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_1573091
_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         'C38 H36 Br2 N2 Ni'
_chemical_formula_sum            'C38 H36 Br2 N2 Ni'
_chemical_formula_weight         739.22
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-10-26
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.05.22 svn.r1d9e7f8d for OlexSys, GUI svn.r6131)
;
_audit_update_record
;
2024-10-26 deposited with the CCDC.	2024-11-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.829(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9593(8)
_cell_length_b                   15.7707(6)
_cell_length_c                   17.4731(10)
_cell_measurement_reflns_used    9937
_cell_measurement_temperature    169.96(13)
_cell_measurement_theta_max      74.2440
_cell_measurement_theta_min      3.8350
_cell_volume                     3337.7(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)'
_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 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      169.96(13)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.928
_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    -43.00  -4.00   0.50    0.80    --  -47.09 106.00  -1.00   78
  2  \w    -79.00 -48.00   0.50    0.80    --  -47.09 106.00  -1.00   62
  3  \w     15.00  57.00   0.50    0.80    --   47.09-106.00-100.00   84
  4  \w     73.00 106.00   0.50    4.60    --  103.25-106.00-100.00   66
  5  \w     90.00 172.00   0.50    4.60    --  103.25 106.00  -1.00  164
  6  \w    -95.00 -69.00   0.50    4.60    -- -104.50 106.00  -1.00   52
  7  \w    -22.00  26.00   0.50    0.80    --  -47.09  19.00   0.00   96
  8  \w    -22.00  26.00   0.50    0.80    --  -47.09  19.00 -90.00   96
  9  \w    -28.00  23.00   0.50    0.80    --  -47.09  38.00 120.00  102
 10  \w     -5.00  22.00   0.50    0.80    --  -47.09  19.00  90.00   54
 11  \w    -26.00  30.00   0.50    0.80    --   47.09 -19.00-150.00  112
 12  \w     65.00 107.00   0.50    4.60    --  103.25 -77.00 -90.00   84
 13  \w     92.00 174.00   0.50    4.60    --  103.25  45.00 -30.00  164
 14  \w     42.00  74.00   0.50    4.60    --  103.25 -61.00 -60.00   64
 15  \w     51.00 106.00   0.50    4.60    --  103.25 -94.00 -90.00  110
 16  \w     31.00  74.00   0.50    4.60    --  103.25 -61.00-120.00   86
 17  \w     32.00  61.00   0.50    4.60    --  103.25 -61.00 -90.00   58
 18  \w    -68.00 -43.00   0.50    4.60    -- -104.50  61.00-150.00   50
 19  \w   -118.00 -92.00   0.50    4.60    -- -104.50 -30.00-180.00   52
 20  \w   -160.00-126.00   0.50    4.60    -- -104.50 -30.00-180.00   68
 21  \w    -67.00 -32.00   0.50    4.60    -- -104.50  61.00  30.00   70
 22  \w    -91.00 -32.00   0.50    4.60    -- -104.50  77.00  60.00  118
 23  \w    -63.00 -36.00   0.50    4.60    -- -104.50  61.00 150.00   54
 24  \w   -121.00 -95.00   0.50    4.60    -- -104.50 -15.00 150.00   52
 25  \w   -164.00-138.00   0.50    4.60    -- -104.50 -15.00 150.00   52
 26  \w    -68.00 -34.00   0.50    4.60    -- -104.50  61.00-180.00   68
 27  \w   -135.00-108.00   0.50    4.60    -- -104.50-106.00-100.00   54
;
_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      -0.0949626000
_diffrn_orient_matrix_UB_12      0.0549751000
_diffrn_orient_matrix_UB_13      -0.0561564000
_diffrn_orient_matrix_UB_21      -0.0390727000
_diffrn_orient_matrix_UB_22      0.0167026000
_diffrn_orient_matrix_UB_23      0.0720564000
_diffrn_orient_matrix_UB_31      0.0752474000
_diffrn_orient_matrix_UB_32      0.0789573000
_diffrn_orient_matrix_UB_33      0.0236066000
_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  0.0513
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.928
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            23084
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.928
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.245
_diffrn_reflns_theta_min         3.897
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.852
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87768
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.94a (Rigaku Oxford Diffraction, 2023)
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    1.471
_exptl_crystal_description       needle
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.342
_refine_diff_density_min         -0.916
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     578
_refine_ls_number_reflns         6489
_refine_ls_number_restraints     876
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1371
_refine_ls_R_factor_gt           0.1279
_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^)+47.1369P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2355
_refine_ls_wR_factor_ref         0.2391
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5535
_reflns_number_total             6489
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4py01110d2.cif
_cod_data_source_block           Ni2
_cod_depositor_comments
'Adding full bibliography for 1573091--1573092.cif.'
