Axial-phenyl-constrained bis(imino)acenaphthene-nickel precatalysts enhance ethylene polymerization
Wang, Quanchao; Zhang, Qiuyue; Wang, Yizhou; Zou, Song; Ma, Yanping; Liang, Tongling; Sun, Wen-Hua; Polymer Chemistry 15 (2024) 4993–5006; doi:10.1039/D4PY01110D

data_1573092
_publ_section_title
;
 Axial-phenyl-constrained bis(imino)acenaphthene-nickel precatalysts
 enhance ethylene polymerization
;
_journal_issue                   48
_journal_name_full               'Polymer Chemistry'
_journal_page_first              4993
_journal_page_last               5006
_journal_paper_doi               10.1039/D4PY01110D
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C84 H88 Br4 N4 Ni2'
_chemical_formula_sum            'C84 H88 Br4 N4 Ni2'
_chemical_formula_weight         1590.64
_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     iterative
_audit_creation_date             2024-08-16
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.05.22 svn.r1d9e7f8d for OlexSys, GUI svn.r6131)
;
_audit_update_record
;
2024-08-25 deposited with the CCDC.	2024-11-11 downloaded from the CCDC.
;
_cell_angle_alpha                100.897(3)
_cell_angle_beta                 90.722(3)
_cell_angle_gamma                104.200(4)
_cell_formula_units_Z            1
_cell_length_a                   10.1206(4)
_cell_length_b                   11.7415(6)
_cell_length_c                   18.2647(5)
_cell_measurement_reflns_used    9719
_cell_measurement_temperature    169.98(11)
_cell_measurement_theta_max      75.5660
_cell_measurement_theta_min      3.9490
_cell_volume                     2062.19(15)
_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-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3-alpha (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      169.98(11)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.953
_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     82.00 176.00   0.50    0.83    --  103.25 125.00  90.00  188
  2  \w    151.00 176.00   0.50    0.83    --  103.25 106.00 -92.00   50
  3  \w     83.00 163.00   0.50    0.83    --  103.25 125.00-150.00  160
  4  \w     90.00 137.00   0.50    0.83    --  103.25 106.00 -92.00   94
  5  \w     87.00 157.00   0.50    0.83    --  103.25  61.00-180.00  140
  6  \w     93.00 178.00   0.50    0.83    --  103.25  30.00-120.00  170
  7  \w    -36.00  23.00   0.50    0.10    --  -46.95  38.00 -90.00  118
  8  \w    -67.00 -41.00   0.50    0.83    -- -104.50  61.00  60.00   52
  9  \w   -102.00 -35.00   0.50    0.83    -- -104.50  77.00 -90.00  134
 10  \w      4.00  61.00   0.50    0.10    --   46.95-106.00 168.00  114
 11  \w     62.00  91.00   0.50    0.10    --   46.95-125.00 150.00   58
 12  \w     54.00  95.00   0.50    0.10    --   46.95-125.00 -60.00   82
 13  \w     35.00 103.00   0.50    0.83    --  103.25-125.00-180.00  136
 14  \w     79.00 105.00   0.50    0.83    --  103.25 -94.00 -60.00   52
 15  \w     34.00 111.00   0.50    0.83    --  103.25-125.00 -30.00  154
 16  \w     32.00 102.00   0.50    0.83    --  103.25-125.00 150.00  140
 17  \w     46.00 107.00   0.50    0.83    --  103.25-106.00 168.00  122
 18  \w     52.00  87.00   0.50    0.83    --  103.25 -94.00   0.00   70
 19  \w     68.00  96.00   0.50    0.83    --  103.25 -94.00-180.00   56
 20  \w     36.00  62.00   0.50    0.83    --  103.25 -61.00-150.00   52
 21  \w    -11.00  30.00   0.50    0.10    --   46.95 -19.00 -90.00   82
 22  \w    -25.00  45.00   0.50    0.10    --   46.95 -38.00  30.00  140
 23  \w   -119.00 -74.00   0.50    0.10    --  -46.95-125.00-150.00   90
 24  \w   -174.00 -80.00   0.50    0.83    -- -104.50 -82.00-153.23  188
