#------------------------------------------------------------------------------
#$Date: 2022-09-06 13:13:25 +0300 (Tue, 06 Sep 2022) $
#$Revision: 277675 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/06/16/7061644.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7061644
loop_
_publ_author_name
'Plaza-Lozano, Diego'
'Ramírez-Palma, David'
'Vela, Alberto'
'Olguín, Juan'
_publ_section_title
;
 High spin iron(ii) complexes based on imidazolyl- and
 1,2,3-triazolyl-thione ligands and NCE (E = S, Se or BH3) co-ligands:
 effect of the S-functional group on the structural and magnetic
 properties
;
_journal_issue                   31
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              14910
_journal_page_last               14921
_journal_paper_doi               10.1039/D2NJ01989B
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety         'C20 H18 Fe N8 S4'
_chemical_formula_sum            'C20 H18 Fe N8 S4'
_chemical_formula_weight         554.51
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2020-05-23 deposited with the CCDC.	2022-07-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.618(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.8211(7)
_cell_length_b                   15.7029(11)
_cell_length_c                   7.7911(6)
_cell_measurement_reflns_used    9991
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      33.16
_cell_measurement_theta_min      2.47
_cell_volume                     1184.65(15)
_computing_cell_refinement       'APEX2 v2012.10.0(Bruker, 2012)'
_computing_data_collection
'Bruker Instrument Service (Bruker AXS Inc., 2015)'
_computing_data_reduction        'SAINT V8.27B (Bruker, 2012)'
_computing_molecular_graphics    'XP V 5.1 (Bruker, 1998)'
_computing_publication_material  'CIFTAB V 2013/2 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2012 (Bruker, 2013)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 VENTURE diffractometer'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0355
_diffrn_reflns_av_unetI/netI     0.0173
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            36368
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.575
_diffrn_reflns_theta_min         2.471
_diffrn_source_type              'Incoatec I\mS HB'
_exptl_absorpt_coefficient_mu    1.016
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.7019
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Sheldrick, 2012)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             568
_exptl_crystal_size_max          0.303
_exptl_crystal_size_mid          0.277
_exptl_crystal_size_min          0.254
_exptl_transmission_factor_max   0.7465
_exptl_transmission_factor_min   0.7019
_refine_diff_density_max         0.417
_refine_diff_density_min         -0.473
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     152
_refine_ls_number_reflns         4290
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0275
_refine_ls_R_factor_gt           0.0244
_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)+(0.0274P)²+0.4383P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0630
_refine_ls_wR_factor_ref         0.0646
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3956
_reflns_number_total             4290
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2nj01989b2.cif
_cod_data_source_block           DPL019
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7061643--7061648.cif.
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7061644
_shelx_shelxl_version_number     2014/7
_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.
;
_shelx_estimated_absorpt_t_min   0.748
_shelx_estimated_absorpt_t_max   0.782
_diffrn_source_source            'microfocus sealed tube'
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_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.5000 0.5000 0.5000 0.01380(5) Uani 1 2 d S . P . .
C1 C 0.76366(10) 0.39438(6) 0.62734(13) 0.01908(17) Uani 1 1 d . . . . .
H1 H 0.7886 0.4243 0.5312 0.023 Uiso 1 1 calc R U . . .
N1 N 0.63284(8) 0.40196(5) 0.65800(10) 0.01664(14) Uani 1 1 d . . . . .
S1 S 0.42252(3) 0.53855(2) 0.77696(3) 0.01825(5) Uani 1 1 d . . . . .
N2 N 0.46413(9) 0.36566(5) 0.82950(11) 0.01867(15) Uani 1 1 d . . . . .
C2 C 0.86308(11) 0.34542(7) 0.72842(14) 0.02221(18) Uani 1 1 d . . . . .
H2 H 0.9534 0.3408 0.7007 0.027 Uiso 1 1 calc R U . . .
S2 S 0.94163(3) 0.63699(2) 0.66335(5) 0.03860(9) Uani 1 1 d . . . . .
C6 C 0.39786(12) 0.29747(7) 0.89663(16) 0.0273(2) Uani 1 1 d . . . . .
