Spin-Crossover Semiconductors Based on Homoleptic Tris-Diimine Fe(II) Complexes with Fractionally Charged TCNQ•δ- Anions
Amanyazova, Botagoz; Shatruk, Michael; Yergeshbayeva, Sandugash; Choi, Eun Sang; Erkasov, Rakhmetulla; Dalton Transactions  (2025) –; doi:10.1039/D5DT02365C

data_7719811
_publ_section_title
;
 Spin-Crossover Semiconductors Based on Homoleptic Tris-Diimine Fe(II)
 Complexes with Fractionally Charged TCNQ&#x2022;\d- Anions
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D5DT02365C
_journal_year                    2025
_chemical_formula_moiety         'C18 H12 Fe N6 S6, 3(C12 H4 N4)'
_chemical_formula_sum            'C54 H24 Fe N18 S6'
_chemical_formula_weight         1173.12
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2025-01-13
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-03-25 deposited with the CCDC.	2025-11-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.523(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   33.0830(6)
_cell_length_b                   9.7943(2)
_cell_length_c                   15.7944(3)
_cell_measurement_reflns_used    21261
_cell_measurement_temperature    100.0(3)
_cell_measurement_theta_max      33.7460
_cell_measurement_theta_min      3.4700
_cell_volume                     5047.25(17)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.0(3)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0559
_diffrn_reflns_av_unetI/netI     0.0297
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            49904
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_min         3.319
_exptl_absorpt_coefficient_mu    0.608
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.794
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.137a (Rigaku Oxford Diffraction, 2024)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_description       plate
_exptl_crystal_F_000             2384
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.612
_refine_diff_density_min         -0.530
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     490
_refine_ls_number_reflns         7690
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0434
_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/[\s^2^(Fo^2^)+(0.0533P)^2^+7.6302P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1079
_refine_ls_wR_factor_ref         0.1144
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6466
_reflns_number_total             7690
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02365c2.cif
_cod_data_source_block           structure2_100K
_cod_database_code               7719811
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.936
_shelx_estimated_absorpt_t_min   0.843
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(S1A) = Uanis(S1B)
Uanis(N4B) = Uanis(N4)
Uanis(S2B) = Uanis(S2A)
Uanis(C10B) = Uanis(C10A)
Uanis(C11B) = Uanis(C11A)
Uanis(S3A) = Uanis(S3B)
Uanis(C12B) = Uanis(C12A)
Uanis(N5B) = Uanis(N5)
Uanis(C13B) = Uanis(C13A)
Uanis(C14B) = Uanis(C14A)
Uanis(C15B) = Uanis(C15A)
Uanis(C16B) = Uanis(C16A)
Uanis(C17B) = Uanis(C17A)
Uanis(C18B) = Uanis(C18A)
Uanis(C19B) = Uanis(C19A)
Uanis(C20B) = Uanis(C20A)
Uanis(N6B) = Uanis(N6)
Uanis(C21B) = Uanis(C21A)
Uanis(N7B) = Uanis(N7)
3. Others
 Sof(S1B)=1-FVAR(1)
 Sof(S1A)=FVAR(1)
 Sof(S2B)=1-FVAR(2)
 Sof(S2A)=FVAR(2)
 Sof(S3B)=1-FVAR(3)
 Sof(S3A)=FVAR(3)
 Sof(C18B)=Sof(H18B)=Sof(N7B)=Sof(C17B)=Sof(H17B)=Sof(C11B)=Sof(C12B)=
 Sof(C21B)=Sof(N5B)=Sof(C19B)=Sof(C15B)=Sof(H15B)=Sof(C10B)=Sof(C13B)=Sof(C16B)=
 Sof(N6B)=Sof(N4B)=Sof(C14B)=Sof(H14B)=Sof(C20B)=1-FVAR(4)
 Sof(N4)=Sof(N7)=Sof(N6)=Sof(C14A)=Sof(H14A)=Sof(C15A)=Sof(H15A)=Sof(C16A)=
 Sof(C19A)=Sof(C10A)=Sof(C11A)=Sof(C13A)=Sof(C20A)=Sof(C18A)=Sof(H18A)=
 Sof(C21A)=Sof(N5)=Sof(C17A)=Sof(H17A)=Sof(C12A)=FVAR(4)
 Fixed Sof: C23(0.5) C25(0.5) C30(0.5) H30(0.5) C26(0.5) H26(0.5) C24(0.5)
 N9(0.5) C27(0.5) H27(0.5) C29(0.5) H29(0.5) C28(0.5) C31(0.5) C32(0.5)
 N10(0.5) N11(0.5) C33(0.5) N8(0.5) C22(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C14A(H14A), C15A(H15A), C8(H8), C9(H9), C1(H1), C5(H5), C18A(H18A),
 C2(H2), C17A(H17A), C18B(H18B), C17B(H17B), C15B(H15B), C14B(H14B), C30(H30),
 C26(H26), C27(H27), C29(H29)
;
_shelx_res_checksum              26819
_olex2_submission_special_instructions 'No special instructions were received'