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_7704108
_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         'C24 H26 N4'
_chemical_formula_sum            'C24 H26 N4'
_chemical_formula_weight         370.49
_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     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-01-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-01-14 deposited with the CCDC.	2020-04-16 downloaded from the CCDC.
;
_cell_angle_alpha                68.670(3)
_cell_angle_beta                 83.291(3)
_cell_angle_gamma                89.466(3)
_cell_formula_units_Z            2
_cell_length_a                   8.6058(4)
_cell_length_b                   10.9184(4)
_cell_length_c                   11.7427(4)
_cell_measurement_reflns_used    11418
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      66.2620
_cell_measurement_theta_min      4.0560
_cell_volume                     1020.09(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_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_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
  1 omega  -12.00  102.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       26.3311   57.0000  150.0000 114

  2 omega  -17.00  111.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       26.3311   77.0000  -60.0000 128

  3 omega  -12.00  102.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       26.3311   57.0000 -150.0000 114

  4 omega  -58.00   70.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       26.3311  -77.0000   30.0000 128

  5 omega   30.00  144.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       67.1656   61.0000  -60.0000 114

  6 omega   57.00  150.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       67.1656  178.0000  -60.0000 93

  7 omega   30.00  144.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       67.1656   61.0000 -120.0000 114

  8 omega  100.00  153.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       67.1656  111.0000 -150.0000 53

  9 omega   30.00  144.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       67.1656   61.0000  -30.0000 114

 10 omega  100.00  153.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       67.1656  111.0000 -180.0000 53

 11 omega  100.00  153.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       67.1656  111.0000 -120.0000 53

 12 omega  100.00  153.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       67.1656  111.0000  120.0000 53

 13 omega  100.00  153.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       67.1656  111.0000  -30.0000 53

 14 omega  100.00  153.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       67.1656  111.0000  -60.0000 53

 15 omega  -10.00  151.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       67.1656   30.0000   60.0000 161

 16 omega   30.00  144.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       67.1656   61.0000  -90.0000 114

 17 omega   12.00  116.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       67.1656 -111.0000  -60.0000 104

 18 omega   86.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  138.0000 -150.0000 92

 19 omega   86.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  138.0000 -120.0000 92

 20 omega  101.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  104.0000  -90.0000 77

 21 omega   71.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   65.0000 -120.0000 107

 22 omega  101.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  104.0000   30.0000 77

 23 omega  101.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  104.0000   60.0000 77

 24 omega   65.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -180.0000 113

 25 omega   29.00  145.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -65.0000  -30.0000 116

 26 omega   86.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  138.0000  120.0000 92

 27 omega   21.00  113.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -104.0000 -150.0000 92

 28 omega   25.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   21.0000  120.0000 153

 29 omega   25.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -32.0000  120.0000 153

 30 omega   25.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -32.0000   30.0000 153

 31 omega  101.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  104.0000  150.0000 77

 32 omega  101.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  104.0000  120.0000 77

 33 omega  101.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  104.0000  -30.0000 77

 34 omega   29.00  145.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -65.0000  -60.0000 116

 35 omega   21.00  113.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -104.0000  -30.0000 92

 36 omega   21.00  113.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -104.0000  -90.0000 92

 37 omega   69.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   70.0000  -33.1474 109

 38 omega   25.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   21.0000  -30.0000 153

 39 omega   21.00  113.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -104.0000   60.0000 92

 40 omega  101.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  104.0000    0.0000 77

 41 omega   27.00  123.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -127.0000 -148.8965 96

 42 omega  -50.00   64.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       26.3311  -57.0000  -90.0000 114

 43 omega  -50.00   64.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       26.3311  -57.0000   60.0000 114

 44 omega  -23.00   31.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       26.3311   90.0000   66.0000 54

 45 omega  -17.00  111.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       26.3311   77.0000  150.0000 128

 46 omega  -50.00   64.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       26.3311  -57.0000 -150.0000 114

 47 omega  -12.00  102.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       26.3311   57.0000   60.0000 114

 48 omega   30.00  144.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       67.1656   61.0000  150.0000 114

 49 omega   24.00  152.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       67.1656   77.0000  150.0000 128

 50 omega   24.00  152.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       67.1656   77.0000   60.0000 128

 51 omega   24.00  152.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       67.1656   77.0000    0.0000 128

 52 omega   24.00  152.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       67.1656   77.0000   30.0000 128

 53 omega   24.00  152.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       67.1656   77.0000  120.0000 128

 54 omega   24.00  152.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       67.1656   77.0000  -60.0000 128

 55 omega   24.00  152.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       67.1656   77.0000 -150.0000 128

 56 omega   24.00  152.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       67.1656   77.0000 -120.0000 128

 57 omega   24.00  152.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       67.1656   77.0000  -30.0000 128

 58 omega   24.00  152.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       67.1656   77.0000   90.0000 128

 59 omega   24.00  152.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       67.1656   77.0000 -180.0000 128

 60 omega   65.00  167.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000    0.0000 102

 61 omega   69.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   54.0000  150.0000 109
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0290936000
_diffrn_orient_matrix_UB_12      -0.0007631000
_diffrn_orient_matrix_UB_13      -0.1267255000
_diffrn_orient_matrix_UB_21      0.1705763000
_diffrn_orient_matrix_UB_22      -0.0381388000
_diffrn_orient_matrix_UB_23      -0.0220133000
_diffrn_orient_matrix_UB_31      -0.0508801000
_diffrn_orient_matrix_UB_32      -0.1466923000
_diffrn_orient_matrix_UB_33      0.0599227000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0194
_diffrn_reflns_av_unetI/netI     0.0128
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            16708
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_diffrn_reflns_theta_max         66.11
_diffrn_reflns_theta_min         4.07
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.562
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69632
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic dark red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.206
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             396
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.426
_refine_diff_density_min         -0.225
_refine_diff_density_rms         0.034
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     257
_refine_ls_number_reflns         3526
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0361
_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^)+(0.0493P)^2^+0.3400P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0972
_refine_ls_wR_factor_ref         0.0991
_reflns_number_gt                3281
_reflns_number_total             3526
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d0dt00466a2.cif
_cod_data_source_block           Lx
_cod_depositor_comments
'Adding full bibliography for 7704099--7704110.cif.'
_cod_database_code               7704108
_chemical_oxdiff_formula         'C H N'
_reflns_odcompleteness_completeness 96.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C22(H22), C19(H19)
2.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C10(H10), C17(H17), C8(H8), C9(H9), C16(H16), C15(H15), C2(H2),
 C1(H1), C5(H5), C3(H3), C4(H4)
2.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C24(H24A,H24B,H24C), C21(H21A,H21B,H21C), C23(H23A,H23B,
 H23C)
;
_olex2_submission_special_instructions 'No special instructions were received'