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_7716146
_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 H28 N8 Ni'
_chemical_formula_sum            'C36 H28 N8 Ni'
_chemical_formula_weight         631.37
_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     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                103.656(2)
_cell_angle_beta                 103.321(2)
_cell_angle_gamma                98.778(2)
_cell_formula_units_Z            2
_cell_length_a                   10.5648(3)
_cell_length_b                   11.4031(3)
_cell_length_c                   13.4514(3)
_cell_measurement_reflns_used    16769
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      66.0730
_cell_measurement_theta_min      3.4980
_cell_volume                     1495.16(7)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (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  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9580
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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    -12.00 102.00   1.00    2.00    --   26.33  57.00 -60.00  114
  2  \w      1.00  81.00   1.00    2.00    --   26.33 -99.00  30.00   80
  3  \w    -12.00 102.00   1.00    2.00    --   26.33  57.00  30.00  114
  4  \w    -12.00 102.00   1.00    2.00    --   26.33  57.00-180.00  114
  5  \w    -12.00 102.00   1.00    2.00    --   26.33  57.00-120.00  114
  6  \w     20.00 147.00   1.00    2.00    --   67.17  45.00 150.00  127
  7  \w     30.00 144.00   1.00    2.00    --   67.17  61.00-150.00  114
  8  \w    -19.00 155.00   1.00    2.00    --   67.17  15.00 -30.00  174
  9  \w     -4.00 109.00   1.00    2.00    --   67.17 -94.00 120.00  113
 10  \w    100.00 153.00   1.00    2.00    --   67.17 111.00  60.00   53
 11  \w     12.00 116.00   1.00    2.00    --   67.17-111.00 -90.00  104
 12  \w    100.00 153.00   1.00    2.00    --   67.17 111.00 -90.00   53
 13  \w     -9.00 104.00   1.00    2.00    --   67.17 -61.00   0.00  113
 14  \w    100.00 153.00   1.00    2.00    --   67.17 111.00  90.00   53
 15  \w    100.00 153.00   1.00    2.00    --   67.17 111.00-180.00   53
 16  \w     86.00 178.00   1.00    2.00    --  108.00 138.00 150.00   92
 17  \w     71.00 178.00   1.00    2.00    --  108.00  65.00-180.00  107
 18  \w     29.00 145.00   1.00    2.00    --  108.00 -65.00  90.00  116
 19  \w     58.00 178.00   1.00    2.00    --  108.00  43.00 -30.00  120
 20  \w     31.00 147.00   1.00    2.00    --  108.00 -54.00-150.00  116
 21  \w     21.00 178.00   1.00    2.00    --  108.00 -21.00  60.00  157
 22  \w     86.00 178.00   1.00    2.00    --  108.00 138.00   0.00   92
 23  \w     86.00 178.00   1.00    2.00    --  108.00 138.00  30.00   92
 24  \w     21.00 113.00   1.00    2.00    --  108.00-104.00 -90.00   92
 25  \w     23.00 151.00   1.00    2.00    --  108.00 -77.00-150.00  128
 26  \w     21.00 113.00   1.00    2.00    --  108.00-104.00  90.00   92
 27  \w     28.00 158.00   1.00    2.00    --  108.00 -43.00  60.00  130
 28  \w     19.00 158.00   1.00    2.00    --  108.00 -89.00 -90.00  139
 29  \w     31.00 147.00   1.00    2.00    --  108.00 -54.00 -30.00  116
 30  \w     86.00 178.00   1.00    2.00    --  108.00 138.00 120.00   92
 31  \w     21.00 113.00   1.00    2.00    --  108.00-104.00  60.00   92
 32  \w     19.00 178.00   1.00    2.00    --  108.00 -11.00-180.00  159
 33  \w     19.00 158.00   1.00    2.00    --  108.00 -89.00  90.00  139
 34  \w     69.00 178.00   1.00    2.00    --  108.00  54.00  90.00  109
 35  \w     71.00 178.00   1.00    2.00    --  108.00  65.00 -60.00  107
 36  \w     23.00 151.00   1.00    2.00    --  108.00 -77.00 -30.00  128
