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_7720209
_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         'C23 H19 Fe N7 S Se2, 2(C2 H3 N), 0.5[C2H3N]'
_chemical_formula_sum            'C28 H26.5 Fe N9.5 S Se2'
_chemical_formula_weight         741.92
_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   mixed
_audit_creation_date             2024-01-23
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2025-08-13 deposited with the CCDC.	2026-01-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.895(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   31.3953(13)
_cell_length_b                   11.8669(5)
_cell_length_c                   17.4680(6)
_cell_measurement_reflns_used    21822
_cell_measurement_temperature    120
_cell_measurement_theta_max      30.39
_cell_measurement_theta_min      2.10
_cell_volume                     6193.1(4)
_computing_cell_refinement
;
X-Area Recipe 1.37.0.0 (STOE, 2021)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.186.0 (STOE, 2022)
;
_computing_data_reduction
;
X-Area Integrate 2.5.3.0 (STOE, 2021)
X-Area LANA 2.7.5.0 (STOE, 2022)
;
_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 0.860
_diffrn_measurement_details
;
 1784 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  0.0275
_diffrn_reflns_av_unetI/netI     0.0277
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.860
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            41065
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.860
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.761
_diffrn_reflns_theta_min         2.097
_exptl_absorpt_coefficient_mu    2.941
_exptl_absorpt_correction_T_max  0.3515
_exptl_absorpt_correction_T_min  0.2933
_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.
Afterwards a spherical absorption correction was performed within STOE LANA.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.591
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2968
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.187
_exptl_crystal_size_min          0.14
_exptl_crystal_size_rad          0.110
_refine_diff_density_max         1.899
_refine_diff_density_min         -0.917
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     417
_refine_ls_number_reflns         9842
_refine_ls_number_restraints     73
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0829
_refine_ls_R_factor_gt           0.0620
_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^)+(0.0663P)^2^+36.1423P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1552
_refine_ls_wR_factor_ref         0.1678
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7415
_reflns_number_total             9842
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02912k2.cif
_cod_data_source_block           jgb-rf-102-03_3d
_cod_original_formula_sum        'C28 H26.50 Fe N9.50 S Se2'
_cod_database_code               7720209
_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, All C(H,H,H,H,H,H) groups
2. Restrained distances
 Se2-C23 \\sim Se2A-C23A
 with sigma of 0.02
 C23-N7 \\sim C23-N7A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
N7A \\sim N7 \\sim C23A \\sim C23 \\sim Se2A \\sim Se2: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08 within 1.7A
Uanis(Fe1A) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(Se2A) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(Se2A) \\sim Ueq, Uanis(C23A) \\sim Ueq, Uanis(N7A) \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.002
4. Others
 Sof(Se2A)=Sof(Fe1A)=Sof(N7A)=Sof(C23A)=1-FVAR(1)
 Sof(Se2)=Sof(Fe1)=Sof(N7)=Sof(C23)=FVAR(1)
 Fixed Sof: N9(0.5) C26(0.5) N9A(0.5) C26A(0.5) H27D(0.5) H27E(0.5) H27F(0.5)
 H27A(0.5) H27B(0.5) H27C(0.5)
5.a Riding coordinates:
 C27(H27D,H27E,H27F), C27(H27A,H27B,H27C)
5.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B), C16(H16A,H16B)
5.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C12(H12), C13(H13), C14(H14),
 C15(H15), C18(H18), C19(H19), C20(H20), C21(H21)
5.d Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              67717
_shelx_fab_checksum              74696
_olex2_submission_special_instructions 'No special instructions were received'