H6 H 0.4294 0.2402 0.9078 0.033 Uiso 1 1 calc R U . . .
C7 C 0.28165(12) 0.32805(7) 0.94216(17) 0.0294(2) Uani 1 1 d . . . . .
H7 H 0.2153 0.2964 0.9914 0.035 Uiso 1 1 calc R U . . .
N3 N 0.27587(9) 0.41421(6) 0.90429(12) 0.02175(16) Uani 1 1 d . . . . .
C3 C 0.82825(12) 0.30319(7) 0.87114(15) 0.0275(2) Uani 1 1 d . . . . .
H3 H 0.8948 0.2697 0.9441 0.033 Uiso 1 1 calc R U . . .
C5 C 0.60094(10) 0.35999(6) 0.79493(12) 0.01735(16) Uani 1 1 d . . . . .
C4 C 0.69527(12) 0.31050(7) 0.90579(14) 0.0254(2) Uani 1 1 d . . . . .
H4 H 0.6688 0.2824 1.0030 0.030 Uiso 1 1 calc R U . . .
N4 N 0.66750(9) 0.58584(6) 0.55993(12) 0.02155(16) Uani 1 1 d . . . . .
C8 C 0.16758(12) 0.47206(8) 0.93835(18) 0.0317(2) Uani 1 1 d . . . . .
H8A H 0.1210 0.4965 0.8283 0.048 Uiso 1 1 calc R U . . .
H8B H 0.2084 0.5179 1.0156 0.048 Uiso 1 1 calc R U . . .
H8C H 0.1004 0.4407 0.9940 0.048 Uiso 1 1 calc R U . . .
C10 C 0.78176(10) 0.60722(6) 0.60228(13) 0.01990(17) Uani 1 1 d . . . . .
C9 C 0.38764(9) 0.43819(6) 0.83662(12) 0.01660(15) Uani 1 1 d . . . . .
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N4 Fe1 N4 180.00(4) 3_666 . ?
N4 Fe1 N1 92.48(3) 3_666 . ?
N4 Fe1 N1 87.52(3) . . ?
N4 Fe1 N1 87.52(3) 3_666 3_666 ?
N4 Fe1 N1 92.48(3) . 3_666 ?
N1 Fe1 N1 180.0 . 3_666 ?
N4 Fe1 S1 90.41(3) 3_666 . ?
N4 Fe1 S1 89.59(3) . . ?
N1 Fe1 S1 85.70(2) . . ?
N1 Fe1 S1 94.30(2) 3_666 . ?
N4 Fe1 S1 89.59(3) 3_666 3_666 ?
N4 Fe1 S1 90.41(3) . 3_666 ?
N1 Fe1 S1 94.30(2) . 3_666 ?
N1 Fe1 S1 85.70(2) 3_666 3_666 ?
S1 Fe1 S1 180.0 . 3_666 ?
N1 C1 C2 123.44(9) . . ?
N1 C1 H1 118.3 . . ?
C2 C1 H1 118.3 . . ?
C5 N1 C1 117.06(8) . . ?
C5 N1 Fe1 125.71(6) . . ?
C1 N1 Fe1 116.48(6) . . ?
C9 S1 Fe1 96.73(3) . . ?
C9 N2 C6 109.18(8) . . ?
C9 N2 C5 127.13(8) . . ?
C6 N2 C5 122.56(8) . . ?
C1 C2 C3 118.56(9) . . ?
C1 C2 H2 120.7 . . ?
C3 C2 H2 120.7 . . ?
C7 C6 N2 107.15(9) . . ?
C7 C6 H6 126.4 . . ?
N2 C6 H6 126.4 . . ?
C6 C7 N3 107.48(9) . . ?
C6 C7 H7 126.3 . . ?
N3 C7 H7 126.3 . . ?
C9 N3 C7 110.44(9) . . ?
C9 N3 C8 124.34(9) . . ?
C7 N3 C8 125.18(9) . . ?
C4 C3 C2 119.02(9) . . ?
C4 C3 H3 120.5 . . ?
C2 C3 H3 120.5 . . ?
