Sub lattice driven spin state ordering and coordination elasticity in Fe(II) 1,3,4-thiadiazole complexes.
Becker, Jens-Georg; Sundaresan, Sriram; Hochdörffer, Tim; Wolny, Juliusz A.; Carrella, Luca M.; Schünemann, Volker; Rentschler, Eva; Dalton transactions (Cambridge, England : 2003) 55 (2026) 2833–2844; doi:10.1039/d5dt02912k

data_7720205
_publ_section_title
;
 Sub lattice driven spin state ordering and coordination elasticity in
 Fe(II) 1,3,4-thiadiazole complexes.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2833
_journal_page_last               2844
_journal_paper_doi               10.1039/d5dt02912k
_journal_volume                  55
_journal_year                    2026
_chemical_formula_moiety         '2(C23 H19 Fe N7 S3), C2 H3 N'
_chemical_formula_sum            'C48 H41 Fe2 N15 S6'
_chemical_formula_weight         1132.02
_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   geom
_audit_creation_date             2025-01-08
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-08-13 deposited with the CCDC.	2026-01-27 downloaded from the CCDC.
;
_cell_angle_alpha                84.104(2)
_cell_angle_beta                 88.812(2)
_cell_angle_gamma                78.965(2)
_cell_formula_units_Z            2
_cell_length_a                   11.1571(2)
_cell_length_b                   13.8853(3)
_cell_length_c                   16.6309(3)
_cell_measurement_reflns_used    47943
_cell_measurement_temperature    120
_cell_measurement_theta_max      33.83
_cell_measurement_theta_min      2.16
_cell_volume                     2515.44(9)
_computing_cell_refinement
;
X-Area Recipe 2.0.2 (STOE, 2024)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.194.0 (STOE, 2023)
;
_computing_data_reduction
;
X-Area Integrate 2.5.18.0 (STOE, 2024)
X-Area LANA 2.8.4 (STOE, 2024)
;
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      120.00
_diffrn_detector_area_resol_mean 13.33
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.854
_diffrn_measurement_details
;
 2698 frames, detector distance = 60 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0154
_diffrn_reflns_av_unetI/netI     0.0184
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.854
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            57581
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.854
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.800
_diffrn_reflns_theta_min         2.157
_exptl_absorpt_coefficient_mu    0.878
_exptl_absorpt_correction_T_max  0.9017
_exptl_absorpt_correction_T_min  0.8539
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens in: F. R. Ahmed (Editor), "Crystallographic Computing", Munksgaard,
Copenhagen (1970), 255 - 270. Afterwards scaling of reflection intensities was
performed within STOE LANA. J. Koziskova, F. Hahn, J. Richter, J. Kozisek, Acta
Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Finally a spherical absorption correction was done within STOE LANA.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.495
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1164
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.123
_exptl_crystal_size_min          0.1
_exptl_crystal_size_rad          0.075
_refine_diff_density_max         0.686
_refine_diff_density_min         -0.529
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     787
_refine_ls_number_reflns         17266
_refine_ls_number_restraints     185
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0381
_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^)+(0.0414P)^2^+1.6759P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0917
_refine_ls_wR_factor_ref         0.0970
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14740
_reflns_number_total             17266
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02912k2.cif
_cod_data_source_block           jgb-435b_3d
_cod_database_code               7720205
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N3-C9 \\sim N3-C9A
 with sigma of 0.02
 C8-C9 \\sim C8A-C9A
 with sigma of 0.02
3. Rigid bond restraints
 N14, N14A, C46, C46A, S6, S6A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C9A \\sim C9: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 1.7A
N14 \\sim N14A \\sim C46 \\sim C46A \\sim S6 \\sim S6A: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08 within 1.7A
Uanis(S6A) \\sim Ueq, Uanis(S6) \\sim Ueq, Uanis(C46A) \\sim Ueq, Uanis(C46)
\\sim Ueq, Uanis(N14A) \\sim Ueq, Uanis(N14) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C8A) \\sim Ueq, Uanis(S1A) \\sim Ueq, Uanis(N2A) \\sim Ueq, Uanis(N1A)
\\sim Ueq, Uanis(C7A) \\sim Ueq, Uanis(C6A) \\sim Ueq, Uanis(C1A) \\sim Ueq,
Uanis(C2A) \\sim Ueq, Uanis(C3A) \\sim Ueq, Uanis(C4A) \\sim Ueq, Uanis(C5A)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C9A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Same fragment restrains
{S6, N14, C46} sigma for 1-2: 0.02, 1-3: 0.04
as in
{S6A, N14A, C46A}
6. Others
 Sof(Fe2A)=Sof(S6A)=Sof(N14A)=Sof(C46A)=1-FVAR(1)
 Sof(Fe2)=Sof(S6)=Sof(N14)=Sof(C46)=FVAR(1)
 Sof(S1A)=Sof(N1A)=Sof(N2A)=Sof(C1A)=Sof(H1A)=Sof(C2A)=Sof(H2A)=Sof(C3A)=
 Sof(H3A)=Sof(C4A)=Sof(H4A)=Sof(C5A)=Sof(H5A)=Sof(C6A)=Sof(C7A)=Sof(C8A)=
 Sof(C9A)=Sof(H9AA)=Sof(H9AB)=1-FVAR(2)
 Sof(S1)=Sof(N1)=Sof(N2)=Sof(C1)=Sof(H1)=Sof(C2)=Sof(H2)=Sof(C3)=Sof(H3)=
 Sof(C4)=Sof(H4)=Sof(C5)=Sof(H5)=Sof(C6)=Sof(C7)=Sof(C8)=Sof(C9)=Sof(H9A)=
 Sof(H9B)=FVAR(2)
7.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C9A(H9AA,H9AB), C10(H10A,H10B), C16(H16A,H16B), C32(H32A,H32B),
 C33(H33A,H33B), C39(H39A,H39B)
7.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C1A(H1A), C2A(H2A), C3A(H3A),
 C4A(H4A), C5A(H5A), C12(H12), C13(H13), C14(H14), C15(H15), C18(H18), C19(H19),
  C20(H20), C21(H21), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28),
 C35(H35), C36(H36), C37(H37), C38(H38), C41(H41), C42(H42), C43(H43), C44(H44)
7.c Idealised Me refined as rotating group:
 C48(H48A,H48B,H48C)
;
_shelx_res_checksum              81918
_olex2_submission_special_instructions 'No special instructions were received'