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_7133370
_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         '2(C44 H48 Fe2 N8), C6 H6'
_chemical_formula_sum            'C94 H102 Fe4 N16'
_chemical_formula_weight         1679.31
_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     dual
_audit_creation_date             2023-06-14
_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                68.265(17)
_cell_angle_beta                 89.15(2)
_cell_angle_gamma                87.363(15)
_cell_formula_units_Z            2
_cell_length_a                   14.495(4)
_cell_length_b                   17.190(5)
_cell_length_c                   20.268(7)
_cell_measurement_reflns_used    9743
_cell_measurement_temperature    150.15
_cell_measurement_theta_max      26.265
_cell_measurement_theta_min      2.374
_cell_volume                     4686(3)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker D8-Venture Duo'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1601
_diffrn_reflns_av_unetI/netI     0.2034
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            67764
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.595
_diffrn_reflns_theta_min         1.899
_exptl_absorpt_coefficient_mu    0.658
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8126
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1621 before and 0.0796 after correction.
The Ratio of minimum to maximum transmission is 0.8126.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.190
_exptl_crystal_description       'irregular prism-like'
_exptl_crystal_F_000             1764
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.425
_refine_diff_density_min         -0.729
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1043
_refine_ls_number_reflns         19187
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.1858
_refine_ls_R_factor_gt           0.0985
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1411P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2482
_refine_ls_wR_factor_ref         0.2968
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9051
_reflns_number_total             19187
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc02522a2.cif
_cod_data_source_block           dal2216
_cod_depositor_comments
'Adding full bibliography for 7133367--7133370.cif.'
_cod_database_code               7133370
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_max   0.974
_shelx_estimated_absorpt_t_min   0.914
_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:
 C4(H4), C5(H5), C6(H6), C7(H7), C10(H10), C11(H11), C12(H12), C13(H13),
 C16(H16), C17(H17), C18(H18), C19(H19), C26(H26), C27(H27), C28(H28), C29(H29),
  C32(H32), C33(H33), C34(H34), C35(H35), C38(H38), C39(H39), C40(H40),
 C41(H41), C48(H48), C49(H49), C50(H50), C51(H51), C54(H54), C55(H55), C56(H56),
  C57(H57), C60(H60), C61(H61), C62(H62), C63(H63), C70(H70), C71(H71),
 C72(H72), C73(H73), C76(H76), C77(H77), C78(H78), C79(H79), C82(H82), C83(H83),
  C84(H84), C85(H85), C89(H89), C90(H90), C91(H91), C92(H92), C93(H93), C94(H94)
2.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C),
 C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C43(H43A,H43B,H43C), C44(H44A,H44B,
 H44C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C65(H65A,H65B,H65C), C66(H66A,
 H66B,H66C), C67(H67A,H67B,H67C), C68(H68A,H68B,H68C), C87(H87A,H87B,H87C),
 C88(H88A,H88B,H88C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              74282
_shelx_hkl_checksum              87415
_shelx_fab_checksum              22109
_olex2_submission_special_instructions 'No special instructions were received'