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_7709263
_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
'2(C31 H24 Cl Fe N5), 2(Cl O4), 4(C6 H6), 2(C6 H5), [+ solvents]'
_chemical_formula_sum            'C104 H90 Cl4 Fe2 N10 O8'
_chemical_formula_weight         1861.35
_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             2021-04-17
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-10-03 deposited with the CCDC.	2021-12-08 downloaded from the CCDC.
;
_cell_angle_alpha                74.903(7)
_cell_angle_beta                 85.255(7)
_cell_angle_gamma                74.213(7)
_cell_formula_units_Z            1
_cell_length_a                   10.045(2)
_cell_length_b                   15.049(4)
_cell_length_c                   15.944(4)
_cell_measurement_reflns_used    3974
_cell_measurement_temperature    100.05
_cell_measurement_theta_max      24.86
_cell_measurement_theta_min      2.38
_cell_volume                     2239.1(9)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_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    'SHELXS-1997  (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.05
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  'Bruker APEX-III CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1180
_diffrn_reflns_av_unetI/netI     0.1648
_diffrn_reflns_Laue_measured_fraction_full 0.956
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16544
_diffrn_reflns_point_group_measured_fraction_full 0.956
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        25.033
_diffrn_reflns_theta_max         25.033
_diffrn_reflns_theta_min         2.384
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.509
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.4774
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1435 before and 0.1056 after correction.
The Ratio of minimum to maximum transmission is 0.6406.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'metallic brownish yellow'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_description       needle
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.154
_refine_diff_density_min         -1.049
_refine_diff_density_rms         0.121
_refine_ls_extinction_coef       0.0018(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     548
_refine_ls_number_reflns         7565
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.1713
_refine_ls_R_factor_gt           0.0915
_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^)+(0.1311P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2166
_refine_ls_wR_factor_ref         0.2819
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4119
_reflns_number_total             7565
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03381f2.cif
_cod_data_source_block           mo_tkp120118a_0m_a
_cod_database_code               7709263
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.975
_shelx_estimated_absorpt_t_min   0.928
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C48) = Uanis(C49) = Uanis(C46) = Uanis(C43) = Uanis(C47) = Uanis(C45)
3.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C14(H14A,H14B)
3.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C13(H13), C15(H15), C16(H16), C17(H17), C18(H18),
 C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26),
  C27(H27), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33),
 C34(H34), C35(H35), C36(H36), C37(H37), C39(H39), C40(H40), C1A(H1A), C41(H41),
  C42(H42), C43(H43), C44(H44), C45(H45), C46(H46), C47(H47), C48(H48),
 C49(H49), C38(H38), C50(H50), C52(H52)
;
_shelx_res_checksum              95664
_shelx_hkl_checksum              9508
_olex2_submission_special_instructions 'No special instructions were received'