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_7720206
_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 H25 B2 Fe N7 S, 2.5(C2 H3 N)'
_chemical_formula_sum            'C28 H32.5 B2 Fe N9.5 S'
_chemical_formula_weight         611.66
_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
_atom_sites_solution_primary     dual
_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                 107.101(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   31.237(2)
_cell_length_b                   12.1599(6)
_cell_length_c                   17.6916(12)
_cell_measurement_reflns_used    29849
_cell_measurement_temperature    230
_cell_measurement_theta_max      32.35
_cell_measurement_theta_min      2.06
_cell_volume                     6422.9(7)
_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      230.00
_diffrn_detector_area_resol_mean 13.33
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.862
_diffrn_measurement_details
;
 1783 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  0.0445
_diffrn_reflns_av_unetI/netI     0.0253
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.862
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            40853
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.862
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.742
_diffrn_reflns_theta_min         2.059
_exptl_absorpt_coefficient_mu    0.568
_exptl_absorpt_correction_T_max  0.9797
_exptl_absorpt_correction_T_min  0.7011
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.265
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2552
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.387
_exptl_crystal_size_min          0.11
_exptl_crystal_size_rad          0.190
_refine_diff_density_max         1.330
_refine_diff_density_min         -0.660
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         10231
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0616
_refine_ls_R_factor_gt           0.0558
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0943P)^2^+6.4783P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1610
_refine_ls_wR_factor_ref         0.1675
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8904
_reflns_number_total             10231
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02912k2.cif
_cod_data_source_block           jgb-rf-150-02_3d
_cod_original_formula_sum        'C28 H32.50 B2 Fe N9.50 S'
_cod_database_code               7720206
_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 B(H,H,H) groups, All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C29) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(N10) \\sim Ueq, Uanis(C28A)
\\sim Ueq, Uanis(N10A) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(N9) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C27) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: N10(0.5) N10A(0.5) C26(0.5) C27(0.5) H27A(0.5) H27B(0.5) H27C(0.5)
 C28(0.5) C28A(0.5) H29A(0.5) H29B(0.5) H29C(0.5) H29D(0.5) H29E(0.5) H29F(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B), C16(H16A,H16B)
4.b 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)
4.c Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C29(H29D,H29E,
 H29F), B1(H1A,H1B,H1C), B2(H2A,H2B,H2C)
;
_shelx_res_checksum              39985
_olex2_submission_special_instructions 'No special instructions were received'