Dehydrogenation of amines in aryl-amine functionalized pincer-like nitrogen-donor redox non-innocent ligands via ligand reduction on a Ni(ii) template.
Khatua, Manas; Goswami, Bappaditya; Samanta, Subhas; Dalton transactions (Cambridge, England : 2003) 49 (2020) 6816–6831; doi:10.1039/d0dt00466a

data_7704100
_publ_section_title
;
 Dehydrogenation of amines in aryl-amine functionalized pincer-like
 nitrogen-donor redox non-innocent ligands via ligand reduction on a
 Ni(ii) template.
;
_journal_issue                   20
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6816
_journal_page_last               6831
_journal_paper_doi               10.1039/d0dt00466a
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C20 H20 Cl2 N4 Ni'
_chemical_formula_sum            'C20 H20 Cl2 N4 Ni'
_chemical_formula_weight         446.01
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-03-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-04-05 deposited with the CCDC.	2020-04-16 downloaded from the CCDC.
;
_cell_angle_alpha                87.050(4)
_cell_angle_beta                 75.671(4)
_cell_angle_gamma                71.025(5)
_cell_formula_units_Z            2
_cell_length_a                   9.0074(5)
_cell_length_b                   9.9859(6)
_cell_length_c                   11.7946(6)
_cell_measurement_reflns_used    5034
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      66.1110
_cell_measurement_theta_min      3.8720
_cell_volume                     971.54(10)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector_area_resol_mean 7.9580
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_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     30.00 123.00   1.00    1.00    --   67.17  61.00  60.00   93
  2  \w     96.00 138.00   1.00    1.00    --   67.17  61.00   0.00   42
  3  \w    106.00 135.00   1.00    1.00    --   67.17  61.00 -30.00   29
  4  \w    112.00 138.00   1.00    1.00    --   67.17 111.00 -30.00   26
  5  \w    133.00 177.00   1.00    1.00    --  108.00 138.00 -90.00   44
  6  \w    132.00 158.00   1.00    1.00    --  108.00 138.00-150.00   26
  7  \w    117.00 152.00   1.00    1.00    --   67.17 111.00-150.00   35
  8  \w    112.00 138.00   1.00    1.00    --  108.00 138.00-180.00   26
  9  \w    104.00 158.00   1.00    1.00    --  108.00 104.00-180.00   54
 10  \w    103.00 148.00   1.00    1.00    --  108.00  84.00-144.00   45
 11  \w    104.00 144.00   1.00    1.00    --  108.00 104.00 -30.00   40
 12  \w     90.00 118.00   1.00    1.00    --  108.00 138.00 -30.00   28
 13  \w     87.00 113.00   1.00    1.00    --  108.00 138.00 -90.00   26
 14  \w     63.00 130.00   1.00    1.00    --   67.17 178.00 -90.00   67
 15  \w     85.00 113.00   1.00    1.00    --   26.33 178.00 -90.00   28
 16  \w     33.00  91.00   1.00    1.00    --   67.17  61.00   0.00   58
 17  \w    101.00 132.00   1.00    1.00    --  108.00 104.00  90.00   31
 18  \w    101.00 177.00   1.00    1.00    --  108.00 104.00 120.00   76
 19  \w    123.00 172.00   1.00    1.00    --  108.00 -32.00 -60.00   49
 20  \w    108.00 147.00   1.00    1.00    --  108.00 -54.00  90.00   39
 21  \w     90.00 116.00   1.00    1.00    --  108.00 -54.00  60.00   26
 22  \w     81.00 133.00   1.00    1.00    --  108.00 -54.00 150.00   52
 23  \w     53.00  89.00   1.00    1.00    --  108.00-104.00  30.00   36
 24  \w     50.00  89.00   1.00    1.00    --  108.00-104.00 -60.00   39
 25  \w     42.00  79.00   1.00    1.00    --  108.00-104.00 -90.00   37
 26  \w     44.00 120.00   1.00    1.00    --  108.00-123.00 -85.80   76
 27  \w     65.00  91.00   1.00    1.00    --  108.00 -89.00-180.00   26
 28  \w     37.00 113.00   1.00    1.00    --   67.17-111.00 -90.00   76
 29  \w     89.00 121.00   1.00    1.00    --   26.33-178.00-180.00   32
 30  \w     56.00  82.00   1.00    1.00    --   26.33-178.00-180.00   26
 31  \w     50.00  80.00   1.00    1.00    --  108.00 -32.00 -60.00   30
 32  \w     28.00 109.00   1.00    1.00    --  108.00-104.00-150.00   81
 33  \w     25.00  74.00   1.00    1.00    --  108.00-104.00   0.00   49
 34  \w     38.00  88.00   1.00    1.00    --  108.00 -54.00  90.00   50
 35  \w     32.00  58.00   1.00    1.00    --  108.00 -54.00  60.00   26
 36  \w     37.00  79.00   1.00    1.00    --  108.00 -65.00  60.00   42
 37  \w     24.00 102.00   1.00    1.00    --  108.00-104.00  60.00   78
 38  \w     23.00  69.00   1.00    1.00    --   26.33 -77.00  30.00   46
 39  \w     23.00 107.00   1.00    1.00    --  108.00-104.00 -30.00   84
 40  \w     44.00 160.00   1.00    1.00    --  108.00  32.00-180.00  116
 41  \w     84.00 126.00   1.00    1.00    --  108.00  54.00 -90.00   42
 42  \w     30.00  55.00   1.00    1.00    --   67.17  61.00 -30.00   25
 43  \w     23.00 143.00   1.00    1.00    --   67.17  45.00 -60.00  120
 44  \w    -19.00 108.00   1.00    1.00    --   26.33  38.00 -30.00  127
 45  \w    -19.00  34.00   1.00    1.00    --   26.33  84.00-144.00   53
 46  \w    -51.00  -5.00   1.00    1.00    --   26.33 -77.00  30.00   46
 47  \w    -18.00  35.00   1.00    1.00    --   67.17 -77.00 120.00   53
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0478
_diffrn_reflns_av_unetI/netI     0.0433
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6286
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        66.252
_diffrn_reflns_theta_max         66.252
_diffrn_reflns_theta_min         3.870
_exptl_absorpt_coefficient_mu    4.064
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59293
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear reddish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             460
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.946
_refine_diff_density_min         -0.951
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         3349
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0563
_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^)+(0.1144P)^2^+0.5782P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1534
_refine_ls_wR_factor_ref         0.1554
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3170
_reflns_number_total             3349
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00466a2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7704099--7704110.cif.'
_cod_database_code               7704100
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Fixed occupancy and ADP/Uiso:
 H006
2.b Secondary CH2 refined with riding coordinates:
 C00B(H00A,H00B)
2.c Aromatic/amide H refined with riding coordinates:
 C00F(H00F), C00G(H00G), C00H(H00H), C00I(H00I), C00J(H00J), C00K(H00K),
 C00L(H00L), C00M(H00M), C00N(H00N), C00O(H00O), C00Q(H00Q)
2.d Idealised Me refined as rotating group:
 C00P(H00C,H00D,H00E), C00R(H00P,H00R,H00S)
;
_shelx_res_checksum              79739
_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
;