 25  \w   -114.00 -25.00   0.50    0.10    --  -46.95 -77.00-180.00  178
 26  \w   -172.00-146.00   0.50    0.83    -- -104.50 -58.00  18.23   52
 27  \w   -137.00 -89.00   0.50    0.83    -- -104.50 -58.00  18.23   96
 28  \w   -146.00 -93.00   0.50    0.83    -- -104.50 -45.00  60.00  106
 29  \w   -163.00 -85.00   0.50    0.83    -- -104.50-106.00 168.00  156
 30  \w   -147.00-120.00   0.50    0.83    -- -104.50 -30.00  90.00   54
 31  \w   -106.00 -80.00   0.50    0.83    -- -104.50 106.00 -92.00   52
 32  \w   -111.00 -72.00   0.50    0.83    -- -104.50 125.00-120.00   78
 33  \w    -80.00 -48.00   0.50    0.10    --  -46.95 106.00 -92.00   64
 34  \w    -40.00   1.00   0.50    0.10    --  -46.95 106.00 -92.00   82
 35  \w   -111.00 -66.00   0.50    0.83    -- -104.50 125.00  30.00   90
 36  \w   -109.00 -45.00   0.50    0.83    -- -104.50 114.00  26.52  128
;
_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      -0.1018674000
_diffrn_orient_matrix_UB_12      -0.0716619000
_diffrn_orient_matrix_UB_13      -0.0657274000
_diffrn_orient_matrix_UB_21      0.0756591000
_diffrn_orient_matrix_UB_22      0.0812154000
_diffrn_orient_matrix_UB_23      -0.0513508000
_diffrn_orient_matrix_UB_31      0.0929983000
_diffrn_orient_matrix_UB_32      -0.0856450000
_diffrn_orient_matrix_UB_33      -0.0211997000
_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  0.0618
_diffrn_reflns_av_unetI/netI     0.0563
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            24318
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.747
_diffrn_reflns_theta_min         3.962
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.153
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69921
_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    1.281
_exptl_crystal_description       plate
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.891
_refine_diff_density_min         -0.960
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         8177
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0866
_refine_ls_R_factor_gt           0.0723
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0869P)^2^+7.3537P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1871
_refine_ls_wR_factor_ref         0.1975
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6582
_reflns_number_total             8177
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4py01110d2.cif
_cod_data_source_block           Ni3
_cod_depositor_comments
'Adding full bibliography for 1573091--1573092.cif.'
_cod_database_code               1573092
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N Ni Br'
_reflns_odcompleteness_completeness 99.26
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Br2 \\sim Br4: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04 within 1.7A
Uanis(Br2) \\sim Ueq, Uanis(Br4) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
3. Others
 Sof(Br2)=1-FVAR(1)
 Sof(Br4)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C37(H37), C40(H40), C28(H28), C25(H25)
4.b Aromatic/amide H refined with riding coordinates:
 C35(H35), C33(H33), C34(H34), C10(H10), C9(H9), C4(H4), C6(H6), C21(H21),
 C18(H18), C23(H23), C22(H22), C17(H17), C5(H5), C16(H16), C14(H14), C15(H15)
4.c Idealised Me refined as rotating group:
 C41(H41A,H41B,H41C), C39(H39A,H39B,H39C), C42(H42A,H42B,H42C), C38(H38A,H38B,
 H38C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C26(H26A,H26B,H26C), C27(H27A,
 H27B,H27C)
;
_shelx_res_checksum              98602
_shelx_fab_checksum              91555
_platon_squeeze_void_probe_radius 1.20
_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 1.876
_oxdiff_exptl_absorpt_empirical_full_min 0.384