Lewis acid modulation in phosphorus phenol nickel catalyzed ethylene polymerization and copolymerization
Wang, Wenbing; Nie, Nan; Xu, Menghe; Zou, Chen; Polymer Chemistry 14 (2023) 4933–4939; doi:10.1039/D3PY00925D

data_1570513
_publ_section_title
;
 Lewis acid modulation in phosphorus phenol nickel catalyzed ethylene
 polymerization and copolymerization
;
_journal_issue                   43
_journal_name_full               'Polymer Chemistry'
_journal_page_first              4933
_journal_page_last               4939
_journal_paper_doi               10.1039/D3PY00925D
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C30 H35 N2 Ni O P'
_chemical_formula_sum            'C30 H35 N2 Ni O P'
_chemical_formula_weight         529.28
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-03-15
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-04-20 deposited with the CCDC.	2023-10-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.6966(6)
_cell_length_b                   15.9160(12)
_cell_length_c                   19.1276(19)
_cell_measurement_reflns_used    1908
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.874
_cell_measurement_theta_min      2.485
_cell_volume                     2647.5(4)
_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 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'D8 VENTURE'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0826
_diffrn_reflns_av_unetI/netI     0.1291
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            11685
_diffrn_reflns_point_group_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.380
_diffrn_reflns_theta_min         2.485
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.819
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6556
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1098 before and 0.0702 after correction.
The Ratio of minimum to maximum transmission is 0.8795.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_description       block
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.429
_refine_diff_density_min         -0.439
_refine_diff_density_rms         0.097
_refine_ls_abs_structure_details
;
 Flack x determined using 1085 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         5167
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0973
_refine_ls_R_factor_gt           0.0572
_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^)+(0.0212P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0925
_refine_ls_wR_factor_ref         0.1121
_reflns_Friedel_coverage         0.714
_reflns_Friedel_fraction_full    0.934
_reflns_Friedel_fraction_max     0.917
_reflns_number_gt                3723
_reflns_number_total             5167
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3py00925d2.cif
_cod_data_source_block           315154ni_0m
_cod_database_code               1570513
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.960
_shelx_estimated_absorpt_t_min   0.860
_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.a Aromatic/amide H refined with riding coordinates:
 C16(H16), C17(H17), C18(H18), C7(H7), C14(H14), C4(H4), C26(H26), C11(H11),
 C13(H13), C10(H10), C27(H27), C6(H6), C5(H5), C12(H12), C25(H25), C28(H28),
 C29(H29)
2.b Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C22(H22A,H22B,H22C),
 C24(H24A,H24B,H24C), C23(H23A,H23B,H23C)
;
_olex2_submission_special_instructions 'No special instructions were received'