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_7704104
_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 H18 Cl2 N4 Ni'
_chemical_formula_sum            'C20 H18 Cl2 N4 Ni'
_chemical_formula_weight         443.97
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-11-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-11-14 deposited with the CCDC.	2020-04-16 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.3625(2)
_cell_length_b                   14.1391(2)
_cell_length_c                   20.0908(2)
_cell_measurement_reflns_used    11819
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      66.1050
_cell_measurement_theta_min      3.1360
_cell_volume                     3795.83(9)
_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 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega   57.00  121.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       26.3311  178.0000   60.0000 64

  2 omega  -12.00  102.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       26.3311   57.0000 -120.0000 114

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

  4 omega  -10.00  151.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       67.1656   30.0000  -30.0000 161

  5 omega  100.00  153.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       67.1656  111.0000 -120.0000 53

  6 omega   57.00  150.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       67.1656  178.0000  -60.0000 93

  7 omega  101.00  178.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  104.0000  150.0000 77

  8 omega   58.00  178.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   43.0000  150.0000 120

  9 omega   21.00  113.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -104.0000  -60.0000 92

 10 omega  101.00  178.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  104.0000   60.0000 77

 11 omega   21.00  113.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -104.0000    0.0000 92

 12 omega   29.00  145.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -65.0000   30.0000 116

 13 omega  101.00  178.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  104.0000 -150.0000 77

 14 omega   93.00  178.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  127.0000  133.0000 85

 15 omega   36.00  178.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   32.0000 -150.0000 142

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

 17 omega  -12.00  102.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       26.3311   57.0000    0.0000 114

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

 19 omega   24.00  144.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       67.1656   77.0000   30.0000 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_UB_11      0.0100368000
_diffrn_orient_matrix_UB_12      -0.0034951000
_diffrn_orient_matrix_UB_13      0.0763910000
_diffrn_orient_matrix_UB_21      -0.1145855000
_diffrn_orient_matrix_UB_22      -0.0065857000
_diffrn_orient_matrix_UB_23      0.0065263000
_diffrn_orient_matrix_UB_31      0.0066713000
_diffrn_orient_matrix_UB_32      -0.1087087000
_diffrn_orient_matrix_UB_33      -0.0028930000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_av_unetI/netI     0.0201
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            16925
_diffrn_reflns_theta_full        66.21
_diffrn_reflns_theta_max         66.21
_diffrn_reflns_theta_min         5.06
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.161
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48978
_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    1.554
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.267
_refine_diff_density_min         -0.349
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     246
_refine_ls_number_reflns         3308
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0281
_refine_ls_R_factor_gt           0.0271
_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^)+(0.0435P)^2^+2.1529P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0747
_refine_ls_wR_factor_ref         0.0755
_reflns_number_gt                3182
_reflns_number_total             3308
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d0dt00466a2.cif
_cod_data_source_block           8
_cod_depositor_comments
'Adding full bibliography for 7704099--7704110.cif.'
_cod_database_code               7704104
_chemical_oxdiff_formula         'C H N Cl Ni'
_reflns_odcompleteness_completeness 97.80
_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 Aromatic/amide H refined with riding coordinates:
 C5(H5), C10(H10), C9(H9), C17(H17), C12(H12), C8(H8), C1(H1), C15(H15),
 C4(H4), C16(H16), C2(H2), C3(H3)
2.b Idealised Me refined as rotating group:
 C20(H20a,H20b,H20c), C19(H19a,H19b,H19c)
;
_olex2_submission_special_instructions 'No special instructions were received'