Investigation for Unique Magnetic Behaviours of Isomers in 1,2-Dithiooxalato-Bridged Diiron(II) Complex
KANETOMO, Takuya; Yokoyama, Koki; Suzuki, Yudai; Ida, Hiromichi; Okazawa, Atsushi; Enomoto, Masaya; Dalton Transactions  (2023) –; doi:10.1039/D3DT01992F

data_7713731
_publ_section_title
;
 Investigation for Unique Magnetic Behaviours of Isomers in
 1,2-Dithiooxalato-Bridged Diiron(II) Complex
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT01992F
_journal_year                    2023
_chemical_formula_moiety         'C38 H36 Fe2 N8 O2 S2, 2(Cl O4)'
_chemical_formula_sum            'C38 H36 Cl2 Fe2 N8 O10 S2'
_chemical_formula_weight         1011.47
_chemical_melting_point          458
_chemical_name_systematic
'[\m-ethanebis(thioic S-acid)ato]-bis{1-(pyridin-2-yl)-N,N-bis[(pyridin-2-yl)methyl]methanamine}-di-iron diperchlorate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-04-12
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2023-06-26 deposited with the CCDC.	2023-08-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.095(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.4258(9)
_cell_length_b                   13.8090(15)
_cell_length_c                   16.7478(16)
_cell_measurement_reflns_used    4640
_cell_measurement_temperature    223
_cell_measurement_theta_max      26.36
_cell_measurement_theta_min      2.67
_cell_volume                     2114.3(4)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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      223
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0535
_diffrn_reflns_av_unetI/netI     0.0547
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            21292
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         1.936
_exptl_absorpt_coefficient_mu    0.978
_exptl_absorpt_correction_T_max  0.9482
_exptl_absorpt_correction_T_min  0.8544
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0779 before and 0.0499 after correction.
The Ratio of minimum to maximum transmission is 0.9011.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_description       block
_exptl_crystal_F_000             1036
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.212
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.153
_refine_diff_density_max         1.235
_refine_diff_density_min         -0.960
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         4706
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0804
_refine_ls_R_factor_gt           0.0523
_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^)+(0.0538P)^2^+2.3012P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1287
_refine_ls_wR_factor_ref         0.1400
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3374
_reflns_number_total             4706
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01992f1.cif
_cod_data_source_block           fetpadto_223k_1stcool_0m
_cod_database_code               7713731
_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
2. Shared sites
{O1B, S1A}
{S1B, O1A}
3. Uiso/Uaniso restraints and constraints
Uanis(O1B) = Uanis(S1A)
Uanis(S1B) = Uanis(O1A)
4. Others
 Sof(O1B)=Sof(S1B)=1-FVAR(1)
 Sof(S1A)=Sof(O1A)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C19(H19A,H19B), C7(H7A,H7B)
5.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C14(H14), C17(H17), C15(H15), C5(H5), C2(H2), C11(H11),
 C10(H10), C16(H16), C3(H3), C4(H4)
;
_shelx_res_checksum              59179
_olex2_submission_special_instructions 'No special instructions were received'