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_1571186
_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         'C88 H76 Br2 N2 Ni'
_chemical_formula_sum            'C88 H76 Br2 N2 Ni'
_chemical_formula_weight         1380.03
_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     dual
_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                 109.5382(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.2367(2)
_cell_length_b                   17.34528(14)
_cell_length_c                   20.7624(2)
_cell_measurement_reflns_used    31392
_cell_measurement_temperature    169.99(10)
_cell_measurement_theta_max      75.0680
_cell_measurement_theta_min      2.1950
_cell_volume                     7207.59(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 1.5 (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    'SHELXT 2018/2 (Sheldrick, 2018)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.971
_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     36.00 121.00   0.50    0.13    --   47.20  31.00 -25.00  170
  2  \w     90.00 141.00   0.50    0.53    --  103.25  61.00  60.00  102
  3  \w    144.00 172.00   0.50    0.53    --  103.25  61.00  60.00   56
  4  \w    134.00 176.00   0.50    0.53    --  103.25  61.00  30.00   84
  5  \w     91.00 177.00   0.50    0.53    --  103.25  31.00 -25.00  172
  6  \w     95.00 125.00   0.50    0.53    --  103.25  61.00  30.00   60
  7  \w    -20.00  19.00   0.50    0.13    --   47.20 -19.00  30.00   78
  8  \w     35.00  74.00   0.50    0.53    --  103.25 -61.00   0.00   78
  9  \w     48.00  75.00   0.50    0.53    --  103.25 -61.00  30.00   54
 10  \w     31.00  56.00   0.50    0.53    --  103.25 -61.00  60.00   50
 11  \w     33.00  73.00   0.50    0.53    --  103.25 -61.00 -30.00   80
 12  \w     31.00  73.00   0.50    0.53    --  103.25 -61.00-180.00   84
 13  \w     35.00  69.00   0.50    0.53    --  103.25 -61.00-150.00   68
 14  \w     31.00 108.00   0.50    0.53    --  103.25 -77.00 -90.00  154
 15  \w     -3.00  26.00   0.50    0.13    --   47.20 -31.00 174.00   58
 16  \w    -28.00   8.00   0.50    0.13    --  -47.20  31.00 -25.00   72
 17  \w    -62.00 -36.00   0.50    0.53    -- -104.50  61.00-120.00   52
 18  \w    -65.00 -40.00   0.50    0.53    -- -104.50  61.00-150.00   50
 19  \w    -99.00 -51.00   0.50    0.53    -- -104.50  77.00 -90.00   96
 20  \w    -63.00 -37.00   0.50    0.53    -- -104.50  61.00  30.00   52
 21  \w    -39.00  25.00   0.50    0.13    --  -47.20  38.00 120.00  128
 22  \w    -68.00 -42.00   0.50    0.53    -- -104.50  61.00 150.00   52
 23  \w    -90.00 -33.00   0.50    0.53    -- -104.50 125.00  60.00  114
 24  \w    -57.00 -32.00   0.50    0.53    -- -104.50 125.00  90.00   50
 25  \w   -111.00 -75.00   0.50    0.53    -- -104.50 125.00  90.00   72
 26  \w   -114.00 -35.00   0.50    0.13    --  -47.20 -31.00 174.00  158
 27  \w   -138.00-111.00   0.50    0.53    -- -104.50 -31.00 174.00   54
 28  \w   -115.00 -90.00   0.50    0.13    --  -47.20-125.00 -60.00   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      0.0077926000
_diffrn_orient_matrix_UB_12      0.0092252000
_diffrn_orient_matrix_UB_13      0.0761074000
_diffrn_orient_matrix_UB_21      0.0706404000
_diffrn_orient_matrix_UB_22      0.0331493000
_diffrn_orient_matrix_UB_23      0.0142502000
_diffrn_orient_matrix_UB_31      -0.0296873000
_diffrn_orient_matrix_UB_32      0.0817738000
_diffrn_orient_matrix_UB_33      -0.0144457000
_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  0.0315
_diffrn_reflns_av_unetI/netI     0.0268
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            56887
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.554
_diffrn_reflns_theta_min         2.208
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.035
_exptl_absorpt_correction_T_max  0.903
_exptl_absorpt_correction_T_min  0.728
_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    1.272
_exptl_crystal_description       block
_exptl_crystal_F_000             2864
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.544
_refine_diff_density_min         -1.164
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     838
_refine_ls_number_reflns         14533
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0545
_refine_ls_R_factor_gt           0.0505
_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^)+(0.0813P)^2^+12.4398P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1491
_refine_ls_wR_factor_ref         0.1521
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13122
_reflns_number_total             14961
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4py00061g2.cif
_cod_data_source_block           tx11383_auto
_cod_depositor_comments
'Adding full bibliography for 1571184--1571186.cif.'
_cod_original_cell_volume        7207.58(13)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1571186
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N'
_shelx_estimated_absorpt_t_max   0.905
_shelx_estimated_absorpt_t_min   0.686
_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:
 C35(H35), C22(H22), C48(H48), C60(H60), C73(H73), C86(H86)
2.b Secondary CH2 refined with riding coordinates:
 C49(H49A,H49B), C87(H87A,H87B), C53(H53A,H53B), C52(H52A,H52B), C50(H50A,
 H50B), C51(H51A,H51B), C90(H90A,H90B), C91(H91A,H91B), C88(H88A,H88B),
 C89(H89A,H89B)
2.c Aromatic/amide H refined with riding coordinates:
 C19(H19), C17(H17), C57(H57), C66(H66), C28(H28), C10(H10), C55(H55),
 C47(H47), C24(H24), C37(H37), C30(H30), C27(H27), C62(H62), C65(H65), C14(H14),
  C34(H34), C68(H68), C25(H25), C43(H43), C9(H9), C41(H41), C46(H46), C63(H63),
 C79(H79), C8(H8), C26(H26), C75(H75), C64(H64), C71(H71), C33(H33), C72(H72),
 C85(H85), C5(H5), C69(H69), C32(H32), C45(H45), C40(H40), C39(H39), C6(H6),
 C70(H70), C78(H78), C84(H84), C31(H31), C77(H77), C44(H44), C38(H38), C81(H81),
  C76(H76), C83(H83), C82(H82)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 152 electrons were 
found in a volume of 736\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1.25[CH2Cl2] per Unit Cell 
which account for 210 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              82301
_shelx_hkl_checksum              79870
_shelx_fab_checksum              35123
_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 1.409
_oxdiff_exptl_absorpt_empirical_full_min 0.811