Hydrogen-atom and oxygen-atom transfer reactivities of iron(iv)-oxo complexes of quinoline-substituted pentadentate ligands
Munshi, Sandip; Sinha, Arup; Yiga, Solomon; Banerjee, Sridhar; Singh, Reena; Hossain, Md. Kamal; Haukka, Matti; Valiati, Andrei Felipe; Huelsmann, Ricardo Dagnoni; Martendal, Edmar; Peralta, Rosely; Xavier, Fernando; Wendt, Ola F.; Paine, Tapan K.; Nordlander, Ebbe; Dalton Transactions  (2022) –; doi:10.1039/D1DT03381F

data_7709265
_publ_section_title
;
 Hydrogen-atom and oxygen-atom transfer reactivities of iron(iv)-oxo
 complexes of quinoline-substituted pentadentate ligands
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT03381F
_journal_year                    2022
_chemical_formula_moiety         'C29 H26 Fe N6, 2(B F4) [+ solvent]'
_chemical_formula_sum            'C29 H26 B2 F8 Fe N6'
_chemical_formula_weight         688.03
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2021-10-03 deposited with the CCDC.	2021-12-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.547(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6887(2)
_cell_length_b                   15.5556(3)
_cell_length_c                   21.2702(5)
_cell_measurement_reflns_used    5992
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.9660
_cell_measurement_theta_min      2.4140
_cell_volume                     3513.51(13)
_computing_cell_refinement
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
;
_computing_data_collection
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
;
_computing_data_reduction
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
;
_computing_molecular_graphics
'CrystaMaker X (CrystalMaker Software ltd., 2018)'
_computing_publication_material  'SHELXL-2017 (Sheldrick, 2017)'
_computing_structure_refinement  'SHELXL-2017 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT (Sheldrick, 2017)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.0107
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.890
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\f scans and \w scans with \k offset'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0280
_diffrn_reflns_av_unetI/netI     0.0449
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.890
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            19839
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.890
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.953
_diffrn_reflns_theta_min         1.927
_diffrn_source                   micro-source
_exptl_absorpt_coefficient_mu    0.499
_exptl_absorpt_correction_T_max  0.987
_exptl_absorpt_correction_T_min  0.980
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_description       block
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.212
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.127
_platon_squeeze_details
;
Solvent of crystallization was disordered and could not be unambiguously 
identified. Therefore, solvent was omitted from the final structure. 
The contribution of the missing solvent to the calculated structure factors 
was taken into account by using the SQUEEZE routine of PLATON (Spek, 2003).
;
_refine_diff_density_max         0.763
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         9939
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0749
_refine_ls_R_factor_gt           0.0581
_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^)+(0.0821P)^2^+2.7914P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1533
_refine_ls_wR_factor_ref         0.1663
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7699
_reflns_number_total             9939
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03381f2.cif
_cod_data_source_block           ads_1044_sq
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7709265
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.902
_shelx_estimated_absorpt_t_max   0.939
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              87069
_shelx_hkl_checksum              99161
_shelx_fab_checksum              26772