2_666 0.95 2.67 3.1894(16) 115
C21 H21 S1 . 0.95 2.92 3.8513(13) 165
C24 H24 N22 1_655 0.95 2.67 3.3082(17) 125
C25 H25 S1 1_655 0.95 3.01 3.8056(13) 142
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
Fe1 N11 C11 C12 . . . . 172.36(9) ?
Fe1 N11 C15 C14 . . . . -172.87(9) ?
N11 C11 C12 C13 . . . . 0.88(18) ?
N11 C11 C12 C16 . . . . -178.52(11) ?
C11 N11 C15 C14 . . . . -0.63(18) ?
C11 C12 C13 C14 . . . . -0.64(18) ?
C12 C13 C14 C15 . . . . -0.17(18) ?
C13 C14 C15 N11 . . . . 0.84(19) ?
C15 N11 C11 C12 . . . . -0.24(17) ?
C16 C12 C13 C14 . . . . 178.74(12) ?
N21 C21 C22 C23 . . . . -0.10(19) ?
N21 C21 C22 C26 . . . . -179.84(11) ?
C21 N21 C25 C24 . . . . 0.17(18) ?
C21 C22 C23 C24 . . . . 0.31(18) ?
C22 C23 C24 C25 . . . . -0.28(19) ?
C23 C24 C25 N21 . . . . 0.04(19) ?
C25 N21 C21 C22 . . . . -0.14(18) ?
C26 C22 C23 C24 . . . . -179.96(12) ?
