Lewis acid-induced homo- and heterogeneous nickel catalysts for ethylene polymerization and copolymerization with polar monomers
Tian, Wanlu; Li, Chao; Tan, Chen; Chen, Min; Polymer Chemistry 15 (2024) 631–638; doi:10.1039/D3PY01266B

data_1570700
_publ_section_title
;
 Lewis acid-induced homo- and heterogeneous nickel catalysts for ethylene
 polymerization and copolymerization with polar monomers
;
_journal_issue                   7
_journal_name_full               'Polymer Chemistry'
_journal_page_first              631
_journal_page_last               638
_journal_paper_doi               10.1039/D3PY01266B
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C19 H26 N Ni O'
_chemical_formula_sum            'C19 H26 N Ni O'
_chemical_formula_weight         343.12
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-12-08
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2021.06.11 svn.re2ff6fc5 for OlexSys, GUI svn.r6348)
;
_audit_update_record
;
2023-09-18 deposited with the CCDC.	2024-01-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            32
_cell_length_a                   32.828(3)
_cell_length_b                   32.828(3)
_cell_length_c                   17.2912(17)
_cell_measurement_reflns_used    9996
_cell_measurement_temperature    170.00
_cell_measurement_theta_max      25.195
_cell_measurement_theta_min      2.203
_cell_volume                     18634(3)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      170.00
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0996
_diffrn_reflns_av_unetI/netI     0.0473
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            88307
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.022
_diffrn_reflns_theta_max         25.022
_diffrn_reflns_theta_min         2.528
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.834
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6437
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0815 before and 0.0576 after correction.
The Ratio of minimum to maximum transmission is 0.8636.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'metallic dark black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    0.978
_exptl_crystal_description       block
_exptl_crystal_F_000             5856
_refine_diff_density_max         0.734
_refine_diff_density_min         -0.582
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         8128
_refine_ls_number_restraints     270
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1118
_refine_ls_R_factor_gt           0.0761
_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^)+(0.0759P)^2^+96.4130P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1774
_refine_ls_wR_factor_ref         0.1992
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5351
_reflns_number_total             8128
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3py01266b2.cif
_cod_data_source_block           1
_cod_depositor_comments          'Adding full bibliography for 1570700.cif.'
_cod_original_cell_volume        18634(4)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               1570700
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C00K \\sim C00P \\sim C00L \\sim C00S \\sim C010 \\sim C011 \\sim C012 \\sim
C014 \\sim C015 \\sim C019 \\sim C01A \\sim C01C \\sim C01F \\sim C01I \\sim
C01K \\sim C01M \\sim C01N \\sim C01R \\sim C01S \\sim C01V \\sim C01W \\sim
C01Z \\sim C022 \\sim C023 \\sim C025 \\sim C027 \\sim C029 \\sim C02F \\sim
C02Q \\sim C7 \\sim C8 \\sim C14 \\sim C3 \\sim C2 \\sim C1 \\sim C6 \\sim C5
\\sim C4: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
C00K \\sim C00P \\sim C00L \\sim C00S \\sim C010 \\sim C011 \\sim C012 \\sim
C014 \\sim C015 \\sim C019 \\sim C01A \\sim C01C \\sim C01F \\sim C01I \\sim
C01K \\sim C01M \\sim C01N \\sim C01R \\sim C01S \\sim C01V \\sim C01W \\sim
C01Z \\sim C022 \\sim C023 \\sim C025 \\sim C027 \\sim C029 \\sim C02F \\sim
C02Q \\sim C7 \\sim C8 \\sim C14 \\sim C3 \\sim C2 \\sim C1 \\sim C6 \\sim C5
\\sim C4 \\sim C14A \\sim C01J: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
3. Rigid body (RIGU) restrains
 C7, C14, C8
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C14A, C8, C7
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C01I, C00K, C019
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Sof(H7BC)=Sof(H7BD)=Sof(H8B)=Sof(C14A)=Sof(H14A)=1-FVAR(1)
 Sof(H7AA)=Sof(H7AB)=Sof(H8A)=Sof(C14)=Sof(H14)=FVAR(1)
 Sof(H00C)=Sof(H00D)=Sof(H01D)=Sof(C01J)=Sof(H01M)=1-FVAR(2)
 Sof(H00A)=Sof(H00B)=Sof(H019)=Sof(C01I)=Sof(H01I)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C012(H012), C01I(H01I), C01V(H01V), C022(H022), C14(H14), C2(H2), C14A(H14A),
 C01J(H01M)
5.b Secondary CH2 refined with riding coordinates:
 C00K(H00A,H00B), C00K(H00C,H00D)
5.c Aromatic/amide H refined with riding coordinates:
 C019(H019), C019(H01D), C01F(H01F), C023(H023), C025(H025), C01Z(H01Z),
 C01W(H01W), C01S(H01S), C8(H8A), C8(H8B)
5.d Fitted hexagon refined as free rotating group:
 C01A(C01F,C023,C025,C01N,C010), C01Z(C01W,C01S,C01C,C011,C01R)
5.e X=CH2 refined with riding coordinates:
 C7(H7AA,H7AB), C7(H7BC,H7BD), C5(H5A,H5B), C4(H4A,H4B)
5.f Idealised Me refined as rotating group:
 C014(H01A,H01B,H01C), C015(H01N,H01O,H01P), C01K(H01E,H01G,H01H), C01M(H01J,
 H01K,H01L), C027(H02A,H02B,H02C), C029(H02D,H02E,H02F), C02F(H02G,H02H,H02I),
 C02Q(H02J,H02K,H02L), C1(H1A,H1B,H1C), C6(H6A,H6B,H6C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              84070
_shelx_fab_checksum              50130
_olex2_submission_special_instructions 'No special instructions were received'