#------------------------------------------------------------------------------
#$Date: 2022-09-06 13:13:25 +0300 (Tue, 06 Sep 2022) $
#$Revision: 277675 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/06/16/7061645.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_7061645
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 H30 B2 Fe N10 S2'
_chemical_formula_sum            'C30 H30 B2 Fe N10 S2'
_chemical_formula_weight         672.23
_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-2014/7
_audit_update_record
;
2020-05-23 deposited with the CCDC.	2022-07-07 downloaded from the CCDC.
;
_cell_angle_alpha                104.846(2)
_cell_angle_beta                 103.820(2)
_cell_angle_gamma                99.454(2)
_cell_formula_units_Z            1
_cell_length_a                   8.2630(4)
_cell_length_b                   8.4919(4)
_cell_length_c                   13.1039(7)
_cell_measurement_reflns_used    9988
_cell_measurement_temperature    302(2)
_cell_measurement_theta_max      27.29
_cell_measurement_theta_min      2.56
_cell_volume                     837.79(7)
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_data_collection       'Bruker Instrument Service vV6.2.6'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_molecular_graphics    'XP V 5.1 (Bruker, 1998)'
_computing_publication_material  'CIFTAB V 2013/2 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      302(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.1880
_diffrn_reflns_av_unetI/netI     0.0417
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_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            87200
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.732
_diffrn_reflns_theta_min         2.556
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_type              'Incoatec I\mS HB'
_exptl_absorpt_coefficient_mu    0.612
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.7265
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       square
_exptl_crystal_F_000             348
_exptl_crystal_size_max          0.088
_exptl_crystal_size_mid          0.058
_exptl_crystal_size_min          0.022
_exptl_transmission_factor_max   0.7457
_exptl_transmission_factor_min   0.7265
_refine_diff_density_max         0.381
_refine_diff_density_min         -0.502
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     246
_refine_ls_number_reflns         3569
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0445
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0451P)²+0.5042P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1053
_refine_ls_wR_factor_ref         0.1096
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3113
_reflns_number_total             3569
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2nj01989b2.cif
_cod_data_source_block           DPL277
_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_database_code               7061645
_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   0.948
_shelx_estimated_absorpt_t_max   0.987
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 1.0000 0.5000 0.5000 0.02593(13) Uani 1 2 d S . P . .
N1 N 0.9242(2) 0.7480(2) 0.54268(15) 0.0307(4) Uani 1 1 d . . . . .
C1 C 1.0437(3) 0.8786(3) 0.6208(2) 0.0397(5) Uani 1 1 d . . . . .
S1 S 0.69780(7) 0.37039(7) 0.48045(5) 0.03248(15) Uani 1 1 d . . . . .
B1 B 0.8067(6) 0.5197(5) 0.1259(3) 0.0621(10) Uani 1 1 d . . . . .
H1C H 0.708(6) 0.413(6) 0.077(4) 0.126(17) Uiso 1 1 d . . . . .
H1B H 0.749(7) 0.622(7) 0.137(4) 0.16(2) Uiso 1 1 d . . . . .
H1A H 0.900(7) 0.499(7) 0.083(4) 0.144(19) Uiso 1 1 d . . . . .
N2 N 0.6484(2) 0.6465(2) 0.41507(15) 0.0311(4) Uani 1 1 d . . . . .
C2 C 1.0152(4) 1.0344(3) 0.6582(2) 0.0466(6) Uani 1 1 d . . . . .
N3 N 0.5537(3) 0.6955(3) 0.33586(17) 0.0401(5) Uani 1 1 d . . . . .
C3 C 0.8565(4) 1.0602(3) 0.6170(3) 0.0506(7) Uani 1 1 d . . . . .
N5 N 0.9334(2) 0.4883(3) 0.32919(16) 0.0363(4) Uani 1 1 d . . . . .
C5 C 0.7726(3) 0.7785(3) 0.50417(18) 0.0317(5) Uani 1 1 d . . . . .
C4 C 0.7312(4) 0.9287(3) 0.5389(2) 0.0460(6) Uani 1 1 d . . . . .
N4 N 0.4535(3) 0.5539(3) 0.26582(17) 0.0397(5) Uani 1 1 d . . . . .
H3 H 0.830(4) 1.156(4) 0.638(3) 0.067(10) Uiso 1 1 d . . . . .
C9 C 0.3866(3) 0.2455(3) 0.22662(19) 0.0376(5) Uani 1 1 d . . . . .
H2 H 1.100(4) 1.119(4) 0.715(3) 0.061(9) Uiso 1 1 d . . . . .
