Ligand redox controlled amine dehydrogenation and imine hemilability in singlet diradical azo-aromatic Ni(II) complexes: characterization of the electron transfer series of azo-imine complexes of Ni(II).
Goswami, Bappaditya; Khatua, Manas; Devi, Ambika; Hans, Shivali; Chatterjee, Robindo; Samanta, Subhas; Dalton transactions (Cambridge, England : 2003) 53 (2024) 10250–10260; doi:10.1039/d3dt03414c

data_7716148
_publ_section_title
;
 Ligand redox controlled amine dehydrogenation and imine hemilability in
 singlet diradical azo-aromatic Ni(II) complexes: characterization of the
 electron transfer series of azo-imine complexes of Ni(II).
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10250
_journal_page_last               10260
_journal_paper_doi               10.1039/d3dt03414c
_journal_volume                  53
_journal_year                    2024
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C36 H26 F2 N8 Ni, 2(Cl O4)'
_chemical_formula_sum            'C36 H26 Cl2 F2 N8 Ni O8'
_chemical_formula_weight         866.24
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2024-05-18
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-05-19 deposited with the CCDC.	2024-05-23 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.5575(19)
_cell_length_b                   8.4204(7)
_cell_length_c                   20.7872(18)
_cell_measurement_reflns_used    9748
_cell_measurement_temperature    298.15
_cell_measurement_theta_max      28.293
_cell_measurement_theta_min      2.723
_cell_volume                     3773.4(6)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 97-2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'D8 VENTURE'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            70247
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         1.96
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.729
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6251
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1256 before and 0.0602 after correction.
The Ratio of minimum to maximum transmission is 0.8383.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear dark green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1768
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.683
_refine_diff_density_min         -0.381
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.045(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     514
_refine_ls_number_reflns         9356
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0393
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0901P)^2^+0.1245P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1193
_refine_ls_wR_factor_ref         0.1224
_reflns_number_gt                8430
_reflns_number_total             9356
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d3dt03414c2.cif
_cod_data_source_block           '[3c]_2ClO4'
_cod_depositor_comments
'Adding full bibliography for 7716146--7716150.cif.'
_cod_database_code               7716148
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C5A(H5A), C8(H8), C18(H18), C12A(H12A), C8A(H8A), C10A(H10A),
 C12(H12), C5(H5), C14(H14), C14A(H14A), C1A(H1A), C3(H3), C4(H4), C18A(H18A),
 C9A(H9A), C10(H10), C9(H9), C4A(H4A), C15(H15), C17A(H17A), C3A(H3A), C17(H17),
  C15A(H15A), C2A(H2A)
;
_olex2_submission_special_instructions 'No special instructions were received'