Closed-shell Phenalenyl-based Dinuclear Iron(III) Complex as a Robust Cathode for One-Compartment H2O2 Fuel Cell
Kamboj, Nisha; Dey, Ayan; Lama, Prem; Majumder, Moumita; Sengupta, Srijan; Metre, Ramesh K.; Dalton Transactions  (2023) –; doi:10.1039/D3DT02975A

data_7714229
_publ_section_title
;
 Closed-shell Phenalenyl-based Dinuclear Iron(III) Complex as a Robust
 Cathode for One-Compartment H2O2 Fuel Cell
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02975A
_journal_year                    2023
_chemical_formula_moiety
'C63 H42 Fe2 N6 O9, C H Cl3, C H Cl2.85, 0.15(Cl)'
_chemical_formula_sum            'C65 H44 Cl6 Fe2 N6 O9'
_chemical_formula_weight         1377.46
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2022-12-23
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-07-21 deposited with the CCDC.	2023-10-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.358(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.2460(12)
_cell_length_b                   13.2054(7)
_cell_length_c                   19.6226(10)
_cell_measurement_reflns_used    9974
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.47
_cell_measurement_theta_min      2.44
_cell_volume                     5905.6(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-III photon detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0501
_diffrn_reflns_av_unetI/netI     0.0430
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            52543
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_min         2.117
_exptl_absorpt_coefficient_mu    0.829
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.549
_exptl_crystal_description       colorless
_exptl_crystal_F_000             2808
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.16
_exptl_transmission_factor_max   0.7453
_exptl_transmission_factor_min   0.6157
_refine_diff_density_max         1.011
_refine_diff_density_min         -1.176
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     805
_refine_ls_number_reflns         10810
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0990
_refine_ls_R_factor_gt           0.0797
_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^)+(0.0792P)^2^+26.0279P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1928
_refine_ls_wR_factor_ref         0.2043
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8627
_reflns_number_total             10810
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02975a3.cif
_cod_data_source_block           1
_cod_database_code               7714229
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.879
_shelx_estimated_absorpt_t_min   0.852
_olex2_refinement_description
;
1. Others
 Fixed Sof: Cl6A(0.85) Cl6B(0.15)
2.a Ternary CH refined with riding coordinates:
 C64(H64), C65(H65)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C7(H7), C12(H12), C13(H13), C14(H14),
 C18(H18), C19(H19), C20(H20), C23(H23), C24(H24), C26(H26), C27(H27), C28(H28),
  C33(H33), C34(H34), C35(H35), C39(H39), C40(H40), C41(H41), C44(H44),
 C45(H45), C47(H47), C48(H48), C49(H49), C54(H54), C55(H55), C56(H56), C60(H60),
  C61(H61), C62(H62)
2.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C42(H42A,H42B,H42C), C63(H63A,H63B,H63C)
;
_shelx_res_checksum              47784
_olex2_submission_special_instructions 'No special instructions were received'