#------------------------------------------------------------------------------
#$Date: 2022-09-06 13:13:25 +0300 (Tue, 06 Sep 2022) $
#$Revision: 277675 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/06/16/7061648.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_7061648
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         'C30 H24 Fe N10 S4'
_chemical_formula_sum            'C30 H24 Fe N10 S4'
_chemical_formula_weight         708.68
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2020-05-23 deposited with the CCDC.	2022-07-07 downloaded from the CCDC.
;
_cell_angle_alpha                106.039(3)
_cell_angle_beta                 102.841(4)
_cell_angle_gamma                99.914(3)
_cell_formula_units_Z            1
_cell_length_a                   8.2200(8)
_cell_length_b                   8.4119(8)
_cell_length_c                   13.0015(13)
_cell_measurement_reflns_used    9601
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      27.91
_cell_measurement_theta_min      2.60
_cell_volume                     815.81(14)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      170(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0678
_diffrn_reflns_av_unetI/netI     0.0194
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_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       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            84766
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.481
_diffrn_reflns_theta_min         2.624
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_type              'Incoatec I\mS HB'
_exptl_absorpt_coefficient_mu    0.757
_exptl_absorpt_correction_T_max  0.7273
_exptl_absorpt_correction_T_min  0.6653
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Sheldrick, 2012)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.442
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             364
_exptl_crystal_size_max          0.263
_exptl_crystal_size_mid          0.177
_exptl_crystal_size_min          0.098
_exptl_transmission_factor_max   0.7273
_exptl_transmission_factor_min   0.6653
_refine_diff_density_max         0.314
_refine_diff_density_min         -0.526
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     242
_refine_ls_number_reflns         3732
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0305
_refine_ls_R_factor_gt           0.0269
_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)+(0.0373P)²+0.3214P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0695
_refine_ls_wR_factor_ref         0.0720
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3425
_reflns_number_total             3732
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2nj01989b2.cif
_cod_data_source_block           DPL290
_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_cell_volume        815.80(14)
_cod_database_code               7061648
_shelx_shelxl_version_number     2017/1
_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   0.826
_shelx_estimated_absorpt_t_max   0.930
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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 1.000000 0.500000 0.500000 0.01872(8) Uani 1 2 d S . P . .
S1 S 0.69485(4) 0.36849(4) 0.48009(3) 0.02232(9) Uani 1 1 d . . . . .
N1 N 0.92833(14) 0.75379(14) 0.54520(9) 0.0222(2) Uani 1 1 d . . . . .
C1 C 1.05006(19) 0.88605(18) 0.62325(12) 0.0273(3) Uani 1 1 d . . . . .
H1 H 1.158(2) 0.862(2) 0.6490(14) 0.027(4) Uiso 1 1 d . . . . .
N2 N 0.65026(14) 0.65016(14) 0.41821(9) 0.0224(2) Uani 1 1 d . . . . .
S2 S 0.80083(9) 0.51408(6) 0.12233(3) 0.05835(16) Uani 1 1 d . . . . .
C2 C 1.0244(2) 1.04740(18) 0.66317(13) 0.0313(3) Uani 1 1 d . . . . .
H2 H 1.116(3) 1.129(3) 0.7155(17) 0.044(5) Uiso 1 1 d . . . . .
N3 N 0.55537(16) 0.69980(15) 0.34031(10) 0.0285(3) Uani 1 1 d . . . . .
C3 C 0.8641(2) 1.07375(19) 0.62433(14) 0.0342(3) Uani 1 1 d . . . . .
H3 H 0.845(2) 1.185(2) 0.6487(16) 0.041(5) Uiso 1 1 d . . . . .
C4 C 0.7362(2) 0.93982(18) 0.54584(13) 0.0317(3) Uani 1 1 d . . . . .
H4 H 0.619(3) 0.947(3) 0.5129(17) 0.049(5) Uiso 1 1 d . . . . .
N4 N 0.45277(16) 0.55586(15) 0.26923(10) 0.0282(3) Uani 1 1 d . . . . .
C5 C 0.77632(17) 0.78428(16) 0.50792(11) 0.0221(3) Uani 1 1 d . . . . .
N5 N 0.93488(15) 0.47831(15) 0.32865(10) 0.0265(2) Uani 1 1 d . . . . .
C6 C 0.3349(3) 0.5614(2) 0.16824(15) 0.0468(4) Uani 1 1 d . . . . .
H6A H 0.354656 0.486392 0.102165 0.070 Uiso 1 1 calc R U . . .
H6B H 0.355516 0.678696 0.166385 0.070 Uiso 1 1 calc R U . . .
H6C H 0.215587 0.522772 0.168647 0.070 Uiso 1 1 calc R U . . .
C8 C 0.47689(17) 0.41595(17) 0.29696(11) 0.0242(3) Uani 1 1 d . . . . .
