#------------------------------------------------------------------------------
#$Date: 2024-01-07 13:50:35 +0200 (Sun, 07 Jan 2024) $
#$Revision: 288943 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/29/2022948.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_2022948
loop_
_publ_author_name
'Müller-Meinhard, Asmus'
'Jess, Inke'
'Näther, Christian'
_publ_section_title
;
 Synthesis, crystal structure and properties of
 chloridotetrakis(pyridine-3-carbonitrile)thiocyanatoiron(II)
;
_journal_coeditor_code           NX2002
_journal_issue                   12
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_page_first              1173
_journal_page_last               1178
_journal_paper_doi               10.1107/S205698902300988X
_journal_volume                  79
_journal_year                    2023
_chemical_formula_iupac          '[Fe Cl (N C S) (C6 H4 N2)4]'
_chemical_formula_moiety         'C25 H16 Cl Fe N9 S'
_chemical_formula_sum            'C25 H16 Cl Fe N9 S'
_chemical_formula_weight         565.83
_chemical_name_systematic
;
Chloridotetrakis(pyridine-3-carbonitrile)thiocyanatoiron(II)
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           104
_space_group_name_Hall           'P 4 -2n'
_space_group_name_H-M_alt        'P 4 n c'
_atom_sites_solution_hydrogens   geom
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.79412(6)
_cell_length_b                   10.79412(6)
_cell_length_c                   11.15065(11)
_cell_measurement_reflns_used    9200
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      79.6630
_cell_measurement_theta_min      5.6860
_cell_volume                     1299.196(16)
_computing_cell_refinement
;
CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)
;
_computing_data_collection
;
CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)
;
_computing_data_reduction
;
CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg & Putz, 1999)
;
_computing_publication_material
;
Publcif (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2016/6 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2014/5 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_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  0.0208
_diffrn_reflns_av_unetI/netI     0.0093
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11711
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.863
_diffrn_reflns_theta_min         5.705
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    6.623
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68557
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2023)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_description       block
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.338
_refine_diff_density_min         -0.345
_refine_ls_abs_structure_details
;
Flack x determined using 652 quotients
[(I⁺)-(I⁻)]/[(I⁺)+(I⁻)]
(Parsons et al.,  2013)
;
_refine_ls_abs_structure_Flack   -0.0059(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     88
_refine_ls_number_reflns         1411
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.138
_refine_ls_R_factor_all          0.0227
_refine_ls_R_factor_gt           0.0225
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0384P)²+0.3704P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0653
_refine_ls_wR_factor_ref         0.0654
_reflns_number_gt                1406
_reflns_number_total             1411
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            nx2002sup1.cif
_cod_data_source_block           I
_cod_depositor_comments          'Adding full bibliography for 2022948.cif.'
_cod_original_cell_volume        1299.20(2)
_cod_database_code               2022948
_cod_database_fobs_code          2022948
_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'
'-y, x, z'
'y, -x, z'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+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
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe Fe1 0.500000 0.500000 0.61306(6) 0.01647(19) Uani d 1 . .
N N1 0.500000 0.500000 0.4248(4) 0.0230(11) Uani d 1 . .
C C1 0.500000 0.500000 0.3226(6) 0.0211(10) Uani d 1 . .
S S1 0.500000 0.500000 0.17570(13) 0.0298(3) Uani d 1 . .
Cl Cl1 0.500000 0.500000 0.82574(10) 0.0218(3) Uani d 1 . .
N N11 0.37363(17) 0.33550(16) 0.59511(18) 0.0205(4) Uani d 1 . .
C C11 0.38831(19) 0.2322(2) 0.6601(2) 0.0215(4) Uani d 1 . .
H H11 0.442330 0.233778 0.727352 0.026 Uiso calc 1 . .
C C12 0.3268(2) 0.12224(19) 0.6321(2) 0.0231(4) Uani d 1 . .
C C13 0.2477(2) 0.1182(2) 0.5330(2) 0.0247(5) Uani d 1 . .
