Synthesis of low-molecular weight and branched polyethylenes <i>via</i> ethylene polymerization using 9-(arylimino)-5,6,7,8-tetrahydrocyclohepta-pyridylnickel precatalysts.
Ning, Zhao; Ma, Yanping; Zeng, Yanning; Wang, Yizhou; Xi, Aoqian; Sun, Wen-Hua; Dalton transactions (Cambridge, England : 2003) 53 (2024) 15968–15983; doi:10.1039/d4dt02159b

data_7716949
_publ_section_title
;
 Synthesis of low-molecular weight and branched polyethylenes <i>via</i>
 ethylene polymerization using
 9-(arylimino)-5,6,7,8-tetrahydrocyclohepta-pyridylnickel precatalysts.
;
_journal_issue                   38
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15968
_journal_page_last               15983
_journal_paper_doi               10.1039/d4dt02159b
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C42 H35 Br2 Cl N2 Ni, C H2 Cl2'
_chemical_formula_sum            'C43 H37 Br2 Cl3 N2 Ni'
_chemical_formula_weight         906.62
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-09-07
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2023-10-22 deposited with the CCDC.	2024-09-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.5690(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.1230(2)
_cell_length_b                   10.94452(8)
_cell_length_c                   30.6237(3)
_cell_measurement_reflns_used    35579
_cell_measurement_temperature    169.99(10)
_cell_measurement_theta_max      76.8870
_cell_measurement_theta_min      3.0020
_cell_volume                     7707.97(12)
_computing_cell_refinement       'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      169.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.980
_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     87.00 173.00   0.50    0.15    --  107.36  77.00-120.00  172
  2  \w     95.00 175.00   0.50    0.15    --  107.36  57.00 -90.00  160
  3  \w    103.00 177.00   0.50    0.15    --  107.36  77.00 150.00  148
  4  \w     43.00  69.00   0.50    0.10    --   47.70-142.00 109.00   52
  5  \w     36.00 124.00   0.50    0.15    --  107.36-142.00 109.00  176
  6  \w     35.00  75.00   0.50    0.15    --  107.36-125.00  30.00   80
  7  \w     63.00  88.00   0.50    0.15    --  107.36 -99.00 -30.00   50
  8  \w     78.00 104.00   0.50    0.15    --  107.36 -99.00 -60.00   52
  9  \w     35.00  62.00   0.50    0.15    --  107.36 -99.00 -30.00   54
 10  \w     35.00 114.00   0.50    0.15    --  107.36-128.00 -79.00  158
 11  \w     35.00  90.00   0.50    0.15    --  107.36-125.00-120.00  110
 12  \w     22.00  64.00   0.50    0.10    --   47.70-128.00 -79.00   84
 13  \w     75.00 101.00   0.50    0.15    --  107.36 -99.00 150.00   52
 14  \w     45.00  72.00   0.50    0.15    --  107.36 -99.00 150.00   54
 15  \w     48.00 101.00   0.50    0.15    --  107.36 -99.00 120.00  106
 16  \w     40.00  66.00   0.50    0.15    --  107.36 -57.00 -90.00   52
 17  \w    -27.00  27.00   0.50    0.10    --   47.70 -19.00 120.00  108
 18  \w     43.00  69.00   0.50    0.15    --  107.36 -57.00 120.00   52
 19  \w    -24.00  29.00   0.50    0.10    --   47.70 -19.00-120.00  106
 20  \w     38.00  68.00   0.50    0.15    --  107.36 -57.00 -30.00   60
 21  \w    104.00 129.00   0.50    0.15    --  107.36 128.00  -4.00   50
 22  \w    133.00 178.00   0.50    0.15    --  107.36 125.00  30.00   90
 23  \w     70.00  95.00   0.50    0.15    --  107.36 142.00 165.00   50
 24  \w     70.00  96.00   0.50    0.10    --   47.70 142.00 165.00   52
 25  \w     81.00 117.00   0.50    0.15    --  107.36 125.00  30.00   72
 26  \w   -111.00 -65.00   0.50    0.15    -- -104.50 125.00  60.00   92
 27  \w   -119.00 -36.00   0.50    0.15    -- -104.50 135.00  32.77  166
 28  \w   -129.00 -81.00   0.50    0.15    -- -104.50 151.00 -60.32   96
 29  \w   -100.00 -55.00   0.50    0.15    -- -104.50 128.00  -4.00   90
 30  \w    -94.00 -30.00   0.50    0.10    --  -47.70 128.00  -4.00  128
 31  \w   -123.00 -85.00   0.50    0.15    -- -104.50 142.00 165.00   76