C7 C 0.60699(16) 0.47623(16) 0.39747(11) 0.0207(2) Uani 1 1 d . . . . .
C9 C 0.38261(18) 0.24138(17) 0.22540(11) 0.0261(3) Uani 1 1 d . . . . .
C10 C 0.2046(2) 0.1886(2) 0.20190(13) 0.0336(3) Uani 1 1 d . . . . .
H10 H 0.145(3) 0.267(3) 0.2352(17) 0.047(5) Uiso 1 1 d . . . . .
C11 C 0.1178(2) 0.0253(2) 0.13042(14) 0.0427(4) Uani 1 1 d . . . . .
H11 H -0.008(3) -0.013(3) 0.1120(18) 0.058(6) Uiso 1 1 d . . . . .
C12 C 0.2072(3) -0.0843(2) 0.08173(14) 0.0463(4) Uani 1 1 d . . . . .
H12 H 0.149(3) -0.195(3) 0.0309(19) 0.060(6) Uiso 1 1 d . . . . .
C13 C 0.3831(3) -0.0325(2) 0.10455(16) 0.0465(4) Uani 1 1 d . . . . .
H13 H 0.450(3) -0.105(3) 0.072(2) 0.068(7) Uiso 1 1 d . . . . .
C14 C 0.4725(2) 0.1303(2) 0.17691(14) 0.0365(3) Uani 1 1 d . . . . .
H14 H 0.597(3) 0.168(2) 0.1928(16) 0.041(5) Uiso 1 1 d . . . . .
C15 C 0.87962(19) 0.49225(17) 0.24246(11) 0.0263(3) 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
N5 Fe1 N5 180.0 2_766 . ?
N5 Fe1 N1 90.99(4) 2_766 2_766 ?
N5 Fe1 N1 89.01(4) . 2_766 ?
N5 Fe1 N1 89.01(4) 2_766 . ?
N5 Fe1 N1 90.99(4) . . ?
N1 Fe1 N1 180.0 2_766 . ?
N5 Fe1 S1 90.29(3) 2_766 2_766 ?
N5 Fe1 S1 89.71(3) . 2_766 ?
N1 Fe1 S1 85.93(3) 2_766 2_766 ?
N1 Fe1 S1 94.06(3) . 2_766 ?
N5 Fe1 S1 89.71(3) 2_766 . ?
N5 Fe1 S1 90.29(3) . . ?
N1 Fe1 S1 94.07(3) 2_766 . ?
N1 Fe1 S1 85.93(3) . . ?
S1 Fe1 S1 180.0 2_766 . ?
C7 S1 Fe1 95.91(4) . . ?
C5 N1 C1 116.35(11) . . ?
C5 N1 Fe1 127.27(9) . . ?
C1 N1 Fe1 116.26(9) . . ?
N1 C1 C2 123.39(14) . . ?
N1 C1 H1 115.1(10) . . ?
C2 C1 H1 121.5(10) . . ?
N3 N2 C7 113.44(11) . . ?
N3 N2 C5 115.47(11) . . ?
C7 N2 C5 131.08(11) . . ?
C3 C2 C1 118.73(14) . . ?
C3 C2 H2 124.7(13) . . ?
C1 C2 H2 116.5(13) . . ?
N4 N3 N2 103.28(10) . . ?
C4 C3 C2 119.08(13) . . ?
C4 C3 H3 120.8(12) . . ?
C2 C3 H3 120.0(12) . . ?
C3 C4 C5 117.90(14) . . ?
C3 C4 H4 124.6(12) . . ?
C5 C4 H4 117.5(12) . . ?
N3 N4 C8 114.05(11) . . ?
N3 N4 C6 118.18(12) . . ?
C8 N4 C6 127.67(13) . . ?
N1 C5 C4 124.48(13) . . ?
N1 C5 N2 117.23(11) . . ?
C4 C5 N2 118.18(12) . . ?
C15 N5 Fe1 165.11(11) . . ?
N4 C6 H6A 109.5 . . ?
N4 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N4 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N4 C8 C7 105.91(12) . . ?
N4 C8 C9 122.84(12) . . ?
C7 C8 C9 131.18(12) . . ?
N2 C7 C8 103.29(11) . . ?
N2 C7 S1 126.53(10) . . ?
C8 C7 S1 130.18(10) . . ?
C10 C9 C14 119.86(14) . . ?
C10 C9 C8 120.89(13) . . ?
C14 C9 C8 119.20(13) . . ?
C11 C10 C9 119.78(16) . . ?
C11 C10 H10 121.5(12) . . ?
C9 C10 H10 118.7(12) . . ?
C12 C11 C10 120.23(17) . . ?
C12 C11 H11 119.0(13) . . ?
C10 C11 H11 120.8(13) . . ?
C13 C12 C11 120.18(16) . . ?
C13 C12 H12 118.9(14) . . ?
C11 C12 H12 120.9(14) . . ?
