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_7133369
_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         'C44 H48 Fe2 N8, 1.5(C6 H6)'
_chemical_formula_sum            'C53 H57 Fe2 N8'
_chemical_formula_weight         917.76
_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             2024-05-22
_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                90
_cell_angle_beta                 101.994(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.1280(14)
_cell_length_b                   17.7302(18)
_cell_length_c                   18.8223(18)
_cell_measurement_reflns_used    9903
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.35
_cell_measurement_theta_min      2.212
_cell_volume                     4611.9(8)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.0261
_diffrn_reflns_av_unetI/netI     0.0192
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            54010
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.353
_diffrn_reflns_theta_min         1.474
_exptl_absorpt_coefficient_mu    0.675
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.7132
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0390 before and 0.0372 after correction.
The Ratio of minimum to maximum transmission is 0.9568.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.322
_exptl_crystal_description       prism-like
_exptl_crystal_F_000             1932
_exptl_crystal_size_max          0.285
_exptl_crystal_size_mid          0.225
_exptl_crystal_size_min          0.215
_refine_diff_density_max         0.410
_refine_diff_density_min         -0.390
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     576
_refine_ls_number_reflns         9396
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0274
_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^)+(0.0342P)^2^+2.0982P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0691
_refine_ls_wR_factor_ref         0.0731
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8041
_reflns_number_total             9396
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc02522a2.cif
_cod_data_source_block           dal2019
_cod_depositor_comments
'Adding full bibliography for 7133367--7133370.cif.'
_cod_database_code               7133369
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_max   0.868
_shelx_estimated_absorpt_t_min   0.831
_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.a Aromatic/amide H refined with riding coordinates:
 C26(H26), C16A(H16A), C23A(H23A), C25(H25), C15A(H15A), C3(H3), C26A(H26A),
 C24A(H24A), C6S(H6S), C5A(H5A), C23(H23), C5(H5), C16(H16), C6A(H6A), C4(H4),
 C3A(H3A), C14A(H14A), C25A(H25A), C15(H15), C4A(H4A), C13A(H13A), C6(H6),
 C24(H24), C5S(H5S), C13(H13), C14(H14), C1S(H1S), C8S(H8S), C4S(H4S), C2S(H2S),
  C3S(H3S), C9S(H9S), C7S(H7S)
2.b Idealised Me refined as rotating group:
 C27A(H27A,H27B,H27C), C28A(H28A,H28B,H28C), C27(H27D,H27E,H27F), C18A(H18A,
 H18B,H18C), C17A(H17A,H17B,H17C), C28(H28D,H28E,H28F), C18(H18D,H18E,H18F),
 C17(H17D,H17E,H17F)
;
_shelx_res_checksum              60636
_shelx_hkl_checksum              20952
_olex2_submission_special_instructions 'No special instructions were received'