#------------------------------------------------------------------------------
#$Date: 2025-07-06 19:42:22 +0300 (Sun, 06 Jul 2025) $
#$Revision: 300920 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/82/7718289.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_7718289
loop_
_publ_author_name
'Cuza, Emmelyne'
'Delsuc, Nicolas'
'Marrot, Jerôme'
'Shepard, William'
'Policar, Clotilde'
'Serre, Christian'
'Tissot, Antoine'
_publ_section_title
;
 Angle-dependent spin crossover properties in polymorphic iron(II)
 complexes based on pyridine-triazole derivatives.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6274
_journal_page_last               6280
_journal_paper_doi               10.1039/d4dt03376k
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C28 H30 Fe N12 O6 S2'
_chemical_formula_sum            'C28 H30 Fe N12 O6 S2'
_chemical_formula_weight         750.61
_chemical_name_systematic        ec103-b1-110k
_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
_audit_creation_date             20245-02-10
_audit_creation_method
;
Olex2 1.5
(compiled 2024.01.12 svn.r2f8d729c for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-02-10 deposited with the CCDC.	2025-03-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.635(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.4990(4)
_cell_length_b                   14.2794(6)
_cell_length_c                   9.1679(3)
_cell_measurement_reflns_used    3029
_cell_measurement_temperature    110
_cell_measurement_theta_max      46.23
_cell_measurement_theta_min      2.93
_cell_volume                     1717.38(11)
_computing_cell_refinement       'CrystFEL (White, 2018)'
_computing_data_collection       MXCuBE
_computing_data_reduction        'CrystFEL (White, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      110.00
_diffrn_detector_area_resol_mean 0.075
_diffrn_detector_type            'DECTRIS EIGER-9M'
_diffrn_measured_fraction_theta_full 0.927
_diffrn_measured_fraction_theta_max 0.801
_diffrn_measurement_device       'Kappa-geometry diffractometer'
_diffrn_measurement_device_type  Synchrotron
_diffrn_measurement_method       'omega rotation shutterless scans'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.72932
_diffrn_reflns_av_R_equivalents  0.0652
_diffrn_reflns_av_unetI/netI     0.0452
_diffrn_reflns_Laue_measured_fraction_full 0.927
_diffrn_reflns_Laue_measured_fraction_max 0.801
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            17135
_diffrn_reflns_point_group_measured_fraction_full 0.927
_diffrn_reflns_point_group_measured_fraction_max 0.801
_diffrn_reflns_theta_full        25.950
_diffrn_reflns_theta_max         27.766
_diffrn_reflns_theta_min         1.593
_diffrn_source                   'Synchrotron SOLEIL'
_diffrn_source_target            Mo
_diffrn_source_type              'U24 Undulator, PROXIMA-2 Beamline'
_exptl_absorpt_coefficient_mu    0.661
_exptl_absorpt_correction_T_max  0.983
_exptl_absorpt_correction_T_min  0.953
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.452
_exptl_crystal_description       needle
_exptl_crystal_F_000             776
_exptl_crystal_preparation       'In fine glass tube'
_exptl_crystal_recrystallization_method 'MeOH H2O'
_exptl_crystal_size_max          0.0728
_exptl_crystal_size_mid          0.055
_exptl_crystal_size_min          0.0256
_refine_diff_density_max         0.962
_refine_diff_density_min         -0.444
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     224
_refine_ls_number_reflns         3006
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0878
_refine_ls_R_factor_gt           0.0714
_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)+(0.1724P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2143
_refine_ls_wR_factor_ref         0.2356
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2065
_reflns_number_total             3006
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt03376k2.cif
_cod_data_source_block           ec103-b1-110k
_cod_depositor_comments
'Adding full bibliography for 7718287--7718289.cif.'
_cod_database_code               7718289
_shelx_shelxl_version_number     2018/3
_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_max   0.993
_shelx_estimated_absorpt_t_min   0.955
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C11(H11A,H11B), C12(H12A,H12B)
2.b Aromatic/amide H refined with riding coordinates:
 N6(H6), C5(H5), C3(H3), C4(H4), C8(H8), C2(H2)
2.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C)
;
_olex2_exptl_crystal_mounting_method loop
_olex2_submission_special_instructions 'No special instructions were received'
_olex2_submission_original_sample_id ec103-b1-110K
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 0.500000 0.500000 0.500000 0.0422(3) Uani 1 2 d S . P . .
