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_7716147
_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_formula_moiety         'C36 H32 N8 Ni0.933, 0.067(Ni)'
_chemical_formula_sum            'C36 H32 N8 Ni'
_chemical_formula_weight         635.41
_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     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-09-25
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-09-24 deposited with the CCDC.	2024-05-23 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 94.537(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.5912(2)
_cell_length_b                   27.4342(6)
_cell_length_c                   11.5190(3)
_cell_measurement_reflns_used    18415
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.0060
_cell_measurement_theta_min      1.7790
_cell_volume                     3021.46(12)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 7.9580
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -123.00 -55.00   1.00    5.00    --  -27.14 178.00 -60.00   68
  2  \w    -31.00 112.00   1.00    5.00    --   28.55  38.00  60.00  143
  3  \w     35.00 126.00   1.00    5.00    --   28.55 178.00 -60.00   91
  4  \w   -104.00  11.00   1.00    5.00    --  -27.14 -57.00  90.00  115
  5  \w    -66.00  50.00   1.00    5.00    --  -27.14  57.00 -30.00  116
  6  \w    -20.00  29.00   1.00    5.00    --  -27.14 -99.00  30.00   49
  7  \w    -16.00 116.00   1.00    5.00    --   28.55  77.00 -90.00  132
  8  \w    -48.00  67.00   1.00    5.00    --   28.55 -57.00  60.00  115
  9  \w    -16.00 116.00   1.00    5.00    --   28.55  77.00-180.00  132
 10  \w    -16.00  47.00   1.00    5.00    --   28.55  77.00 -30.00   63
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0480
_diffrn_reflns_av_unetI/netI     0.0268
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            43336
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         2.26
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.683
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55701
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic dark brown'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.592
_refine_diff_density_min         -0.278
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     446
_refine_ls_number_reflns         6243
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0516
_refine_ls_R_factor_gt           0.0470
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0386P)^2^+4.3444P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1117
_refine_ls_wR_factor_ref         0.1144
_reflns_number_gt                5733
_reflns_number_total             6243
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d3dt03414c2.cif
_cod_data_source_block           '[1]'
_cod_depositor_comments
'Adding full bibliography for 7716146--7716150.cif.'
_cod_database_code               7716147
_olex2_refinement_description
;
1. Others
 Sof(Ni1A)=1-FVAR(1)
 Sof(Ni1)=FVAR(1)
2.a Secondary CH2 refined with riding coordinates:
 C12(H12a,H12b), C12A(H12c,H12d)
2.b Aromatic/amide H refined with riding coordinates:
 N4(H4), N4A(H4A), C8(H8), C10(H10), C9(H9), C1(H1), C14(H14), C5(H5), C2(H2),
 C19(H19), C18A(H18A), C3(H3), C15(H15), C10A(H10A), C4(H4b), C5A(H5A),
 C17(H17), C8A(H8A), C3A(H3A), C14A(H14A), C9A(H9A), C17A(H17A), C4A(H4Aa),
 C16A(H16A), C16(H16), C2A(H2A), C15A(H15A)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;