N1 C5 C4 123.38(9) . . ?
N1 C5 N2 118.52(8) . . ?
C4 C5 N2 118.09(9) . . ?
C3 C4 C5 118.53(10) . . ?
C3 C4 H4 120.7 . . ?
C5 C4 H4 120.7 . . ?
C10 N4 Fe1 157.21(8) . . ?
N3 C8 H8A 109.5 . . ?
N3 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N3 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N4 C10 S2 179.50(10) . . ?
N3 C9 N2 105.74(8) . . ?
N3 C9 S1 125.60(7) . . ?
N2 C9 S1 128.65(7) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N4 2.1177(9) 3_666 ?
Fe1 N4 2.1177(9) . ?
Fe1 N1 2.2474(8) . ?
Fe1 N1 2.2474(8) 3_666 ?
Fe1 S1 2.4800(3) . ?
Fe1 S1 2.4800(3) 3_666 ?
C1 N1 1.3507(12) . ?
C1 C2 1.3812(14) . ?
C1 H1 0.9500 . ?
N1 C5 1.3351(12) . ?
S1 C9 1.6942(10) . ?
N2 C9 1.3705(12) . ?
N2 C6 1.3991(13) . ?
N2 C5 1.4166(13) . ?
C2 C3 1.3857(15) . ?
C2 H2 0.9500 . ?
S2 C10 1.6312(11) . ?
C6 C7 1.3395(16) . ?
C6 H6 0.9500 . ?
C7 N3 1.3840(15) . ?
C7 H7 0.9500 . ?
N3 C9 1.3484(12) . ?
N3 C8 1.4564(14) . ?
C3 C4 1.3818(16) . ?
C3 H3 0.9500 . ?
C5 C4 1.3931(13) . ?
C4 H4 0.9500 . ?
N4 C10 1.1649(13) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C6 H6 N4 0.95 2.63 3.4122(14) 139.7 2_646
C1 H1 S1 0.95 2.96 3.5285(10) 120.0 3_666
C8 H8A S2 0.98 2.98 3.8254(14) 145.5 1_455
C8 H8C S2 0.98 3.03 3.8503(14) 142.6 3_667
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 C1 N1 C5 0.67(14) . . . . ?
C2 C1 N1 Fe1 171.28(8) . . . . ?
N1 C1 C2 C3 -1.45(16) . . . . ?
C9 N2 C6 C7 0.68(13) . . . . ?
C5 N2 C6 C7 169.32(10) . . . . ?
N2 C6 C7 N3 -0.16(14) . . . . ?
C6 C7 N3 C9 -0.43(14) . . . . ?
C6 C7 N3 C8 -178.24(11) . . . . ?
C1 C2 C3 C4 0.93(17) . . . . ?
C1 N1 C5 C4 0.62(14) . . . . ?
Fe1 N1 C5 C4 -169.01(8) . . . . ?
C1 N1 C5 N2 -179.19(8) . . . . ?
Fe1 N1 C5 N2 11.18(12) . . . . ?
C9 N2 C5 N1 -48.64(14) . . . . ?
C6 N2 C5 N1 144.85(10) . . . . ?
C9 N2 C5 C4 131.54(11) . . . . ?
C6 N2 C5 C4 -34.97(14) . . . . ?
C2 C3 C4 C5 0.25(17) . . . . ?
N1 C5 C4 C3 -1.08(16) . . . . ?
N2 C5 C4 C3 178.73(10) . . . . ?
C7 N3 C9 N2 0.84(12) . . . . ?
C8 N3 C9 N2 178.66(10) . . . . ?
C7 N3 C9 S1 -178.51(8) . . . . ?
C8 N3 C9 S1 -0.68(15) . . . . ?
C6 N2 C9 N3 -0.92(11) . . . . ?
C5 N2 C9 N3 -168.91(9) . . . . ?
C6 N2 C9 S1 178.39(8) . . . . ?
C5 N2 C9 S1 10.41(15) . . . . ?
Fe1 S1 C9 N3 -137.16(8) . . . . ?
Fe1 S1 C9 N2 43.65(9) . . . . ?