S1 S 0.26941(12) 0.49191(9) 0.01730(16) 0.0702(5) Uani 1 1 d . . . . .
O1 O 0.1588(2) 0.2547(3) 0.4538(3) 0.0683(10) Uani 1 1 d . . . . .
N2 N 0.5715(2) 0.3931(2) 0.4148(3) 0.0433(8) Uani 1 1 d . . . . .
N1 N 0.3962(3) 0.5016(2) 0.3070(5) 0.0502(9) Uani 1 1 d . . . . .
N3 N 0.4313(2) 0.3877(3) 0.5651(4) 0.0474(8) Uani 1 1 d . . . . .
N5 N 0.3440(2) 0.2827(3) 0.6391(3) 0.0479(9) Uani 1 1 d . . . . .
N4 N 0.3582(3) 0.3742(3) 0.6347(4) 0.0510(9) Uani 1 1 d . . . . .
N6 N 0.0866(3) 0.2049(3) 0.6389(4) 0.0633(11) Uani 1 1 d . . . . .
H6 H 0.095724 0.200276 0.736925 0.076 Uiso 1 1 calc R U . . .
C6 C 0.5447(3) 0.3048(3) 0.4425(4) 0.0426(9) Uani 1 1 d . . . . .
C7 C 0.4629(3) 0.3032(3) 0.5234(4) 0.0430(9) Uani 1 1 d . . . . .
C5 C 0.5878(3) 0.2257(3) 0.3955(4) 0.0472(10) Uani 1 1 d . . . . .
H5 H 0.567964 0.164804 0.419304 0.057 Uiso 1 1 calc R U . . .
C3 C 0.6866(3) 0.3273(3) 0.2803(5) 0.0517(11) Uani 1 1 d . . . . .
H3 H 0.735450 0.336902 0.222273 0.062 Uiso 1 1 calc R U . . .
C4 C 0.6605(3) 0.2376(3) 0.3129(4) 0.0522(11) Uani 1 1 d . . . . .
H4 H 0.691981 0.184933 0.279229 0.063 Uiso 1 1 calc R U . . .
C8 C 0.4065(3) 0.2341(3) 0.5699(4) 0.0476(10) Uani 1 1 d . . . . .
H8 H 0.410322 0.168335 0.556899 0.057 Uiso 1 1 calc R U . . .
C2 C 0.6416(3) 0.4028(3) 0.3318(5) 0.0510(10) Uani 1 1 d . . . . .
H2 H 0.660481 0.464100 0.308346 0.061 Uiso 1 1 calc R U . . .
C9 C 0.2622(3) 0.2459(3) 0.7045(4) 0.0508(11) Uani 1 1 d . . . . .
H9A H 0.251824 0.288679 0.784570 0.061 Uiso 1 1 calc R U . . .
H9B H 0.282362 0.183926 0.750176 0.061 Uiso 1 1 calc R U . . .
C10 C 0.1632(3) 0.2366(3) 0.5850(5) 0.0544(11) Uani 1 1 d . . . . .
O3 O -0.1318(3) 0.3828(5) 0.6516(6) 0.1196(18) Uani 1 1 d . . . . .
C1 C 0.3436(4) 0.4980(3) 0.1861(6) 0.0517(11) Uani 1 1 d . . . . .
O2 O -0.0615(3) 0.3639(4) 0.4486(5) 0.1024(14) Uani 1 1 d . . . . .
C11 C -0.0118(3) 0.1774(5) 0.5449(6) 0.0750(16) Uani 1 1 d . . . . .
H11A H -0.022027 0.109364 0.555962 0.090 Uiso 1 1 calc R U . . .
H11B H -0.012901 0.190093 0.438387 0.090 Uiso 1 1 calc R U . . .
C12 C -0.0950(4) 0.2294(5) 0.5875(6) 0.0862(18) Uani 1 1 d . . . . .
H12A H -0.089579 0.221242 0.696374 0.103 Uiso 1 1 calc R U . . .
H12B H -0.161211 0.202891 0.533156 0.103 Uiso 1 1 calc R U . . .
C13 C -0.0930(4) 0.3325(6) 0.5529(6) 0.0898(19) Uani 1 1 d . . . . .
