2-(N,N-Diethylaminomethyl)-6,7-trihydroquinolinyl-8-ylideneamine-Ni(ii) chlorides: application in ethylene dimerization and trimerization
Li, Jiaxin; Ma, Yanping; Hu, Xinquan; Flisak, Zygmunt; Tongling, Liang; Sun, Wen-Hua; New Journal of Chemistry 44 (2020) 17047–17052; doi:10.1039/D0NJ04003G

data_7059978
_publ_section_title
;
 2-(N,N-Diethylaminomethyl)-6,7-trihydroquinolinyl-8-ylideneamine-Ni(ii)
 chlorides: application in ethylene dimerization and trimerization
;
_journal_issue                   39
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              17047
_journal_page_last               17052
_journal_paper_doi               10.1039/D0NJ04003G
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety         'C26 H37 Cl2 N3 Ni'
_chemical_formula_sum            'C26 H37 Cl2 N3 Ni'
_chemical_formula_weight         521.19
_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     direct
_audit_creation_date             2019-06-28
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2020-05-27 deposited with the CCDC.	2020-09-11 downloaded from the CCDC.
;
_cell_angle_alpha                94.937(2)
_cell_angle_beta                 95.5750(10)
_cell_angle_gamma                92.089(2)
_cell_formula_units_Z            2
_cell_length_a                   9.5112(2)
_cell_length_b                   10.9618(3)
_cell_length_c                   12.9408(2)
_cell_measurement_reflns_used    13349
_cell_measurement_temperature    170.00(11)
_cell_measurement_theta_max      75.2230
_cell_measurement_theta_min      4.0420
_cell_volume                     1336.48(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      170.00(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.959
_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    -64.00 -39.00   0.50    0.05    --  -47.20 146.00  14.00   50
  2  \w    -90.00 -58.00   0.50    0.05    --  -47.20-146.00 -36.00   64
  3  \w    -95.00 -62.00   0.50    0.05    --  -47.20 125.00-151.00   66
  4  \w   -101.00 -75.00   0.50    0.05    --  -47.20-125.00 130.00   52
  5  \w     27.00  91.00   0.50    0.05    --   47.20-125.00 130.00  128
  6  \w     45.00 106.00   0.50    0.05    --   47.20-146.00 -36.00  122
  7  \w     67.00  94.00   0.50    0.05    --   47.20 146.00  14.00   54
  8  \w   -116.00 -90.00   0.50    0.05    --  -99.00 125.00-151.00   52
  9  \w   -134.00 -67.00   0.50    0.05    --  -99.00-146.00 -36.00  134
 10  \w   -110.00 -78.00   0.50    0.05    --  -99.00 146.00  14.00   64
 11  \w    102.00 131.00   0.50    0.05    --  103.25-146.00 -36.00   58
 12  \w    123.00 148.00   0.50    0.05    --  103.25 125.00-151.00   50
 13  \w     99.00 140.00   0.50    0.05    --  103.25 146.00  14.00   82
 14  \w     32.00 112.00   0.50    0.05    --  103.25-125.00 130.00  160
 15  \w   -120.00 -25.00   0.50    0.05    --  -47.20 -77.00 -30.00  190
 16  \w    -59.00  24.00   0.50    0.05    --  -47.20  19.00 -60.00  166
 17  \w     73.00 114.00   0.50    0.05    --   47.20  38.00 -60.00   82
 18  \w   -111.00 -86.00   0.50    0.05    --  -99.00  30.00  90.00   50
 19  \w    -70.00 -25.00   0.50    0.05    --  -99.00  30.00  90.00   90
 20  \w   -162.00 -87.00   0.50    0.05    --  -99.00 -30.00-180.00  150
 21  \w   -167.00 -88.00   0.50    0.05    --  -99.00 -45.00 120.00  158
 22  \w     52.00 109.00   0.50    0.05    --  103.25 -94.00  30.00  114
 23  \w     32.00  91.00   0.50    0.05    --  103.25 -61.00-150.00  118
 24  \w     33.00 111.00   0.50    0.05    --  103.25 -45.00  90.00  156
 25  \w     91.00 163.00   0.50    0.05    --  103.25  30.00  30.00  144
 26  \w     33.00  93.00   0.50    0.05    --  103.25 -94.00   0.00  120
 27  \w     31.00 103.00   0.50    0.05    --  103.25 -94.00 -90.00  144
 28  \w     57.00 119.00   0.50    0.05    --  103.25 -61.00  90.00  124
 29  \w     94.00 165.00   0.50    0.05    --  103.25  45.00 -60.00  142
 30  \w    129.00 169.00   0.50    0.05    --  103.25  45.00-150.00   80
 31  \w     77.00 108.00   0.50    0.05    --  103.25 -94.00-180.00   62
 32  \w     36.00  90.00   0.50    0.05    --  103.25 -45.00 -90.00  108
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0111570000
_diffrn_orient_matrix_UB_12      0.0264646000
_diffrn_orient_matrix_UB_13      0.1177100000
_diffrn_orient_matrix_UB_21      -0.1597321000
_diffrn_orient_matrix_UB_22      0.0174987000
_diffrn_orient_matrix_UB_23      -0.0221973000
_diffrn_orient_matrix_UB_31      -0.0300162000
_diffrn_orient_matrix_UB_32      -0.1375963000
_diffrn_orient_matrix_UB_33      0.0087143000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0198
_diffrn_reflns_av_unetI/netI     0.0177
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16013
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.504
_diffrn_reflns_theta_min         4.052
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.011
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58287
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.14e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.295
_exptl_crystal_description       block
_exptl_crystal_F_000             552
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.283
_refine_diff_density_min         -0.365
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         5313
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0339
_refine_ls_R_factor_gt           0.0293
_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^)+(0.0420P)^2^+0.6890P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0782
_refine_ls_wR_factor_ref         0.0886
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4985
_reflns_number_total             5313
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj04003g2.cif
_cod_data_source_block           Ni3
_cod_depositor_comments
'Adding full bibliography for 7059977--7059978.cif.'
_cod_database_code               7059978
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_usercomment     'C H N Ni Cl'
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C20(H20), C17(H17)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C23(H23A,H23B), C25(H25A,H25B), C6(H6A,H6B), C8(H8A,H8B), C7(H7A,
 H7B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C14(H14), C13(H13), C15(H15)
2.d Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C21(H21A,H21B,H21C), C19(H19A,H19B,
 H19C), C22(H22A,H22B,H22C), C18(H18A,H18B,H18C)
;
_shelx_res_checksum              61575
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.521
_oxdiff_exptl_absorpt_empirical_full_min 0.675