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_7059977
_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         'C22 H29 Cl2 N3 Ni'
_chemical_formula_sum            'C22 H29 Cl2 N3 Ni'
_chemical_formula_weight         465.09
_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
_atom_sites_solution_primary     dual
_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                90
_cell_angle_beta                 107.7540(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.0468(2)
_cell_length_b                   8.48720(10)
_cell_length_c                   15.8299(2)
_cell_measurement_reflns_used    13020
_cell_measurement_temperature    169.99(11)
_cell_measurement_theta_max      75.0810
_cell_measurement_theta_min      2.7100
_cell_volume                     2181.19(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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      169.99(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.968
_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    -80.00 -55.00   0.50    0.05    --  -47.20 131.00-158.00   50
  2  \w   -115.00 -90.00   0.50    0.05    --  -47.20-138.00 -44.00   50
  3  \w   -118.00 -86.00   0.50    0.05    --  -47.20-131.00 130.00   64
  4  \w     54.00  86.00   0.50    0.05    --   47.20-138.00 -44.00   64
  5  \w     73.00  98.00   0.50    0.05    --   47.20 131.00-158.00   50
  6  \w     70.00  95.00   0.50    0.05    --   47.20 138.00  16.00   50
  7  \w     27.00  98.00   0.50    0.05    --   47.20-131.00 130.00  142
  8  \w   -100.00 -75.00   0.50    0.05    --  -99.00 138.00  16.00   50
  9  \w     31.00 121.00   0.50    0.05    --  103.25-138.00 -44.00  180
 10  \w     77.00 104.00   0.50    0.05    --  103.25 131.00-158.00   54
 11  \w     76.00 101.00   0.50    0.05    --  103.25-131.00 130.00   50
 12  \w     95.00 120.00   0.50    0.05    --  103.25 138.00  16.00   50
 13  \w   -120.00 -72.00   0.50    0.05    --  -47.20-125.00-180.00   96
 14  \w   -119.00 -25.00   0.50    0.05    --  -47.20 -77.00 120.00  188
 15  \w     36.00  89.00   0.50    0.05    --   47.20  38.00 -60.00  106
 16  \w     94.00 120.00   0.50    0.05    --   47.20  38.00 -60.00   52
 17  \w    -56.00 -27.00   0.50    0.05    --  -99.00 125.00  30.00   58
 18  \w   -117.00 -64.00   0.50    0.05    --  -99.00 125.00  30.00  106
 19  \w     39.00 100.00   0.50    0.05    --  103.25 -94.00 -30.00  122
 20  \w     62.00 116.00   0.50    0.05    --  103.25 -45.00  90.00  108
 21  \w     81.00 160.00   0.50    0.05    --  103.25  77.00 -90.00  158
 22  \w    100.00 148.00   0.50    0.05    --  103.25  45.00 150.00   96
 23  \w     31.00 108.00   0.50    0.05    --  103.25 -94.00 120.00  154
 24  \w     33.00  58.00   0.50    0.05    --  103.25 -45.00  90.00   50
 25  \w     90.00 167.00   0.50    0.05    --  103.25  61.00 -60.00  154
;
_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      0.0236113000
_diffrn_orient_matrix_UB_12      -0.1758752000
_diffrn_orient_matrix_UB_13      0.0072718000
_diffrn_orient_matrix_UB_21      0.0915780000
_diffrn_orient_matrix_UB_22      0.0448099000
_diffrn_orient_matrix_UB_23      0.0386571000
_diffrn_orient_matrix_UB_31      -0.0080488000
_diffrn_orient_matrix_UB_32      -0.0048920000
_diffrn_orient_matrix_UB_33      0.0942484000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0300
_diffrn_reflns_av_unetI/netI     0.0239
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            17597
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.407
_diffrn_reflns_theta_min         2.722
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.623
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.37975
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.416
_exptl_crystal_description       needle
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.311
_refine_diff_density_min         -0.513
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     257
_refine_ls_number_reflns         4381
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.145
_refine_ls_R_factor_all          0.0391
_refine_ls_R_factor_gt           0.0328
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0570P)^2^+1.5830P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0880
_refine_ls_wR_factor_ref         0.1124
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3969
_reflns_number_total             4381
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj04003g2.cif
_cod_data_source_block           Ni1
_cod_depositor_comments
'Adding full bibliography for 7059977--7059978.cif.'
_cod_database_code               7059977
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_usercomment     'C H N Ni Cl'
_reflns_odcompleteness_completeness 99.95
_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 Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C19(H19A,H19B), C21(H21A,
 H21B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C13(H13), C14(H14), C15(H15)
2.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C17(H17A,H17B,H17C), C22(H22A,H22B,
 H22C)
;
_shelx_res_checksum              73945
_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 1.994
_oxdiff_exptl_absorpt_empirical_full_min 0.564