High molecular weight polyethylene via the spatial proximity of benzosuberyl in iminopyridine nickel catalysts
Khalid, Areej; Mahmood, Qaiser; Razzaq, Ayesha; Ma, Yanping; Ren, Geng; Wang, Yizhou; Liang, Tongling; Sun, Wen-Hua; RSC Advances 15 (2025) 31597–31608; doi:10.1039/D5RA05407A

data_7250832
_publ_section_title
;
 High molecular weight polyethylene via the spatial proximity of
 benzosuberyl in iminopyridine nickel catalysts
;
_journal_issue                   38
_journal_name_full               'RSC Advances'
_journal_page_first              31597
_journal_page_last               31608
_journal_paper_doi               10.1039/D5RA05407A
_journal_volume                  15
_journal_year                    2025
_chemical_formula_moiety         'C44 H38 Br2 N2 Ni'
_chemical_formula_sum            'C44 H38 Br2 N2 Ni'
_chemical_formula_weight         813.29
_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     iterative
_audit_creation_date             2025-01-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2025-06-23 deposited with the CCDC.	2025-08-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.533(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.2626(2)
_cell_length_b                   25.2521(4)
_cell_length_c                   15.1940(2)
_cell_measurement_reflns_used    13079
_cell_measurement_temperature    170.0(4)
_cell_measurement_theta_max      75.1400
_cell_measurement_theta_min      3.4900
_cell_volume                     3537.32(11)
_computing_cell_refinement       'CrysAlisPro 1.171.42.96a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.96a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.96a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      170.0(4)
_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 0.963
_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  36.00   0.50    0.05    --  -42.87  19.00-120.00   56
  2  \w    -58.00 -30.00   0.50    0.06    -- -104.50  61.00-150.00   56
  3  \w    -68.00 -40.00   0.50    0.06    -- -104.50  61.00 -60.00   56
  4  \w    -62.00 -37.00   0.50    0.06    -- -104.50  61.00   0.00   50
  5  \w    -85.00  -2.00   0.50    0.05    --  -42.87 110.00 135.00  166
  6  \w   -106.00 -67.00   0.50    0.06    -- -104.50 110.00 135.00   78
  7  \w   -163.00 -89.00   0.50    0.06    -- -104.50 -30.00 -60.00  148
  8  \w   -115.00 -90.00   0.50    0.06    -- -104.50-110.00  39.00   50
  9  \w     36.00 105.00   0.50    0.06    --  108.44 -94.00  60.00  138
 10  \w     68.00 107.00   0.50    0.06    --  108.44-110.00  39.00   78
 11  \w     37.00  76.00   0.50    0.06    --  108.44-125.00 -30.00   78
 12  \w     46.00 111.00   0.50    0.06    --  108.44-125.00 -90.00  130
 13  \w     45.00  75.00   0.50    0.05    --   42.87-110.00  39.00   60
 14  \w     11.00  37.00   0.50    0.05    --   42.87-110.00  39.00   52
 15  \w    -22.00  19.00   0.50    0.05    --   42.87 -38.00 -90.00   82
 16  \w     37.00  63.00   0.50    0.06    --  108.44 -61.00-120.00   52
 17  \w     47.00  73.00   0.50    0.06    --  108.44 -61.00 -90.00   52
 18  \w     38.00  75.00   0.50    0.06    --  108.44 -61.00  30.00   74
 19  \w     35.00  73.00   0.50    0.06    --  108.44 -61.00 120.00   76
 20  \w    -34.00  46.00   0.50    0.05    --   42.87 -38.00 -60.00  160
 21  \w     63.00 120.00   0.50    0.05    --   42.87  38.00-120.00  114
 22  \w     31.00  56.00   0.50    0.05    --   42.87  38.00-120.00   50
 23  \w    105.00 159.00   0.50    0.06    --  108.44 125.00 -90.00  108
 24  \w     81.00 178.00   0.50    0.06    --  108.44  77.00  90.00  194
 25  \w     88.00 162.00   0.50    0.06    --  108.44 110.00 135.00  148
;
_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      0.1282349000
_diffrn_orient_matrix_UB_12      0.0032262000
_diffrn_orient_matrix_UB_13      0.0723490000
_diffrn_orient_matrix_UB_21      -0.0304124000
_diffrn_orient_matrix_UB_22      0.0594195000
_diffrn_orient_matrix_UB_23      0.0122108000
_diffrn_orient_matrix_UB_31      -0.1026682000
_diffrn_orient_matrix_UB_32      -0.0135189000
_diffrn_orient_matrix_UB_33      0.0706677000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0720
_diffrn_reflns_av_unetI/netI     0.0562
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            22743
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.731
_diffrn_reflns_theta_min         3.406
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.696
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.35201
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.96a (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    1.527
_exptl_crystal_description       block
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.941
_refine_diff_density_min         -1.454
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     444
_refine_ls_number_reflns         7098
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0573
_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^)+(0.0974P)^2^+2.3731P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1615
_refine_ls_wR_factor_ref         0.1713
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5702
_reflns_number_total             7098
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ra05407a2.cif
_cod_data_source_block           tx17147_auto_sq
_cod_database_code               7250832
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHNNiBr
_shelx_estimated_absorpt_t_max   0.556
_shelx_estimated_absorpt_t_min   0.384
_diffrn_oxdiff_digest_frames
;
015823ca2a48f7444aecc63c9c0f5dc38a023060414
;
_diffrn_oxdiff_digest_hkl
;
01e027d03a9fd64de670d00b99b0fad1d0ea90
;
_reflns_odcompleteness_completeness 99.88
_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:
 C4(H4), C25(H25)
2.b Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C11(H11A,H11B), C33(H33A,H33B), C32(H32A,H32B)
2.c Aromatic/amide H refined with riding coordinates:
 C24(H24), C22(H22), C17(H17), C14(H14), C6(H6), C16(H16), C9(H9), C46(H46),
 C7(H7), C38(H38), C15(H15), C8(H8), C49(H49), C47(H47), C48(H48), C37(H37),
 C35(H35), C36(H36), C27(H27), C30(H30), C29(H29), C28(H28)
2.d Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C), C43(H43A,H43B,H43C)
;
_shelx_res_checksum              90733
_shelx_fab_checksum              20505
_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 2.736
_oxdiff_exptl_absorpt_empirical_full_min 0.220