C8 C 0.4782(3) 0.4166(3) 0.29591(19) 0.0332(5) Uani 1 1 d . . . . .
H1 H 1.153(4) 0.855(4) 0.647(2) 0.051(8) Uiso 1 1 d . . . . .
C7 C 0.6070(3) 0.4756(3) 0.39582(18) 0.0289(4) Uani 1 1 d . . . . .
C6 C 0.3365(4) 0.5597(4) 0.1637(3) 0.0636(9) Uani 1 1 d . . . . .
H6A H 0.3544 0.4846 0.1011 0.095 Uiso 1 1 calc R U . . .
H6B H 0.3589 0.6719 0.1592 0.095 Uiso 1 1 calc R U . . .
H6C H 0.2199 0.5264 0.1640 0.095 Uiso 1 1 calc R U . . .
H4 H 0.625(4) 0.938(4) 0.509(2) 0.053(8) Uiso 1 1 d . . . . .
C10 C 0.2091(3) 0.1937(4) 0.2027(2) 0.0514(7) Uani 1 1 d . . . . .
H10 H 0.1477 0.2660 0.2329 0.062 Uiso 1 1 calc R U . . .
C14 C 0.4757(4) 0.1367(4) 0.1827(3) 0.0568(7) Uani 1 1 d . . . . .
C12 C 0.2144(5) -0.0728(4) 0.0890(3) 0.0730(11) Uani 1 1 d . . . . .
H12 H 0.1565 -0.1801 0.0423 0.088 Uiso 1 1 calc R U . . .
C11 C 0.1250(5) 0.0333(5) 0.1333(3) 0.0667(10) Uani 1 1 d . . . . .
H14 H 0.591(4) 0.165(4) 0.194(3) 0.060(9) Uiso 1 1 d . . . . .
C13 C 0.3888(6) -0.0230(4) 0.1124(3) 0.0753(10) Uani 1 1 d . . . . .
H13 H 0.454(5) -0.096(6) 0.080(4) 0.101(14) Uiso 1 1 d . . . . .
H11 H 0.010(5) 0.002(5) 0.120(3) 0.082(12) Uiso 1 1 d . . . . .
C15 C 0.8820(3) 0.5012(3) 0.24405(19) 0.0356(5) 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'
B B 0.0013 0.0007 '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 89.71(7) 2_766 2_766 ?
N5 Fe1 N1 90.29(7) . 2_766 ?
N5 Fe1 N1 90.29(7) 2_766 . ?
N5 Fe1 N1 89.71(7) . . ?
N1 Fe1 N1 180.0 2_766 . ?
N5 Fe1 S1 90.96(5) 2_766 2_766 ?
N5 Fe1 S1 89.04(5) . 2_766 ?
N1 Fe1 S1 85.47(5) 2_766 2_766 ?
N1 Fe1 S1 94.53(5) . 2_766 ?
N5 Fe1 S1 89.04(5) 2_766 . ?
N5 Fe1 S1 90.96(5) . . ?
N1 Fe1 S1 94.54(5) 2_766 . ?
N1 Fe1 S1 85.47(5) . . ?
S1 Fe1 S1 180.0 2_766 . ?
C5 N1 C1 115.7(2) . . ?
C5 N1 Fe1 127.59(15) . . ?
C1 N1 Fe1 116.60(15) . . ?
N1 C1 C2 123.5(2) . . ?
C7 S1 Fe1 96.00(7) . . ?
N3 N2 C7 113.22(18) . . ?
N3 N2 C5 115.50(18) . . ?
C7 N2 C5 131.28(18) . . ?
C1 C2 C3 118.9(3) . . ?
N4 N3 N2 103.25(17) . . ?
C2 C3 C4 118.9(2) . . ?
C15 N5 Fe1 168.2(2) . . ?
N1 C5 C4 124.8(2) . . ?
N1 C5 N2 116.76(19) . . ?
C4 C5 N2 118.3(2) . . ?
C5 C4 C3 118.1(2) . . ?
N3 N4 C8 114.04(18) . . ?
N3 N4 C6 118.1(2) . . ?
C8 N4 C6 127.8(2) . . ?
C14 C9 C10 119.7(3) . . ?
C14 C9 C8 119.7(2) . . ?
C10 C9 C8 120.5(2) . . ?
N4 C8 C7 105.9(2) . . ?
N4 C8 C9 122.9(2) . . ?
C7 C8 C9 131.1(2) . . ?
N2 C7 C8 103.59(18) . . ?
