Mononuclear Iron(III) Complex with Unusual Temperature Change of Color and Magneto-Structural Properties: Synthesis, Structure, Magnetization, Multi-frequency ESR and DFT Study
Garg, Nitish Kumar; Goriya, Yogesh; Seetharaman, Manojveer; Muratović, Senada; Pajić, Damir; Cetina, Mario; Petreska, Irina; Krupskaya, Yulia; Kataev, Vladislav; Johnson, Magnus T.; Wendt, Ola F.; Žilić, Dijana; Dalton Transactions  (2022) –; doi:10.1039/D1DT03751J

data_7709234
_publ_section_title
;
 Mononuclear Iron(III) Complex with Unusual Temperature Change of Color
 and Magneto-Structural Properties: Synthesis, Structure, Magnetization,
 Multi-frequency ESR and DFT Study
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT03751J
_journal_year                    2022
_chemical_formula_moiety         'C36 H42 Fe1 N6 O6, 3(B F4), 0.8[C5H12]'
_chemical_formula_sum            'C36 H42 B3 F12 Fe N6 O6'
_chemical_formula_weight         971.03
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2021-03-17
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-12-09 deposited with the CCDC.	2022-01-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   14.3913(7)
_cell_length_b                   14.3913(7)
_cell_length_c                   38.125(4)
_cell_measurement_reflns_used    2084
_cell_measurement_temperature    125
_cell_measurement_theta_max      22.8160
_cell_measurement_theta_min      3.9000
_cell_volume                     6838.2(9)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      125
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1367
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0895
_diffrn_reflns_av_unetI/netI     0.0407
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            18022
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         3.440
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.428
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68690
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2982
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: pentane'
_exptl_crystal_size_max          0.533
_exptl_crystal_size_mid          0.293
_exptl_crystal_size_min          0.186
_refine_diff_density_max         0.576
_refine_diff_density_min         -0.766
_refine_diff_density_rms         0.071
_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     99
_refine_ls_number_reflns         1341
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.1360
_refine_ls_R_factor_gt           0.0826
_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^)+(0.1073P)^2^+58.3106P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2167
_refine_ls_wR_factor_ref         0.2693
_reflns_Friedel_coverage         0.000
_reflns_number_gt                744
_reflns_number_total             1341
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03751j2.cif
_cod_data_source_block           FeL6(BF4)3_125K
_cod_original_cell_volume        6838.3(10)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               7709234
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(F2) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
3.a Aromatic/amide H refined with riding coordinates:
 N1(H1), C3(H3), C4(H4), C5(H5)
3.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 210 electrons were 
found in a volume of 762\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
0.8[C5H12] per Formula Unit 
which account for 202 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              84677
_shelx_fab_checksum              27443