C14 C -0.1307(8) 0.4897(5) 0.6243(14) 0.134(4) Uani 1 1 d . . . . .
H14A H -0.099743 0.502471 0.539850 0.202 Uiso 1 1 calc R U . . .
H14B H -0.091033 0.520741 0.714645 0.202 Uiso 1 1 calc R U . . .
H14C H -0.200761 0.513600 0.601098 0.202 Uiso 1 1 calc R U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017 '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'
Fe Fe 0.3512 0.8903 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0065 0.0035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0115 0.0065 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1301 0.1311 '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
N2 Fe1 N2 180.0 3_666 . ?
N1 Fe1 N2 91.96(13) 3_666 . ?
N1 Fe1 N2 88.04(13) . . ?
N1 Fe1 N2 88.04(13) 3_666 3_666 ?
N1 Fe1 N2 91.96(13) . 3_666 ?
N1 Fe1 N1 180.0 3_666 . ?
N1 Fe1 N3 90.26(14) 3_666 . ?
N1 Fe1 N3 90.26(14) . 3_666 ?
N1 Fe1 N3 89.74(14) 3_666 3_666 ?
N1 Fe1 N3 89.74(14) . . ?
N3 Fe1 N2 79.15(14) . . ?
N3 Fe1 N2 100.85(14) . 3_666 ?
N3 Fe1 N2 79.15(14) 3_666 3_666 ?
N3 Fe1 N2 100.85(14) 3_666 . ?
N3 Fe1 N3 180.0 . 3_666 ?
C6 N2 Fe1 116.8(2) . . ?
C6 N2 C2 117.0(3) . . ?
C2 N2 Fe1 126.2(3) . . ?
C1 N1 Fe1 172.1(4) . . ?
N4 N3 Fe1 135.6(3) . . ?
N4 N3 C7 109.2(3) . . ?
C7 N3 Fe1 115.2(2) . . ?
N4 N5 C8 112.3(3) . . ?
N4 N5 C9 119.5(3) . . ?
C8 N5 C9 128.0(4) . . ?
N3 N4 N5 106.9(3) . . ?
C10 N6 H6 118.2 . . ?
C10 N6 C11 123.6(4) . . ?
C11 N6 H6 118.2 . . ?
N2 C6 C7 112.0(3) . . ?
N2 C6 C5 123.5(3) . . ?
C5 C6 C7 124.5(4) . . ?
N3 C7 C6 116.8(3) . . ?
N3 C7 C8 108.4(3) . . ?
C8 C7 C6 134.8(4) . . ?
C6 C5 H5 120.9 . . ?
C4 C5 C6 118.3(4) . . ?
C4 C5 H5 120.9 . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C2 C3 C4 119.9(4) . . ?
C5 C4 H4 120.6 . . ?
C3 C4 C5 118.8(4) . . ?
C3 C4 H4 120.6 . . ?
N5 C8 C7 103.2(4) . . ?
N5 C8 H8 128.4 . . ?
C7 C8 H8 128.4 . . ?
N2 C2 C3 122.5(4) . . ?
N2 C2 H2 118.8 . . ?
C3 C2 H2 118.8 . . ?
N5 C9 H9A 109.5 . . ?
N5 C9 H9B 109.5 . . ?
N5 C9 C10 110.8(3) . . ?
H9A C9 H9B 108.1 . . ?
C10 C9 H9A 109.5 . . ?
C10 C9 H9B 109.5 . . ?
O1 C10 N6 125.4(4) . . ?
O1 C10 C9 121.5(4) . . ?
N6 C10 C9 113.0(4) . . ?
C13 O3 C14 113.3(6) . . ?
N1 C1 S1 179.4(4) . . ?
N6 C11 H11A 109.5 . . ?
N6 C11 H11B 109.5 . . ?
N6 C11 C12 110.7(5) . . ?
H11A C11 H11B 108.1 . . ?
C12 C11 H11A 109.5 . . ?
C12 C11 H11B 109.5 . . ?
C11 C12 H12A 109.1 . . ?
C11 C12 H12B 109.1 . . ?
C11 C12 C13 112.5(5) . . ?
H12A C12 H12B 107.8 . . ?
C13 C12 H12A 109.1 . . ?
