#------------------------------------------------------------------------------
#$Date: 2022-09-06 13:13:25 +0300 (Tue, 06 Sep 2022) $
#$Revision: 277675 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/06/16/7061647.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_7061647
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   difmap
_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                104.946(4)
_cell_angle_beta                 103.136(3)
_cell_angle_gamma                99.831(3)
_cell_formula_units_Z            1
_cell_length_a                   8.2367(7)
_cell_length_b                   8.4429(9)
_cell_length_c                   12.9792(13)
_cell_measurement_reflns_used    9613
_cell_measurement_temperature    166(2)
_cell_measurement_theta_max      25.01
_cell_measurement_theta_min      2.57
_cell_volume                     823.62(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      166(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0804
_diffrn_reflns_av_unetI/netI     0.0227
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            64134
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.124
_diffrn_reflns_theta_max         25.124
_diffrn_reflns_theta_min         2.575
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_type              'Incoatec I\mS HB'
_exptl_absorpt_coefficient_mu    0.622
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6934
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Sheldrick, 2012)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.355
_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   0.7452
_exptl_transmission_factor_min   0.6934
_refine_diff_density_max         0.213
_refine_diff_density_min         -0.238
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         2923
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0281
_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)+(0.0215P)²+0.4975P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0606
_refine_ls_wR_factor_ref         0.0637
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2536
_reflns_number_total             2923
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2nj01989b2.cif
_cod_data_source_block           DPL277BT
_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               7061647
_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   0.947
_shelx_estimated_absorpt_t_max   0.986
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 0.01700(11) Uani 1 2 d S . P . .
C1 C 1.0449(2) 0.8803(2) 0.62126(16) 0.0254(4) Uani 1 1 d . . . . .
N1 N 0.92509(18) 0.74912(18) 0.54360(12) 0.0200(3) Uani 1 1 d . . . . .
S1 S 0.69743(5) 0.36804(6) 0.48079(4) 0.02101(12) Uani 1 1 d . . . . .
B1 B 1.2016(4) 0.4819(4) 0.8757(2) 0.0382(6) Uani 1 1 d . . . . .
H1A H 1.106(4) 0.475(4) 0.916(2) 0.086(10) Uiso 1 1 d . . . . .
H1B H 1.307(4) 0.586(4) 0.924(2) 0.080(9) Uiso 1 1 d . . . . .
H1C H 1.262(4) 0.373(4) 0.864(2) 0.081(9) Uiso 1 1 d . . . . .
N2 N 0.64827(18) 0.64647(18) 0.41607(12) 0.0200(3) Uani 1 1 d . . . . .
C2 C 1.0165(3) 1.0382(2) 0.65938(17) 0.0296(4) Uani 1 1 d . . . . .
C4 C 0.7311(3) 0.9314(2) 0.54100(18) 0.0298(5) Uani 1 1 d . . . . .
N4 N 0.4524(2) 0.5531(2) 0.26653(13) 0.0255(4) Uani 1 1 d . . . . .
N3 N 0.55333(19) 0.6955(2) 0.33695(13) 0.0259(4) Uani 1 1 d . . . . .
C3 C 0.8569(3) 1.0634(3) 0.61897(18) 0.0328(5) Uani 1 1 d . . . . .
N5 N 1.06593(19) 0.51280(19) 0.67206(13) 0.0235(3) Uani 1 1 d . . . . .
C5 C 0.7726(2) 0.7785(2) 0.50505(15) 0.0205(4) Uani 1 1 d . . . . .
H4 H 0.623(3) 0.940(3) 0.5109(18) 0.042(6) Uiso 1 1 d . . . . .
C10 C 0.2071(3) 0.1897(3) 0.20131(17) 0.0324(5) Uani 1 1 d . . . . .
C12 C 0.2138(3) -0.0789(3) 0.0860(2) 0.0463(6) Uani 1 1 d . . . . .
C11 C 0.1225(3) 0.0283(3) 0.13124(18) 0.0416(6) Uani 1 1 d . . . . .
H14 H 0.600(3) 0.171(3) 0.1975(18) 0.041(6) Uiso 1 1 d . . . . .
C13 C 0.3900(3) -0.0279(3) 0.1104(2) 0.0458(6) Uani 1 1 d . . . . .
H13 H 0.455(4) -0.102(4) 0.077(2) 0.070(9) Uiso 1 1 d . . . . .
H12 H 0.157(3) -0.189(3) 0.039(2) 0.060(8) Uiso 1 1 d . . . . .
C14 C 0.4765(3) 0.1323(3) 0.18105(18) 0.0350(5) Uani 1 1 d . . . . .
H11 H 0.001(3) -0.002(3) 0.1148(19) 0.047(7) Uiso 1 1 d . . . . .
C15 C 1.1216(2) 0.5001(2) 0.75799(15) 0.0227(4) Uani 1 1 d . . . . .
H10 H 0.145(3) 0.264(3) 0.2291(18) 0.038(6) Uiso 1 1 d . . . . .
