High-performance polyethylene elastomers using a hybrid steric approach in α-diimine nickel precatalysts
Saeed, Hassan; Mahmood, Qaiser; Yuan, Rongyan; Wang, Yizhou; Zou, Song; Tahir, Kainat Fatima; Ma, Yanping; Liang, Tongling; Sun, Wen-Hua; Polymer Chemistry 15 (2024) 1437–1452; doi:10.1039/D4PY00061G

data_1571184
_publ_section_title
;
 High-performance polyethylene elastomers using a hybrid steric approach
 in \a-diimine nickel precatalysts
;
_journal_issue                   14
_journal_name_full               'Polymer Chemistry'
_journal_page_first              1437
_journal_page_last               1452
_journal_paper_doi               10.1039/D4PY00061G
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C86 H72 Br2 N2 Ni'
_chemical_formula_sum            'C86 H72 Br2 N2 Ni'
_chemical_formula_weight         1351.98
_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     direct
_audit_creation_date             2024-01-18
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-01-18 deposited with the CCDC.	2024-03-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.0777(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.98915(15)
_cell_length_b                   17.36611(9)
_cell_length_c                   20.56133(13)
_cell_measurement_reflns_used    58673
_cell_measurement_temperature    169.99(10)
_cell_measurement_theta_max      75.4560
_cell_measurement_theta_min      2.2230
_cell_volume                     7039.14(8)
_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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_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 0.988
_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     90.00 157.00   0.50    0.33    --  103.25  61.00 150.00  134
  2  \w     87.00 144.00   0.50    0.33    --  103.25  61.00  90.00  114
  3  \w    117.00 178.00   0.50    0.33    --  103.25  15.00 -60.00  122
  4  \w     91.00 178.00   0.50    0.33    --  103.25  30.00-120.00  174
  5  \w    -11.00  27.00   0.50    0.08    --  -47.20  19.00   0.00   76
  6  \w    -23.00  27.00   0.50    0.08    --  -47.20  19.00 -90.00  100
  7  \w    -23.00  27.00   0.50    0.08    --  -47.20  19.00-150.00  100
  8  \w    -26.00  29.00   0.50    0.08    --   47.20 -19.00 -60.00  110
  9  \w     40.00  75.00   0.50    0.33    --  103.25 -61.00-120.00   70
 10  \w    -25.00  29.00   0.50    0.08    --   47.20 -19.00  60.00  108
 11  \w     36.00  90.00   0.50    0.33    --  103.25 -94.00   0.00  108
 12  \w     76.00 112.00   0.50    0.08    --   47.20-160.00  63.00   72
 13  \w     86.00 123.00   0.50    0.33    --  103.25-160.00  63.00   74
 14  \w     43.00 100.00   0.50    0.33    --  103.25 -94.00  60.00  114
 15  \w     31.00 103.00   0.50    0.33    --  103.25 -94.00  30.00  144
 16  \w     40.00  77.00   0.50    0.33    --  103.25 -94.00 -90.00   74
 17  \w     32.00 105.00   0.50    0.33    --  103.25-118.00-143.00  146
 18  \w     29.00  55.00   0.50    0.08    --   47.20-118.00-143.00   52
 19  \w     58.00  93.00   0.50    0.08    --   47.20 160.00  94.00   70
 20  \w     83.00 108.00   0.50    0.33    --  103.25 160.00  94.00   50
 21  \w     85.00 116.00   0.50    0.33    --  103.25 118.00 -57.00   62
 22  \w    -62.00 -33.00   0.50    0.33    -- -104.50  77.00 150.00   58
 23  \w    -99.00 -67.00   0.50    0.33    -- -104.50  77.00 150.00   64
 24  \w    -60.00 -35.00   0.50    0.33    -- -104.50  61.00 150.00   50
 25  \w    -67.00 -33.00   0.50    0.33    -- -104.50  61.00  60.00   68
 26  \w    -68.00 -32.00   0.50    0.33    -- -104.50  61.00 -60.00   72
 27  \w    -64.00 -33.00   0.50    0.33    -- -104.50  61.00 -90.00   62
 28  \w   -108.00 -34.00   0.50    0.33    -- -104.50 112.00 -72.41  148
 29  \w    -64.00 -38.00   0.50    0.33    -- -104.50 142.00   8.10   52
 30  \w   -122.00 -33.00   0.50    0.33    -- -104.50 141.00  83.07  178
 31  \w   -122.00 -79.00   0.50    0.33    -- -104.50 160.00  94.00   86
 32  \w    -98.00 -73.00   0.50    0.08    --  -47.20 160.00  94.00   50
