Effect of Ligand Modulation on Metal-to-Metal Electron Transfer in a Series of [Fe2Co2] Molecular Square Complexes
Kamilya, Sujit; Ghosh, Subrata; Mehta, Sakshi; Mondal, Abhishake; The Journal of Physical Chemistry A  (2021) –; doi:10.1021/acs.jpca.1c02032

data_1562054
_publ_section_title
;
 Effect of Ligand Modulation on Metal-to-Metal Electron Transfer in a
 Series of [Fe2Co2] Molecular Square Complexes
;
_journal_name_full               'The Journal of Physical Chemistry A'
_journal_paper_doi               10.1021/acs.jpca.1c02032
_journal_year                    2021
_chemical_formula_moiety
'C72 H84 B2 Co2 Fe2 N34 O4, 2(B F4), 2(C3 H7 N O)'
_chemical_formula_sum            'C78 H98 B4 Co2 F8 Fe2 N36 O6'
_chemical_formula_weight         2060.72
_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
_audit_creation_date             2021-02-18
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_cell_angle_alpha                88.755(3)
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_cell_angle_gamma                82.435(3)
_cell_formula_units_Z            1
_cell_length_a                   13.1307(6)
_cell_length_b                   13.1529(6)
_cell_length_c                   15.5247(7)
_cell_measurement_reflns_used    9030
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.79
_cell_measurement_theta_min      2.46
_cell_volume                     2504.9(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_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)'
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_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1024
_diffrn_reflns_av_unetI/netI     0.0709
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            111720
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.592
_diffrn_reflns_theta_min         1.775
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.691
_exptl_absorpt_correction_T_max  0.842
_exptl_absorpt_correction_T_min  0.731
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.27
_refine_diff_density_max         4.241
_refine_diff_density_min         -1.004
_refine_diff_density_rms         0.166
_refine_ls_extinction_coef       0.0140(19)
_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   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     616
_refine_ls_number_reflns         15283
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.1357
_refine_ls_R_factor_gt           0.0908
_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^)+(0.1693P)^2^+2.9263P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2418
_refine_ls_wR_factor_ref         0.2806
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9589
_reflns_number_total             15283
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jp1c02032_si_003.cif
_cod_data_source_block           Complex1_100K
_cod_database_code               1562054
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 B1(H1)
2.b Me refined with riding coordinates:
 C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C27(H27A,H27B,H27C), C26(H26A,H26B,
 H26C), C12(H12A,H12B,H12C), C18(H18A,H18B,H18C), C17(H17A,H17B,H17C), C7(H7A,
 H7B,H7C), C8(H8A,H8B,H8C), C13(H13A,H13B,H13C)
2.c Aromatic/amide H refined with riding coordinates:
 C34(H34), C33(H33), C29(H29), C28(H28), C24(H24), C25(H25), C20(H20),
 C19(H19), C10(H10), C15(H15), C5(H5), C39(H39)
2.d Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C38(H38A,H38B,H38C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              82869
_shelx_hkl_checksum              36491
_shelx_fab_checksum              68774
_olex2_submission_special_instructions 'No special instructions were received'