H6C H 0.347(4) 0.484(4) 0.105(3) 0.080(11) Uiso 1 1 d . . . . .
H6B H 0.218(4) 0.530(4) 0.169(3) 0.091(11) Uiso 1 1 d . . . . .
H6A H 0.361(4) 0.665(4) 0.163(2) 0.075(10) Uiso 1 1 d . . . . .
H3 H 0.835(3) 1.170(3) 0.6436(19) 0.044(6) Uiso 1 1 d . . . . .
C9 C 0.3851(2) 0.2423(2) 0.22619(15) 0.0243(4) Uani 1 1 d . . . . .
H2 H 1.105(3) 1.122(3) 0.7111(18) 0.037(6) Uiso 1 1 d . . . . .
C8 C 0.4777(2) 0.4147(2) 0.29644(15) 0.0219(4) Uani 1 1 d . . . . .
H1 H 1.156(3) 0.861(2) 0.6488(16) 0.028(5) Uiso 1 1 d . . . . .
C7 C 0.6065(2) 0.4740(2) 0.39640(14) 0.0189(4) Uani 1 1 d . . . . .
C6 C 0.3355(3) 0.5582(4) 0.1645(2) 0.0424(6) 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 89.86(5) . 2_766 ?
N5 Fe1 N1 90.14(5) 2_766 2_766 ?
N5 Fe1 N1 90.14(5) . . ?
N5 Fe1 N1 89.86(5) 2_766 . ?
N1 Fe1 N1 180.00(7) 2_766 . ?
N5 Fe1 S1 90.68(4) . 2_766 ?
N5 Fe1 S1 89.32(4) 2_766 2_766 ?
N1 Fe1 S1 85.76(4) 2_766 2_766 ?
N1 Fe1 S1 94.24(4) . 2_766 ?
N5 Fe1 S1 89.32(4) . . ?
N5 Fe1 S1 90.68(4) 2_766 . ?
N1 Fe1 S1 94.24(4) 2_766 . ?
N1 Fe1 S1 85.76(4) . . ?
S1 Fe1 S1 180.0 2_766 . ?
N1 C1 C2 123.33(18) . . ?
N1 C1 H1 117.1(12) . . ?
C2 C1 H1 119.5(12) . . ?
C5 N1 C1 116.30(15) . . ?
C5 N1 Fe1 127.11(12) . . ?
C1 N1 Fe1 116.50(12) . . ?
C7 S1 Fe1 96.26(6) . . ?
C15 B1 H1A 108.4(17) . . ?
C15 B1 H1B 110.8(16) . . ?
H1A B1 H1B 110(2) . . ?
C15 B1 H1C 108.7(15) . . ?
H1A B1 H1C 115(2) . . ?
H1B B1 H1C 103(2) . . ?
N3 N2 C7 113.10(14) . . ?
N3 N2 C5 115.78(14) . . ?
C7 N2 C5 131.12(14) . . ?
C3 C2 C1 118.83(19) . . ?
C3 C2 H2 122.5(14) . . ?
C1 C2 H2 118.6(14) . . ?
C3 C4 C5 117.97(19) . . ?
C3 C4 H4 123.6(14) . . ?
C5 C4 H4 118.5(15) . . ?
N3 N4 C8 113.74(15) . . ?
N3 N4 C6 118.49(17) . . ?
C8 N4 C6 127.67(18) . . ?
N4 N3 N2 103.50(14) . . ?
C4 C3 C2 119.23(19) . . ?
C4 C3 H3 120.6(14) . . ?
C2 C3 H3 120.2(14) . . ?
C15 N5 Fe1 166.69(15) . . ?
N1 C5 C4 124.30(17) . . ?
N1 C5 N2 117.47(15) . . ?
C4 C5 N2 118.11(16) . . ?
C11 C10 C9 119.6(2) . . ?
C11 C10 H10 120.2(14) . . ?
C9 C10 H10 120.1(14) . . ?
C11 C12 C13 120.6(2) . . ?
C11 C12 H12 120.2(16) . . ?
C13 C12 H12 119.2(16) . . ?
C12 C11 C10 120.1(2) . . ?
C12 C11 H11 122.5(14) . . ?
C10 C11 H11 117.4(14) . . ?
C12 C13 C14 120.0(2) . . ?
C12 C13 H13 121.1(17) . . ?
C14 C13 H13 118.9(17) . . ?
C13 C14 C9 119.8(2) . . ?
C13 C14 H14 121.0(13) . . ?
C9 C14 H14 119.1(13) . . ?
N5 C15 B1 178.9(2) . . ?
C14 C9 C10 119.81(19) . . ?
C14 C9 C8 119.19(17) . . ?
C10 C9 C8 120.97(18) . . ?
N4 C8 C7 106.06(16) . . ?
N4 C8 C9 122.50(16) . . ?
C7 C8 C9 131.36(16) . . ?
N2 C7 C8 103.59(15) . . ?
N2 C7 S1 125.85(13) . . ?
C8 C7 S1 130.56(14) . . ?
