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_7704103
_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         'C36 H28 Cl2.644 I1.356 N8 Ni2, 2(C H2 Cl2)'
_chemical_formula_sum            'C38 H32 Cl6.64 I1.36 N8 Ni2'
_chemical_formula_weight         1126.11
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-02-11
_audit_creation_method
;
Olex2 1.3-dev
(compiled 2020.01.20 svn.r60d3a05a for OlexSys, GUI svn.r5830)
;
_audit_update_record
;
2020-04-05 deposited with the CCDC.	2020-04-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.576(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.4316(3)
_cell_length_b                   15.7887(4)
_cell_length_c                   13.0106(3)
_cell_measurement_reflns_used    9475
_cell_measurement_temperature    100.03(11)
_cell_measurement_theta_max      66.1900
_cell_measurement_theta_min      4.2540
_cell_volume                     2106.46(10)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.03(11)
_diffrn_detector_area_resol_mean 7.9580
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    4.00    --   26.33  57.00 -90.00  114
  2  \w     57.00 121.00   1.00    4.00    --   26.33 178.00-120.00   64
  3  \w     57.00 121.00   1.00    4.00    --   26.33 178.00-150.00   64
  4  \w     57.00 121.00   1.00    4.00    --   26.33 178.00  30.00   64
  5  \w    100.00 153.00   1.00   15.00    --   67.17 111.00  60.00   53
  6  \w     30.00 144.00   1.00   15.00    --   67.17  61.00 -90.00  114
  7  \w    100.00 153.00   1.00   15.00    --   67.17 111.00-180.00   53
  8  \w    100.00 153.00   1.00   15.00    --   67.17 111.00-120.00   53
  9  \w    100.00 153.00   1.00   15.00    --   67.17 111.00   0.00   53
 10  \w    100.00 153.00   1.00   15.00    --   67.17 111.00-150.00   53
 11  \w     57.00 150.00   1.00   15.00    --   67.17 178.00  60.00   93
 12  \w     20.00 147.00   1.00   15.00    --   67.17  45.00-150.00  127
 13  \w     86.00 178.00   1.00   20.00    --  108.00 138.00 -60.00   92
 14  \w     21.00 113.00   1.00   20.00    --  108.00-104.00   0.00   92
 15  \w     20.00 178.00   1.00   20.00    --  108.00  11.00 -90.00  158
 16  \w    101.00 178.00   1.00   20.00    --  108.00 104.00  30.00   77
 17  \w     21.00 113.00   1.00   20.00    --  108.00-104.00 -60.00   92
 18  \w    101.00 178.00   1.00   20.00    --  108.00 104.00  60.00   77
 19  \w     86.00 178.00   1.00   20.00    --  108.00 138.00-180.00   92
 20  \w     21.00 113.00   1.00   20.00    --  108.00-104.00-180.00   92
 21  \w     29.00 145.00   1.00   20.00    --  108.00 -65.00  60.00  116
 22  \w    101.00 178.00   1.00   20.00    --  108.00 104.00-120.00   77
 23  \w     21.00 113.00   1.00   20.00    --  108.00-104.00 -90.00   92
 24  \w     86.00 178.00   1.00   20.00    --  108.00 138.00  60.00   92
 25  \w     69.00 178.00   1.00   20.00    --  108.00  54.00-120.00  109
 26  \w     65.00 178.00   1.00   20.00    --  108.00  77.00 -60.00  113
 27  \w     66.00 178.00   1.00   20.00    --  108.00  74.00 -45.29  112
 28  \w     36.00 178.00   1.00   20.00    --  108.00  32.00-150.00  142
 29  \w    -12.00 102.00   1.00    4.00    --   26.33  57.00 120.00  114
 30  \w    -55.00  82.00   1.00    4.00    --   26.33 -38.00 -90.00  137
 31  \w    -50.00  64.00   1.00    4.00    --   26.33 -57.00 150.00  114
 32  \w    -17.00 111.00   1.00    4.00    --   26.33  77.00   0.00  128
 33  \w    -10.00 123.00   1.00   15.00    --   67.17  30.00 120.00  133
;
_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  0.0303
_diffrn_reflns_av_unetI/netI     0.0217
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            17206
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        66.211
_diffrn_reflns_theta_max         66.211
_diffrn_reflns_theta_min         4.312
_exptl_absorpt_coefficient_mu    13.134
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68752
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic dark black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.775
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1114
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.066
_exptl_crystal_size_min          0.051
_refine_diff_density_max         0.821
_refine_diff_density_min         -0.641
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     257
_refine_ls_number_reflns         3692
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0289
_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
'w=1/[\s^2^(Fo^2^)+(0.0386P)^2^+1.5193P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0697
_refine_ls_wR_factor_ref         0.0707
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3491
_reflns_number_total             3692
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00466a2.cif
_cod_data_source_block           11
_cod_depositor_comments
'Adding full bibliography for 7704099--7704110.cif.'
_cod_database_code               7704103
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.554
_shelx_estimated_absorpt_t_min   0.280
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(I1A) = Uanis(Cl1)
3. Others
 Sof(Cl1)=1-FVAR(1)
 Sof(I1A)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B)
4.b Aromatic/amide H refined with riding coordinates:
 C12A(H12A), C9A(H9A), C10A(H10A), C8A(H8A), C16A(H16A), C15A(H15A),
 C14A(H14A), C18A(H18A), C17A(H17A), C5A(H5A), C3A(H3A), C4A(H4A), C1A(H1A),
 C2A(H2A)
;
_shelx_res_checksum              90055
_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
;