C12 C13 C14 120.37(17) . . ?
C12 C13 H13 122.9(15) . . ?
C14 C13 H13 116.8(15) . . ?
C13 C14 C9 119.58(16) . . ?
C13 C14 H14 120.9(11) . . ?
C9 C14 H14 119.5(11) . . ?
N5 C15 S2 179.15(13) . . ?
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 N5 2.1200(12) 2_766 ?
Fe1 N5 2.1201(12) . ?
Fe1 N1 2.2680(11) 2_766 ?
Fe1 N1 2.2680(11) . ?
Fe1 S1 2.4860(4) 2_766 ?
Fe1 S1 2.4860(4) . ?
S1 C7 1.7074(13) . ?
N1 C5 1.3311(17) . ?
N1 C1 1.3455(18) . ?
C1 C2 1.383(2) . ?
C1 H1 0.954(17) . ?
N2 N3 1.3429(15) . ?
N2 C7 1.3785(16) . ?
N2 C5 1.4283(17) . ?
S2 C15 1.6256(14) . ?
C2 C3 1.381(2) . ?
C2 H2 0.91(2) . ?
N3 N4 1.3096(17) . ?
C3 C4 1.377(2) . ?
C3 H3 0.957(19) . ?
C4 C5 1.3886(18) . ?
C4 H4 0.99(2) . ?
N4 C8 1.3555(17) . ?
N4 C6 1.4660(18) . ?
N5 C15 1.1577(18) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C8 C7 1.3909(18) . ?
C8 C9 1.4680(19) . ?
C9 C10 1.391(2) . ?
C9 C14 1.392(2) . ?
C10 C11 1.386(2) . ?
C10 H10 0.96(2) . ?
C11 C12 1.382(3) . ?
C11 H11 0.98(2) . ?
C12 C13 1.375(3) . ?
C12 H12 0.95(2) . ?
C13 C14 1.391(2) . ?
C13 H13 0.96(3) . ?
C14 H14 0.974(19) . ?
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
C5 N1 C1 C2 -1.1(2) . . . . ?
Fe1 N1 C1 C2 -177.40(11) . . . . ?
N1 C1 C2 C3 2.4(2) . . . . ?
C7 N2 N3 N4 -0.69(15) . . . . ?
C5 N2 N3 N4 179.81(11) . . . . ?
C1 C2 C3 C4 -1.2(2) . . . . ?
C2 C3 C4 C5 -1.1(2) . . . . ?
N2 N3 N4 C8 -0.23(15) . . . . ?
N2 N3 N4 C6 -176.86(14) . . . . ?
C1 N1 C5 C4 -1.4(2) . . . . ?
Fe1 N1 C5 C4 174.37(11) . . . . ?
C1 N1 C5 N2 174.67(12) . . . . ?
Fe1 N1 C5 N2 -9.51(16) . . . . ?
C3 C4 C5 N1 2.6(2) . . . . ?
C3 C4 C5 N2 -173.50(13) . . . . ?
N3 N2 C5 N1 -140.52(12) . . . . ?
C7 N2 C5 N1 40.09(19) . . . . ?
N3 N2 C5 C4 35.84(17) . . . . ?
C7 N2 C5 C4 -143.55(14) . . . . ?
N3 N4 C8 C7 1.01(16) . . . . ?
C6 N4 C8 C7 177.26(15) . . . . ?
N3 N4 C8 C9 -176.28(13) . . . . ?
C6 N4 C8 C9 0.0(2) . . . . ?
N3 N2 C7 C8 1.27(15) . . . . ?
C5 N2 C7 C8 -179.33(12) . . . . ?
N3 N2 C7 S1 -177.82(10) . . . . ?
C5 N2 C7 S1 1.6(2) . . . . ?
N4 C8 C7 N2 -1.29(14) . . . . ?
C9 C8 C7 N2 175.68(14) . . . . ?
N4 C8 C7 S1 177.75(10) . . . . ?
C9 C8 C7 S1 -5.3(2) . . . . ?
Fe1 S1 C7 N2 -50.75(11) . . . . ?
Fe1 S1 C7 C8 130.41(12) . . . . ?
N4 C8 C9 C10 -63.44(19) . . . . ?
C7 C8 C9 C10 120.03(17) . . . . ?
N4 C8 C9 C14 113.81(16) . . . . ?
C7 C8 C9 C14 -62.7(2) . . . . ?
C14 C9 C10 C11 0.1(2) . . . . ?
C8 C9 C10 C11 177.35(14) . . . . ?
C9 C10 C11 C12 -0.6(2) . . . . ?
C10 C11 C12 C13 0.5(3) . . . . ?
C11 C12 C13 C14 0.1(3) . . . . ?
C12 C13 C14 C9 -0.6(3) . . . . ?
C10 C9 C14 C13 0.5(2) . . . . ?
C8 C9 C14 C13 -176.78(15) . . . . ?
