2-[2,6-Bis(4,4′-difluorobenzhydryl)-4-methylphenylimino]-3-aryliminobutylnickel complex precatalysts tuning polyethylene elastomers with different molecular weights
Zhu, Dongzhi; Zhang, Qiuyue; Jia, Dedong; Ma, Yanping; Sun, Wen-Hua; RSC Advances 15 (2025) 28601–28612; doi:10.1039/D5RA04501K

data_7250790
_publ_section_title
;
 2-[2,6-Bis(4,4&#x2032;-difluorobenzhydryl)-4-methylphenylimino]-3-aryliminobutylnickel
 complex precatalysts tuning polyethylene elastomers with different
 molecular weights
;
_journal_issue                   35
_journal_name_full               'RSC Advances'
_journal_page_first              28601
_journal_page_last               28612
_journal_paper_doi               10.1039/D5RA04501K
_journal_volume                  15
_journal_year                    2025
_chemical_formula_moiety         'C45 H38 Br2 F4 N2 Ni'
_chemical_formula_sum            'C45 H38 Br2 F4 N2 Ni'
_chemical_formula_weight         901.30
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2025-01-16
_audit_creation_method
;
Olex2 1.5
(compiled 2021.07.19 svn.r715e62df for OlexSys, GUI svn.r6383)
;
_audit_update_record
;
2025-05-19 deposited with the CCDC.	2025-07-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 120.11(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.453(5)
_cell_length_b                   11.045(2)
_cell_length_c                   16.646(3)
_cell_measurement_reflns_used    4999
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      2.23
_cell_volume                     3889.2(17)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1017
_diffrn_reflns_av_unetI/netI     0.1031
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12876
_diffrn_reflns_point_group_measured_fraction_full 0.765
_diffrn_reflns_point_group_measured_fraction_max 0.742
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.459
_diffrn_reflns_theta_min         2.227
_exptl_absorpt_coefficient_mu    2.608
_exptl_absorpt_correction_T_max  .0000
_exptl_absorpt_correction_T_min  .0000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.202
_exptl_crystal_size_mid          0.122
_exptl_crystal_size_min          0.038
_refine_diff_density_max         0.973
_refine_diff_density_min         -0.822
_refine_diff_density_rms         0.107
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.011(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     492
_refine_ls_number_reflns         6602
_refine_ls_number_restraints     44
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0764
_refine_ls_R_factor_gt           0.0693
_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^)+(0.0696P)^2^+4.5384P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1636
_refine_ls_wR_factor_ref         0.1704
_reflns_Friedel_coverage         0.493
_reflns_Friedel_fraction_full    0.535
_reflns_Friedel_fraction_max     0.490
_reflns_number_gt                5947
_reflns_number_total             6602
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ra04501k2.cif
_cod_data_source_block           Ni1
_cod_original_cell_volume        3889.3(17)
_cod_database_code               7250790
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.907
_shelx_estimated_absorpt_t_min   0.621
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C21 \\sim C20 \\sim C1 \\sim C4 \\sim C11 \\sim C12 \\sim C13: within 1.7A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 1.7A
Uanis(C21) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C4)
\\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C12) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Ternary CH refined with riding coordinates:
 C12(H12), C13(H13)
3.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C36(H36), C7(H7), C30(H30), C44(H44), C41(H41), C38(H38), C29(H29),
 C45(H45), C39(H39), C35(H35), C33(H33), C23(H23), C16(H16), C27(H27), C32(H32),
  C42(H42), C24(H24), C18(H18), C17(H17), C26(H26)
3.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C20(H20A,H20B,H20C), C4(H4A,H4B,H4C), C11(H11A,H11B,H11C),
 C21(H21A,H21B,H21C)
;
_shelx_res_checksum              76103
_olex2_submission_special_instructions 'No special instructions were received'