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_7716948
_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         'C45 H42 Br2 N2 Ni'
_chemical_formula_sum            'C45 H42 Br2 N2 Ni'
_chemical_formula_weight         829.33
_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     iterative
_audit_creation_date             2022-10-19
_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                 93.252(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.1583(5)
_cell_length_b                   22.9892(6)
_cell_length_c                   9.3758(3)
_cell_measurement_reflns_used    9562
_cell_measurement_temperature    169.99(10)
_cell_measurement_theta_max      76.4870
_cell_measurement_theta_min      2.5660
_cell_volume                     3692.38(19)
_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 0.999
_diffrn_measured_fraction_theta_max 0.966
_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     -8.00  19.00   0.50    0.40    --  -47.70  33.00 -66.00   54
  2  \w   -120.00 -52.00   0.50    0.40    --  -47.70 -33.00 134.00  136
  3  \w     54.00 106.00   0.50    0.40    --   47.70  33.00 -66.00  104
  4  \w    -26.00  41.00   0.50    0.40    --   47.70 -33.00 134.00  134
  5  \w   -168.00-131.00   0.50    2.50    -- -104.50 -33.00 134.00   74
  6  \w     94.00 177.00   0.50    2.50    --  107.36  33.00 -66.00  166
  7  \w    -19.00  25.00   0.50    0.40    --   47.70 -19.00   0.00   88
  8  \w     19.00  91.00   0.50    0.40    --   47.70-125.00   0.00  144
  9  \w    -62.00 -37.00   0.50    2.50    -- -104.50  57.00 150.00   50
 10  \w   -102.00 -41.00   0.50    2.50    -- -104.50  77.00   0.00  122
 11  \w    -61.00 -32.00   0.50    2.50    -- -104.50  57.00 -60.00   58
 12  \w    -62.00 -32.00   0.50    2.50    -- -104.50  57.00 -90.00   60
 13  \w     36.00 105.00   0.50    2.50    --  107.36 -77.00-150.00  138
 14  \w     36.00  72.00   0.50    2.50    --  107.36 -77.00 120.00   72
 15  \w     38.00  67.00   0.50    2.50    --  107.36 -57.00  30.00   58
 16  \w     40.00  66.00   0.50    2.50    --  107.36 -57.00 150.00   52
 17  \w     39.00  67.00   0.50    2.50    --  107.36 -57.00 -90.00   56
 18  \w     37.00 108.00   0.50    2.50    --  107.36-125.00  60.00  142
 19  \w     36.00  92.00   0.50    2.50    --  107.36 -77.00  30.00  112
 20  \w     42.00  97.00   0.50    2.50    --  107.36 -99.00-150.00  110
 21  \w    102.00 174.00   0.50    2.50    --  107.36  57.00 150.00  144
 22  \w     36.00  67.00   0.50    2.50    --  107.36 -57.00 -30.00   62
;
_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      -0.0398269000
_diffrn_orient_matrix_UB_12      0.0234016000
_diffrn_orient_matrix_UB_13      -0.1397673000
_diffrn_orient_matrix_UB_21      -0.0730185000
_diffrn_orient_matrix_UB_22      0.0157711000
_diffrn_orient_matrix_UB_23      0.0803252000
_diffrn_orient_matrix_UB_31      0.0342407000
_diffrn_orient_matrix_UB_32      0.0608013000
_diffrn_orient_matrix_UB_33      0.0327239000
_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  0.0496
_diffrn_reflns_av_unetI/netI     0.0483
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            25573
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.022
_diffrn_reflns_theta_min         2.579
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.551
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54336
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_description       block
_exptl_crystal_F_000             1696
_refine_diff_density_max         0.744
_refine_diff_density_min         -0.476
_refine_diff_density_rms         0.083
_refine_ls_extinction_coef       0.00009(3)
_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   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     454
_refine_ls_number_reflns         7534
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0633
_refine_ls_R_factor_gt           0.0515
_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^)+(0.0162P)^2^+9.7559P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1039
_refine_ls_wR_factor_ref         0.1085
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6443
_reflns_number_total             7534
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02159b2.cif
_cod_data_source_block           Ni3
_cod_depositor_comments
'Adding full bibliography for 7716948--7716949.cif.'
_cod_database_code               7716948
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N Ni Br'
_reflns_odcompleteness_completeness 99.96
_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
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C17(H17), C30(H30), C43(H43)
2.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C10(H10A,H10B), C8(H8A,H8B), C9(H9A,H9B)
2.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C15(H15), C25(H25), C29(H29), C20(H20), C19(H19), C21(H21),
 C38(H38), C32(H32), C23(H23), C28(H28), C3(H3), C40(H40), C41(H41), C39(H39),
 C1(H1), C42(H42), C22(H22), C27(H27), C36(H36), C26(H26), C2(H2), C33(H33),
 C35(H35), C34(H34)
2.d Idealised Me refined as rotating group:
 C45(H45A,H45B,H45C), C44(H44A,H44B,H44C)
;
_shelx_res_checksum              35950
_shelx_hkl_checksum              12237
_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 1.871
_oxdiff_exptl_absorpt_empirical_full_min 0.686