N4 C6 H6C 110(2) . . ?
N4 C6 H6B 108.3(19) . . ?
H6C C6 H6B 110(3) . . ?
N4 C6 H6A 106.7(19) . . ?
H6C C6 H6A 113(3) . . ?
H6B C6 H6A 109(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 2.1443(16) . ?
Fe1 N5 2.1443(16) 2_766 ?
Fe1 N1 2.2611(14) 2_766 ?
Fe1 N1 2.2611(14) . ?
Fe1 S1 2.4780(5) 2_766 ?
Fe1 S1 2.4780(5) . ?
C1 N1 1.347(2) . ?
C1 C2 1.376(3) . ?
C1 H1 0.96(2) . ?
N1 C5 1.332(2) . ?
S1 C7 1.7094(17) . ?
B1 C15 1.579(3) . ?
B1 H1A 1.04(3) . ?
B1 H1B 1.06(3) . ?
B1 H1C 1.11(3) . ?
N2 N3 1.343(2) . ?
N2 C7 1.379(2) . ?
N2 C5 1.426(2) . ?
C2 C3 1.374(3) . ?
C2 H2 0.92(2) . ?
C4 C3 1.374(3) . ?
C4 C5 1.384(3) . ?
C4 H4 0.91(2) . ?
N4 N3 1.311(2) . ?
N4 C8 1.356(2) . ?
N4 C6 1.466(3) . ?
C3 H3 0.94(2) . ?
N5 C15 1.145(2) . ?
C10 C11 1.385(3) . ?
C10 C9 1.393(3) . ?
C10 H10 0.93(2) . ?
C12 C11 1.374(4) . ?
C12 C13 1.378(4) . ?
C12 H12 0.94(3) . ?
C11 H11 0.95(2) . ?
C13 C14 1.382(3) . ?
C13 H13 0.97(3) . ?
C14 C9 1.390(3) . ?
C14 H14 0.97(2) . ?
C9 C8 1.467(3) . ?
C8 C7 1.385(2) . ?
C6 H6C 0.90(3) . ?
C6 H6B 0.97(3) . ?
C6 H6A 0.90(3) . ?
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 -0.9(3) . . . . ?
C2 C1 N1 Fe1 -177.66(15) . . . . ?
N1 C1 C2 C3 1.9(3) . . . . ?
C8 N4 N3 N2 0.0(2) . . . . ?
C6 N4 N3 N2 -176.64(19) . . . . ?
C7 N2 N3 N4 -0.62(19) . . . . ?
C5 N2 N3 N4 179.66(14) . . . . ?
C5 C4 C3 C2 -1.1(3) . . . . ?
C1 C2 C3 C4 -0.7(3) . . . . ?
C1 N1 C5 C4 -1.1(3) . . . . ?
Fe1 N1 C5 C4 175.19(14) . . . . ?
C1 N1 C5 N2 174.73(15) . . . . ?
Fe1 N1 C5 N2 -8.9(2) . . . . ?
C3 C4 C5 N1 2.2(3) . . . . ?
C3 C4 C5 N2 -173.66(17) . . . . ?
N3 N2 C5 N1 -140.27(16) . . . . ?
C7 N2 C5 N1 40.1(3) . . . . ?
N3 N2 C5 C4 35.9(2) . . . . ?
C7 N2 C5 C4 -143.79(19) . . . . ?
C13 C12 C11 C10 0.5(4) . . . . ?
C9 C10 C11 C12 -0.4(3) . . . . ?
C11 C12 C13 C14 0.1(4) . . . . ?
C12 C13 C14 C9 -0.8(3) . . . . ?
C13 C14 C9 C10 0.9(3) . . . . ?
C13 C14 C9 C8 -176.91(19) . . . . ?
C11 C10 C9 C14 -0.3(3) . . . . ?
C11 C10 C9 C8 177.48(18) . . . . ?
N3 N4 C8 C7 0.5(2) . . . . ?
C6 N4 C8 C7 176.8(2) . . . . ?
N3 N4 C8 C9 -176.47(16) . . . . ?
C6 N4 C8 C9 -0.2(3) . . . . ?
C14 C9 C8 N4 114.8(2) . . . . ?
C10 C9 C8 N4 -63.1(3) . . . . ?
C14 C9 C8 C7 -61.4(3) . . . . ?
C10 C9 C8 C7 120.7(2) . . . . ?
N3 N2 C7 C8 0.94(19) . . . . ?
C5 N2 C7 C8 -179.39(17) . . . . ?
N3 N2 C7 S1 -178.53(12) . . . . ?
C5 N2 C7 S1 1.1(3) . . . . ?
N4 C8 C7 N2 -0.85(19) . . . . ?
C9 C8 C7 N2 175.80(18) . . . . ?
N4 C8 C7 S1 178.58(14) . . . . ?
C9 C8 C7 S1 -4.8(3) . . . . ?
Fe1 S1 C7 N2 -50.65(15) . . . . ?
Fe1 S1 C7 C8 130.03(17) . . . . ?