 33  \w   -124.00 -98.00   0.50    0.33    -- -104.50 142.00   8.10   52
 34  \w   -109.00 -32.00   0.50    0.33    -- -104.50 118.00 -57.00  154
 35  \w   -107.00 -32.00   0.50    0.33    -- -104.50 125.00-180.00  150
 36  \w   -109.00 -64.00   0.50    0.33    -- -104.50 117.00-147.26   90
 37  \w    -91.00 -34.00   0.50    0.08    --  -47.20 118.00 -57.00  114
 38  \w   -174.00 -91.00   0.50    0.33    -- -104.50 -15.00  30.00  166
 39  \w   -174.00-135.00   0.50    0.33    -- -104.50 -64.00  68.73   78
 40  \w   -112.00 -87.00   0.50    0.33    -- -104.50 -64.00  68.73   50
 41  \w   -119.00 -25.00   0.50    0.08    --  -47.20 -77.00 -60.00  188
 42  \w   -173.00-104.00   0.50    0.33    -- -104.50 -81.00 -30.90  138
 43  \w   -118.00 -56.00   0.50    0.08    --  -47.20-160.00  63.00  124
 44  \w   -128.00-103.00   0.50    0.33    -- -104.50-160.00  63.00   50
 45  \w   -119.00 -78.00   0.50    0.08    --  -47.20-125.00 -90.00   82
 46  \w   -126.00 -92.00   0.50    0.33    -- -104.50-118.00-143.00   68
;
_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      -0.0145804000
_diffrn_orient_matrix_UB_12      -0.0417064000
_diffrn_orient_matrix_UB_13      -0.0697511000
_diffrn_orient_matrix_UB_21      -0.0761035000
_diffrn_orient_matrix_UB_22      -0.0023377000
_diffrn_orient_matrix_UB_23      -0.0097870000
_diffrn_orient_matrix_UB_31      -0.0100716000
_diffrn_orient_matrix_UB_32      0.0782390000
_diffrn_orient_matrix_UB_33      -0.0374963000
_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  0.0364
_diffrn_reflns_av_unetI/netI     0.0214
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            106589
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.759
_diffrn_reflns_theta_min         2.241
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.073
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82130
_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_density_diffrn    1.276
_exptl_crystal_description       block
_exptl_crystal_F_000             2800
_refine_diff_density_max         0.743
_refine_diff_density_min         -1.695
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.175
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     820
_refine_ls_number_reflns         14459
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.175
_refine_ls_R_factor_all          0.0604
_refine_ls_R_factor_gt           0.0578
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2423
_refine_ls_wR_factor_ref         0.2479
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13307
_reflns_number_total             14633
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4py00061g2.cif
_cod_data_source_block           tx11828c_auto
_cod_depositor_comments
'Adding full bibliography for 1571184--1571186.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1571184
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N'
_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:
 C85(H85), C35(H35), C59(H59), C22(H22), C48(H48), C72(H72)
2.b Secondary CH2 refined with riding coordinates:
 C89(H89A,H89B), C52(H52A,H52B), C86(H86A,H86B), C49(H49A,H49B), C51(H51A,
 H51B), C50(H50A,H50B), C88(H88A,H88B), C87(H87A,H87B)
2.c Aromatic/amide H refined with riding coordinates:
 C58(H58), C21(H21), C56(H56), C19(H19), C14(H14), C61(H61), C24(H24),
 C34(H34), C65(H65), C10(H10), C64(H64), C28(H28), C71(H71), C84(H84), C8(H8),
 C5(H5), C9(H9), C41(H41), C33(H33), C30(H30), C47(H47), C37(H37), C63(H63),
 C67(H67), C32(H32), C40(H40), C80(H80), C6(H6), C62(H62), C27(H27), C83(H83),
 C70(H70), C31(H31), C78(H78), C25(H25), C69(H69), C26(H26), C81(H81), C39(H39),
  C46(H46), C68(H68), C82(H82), C43(H43), C74(H74), C77(H77), C76(H76),
 C38(H38), C45(H45), C75(H75), C44(H44)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              25959
_shelx_hkl_checksum              38272
_shelx_fab_checksum              22636
_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 2.013
_oxdiff_exptl_absorpt_empirical_full_min 0.616