H H13 0.206877 0.043560 0.511051 0.030 Uiso calc 1 . .
C C14 0.2307(2) 0.2254(2) 0.4677(3) 0.0235(5) Uani d 1 . .
H H14 0.176720 0.226567 0.400458 0.028 Uiso calc 1 . .
C C15 0.2940(2) 0.3315(2) 0.5023(2) 0.0216(4) Uani d 1 . .
H H15 0.280313 0.405460 0.457985 0.026 Uiso calc 1 . .
C C16 0.3447(2) 0.0135(2) 0.7051(3) 0.0278(5) Uani d 1 . .
N N12 0.3583(2) -0.0743(2) 0.7610(2) 0.0362(5) 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 0.0181 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'
Cl Cl 0.3639 0.7018 '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'
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 Cl1 . . 180.0 y
N1 Fe1 N11 . 4_565 84.89(6) ?
N1 Fe1 N11 . 2_665 84.89(6) ?
N1 Fe1 N11 . . 84.89(6) y
N1 Fe1 N11 . 3_655 84.89(6) ?
N11 Fe1 Cl1 3_655 . 95.11(6) ?
N11 Fe1 Cl1 4_565 . 95.11(6) ?
N11 Fe1 Cl1 2_665 . 95.11(6) ?
N11 Fe1 Cl1 . . 95.11(6) y
N11 Fe1 N11 2_665 4_565 89.546(11) y
N11 Fe1 N11 . 4_565 89.547(11) ?
N11 Fe1 N11 2_665 3_655 89.546(11) ?
N11 Fe1 N11 4_565 3_655 169.78(12) ?
N11 Fe1 N11 2_665 . 169.79(12) y
N11 Fe1 N11 . 3_655 89.545(11) y
C1 N1 Fe1 . . 180.0 ?
N1 C1 S1 . . 180.0 ?
C11 N11 Fe1 . . 122.53(15) ?
C11 N11 C15 . . 117.71(19) ?
C15 N11 Fe1 . . 118.75(14) ?
N11 C11 H11 . . 119.0 ?
N11 C11 C12 . . 122.1(2) ?
C12 C11 H11 . . 119.0 ?
C11 C12 C13 . . 119.6(2) ?
C11 C12 C16 . . 120.1(2) ?
C13 C12 C16 . . 120.2(2) ?
C12 C13 H13 . . 120.9 ?
C14 C13 C12 . . 118.2(2) ?
C14 C13 H13 . . 120.9 ?
C13 C14 H14 . . 120.6 ?
C13 C14 C15 . . 118.7(2) ?
C15 C14 H14 . . 120.6 ?
N11 C15 C14 . . 123.6(2) ?
N11 C15 H15 . . 118.2 ?
C14 C15 H15 . . 118.2 ?
N12 C16 C12 . . 178.5(3) ?
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 . 2.099(4) y
Fe1 Cl1 . 2.3716(12) y
Fe1 N11 4_565 2.2480(18) ?
Fe1 N11 2_665 2.2480(18) ?
Fe1 N11 . 2.2480(18) y
Fe1 N11 3_655 2.2480(18) ?
N1 C1 . 1.140(8) ?
C1 S1 . 1.638(7) ?
N11 C11 . 1.340(3) ?
N11 C15 . 1.346(3) ?
C11 H11 . 0.9500 ?
C11 C12 . 1.395(3) ?
C12 C13 . 1.397(3) ?
C12 C16 . 1.441(3) ?
C13 H13 . 0.9500 ?
C13 C14 . 1.379(3) ?
C14 H14 . 0.9500 ?
C14 C15 . 1.389(3) ?
C15 H15 . 0.9500 ?
C16 N12 . 1.144(3) ?
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
C14 H14 N12 6_554 0.95 2.68 3.304(3) 123.8
C15 H15 N12 6_554 0.95 2.67 3.313(3) 125.8
