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_7704110
_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 Cl2 N4 Ni'
_chemical_formula_sum            'C24 H26 Cl2 N4 Ni'
_chemical_formula_weight         500.10
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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                 90.436(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.0222(4)
_cell_length_b                   12.3486(2)
_cell_length_c                   20.4706(4)
_cell_measurement_reflns_used    21647
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      66.4460
_cell_measurement_theta_min      3.1780
_cell_volume                     4808.35(16)
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
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omega____ theta____ kappa____ phi______ frames
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  2 omega   87.00  114.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       67.1656   61.0000  -60.0000 27

  3 omega   87.00  177.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   32.0000  -60.0000 90

  4 omega  144.00  169.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -120.0000 25

  5 omega  134.00  161.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   21.0000 -150.0000 27

  6 omega  127.00  178.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -21.0000  -90.0000 51

  7 omega  131.00  174.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
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  8 omega  109.00  136.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
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  9 omega  108.00  144.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -65.0000   30.0000 36

 10 omega   86.00  144.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
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 11 omega  103.00  130.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -65.0000 -120.0000 27

 12 omega  106.00  177.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
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 13 omega  106.00  133.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
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 14 omega  101.00  152.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
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 15 omega  122.00  177.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  104.0000 -180.0000 55

 16 omega  150.00  177.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  138.0000 -120.0000 27

 17 omega  136.00  161.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
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 18 omega  129.00  157.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
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 19 omega  111.00  138.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
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 20 omega  112.00  154.00   1.0000    3.0000
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 21 omega  101.00  151.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
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 22 omega   95.00  122.00   1.0000    3.0000
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 23 omega   72.00  177.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
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 24 omega  112.00  166.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   11.0000    0.0000 54

 25 omega  134.00  161.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  104.0000   90.0000 27

 26 omega  148.00  175.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   65.0000  150.0000 27

 27 omega  112.00  163.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
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 28 omega  101.00  153.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
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 29 omega   99.00  126.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
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 30 omega   83.00  136.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       67.1656   61.0000   90.0000 53

 31 omega   97.00  131.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  138.0000  150.0000 34

 32 omega   73.00  103.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   54.0000   30.0000 30

 33 omega   74.00  123.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   43.0000  -30.0000 49

 34 omega   74.00   99.00   1.0000    3.0000
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 35 omega   60.00   88.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
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 36 omega   71.00  102.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
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 37 omega   89.00  116.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
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 38 omega   63.00   96.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
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 39 omega   82.00  117.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
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 40 omega   67.00  118.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
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 41 omega   90.00  146.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
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 42 omega   68.00  120.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
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 43 omega   52.00   82.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
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 44 omega   29.00   89.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
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 45 omega   42.00   67.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -54.0000   60.0000 25

 46 omega   23.00   50.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -104.0000   60.0000 27

 47 omega   22.00   82.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -104.0000  150.0000 60

 48 omega   25.00   61.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -117.0000  176.4070 36

 49 omega    8.00   47.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
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 50 omega  -38.00   60.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
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 51 omega   37.00  137.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
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 52 omega   59.00  119.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       26.3311  178.0000   90.0000 60

 53 omega   33.00  152.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
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 54 omega   57.00  149.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
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 55 omega   38.00   81.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   32.0000  -60.0000 43

 56 omega   67.00   97.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   21.0000 -150.0000 30

 57 omega   24.00   49.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -21.0000  -90.0000 25

 58 omega   28.00   57.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -32.0000  -60.0000 29

 59 omega   39.00   80.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000  -90.0000 41

 60 omega   99.00  155.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -89.0000 -150.0000 56

 61 omega   92.00  119.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -89.0000 -180.0000 27

 62 omega   53.00   91.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
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 63 omega   26.00  110.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
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 64 omega   28.00   53.00   1.0000    3.0000
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 65 omega   31.00  143.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
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 66 omega   33.00   90.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
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 67 omega   13.00  114.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
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 68 omega   24.00  103.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
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 69 omega   25.00   50.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
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 70 omega  -48.00   97.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       26.3311  -19.0000  -60.0000 145

 71 omega   -3.00   22.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       26.3311   57.0000 -180.0000 25
;
_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      0.0586691000
_diffrn_orient_matrix_UB_12      0.0668104000
_diffrn_orient_matrix_UB_13      0.0330821000
_diffrn_orient_matrix_UB_21      -0.0558401000
_diffrn_orient_matrix_UB_22      0.0680613000
_diffrn_orient_matrix_UB_23      0.0355334000
_diffrn_orient_matrix_UB_31      0.0014614000
_diffrn_orient_matrix_UB_32      -0.0804422000
_diffrn_orient_matrix_UB_33      0.0574737000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0761
_diffrn_reflns_av_unetI/netI     0.0417
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            43122
_diffrn_reflns_theta_full        66.36
_diffrn_reflns_theta_max         66.36
_diffrn_reflns_theta_min         3.16
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.345
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42449
_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    1.382
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2080
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.656
_refine_diff_density_min         -0.640
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     567
_refine_ls_number_reflns         8387
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0468
_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^)+(0.0847P)^2^+1.9865P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1267
_refine_ls_wR_factor_ref         0.1297
_reflns_number_gt                7782
_reflns_number_total             8387
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d0dt00466a2.cif
_cod_data_source_block           7
_cod_depositor_comments
'Adding full bibliography for 7704099--7704110.cif.'
_cod_original_cell_volume        4808.36(16)
_cod_database_code               7704110
_chemical_oxdiff_formula         'C H N Ni Cl'
_reflns_odcompleteness_completeness 97.59
_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:
 C00W(H00W), C012(H012), C018(H018), C01F(H01F)
2.b Aromatic/amide H refined with riding coordinates:
 C00K(H00K), C00Q(H00Q), C00R(H00R), C00T(H00T), C00V(H00V), C00X(H00X),
 C00Y(H00Y), C00Z(H00Z), C010(H010), C011(H011), C013(H013), C014(H014),
 C015(H015), C016(H016), C017(H017), C019(H019), C01A(H01Q), C01B(H01R),
 C01C(H01C), C01D(H01S), C01E(H01E), C01H(H01H), C01I(H01W), C01J(H01X)
2.c Idealised Me refined as rotating group:
 C01G(H01T,H01U,H01V), C01K(H01Y,H,HA), C01L(H01Z,HB,HC), C01M(H01A,H01B,H01D),
  C01N(H01G,H01I,H01J), C01O(H01K,H01L,H01M), C01P(H01N,H01O,H01P), C01Q(H01,HD,
 HE)
;
_olex2_submission_special_instructions 'No special instructions were received'