C13 C12 H12B 109.1 . . ?
O3 C13 C12 110.4(5) . . ?
O2 C13 O3 126.1(8) . . ?
O2 C13 C12 123.5(6) . . ?
O3 C14 H14A 109.5 . . ?
O3 C14 H14B 109.5 . . ?
O3 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
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 N2 2.055(3) 3_666 ?
Fe1 N2 2.056(3) . ?
Fe1 N1 1.981(5) 3_666 ?
Fe1 N1 1.981(5) . ?
Fe1 N3 2.012(3) . ?
Fe1 N3 2.013(3) 3_666 ?
S1 C1 1.636(6) . ?
O1 C10 1.218(5) . ?
N2 C6 1.353(5) . ?
N2 C2 1.354(5) . ?
N1 C1 1.168(7) . ?
N3 N4 1.310(4) . ?
N3 C7 1.364(5) . ?
N5 N4 1.323(5) . ?
N5 C8 1.359(5) . ?
N5 C9 1.471(5) . ?
N6 H6 0.8800 . ?
N6 C10 1.326(5) . ?
N6 C11 1.457(6) . ?
C6 C7 1.468(5) . ?
C6 C5 1.385(6) . ?
C7 C8 1.374(6) . ?
C5 H5 0.9500 . ?
C5 C4 1.385(6) . ?
C3 H3 0.9500 . ?
C3 C4 1.380(7) . ?
C3 C2 1.374(6) . ?
C4 H4 0.9500 . ?
C8 H8 0.9500 . ?
C2 H2 0.9500 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C9 C10 1.521(6) . ?
O3 C13 1.354(7) . ?
O3 C14 1.547(9) . ?
O2 C13 1.220(7) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.475(8) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 C13 1.507(10) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
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
Fe1 N2 C6 C7 3.3(4) . . . . ?
Fe1 N2 C6 C5 -178.5(3) . . . . ?
Fe1 N2 C2 C3 179.4(3) . . . . ?
Fe1 N3 N4 N5 177.3(3) . . . . ?
Fe1 N3 C7 C6 2.3(4) . . . . ?
Fe1 N3 C7 C8 -177.5(3) . . . . ?
N2 C6 C7 N3 -3.6(5) . . . . ?
N2 C6 C7 C8 176.0(4) . . . . ?
N2 C6 C5 C4 -1.6(6) . . . . ?
N3 C7 C8 N5 -0.5(4) . . . . ?
N5 C9 C10 O1 2.8(6) . . . . ?
N5 C9 C10 N6 -179.1(4) . . . . ?
N4 N3 C7 C6 179.6(3) . . . . ?
N4 N3 C7 C8 -0.2(4) . . . . ?
N4 N5 C8 C7 1.0(4) . . . . ?
N4 N5 C9 C10 89.9(5) . . . . ?
N6 C11 C12 C13 67.3(6) . . . . ?
C6 N2 C2 C3 -1.7(6) . . . . ?
C6 C7 C8 N5 179.8(4) . . . . ?
C6 C5 C4 C3 -0.3(6) . . . . ?
C7 N3 N4 N5 0.8(4) . . . . ?
C7 C6 C5 C4 176.5(4) . . . . ?
C5 C6 C7 N3 178.1(3) . . . . ?
C5 C6 C7 C8 -2.2(7) . . . . ?
C4 C3 C2 N2 0.0(7) . . . . ?
C8 N5 N4 N3 -1.1(4) . . . . ?
C8 N5 C9 C10 -85.2(5) . . . . ?
C2 N2 C6 C7 -175.7(3) . . . . ?
C2 N2 C6 C5 2.6(6) . . . . ?
C2 C3 C4 C5 1.1(6) . . . . ?
C9 N5 N4 N3 -176.9(3) . . . . ?
C9 N5 C8 C7 176.3(3) . . . . ?
C10 N6 C11 C12 -124.5(5) . . . . ?
C11 N6 C10 O1 6.9(8) . . . . ?
C11 N6 C10 C9 -171.0(5) . . . . ?
C11 C12 C13 O3 -150.0(5) . . . . ?
C11 C12 C13 O2 30.8(8) . . . . ?
C14 O3 C13 O2 -1.7(10) . . . . ?
C14 O3 C13 C12 179.2(6) . . . . ?
