Modulation of Fe-Fe distance and spin in diiron complexes using tetradentate ligands with different flanking donors.
Spielvogel, Kyle D.; Campbell, Emily J.; Chowdhury, Sabyasachi Roy; Benner, Florian; Demir, Selvan; Hatzis, Gillian P.; Petras, Hayley R.; Sembukuttiarachchige, Dunya; Shepherd, James J.; Thomas, Christine M.; Vlaisavljevich, Bess; Daly, Scott R.; Chemical communications (Cambridge, England) 60 (2024) 8399–8402; doi:10.1039/d4cc02522a

data_7133367
_publ_section_title
;
 Modulation of Fe-Fe distance and spin in diiron complexes using
 tetradentate ligands with different flanking donors.
;
_journal_issue                   64
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              8399
_journal_page_last               8402
_journal_paper_doi               10.1039/d4cc02522a
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C40 H36 Fe2 N4 S4, 2(C6 H6)'
_chemical_formula_sum            'C52 H48 Fe2 N4 S4'
_chemical_formula_weight         968.88
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2024-04-30
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-05-22 deposited with the CCDC.	2024-07-11 downloaded from the CCDC.
;
_cell_angle_alpha                72.756(5)
_cell_angle_beta                 80.477(5)
_cell_angle_gamma                67.034(5)
_cell_formula_units_Z            2
_cell_length_a                   11.2216(11)
_cell_length_b                   12.4643(12)
_cell_length_c                   19.1311(19)
_cell_measurement_reflns_used    8412
_cell_measurement_temperature    150.15
_cell_measurement_theta_max      26.39
_cell_measurement_theta_min      2.232
_cell_volume                     2349.2(4)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/4 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker Nonius Kappa Apex II'
_diffrn_measurement_method       'Phi and Omega Scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_av_unetI/netI     0.0437
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            28048
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.487
_diffrn_reflns_theta_min         2.502
_exptl_absorpt_coefficient_mu    0.836
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.7040
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0454 before and 0.0403 after correction.
The Ratio of minimum to maximum transmission is 0.9445.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.370
_exptl_crystal_description       prism
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.977
_refine_diff_density_min         -0.526
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     541
_refine_ls_number_reflns         9528
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0607
_refine_ls_R_factor_gt           0.0425
_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^)+(0.0447P)^2^+2.6941P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0982
_refine_ls_wR_factor_ref         0.1075
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7525
_reflns_number_total             9528
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc02522a2.cif
_cod_data_source_block           dal1876
_cod_depositor_comments
'Adding full bibliography for 7133367--7133370.cif.'
_cod_database_code               7133367
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_max   0.914
_shelx_estimated_absorpt_t_min   0.906
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C51-C52 = C52-C53 = C53-C54 = C54-C55 = C55-C56
 1.39 with sigma of 0.005
 C61-C62 = C62-C63 = C63-C64 = C64-C65 = C65-C66
 1.39 with sigma of 0.005
3.a :
 C61(C62,C63,C64,C65,C66), C51(C52,C53,C54,C55,C56)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C11(H11), C14(H14),
 C15(H15), C16(H16), C17(H17), C22(H22), C23(H23), C24(H24), C25(H25), C28(H28),
  C29(H29), C30(H30), C31(H31), C34(H34), C35(H35), C36(H36), C37(H37),
 C61(H61), C62(H62), C63(H63), C64(H64), C65(H65), C66(H66), C51(H51), C52(H52),
  C53(H53), C54(H54), C55(H55), C56(H56)
3.c Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C39(H39A,H39B,H39C), C40(H40A,H40B,
 H40C)
;
_shelx_res_checksum              91899
_shelx_hkl_checksum              20491
_olex2_submission_special_instructions 'No special instructions were received'