N2 C7 S1 125.89(16) . . ?
C8 C7 S1 130.52(17) . . ?
C11 C10 C9 119.2(3) . . ?
C9 C14 C13 120.1(3) . . ?
C11 C12 C13 120.6(3) . . ?
C12 C11 C10 120.5(3) . . ?
C12 C13 C14 119.8(4) . . ?
N5 C15 B1 178.8(3) . . ?
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 2.1453(19) 2_766 ?
Fe1 N5 2.1453(19) . ?
Fe1 N1 2.2663(18) 2_766 ?
Fe1 N1 2.2663(18) . ?
Fe1 S1 2.4818(5) 2_766 ?
Fe1 S1 2.4818(5) . ?
N1 C5 1.328(3) . ?
N1 C1 1.352(3) . ?
C1 C2 1.368(4) . ?
S1 C7 1.709(2) . ?
B1 C15 1.582(4) . ?
N2 N3 1.343(2) . ?
N2 C7 1.377(3) . ?
N2 C5 1.433(3) . ?
C2 C3 1.369(4) . ?
N3 N4 1.311(3) . ?
C3 C4 1.376(4) . ?
N5 C15 1.135(3) . ?
C5 C4 1.368(3) . ?
N4 C8 1.353(3) . ?
N4 C6 1.470(3) . ?
C9 C14 1.372(4) . ?
C9 C10 1.393(4) . ?
C9 C8 1.464(3) . ?
C8 C7 1.386(3) . ?
C10 C11 1.385(4) . ?
C14 C13 1.388(5) . ?
C12 C11 1.360(6) . ?
C12 C13 1.368(6) . ?
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(4) . . . . ?
Fe1 N1 C1 C2 -177.7(2) . . . . ?
N1 C1 C2 C3 1.7(4) . . . . ?
C7 N2 N3 N4 -0.7(3) . . . . ?
C5 N2 N3 N4 179.68(19) . . . . ?
C1 C2 C3 C4 -0.4(4) . . . . ?
C1 N1 C5 C4 -0.9(3) . . . . ?
Fe1 N1 C5 C4 175.27(19) . . . . ?
C1 N1 C5 N2 175.1(2) . . . . ?
Fe1 N1 C5 N2 -8.8(3) . . . . ?
N3 N2 C5 N1 -140.1(2) . . . . ?
C7 N2 C5 N1 40.3(3) . . . . ?
N3 N2 C5 C4 36.1(3) . . . . ?
C7 N2 C5 C4 -143.5(2) . . . . ?
N1 C5 C4 C3 2.1(4) . . . . ?
N2 C5 C4 C3 -173.8(2) . . . . ?
C2 C3 C4 C5 -1.4(4) . . . . ?
N2 N3 N4 C8 0.2(3) . . . . ?
N2 N3 N4 C6 -176.8(2) . . . . ?
N3 N4 C8 C7 0.3(3) . . . . ?
C6 N4 C8 C7 176.9(3) . . . . ?
N3 N4 C8 C9 -176.5(2) . . . . ?
C6 N4 C8 C9 0.1(4) . . . . ?
C14 C9 C8 N4 114.1(3) . . . . ?
C10 C9 C8 N4 -64.2(3) . . . . ?
C14 C9 C8 C7 -61.8(4) . . . . ?
C10 C9 C8 C7 119.9(3) . . . . ?
N3 N2 C7 C8 0.8(3) . . . . ?
C5 N2 C7 C8 -179.6(2) . . . . ?
N3 N2 C7 S1 -178.52(16) . . . . ?
C5 N2 C7 S1 1.1(3) . . . . ?
N4 C8 C7 N2 -0.6(2) . . . . ?
C9 C8 C7 N2 175.8(2) . . . . ?
N4 C8 C7 S1 178.67(18) . . . . ?
C9 C8 C7 S1 -4.9(4) . . . . ?
Fe1 S1 C7 N2 -51.05(19) . . . . ?
Fe1 S1 C7 C8 129.8(2) . . . . ?
C14 C9 C10 C11 -0.9(4) . . . . ?
C8 C9 C10 C11 177.4(2) . . . . ?
C10 C9 C14 C13 1.6(4) . . . . ?
C8 C9 C14 C13 -176.8(3) . . . . ?
C13 C12 C11 C10 0.2(5) . . . . ?
C9 C10 C11 C12 0.0(5) . . . . ?
C11 C12 C13 C14 0.5(6) . . . . ?
C9 C14 C13 C12 -1.3(5) . . . . ?