 37  \w     25.00 178.00   1.00    2.00    --  108.00 -32.00 -90.00  153
 38  \w     28.00 125.00   1.00    2.00    --  108.00-132.00 -99.57   97
 39  \w    -17.00 111.00   1.00    2.00    --   26.33  77.00  30.00  128
 40  \w    -50.00  64.00   1.00    2.00    --   26.33 -57.00-120.00  114
 41  \w    -17.00 111.00   1.00    2.00    --   26.33  77.00  90.00  128
 42  \w     57.00 121.00   1.00    2.00    --   26.33 178.00 -60.00   64
 43  \w    -50.00  64.00   1.00    2.00    --   26.33 -57.00 150.00  114
 44  \w     24.00 152.00   1.00    2.00    --   67.17  77.00 -30.00  128
 45  \w     24.00 152.00   1.00    2.00    --   67.17  77.00  30.00  128
 46  \w     30.00 144.00   1.00    2.00    --   67.17  61.00  30.00  114
 47  \w     24.00 152.00   1.00    2.00    --   67.17  77.00-120.00  128
 48  \w     24.00 152.00   1.00    2.00    --   67.17  77.00 150.00  128
 49  \w     24.00 152.00   1.00    2.00    --   67.17  77.00 -90.00  128
 50  \w     24.00 152.00   1.00    2.00    --   67.17  77.00 108.02  128
 51  \w     24.00 152.00   1.00    2.00    --   67.17  77.00 -60.00  128
 52  \w     24.00 152.00   1.00    2.00    --   67.17  77.00-150.00  128
 53  \w     30.00 144.00   1.00    2.00    --   67.17  61.00  90.00  114
 54  \w     65.00 149.00   1.00    2.00    --  108.00  77.00 120.00   84
 55  \w     58.00 178.00   1.00    2.00    --  108.00  43.00 -90.00  120
 56  \w     58.00 178.00   1.00    2.00    --  108.00  43.00  30.00  120
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0170078000
_diffrn_orient_matrix_UB_12      0.1412743000
_diffrn_orient_matrix_UB_13      0.0231974000
_diffrn_orient_matrix_UB_21      -0.1525910000
_diffrn_orient_matrix_UB_22      -0.0158747000
_diffrn_orient_matrix_UB_23      -0.0343927000
_diffrn_orient_matrix_UB_31      -0.0035986000
_diffrn_orient_matrix_UB_32      0.0095891000
_diffrn_orient_matrix_UB_33      0.1154485000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0341
_diffrn_reflns_av_unetI/netI     0.0217
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            26354
_diffrn_reflns_theta_full        66.25
_diffrn_reflns_theta_max         66.25
_diffrn_reflns_theta_min         3.52
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.257
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72992
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear brownish black'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             656
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.266
_refine_diff_density_min         -0.463
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         5224
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0330
_refine_ls_R_factor_gt           0.0312
_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^)+(0.0431P)^2^+0.9499P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0846
_refine_ls_wR_factor_ref         0.0863
_reflns_number_gt                4929
_reflns_number_total             5224
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d3dt03414c2.cif
_cod_data_source_block           '[2]'
_cod_depositor_comments
'Adding full bibliography for 7716146--7716150.cif.'
_cod_database_code               7716146
_chemical_oxdiff_formula         'C H N Ni'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C12A(H12A), C9A(H9A), C8A(H8A), C1A(H1A), C10(H10), C18A(H18A), C1(H1),
 C17A(H17A), C10A(H10A), C12(H12), C14A(H14A), C5A(H5A), C15A(H15A), C4A(H4A),
 C18(H18), C8(H8), C16A(H16A), C5(H5), C3A(H3A), C9(H9), C14(H14), C2A(H2A),
 C3(H3), C4(H4), C15(H15), C2(H2), C17(H17), C16(H16)
;
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.319
_oxdiff_exptl_absorpt_empirical_full_min 0.762