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_1570476
_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_absolute_configuration S
_chemical_formula_moiety         'C26 H35 Cl N2 Pd'
_chemical_formula_sum            'C26 H35 Cl N2 Pd'
_chemical_formula_weight         517.41
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-05-05
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2021.06.11 svn.re2ff6fc5 for OlexSys, GUI svn.r6348)
;
_audit_update_record
;
2023-05-29 deposited with the CCDC.	2023-11-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.91(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.119(3)
_cell_length_b                   15.120(3)
_cell_length_c                   24.857(5)
_cell_measurement_reflns_used    9880
_cell_measurement_temperature    170.00
_cell_measurement_theta_max      23.74
_cell_measurement_theta_min      2.16
_cell_volume                     5516(2)
_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 0.974
_diffrn_measured_fraction_theta_max 0.974
_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  0.1292
_diffrn_reflns_av_unetI/netI     0.0983
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            29396
_diffrn_reflns_point_group_measured_fraction_full 0.507
_diffrn_reflns_point_group_measured_fraction_max 0.507
_diffrn_reflns_theta_full        24.710
_diffrn_reflns_theta_max         24.710
_diffrn_reflns_theta_min         0.844
_exptl_absorpt_coefficient_mu    0.783
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_description       block
_exptl_crystal_F_000             2144
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         4.062
_refine_diff_density_min         -1.731
_refine_diff_density_rms         0.266
_refine_ls_abs_structure_details
;
No quotients, so Flack parameter determined by classical intensity fit
;
_refine_ls_abs_structure_Flack   0.02(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.300
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1109
_refine_ls_number_reflns         9542
_refine_ls_number_restraints     704
_refine_ls_restrained_S_all      1.268
_refine_ls_R_factor_all          0.1360
_refine_ls_R_factor_gt           0.1223
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3000
_refine_ls_wR_factor_ref         0.3147
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    0.000
_reflns_Friedel_fraction_max     0.000
_reflns_number_gt                7948
_reflns_number_total             9542
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3py01011b2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 1570475--1570477.cif.'
_cod_database_code               1570476
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C01I-C01P
 1.43 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
4.a Ternary CH refined with riding coordinates:
 C00G(H00G), C00P(H00P), C00Q(H00Q), C00V(H00V), C013(H013), C01D(H01D),
 C01G(H01G), C01N(H01N), C02G(H02G), C02J(H8), C02U(H1), C02X(H02X)
4.b Secondary CH2 refined with riding coordinates:
 C01L(H01F,H01H), C022(H02V,H02W), C024(H5,HB), C027(H02K,H02L), C02I(H02D,
 H02E), C035(H03A,H03B), C03A(H12,HK), C03L(H3,HT)
4.c Aromatic/amide H refined with riding coordinates:
 C00U(H00U), C010(H010), C011(H011), C012(H012), C014(H014), C01B(H01I),
 C01E(H01E), C01I(H01M), C01K(H01), C01P(H01P), C01R(H01R), C01S(H01S),
 C01T(H01T), C01Y(H01Y), C01Z(H01Z), C020(H020), C025(H025), C02B(H02M),
 C02D(H7), C02E(H02Z), C02F(H02F), C02N(H9), C02P(H02P), C02Q(H02Q), C02Y(H02Y),
  C030(H030), C033(H033), C03K(H03U)
4.d Idealised Me refined as rotating group:
 C00L(H00A,H00B,H00C), C00Y(H00D,H00E,H00F), C015(H01O,H01Q,H01U), C016(H01A,
 H01B,H01C), C019(H01V,H01W,H01X), C01C(H01J,H01K,H01L), C023(H4,H,HA),
 C028(H02A,H02B,H02C), C02C(H6,HC,HD), C02H(H02N,H02O,H02R), C02R(H02,HE,HF),
 C02S(H10,HG,HH), C02T(H02H,H02I,H02J), C02V(H02S,H02T,H02U), C031(H11,HI,HJ),
 C038(H03V,H03W,H03X), C039(H03R,H03S,H03T), C03B(H03Y,HL,HM), C03C(H03Z,HN,HO),
  C03D(H03,HP,HQ), C03G(H03C,H03D,H03E), C03H(H2,HR,HS), C03I(H03F,H03G,H03H),
 C03J(H03I,H03J,H03K), C03M(H03L,H03M,H03N), C03R(H03O,H03P,H03Q), C040(H04A,
 H04B,H04C), C12(H12A,H12B,H12C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              23114
_shelx_hkl_checksum              91319
_shelx_fab_checksum              3371
_olex2_submission_special_instructions 'No special instructions were received'