Ligand pre-inserted α-diimine palladium catalysts and mechanism studies in olefin polymerization
Liu, Yue; Yang, Gang; Li, Chao; Tan, Chen; Chen, Min; Polymer Chemistry 15 (2024) 40–45; doi:10.1039/D3PY01011B

data_1570477
_publ_section_title
;
 Ligand pre-inserted \a-diimine palladium catalysts and mechanism studies
 in olefin polymerization
;
_journal_issue                   1
_journal_name_full               'Polymer Chemistry'
_journal_page_first              40
_journal_page_last               45
_journal_paper_doi               10.1039/D3PY01011B
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C49 H48 N3 Pd, C32 H12 B F24'
_chemical_formula_sum            'C81 H60 B F24 N3 Pd'
_chemical_formula_weight         1648.53
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-05-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-05-29 deposited with the CCDC.	2023-11-29 downloaded from the CCDC.
;
_cell_angle_alpha                100.5850(10)
_cell_angle_beta                 95.0430(10)
_cell_angle_gamma                104.5800(10)
_cell_formula_units_Z            2
_cell_length_a                   10.0340(3)
_cell_length_b                   19.1514(7)
_cell_length_c                   20.3631(6)
_cell_measurement_reflns_used    9080
_cell_measurement_temperature    150
_cell_measurement_theta_max      26.367
_cell_measurement_theta_min      2.321
_cell_volume                     3685.4(2)
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.993
_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  0.0508
_diffrn_reflns_av_unetI/netI     0.0592
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            43578
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.381
_diffrn_reflns_theta_min         2.118
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.360
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5480
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1046 before and 0.0625 after correction. The Ratio of minimum to maximum transmission is 0.7352. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.486
_exptl_crystal_description       block
_exptl_crystal_F_000             1668
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.917
_refine_diff_density_min         -1.096
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1023
_refine_ls_number_reflns         14994
_refine_ls_number_restraints     1116
_refine_ls_restrained_S_all      1.225
_refine_ls_R_factor_all          0.0679
_refine_ls_R_factor_gt           0.0553
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0621P)^2^+5.8445P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1375
_refine_ls_wR_factor_ref         0.1478
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12599
_reflns_number_total             14994
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3py01011b2.cif
_cod_data_source_block           52lypd2cn_0m
_cod_depositor_comments
'Adding full bibliography for 1570475--1570477.cif.'
_cod_database_code               1570477
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.989
_shelx_estimated_absorpt_t_min   0.948
_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 bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F15, C72
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
C72 \\sim F15: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.01
Uanis(F2) \\sim Ueq, Uanis(F15) \\sim Ueq, Uanis(F13) \\sim Ueq, Uanis(F25)
\\sim Ueq, Uanis(F26) \\sim Ueq, Uanis(F27) \\sim Ueq, Uanis(F24) \\sim Ueq,
Uanis(F23) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Others
 Fixed Sof: F26(0.75) F28(0.75) F24(0.75) F23(0.25) F27(0.25) F25(0.25)
5.a Ternary CH refined with riding coordinates:
 C7(H7), C45(H45), C21(H21)
5.b Secondary CH2 refined with riding coordinates:
 C44(H44A,H44B), C46(H46A,H46B)
5.c Aromatic/amide H refined with riding coordinates:
 C17(H17), C55(H55), C19(H19), C63(H63), C59(H59), C29(H29), C80(H80),
 C67(H67), C71(H71), C53(H53), C39(H39), C51(H51), C2(H2), C6(H6), C61(H61),
 C69(H69), C75(H75), C30(H30), C33(H33), C27(H27), C41(H41), C42(H42), C32(H32),
  C3(H3), C4(H4), C31(H31), C23(H23), C78(H78), C5(H5), C40(H40), C13(H13),
 C11(H11), C26(H26), C24(H24), C12(H12), C9(H9), C25(H25), C10(H10)
5.d Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C34(H34A,H34B,H34C), C37(H37A,H37B,H37C), C49(H49A,H49B,
 H49C), C47(H47A,H47B,H47C)
;
_olex2_submission_special_instructions 'No special instructions were received'