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_1570475
_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         'C47 H44 Cl N2 Pd'
_chemical_formula_sum            'C47 H44 Cl N2 Pd'
_chemical_formula_weight         778.69
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-05-20
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-05-29 deposited with the CCDC.	2023-11-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.6140(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.1884(5)
_cell_length_b                   10.6212(3)
_cell_length_c                   20.1144(5)
_cell_measurement_reflns_used    9491
_cell_measurement_temperature    170
_cell_measurement_theta_max      26.354
_cell_measurement_theta_min      2.600
_cell_volume                     3907.20(18)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      170
_diffrn_measured_fraction_theta_full 0.993
_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  0.0602
_diffrn_reflns_av_unetI/netI     0.0478
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            37208
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.413
_diffrn_reflns_theta_min         2.125
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.578
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5184
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1367 before and 0.0656 after correction.
The Ratio of minimum to maximum transmission is 0.6955.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_description       block
_exptl_crystal_F_000             1612
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.271
_refine_diff_density_min         -0.886
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         7963
_refine_ls_number_restraints     485
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0662
_refine_ls_R_factor_gt           0.0596
_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^)+(0.0890P)^2^+8.9186P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1702
_refine_ls_wR_factor_ref         0.1758
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7087
_reflns_number_total             7963
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3py01011b2.cif
_cod_data_source_block           lpd2_0m
_cod_depositor_comments
'Adding full bibliography for 1570475--1570477.cif.'
_cod_database_code               1570475
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.977
_shelx_estimated_absorpt_t_min   0.939
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H48A,H48B} of C48, {H46A,H46B} of C46
 At 1.5 times of:
  All C(H,H,H) groups, {H39A,H39B} of C39
2. Restrained distances
 Pd1-C50 = Pd1-C51
 2.1 with sigma of 0.02
 Pd1-Cl1 \\sim Pd1-Cl00
 with sigma of 0.02
3. 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
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. 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 within 2A
All non-hydrogen atoms have similar U: within 2A with sigma of 0.005 and sigma
for terminal atoms of 0.01 within 2A
Uanis(C51) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
5. Others
 Fixed Sof: Cl00(0.5) Cl1(0.5) C51(0.5) H51A(0.5) H51B(0.5) H51C(0.5) C50(0.5)
 H50A(0.5) H50B(0.5) H50C(0.5)
6.a Ternary CH refined with riding coordinates:
 C21(H21), C1(H1)
6.b Secondary CH2 refined with riding coordinates:
 C46(H46A,H46B)
6.c Aromatic/amide H refined with riding coordinates:
 C15(H15), C18(H18), C7(H7), C3(H3), C9(H9), C11(H11), C23(H23), C27(H27),
 C10(H10), C6(H6), C29(H29), C25(H25), C26(H26), C24(H24), C5(H5), C4(H4),
 C13(H13), C38(H38), C12(H12), C30(H30), C31(H31), C41(H41), C32(H32), C44(H44),
  C43(H43), C42(H42), C47(H47)
6.d X=CH2 refined with riding coordinates:
 C48(H48A,H48B)
6.e Idealised Me refined as rotating group:
 C35(H35A,H35B,H35C), C17(H17A,H17B,H17C), C51(H51A,H51B,H51C), C50(H50A,H50B,
 H50C)
;
_olex2_submission_special_instructions 'No special instructions were received'