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_7250831
_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         'C46 H42 Br2 N2 Ni'
_chemical_formula_sum            'C46 H42 Br2 N2 Ni'
_chemical_formula_weight         841.34
_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             2025-01-14
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2025-06-23 deposited with the CCDC.	2025-08-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.4590(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.37370(10)
_cell_length_b                   25.5882(3)
_cell_length_c                   15.62100(10)
_cell_measurement_reflns_used    19046
_cell_measurement_temperature    170.2(5)
_cell_measurement_theta_max      75.1500
_cell_measurement_theta_min      2.7490
_cell_volume                     3743.34(6)
_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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      170.2(5)
_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 0.959
_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     41.00 102.00   0.50    0.05    --   42.87-135.00 168.00  122
  2  \w     34.00 115.00   0.50    0.05    --  108.44-135.00 168.00  162
  3  \w     35.00 100.00   0.50    0.05    --  108.44 -94.00 -30.00  130
  4  \w     77.00 108.00   0.50    0.05    --  108.44-125.00-150.00   62
  5  \w     46.00  72.00   0.50    0.05    --  108.44 -61.00 120.00   52
  6  \w     93.00 174.00   0.50    0.05    --  108.44 134.00  54.00  162
  7  \w    -99.00 -74.00   0.50    0.05    -- -104.50 134.00  54.00   50
  8  \w   -127.00 -95.00   0.50    0.05    -- -104.50 146.00  11.63   64
  9  \w   -119.00 -92.00   0.50    0.05    -- -104.50 135.00-125.00   54
 10  \w    -59.00 -27.00   0.50    0.05    --  -42.87 135.00-125.00   64
 11  \w    -83.00 -58.00   0.50    0.05    --  -42.87 134.00  54.00   50
 12  \w   -101.00 -31.00   0.50    0.05    -- -104.50  77.00  60.00  140
 13  \w    -68.00 -36.00   0.50    0.05    -- -104.50  61.00   0.00   64
 14  \w      2.00  37.00   0.50    0.05    --  -42.87  19.00  30.00   70
 15  \w    -22.00  36.00   0.50    0.05    --  -42.87  19.00-180.00  116
 16  \w    -68.00 -40.00   0.50    0.05    -- -104.50  61.00-150.00   56
 17  \w   -106.00 -81.00   0.50    0.05    -- -104.50 -37.00-127.84   50
 18  \w   -116.00 -20.00   0.50    0.05    --  -42.87 -57.00-120.00  192
 19  \w   -124.00 -79.00   0.50    0.05    -- -104.50 -70.00-103.02   90
 20  \w   -174.00-138.00   0.50    0.05    -- -104.50 -70.00-103.02   72
 21  \w   -162.00-123.00   0.50    0.05    -- -104.50 -37.00-127.84   78
 22  \w   -174.00 -82.00   0.50    0.05    -- -104.50 -40.00 -19.11  184
 23  \w   -173.00 -81.00   0.50    0.05    -- -104.50 -44.00  69.07  184
 24  \w   -110.00 -84.00   0.50    0.05    --  -42.87-135.00 168.00   52
 25  \w   -145.00-120.00   0.50    0.05    -- -104.50-135.00 168.00   50
 26  \w   -121.00 -93.00   0.50    0.05    -- -104.50-134.00 -12.00   56
 27  \w   -103.00 -75.00   0.50    0.05    --  -42.87-134.00 -12.00   56
;
_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      0.0559300000
_diffrn_orient_matrix_UB_12      -0.0563596000
_diffrn_orient_matrix_UB_13      0.0106480000
_diffrn_orient_matrix_UB_21      -0.1479560000
_diffrn_orient_matrix_UB_22      -0.0212014000
_diffrn_orient_matrix_UB_23      -0.0292244000
_diffrn_orient_matrix_UB_31      0.0449801000
_diffrn_orient_matrix_UB_32      0.0002898000
_diffrn_orient_matrix_UB_33      -0.0937034000
_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  0.0539
_diffrn_reflns_av_unetI/netI     0.0392
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.959
_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       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            26446
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.277
_diffrn_reflns_theta_min         3.317
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.512
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.20821
_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    1.493
_exptl_crystal_description       block
_exptl_crystal_F_000             1720
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.846
_refine_diff_density_min         -0.756
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.858
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     473
_refine_ls_number_reflns         7431
_refine_ls_number_restraints     456
_refine_ls_restrained_S_all      0.832
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0414
_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^)+(0.0780P)^2^+4.7534P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1099
_refine_ls_wR_factor_ref         0.1126
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6715
_reflns_number_total             7431
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ra05407a2.cif
_cod_data_source_block           tx17146_auto
_cod_database_code               7250831
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         CHNNiBr
_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. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.04 and sigma for 1-3 distances of 0.04
3. Others
 Sof(Br2A)=1-FVAR(1)
 Sof(Br2)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C4(H4), C25(H25), C43(H43)
4.b Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C11(H11A,H11B), C33(H33A,H33B), C32(H32A,H32B)
4.c Aromatic/amide H refined with riding coordinates:
 C24(H24), C22(H22), C6(H6), C17(H17), C7(H7), C38(H38), C35(H35), C14(H14),
 C9(H9), C8(H8), C48(H48), C16(H16), C51(H51), C36(H36), C37(H37), C15(H15),
 C27(H27), C49(H49), C50(H50), C29(H29), C28(H28), C30(H30)
4.d Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C), C45(H45A,H45B,H45C), C44(H44A,H44B,H44C)
;
_shelx_res_checksum              44447
_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 3.254
_oxdiff_exptl_absorpt_empirical_full_min 0.308