 32  \w   -103.00 -45.00   0.50    0.10    --  -47.70 142.00 165.00  116
 33  \w    -22.00  27.00   0.50    0.10    --  -47.70  19.00  90.00   98
 34  \w    -62.00 -37.00   0.50    0.15    -- -104.50  57.00   0.00   50
 35  \w    -59.00 -33.00   0.50    0.15    -- -104.50  57.00 -30.00   52
 36  \w    -64.00 -38.00   0.50    0.15    -- -104.50  77.00-180.00   52
 37  \w   -150.00 -98.00   0.50    0.15    -- -104.50 -19.00  30.00  104
 38  \w   -117.00 -40.00   0.50    0.10    --  -47.70 -77.00 120.00  154
 39  \w   -121.00 -95.00   0.50    0.15    -- -104.50 -49.00 -14.12   52
 40  \w   -171.00-136.00   0.50    0.15    -- -104.50 -49.00 -14.12   70
 41  \w   -168.00 -94.00   0.50    0.15    -- -104.50 -46.00-169.83  148
 42  \w   -107.00 -80.00   0.50    0.10    --  -47.70-125.00-150.00   54
 43  \w    -93.00 -63.00   0.50    0.10    --  -47.70-142.00 109.00   60
 44  \w   -117.00 -80.00   0.50    0.10    --  -47.70-125.00  60.00   74
 45  \w    -98.00 -73.00   0.50    0.10    --  -47.70-128.00 -79.00   50
 46  \w   -147.00-122.00   0.50    0.15    -- -104.50-128.00 -79.00   50
 47  \w   -135.00 -92.00   0.50    0.15    -- -104.50-142.00 109.00   86
 48  \w    -87.00 -62.00   0.50    0.15    -- -104.50-142.00 109.00   50
;
_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      -0.0112299000
_diffrn_orient_matrix_UB_12      -0.0943355000
_diffrn_orient_matrix_UB_13      -0.0390542000
_diffrn_orient_matrix_UB_21      0.0231539000
_diffrn_orient_matrix_UB_22      -0.1023156000
_diffrn_orient_matrix_UB_23      0.0353541000
_diffrn_orient_matrix_UB_31      -0.0618355000
_diffrn_orient_matrix_UB_32      -0.0211535000
_diffrn_orient_matrix_UB_33      0.0030911000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0439
_diffrn_reflns_av_unetI/netI     0.0237
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            52421
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.188
_diffrn_reflns_theta_min         3.027
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.326
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48202
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.121a (Rigaku Oxford Diffraction, 2021)
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    1.563
_exptl_crystal_description       block
_exptl_crystal_F_000             3664
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.624
_refine_diff_density_min         -1.407
_refine_diff_density_rms         0.087
_refine_ls_extinction_coef       0.000051(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     456
_refine_ls_number_reflns         8019
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0411
_refine_ls_shift/su_max          0.058
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0579P)^2^+26.8081P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1117
_refine_ls_wR_factor_ref         0.1138
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7381
_reflns_number_total             8019
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02159b2.cif
_cod_data_source_block           Ni4
_cod_depositor_comments
'Adding full bibliography for 7716948--7716949.cif.'
_cod_original_cell_volume        7707.96(12)
_cod_database_code               7716949
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N F Ni Cl'
_shelx_estimated_absorpt_t_max   0.447
_shelx_estimated_absorpt_t_min   0.349
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Ternary CH refined with riding coordinates:
 C30(H30), C17(H17)
2.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C50(H50A,H50B)
2.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C15(H15), C36(H36), C1(H1), C42(H42), C38(H38), C3(H3), C23(H23),
 C2(H2), C41(H41), C29(H29), C25(H25), C22(H22), C39(H39), C32(H32), C19(H19),
 C34(H34), C40(H40), C33(H33), C35(H35), C26(H26), C21(H21), C20(H20), C27(H27),
  C28(H28)
;
_shelx_res_checksum              88340
_shelx_hkl_checksum              22506
_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 2.597
_oxdiff_exptl_absorpt_empirical_full_min 0.520