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_7720208
_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             2025-01-30
_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                84.30(6)
_cell_angle_beta                 89.04(6)
_cell_angle_gamma                79.39(6)
_cell_formula_units_Z            2
_cell_length_a                   11.203(7)
_cell_length_b                   14.143(11)
_cell_length_c                   16.910(13)
_cell_measurement_reflns_used    16108
_cell_measurement_temperature    240
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      2.12
_cell_volume                     2620(3)
_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      240.00
_diffrn_detector_area_resol_mean 13.33
_diffrn_measured_fraction_theta_full 0.754
_diffrn_measured_fraction_theta_max 0.510
_diffrn_measurement_details
;
 1456 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  0.0372
_diffrn_reflns_av_unetI/netI     0.1223
_diffrn_reflns_Laue_measured_fraction_full 0.754
_diffrn_reflns_Laue_measured_fraction_max 0.510
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            15053
_diffrn_reflns_point_group_measured_fraction_full 0.754
_diffrn_reflns_point_group_measured_fraction_max 0.510
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.950
_diffrn_reflns_theta_min         2.209
_exptl_absorpt_coefficient_mu    0.843
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  1.0000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1164
_refine_diff_density_max         0.608
_refine_diff_density_min         -0.572
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.871
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     750
_refine_ls_number_reflns         10872
_refine_ls_number_restraints     252
_refine_ls_restrained_S_all      0.862
_refine_ls_R_factor_all          0.1551
_refine_ls_R_factor_gt           0.0540
_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^)+(0.0782P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1225
_refine_ls_wR_factor_ref         0.1507
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4696
_reflns_number_total             10872
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02912k2.cif
_cod_data_source_block           jgb-jdg-26-240k
_cod_database_code               7720208
_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. Uiso/Uaniso restraints and constraints
C6 \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C7 \\sim S1 \\sim C8
\\sim C9 \\sim C9A \\sim C8A \\sim N2A \\sim N1 \\sim N2 \\sim N1A \\sim S1A
\\sim C7A \\sim C6A \\sim C5A \\sim C4A \\sim C3A \\sim C2A \\sim C1A: within
1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04 within 1.7A
Uanis(C8A) \\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
3. Same fragment restrains
{S1, N1, N2, C1, C2, C3, C4, C5, C6, C7, C8, C9} sigma for 1-2: 0.02, 1-3: 0.04
as in
{S1A, N1A, N2A, C1A, C2A, C3A, C4A, C5A, C6A, C7A, C8A, C9A}
4. Others
 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(1)
 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(1)
5.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)
5.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)
5.c Idealised Me refined as rotating group:
 C48(H48A,H48B,H48C)
;
_shelx_res_checksum              39822
_olex2_submission_special_instructions 'No special instructions were received'