_cod_database_code               1573091
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C H N Ni Br'
_reflns_odcompleteness_completeness 96.63
_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. Restrained distances
 C2AA-C1AA = C6AA-C1AA = C6AA-C5AA = C5AA-C4AA = C4AA-C3AA = C3AA-C2AA
 1.4 with sigma of 0.02
 C38-C37 = C0AA-C013 = C28-C27 = C36-C35
 1.54 with sigma of 0.01
 C26-C25 = C13A-C0 = C5BA-C39 = C7AB-C1BA
 1.54 with sigma of 0.01
 C5AA-C25 = C1AA-C0 = C5BA-C4BA = C8AA-C1BA
 1.49 with sigma of 0.02
 C24-C013 = C27-C20 = C37-C34 = C35-C30
 1.49 with sigma of 0.02
 C13-C14 = C18-C17 = C16-C15
 1.39 with sigma of 0.01
 C5-C4 = C4-C3 = C3-C12 = C12-C11 = C11-C10 = C9-C10 = C9-C8 = C6-C5 = C7-C12 =
  C8-C7
 1.39 with sigma of 0.01
3. Rigid bond restraints
 C27, C28
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
C27 \\sim C28 \\sim C13A \\sim C0 \\sim C1AA \\sim C2AA \\sim C19 \\sim C23
\\sim C20 \\sim C24 \\sim C21 \\sim C22 \\sim C3AA \\sim C4AA \\sim C5AA \\sim
C6AA \\sim C013 \\sim C0AA \\sim C25 \\sim C26: within 1.7A with sigma of 0.02
and sigma for terminal atoms of 0.04 within 1.7A
C29 \\sim C30 \\sim C34 \\sim C31 \\sim C32 \\sim C33 \\sim C37 \\sim C38 \\sim
C36 \\sim C8AA \\sim C9AA \\sim C0BA \\sim C2BA \\sim C3BA \\sim C4BA \\sim
C5BA \\sim C39 \\sim C35 \\sim C1BA \\sim C7AB: within 1.7A with sigma of 0.02
and sigma for terminal atoms of 0.04 within 1.7A
Uanis(C20) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C13A)
\\sim Ueq, Uanis(C0) \\sim Ueq, Uanis(C1AA) \\sim Ueq, Uanis(C2AA) \\sim Ueq,
Uanis(C6AA) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C22)
\\sim Ueq, Uanis(C013) \\sim Ueq, Uanis(C0AA) \\sim Ueq, Uanis(C3AA) \\sim Ueq,
Uanis(C4AA) \\sim Ueq, Uanis(C5AA) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C26)
\\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C21) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C30) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C32)
\\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C38) \\sim Ueq,
Uanis(C9AA) \\sim Ueq, Uanis(C2BA) \\sim Ueq, Uanis(C3BA) \\sim Ueq,
Uanis(C4BA) \\sim Ueq, Uanis(C5BA) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C35)
\\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C8AA) \\sim Ueq, Uanis(C1BA) \\sim Ueq,
Uanis(C7AB) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C0BA) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C15) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C18)
\\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C7) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C4) \\sim
Ueq, Uanis(C3) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C11) \\sim Ueq,
Uanis(C10) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C8) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(C13A)=Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(C0)=Sof(H0A)=Sof(H0B)=Sof(C1AA)=
 Sof(C2AA)=Sof(H2AA)=Sof(C3AA)=Sof(H3AA)=Sof(C4AA)=Sof(H4AA)=Sof(C5AA)=Sof(C25)=
 Sof(H25A)=Sof(H25B)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=Sof(C6AA)=1-FVAR(1)
 Sof(C19)=Sof(C23)=Sof(H23)=Sof(C20)=Sof(C24)=Sof(C21)=Sof(H21)=Sof(C22)=
 Sof(H22)=Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(C013)=Sof(H01A)=Sof(H01B)=Sof(C28)=
 Sof(H28A)=Sof(H28B)=Sof(H28C)=Sof(C0AA)=Sof(H0AA)=Sof(H0AB)=Sof(H0AC)=FVAR(1)
 Sof(C8AA)=Sof(C9AA)=Sof(H9AA)=Sof(C0BA)=Sof(C1BA)=Sof(H1BA)=Sof(H1BB)=
 Sof(C7AB)=Sof(H7AA)=Sof(H7AB)=Sof(H7AC)=Sof(C2BA)=Sof(H2BA)=Sof(C3BA)=
 Sof(H3BA)=Sof(C4BA)=Sof(C5BA)=Sof(H5BA)=Sof(H5BB)=Sof(C39)=Sof(H39A)=Sof(H39B)=
 Sof(H39C)=1-FVAR(2)
 Sof(C29)=Sof(C30)=Sof(C34)=Sof(C31)=Sof(H31)=Sof(C32)=Sof(H32)=Sof(C33)=
 Sof(H33)=Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(C38)=
 Sof(H38A)=Sof(H38B)=Sof(H38C)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H36C)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C35(H35A,H35B), C37(H37A,H37B), C27(H27A,H27B), C013(H01A,H01B), C0(H0A,H0B),
 C25(H25A,H25B), C1BA(H1BA,H1BB), C5BA(H5BA,H5BB)
6.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C9(H9), C4(H4), C23(H23), C6(H6), C31(H31), C32(H32), C33(H33),
 C5(H5), C14(H14), C21(H21), C18(H18), C22(H22), C17(H17), C16(H16), C15(H15),
 C2AA(H2AA), C3AA(H3AA), C4AA(H4AA), C9AA(H9AA), C2BA(H2BA), C3BA(H3BA)
6.c Idealised Me refined as rotating group:
 C38(H38A,H38B,H38C), C28(H28A,H28B,H28C), C0AA(H0AA,H0AB,H0AC), C13A(H13A,
 H13B,H13C), C26(H26A,H26B,H26C), C36(H36A,H36B,H36C), C7AB(H7AA,H7AB,H7AC),
 C39(H39A,H39B,H39C)
;
_shelx_res_checksum              12030
_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 2.151
_oxdiff_exptl_absorpt_empirical_full_min 0.674