Unexpected o-aryl tBu group effect on suppression of chain transfer in pyridine–imine Ni(ii) and Pd(ii) catalyzed ethylene (co)polymerization
Yan, Zhengpeng; Zou, Wenping; Dai, Shengyu; Polymer Chemistry 14 (2023) 2107–2116; doi:10.1039/D3PY00146F

data_1568726
_publ_section_title
;
 Unexpected o-aryl tBu group effect on suppression of chain transfer in
 pyridine--imine Ni(ii) and Pd(ii) catalyzed ethylene (co)polymerization
;
_journal_issue                   17
_journal_name_full               'Polymer Chemistry'
_journal_page_first              2107
_journal_page_last               2116
_journal_paper_doi               10.1039/D3PY00146F
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C43 H41 Cl N2 Pd'
_chemical_formula_sum            'C43 H41 Cl N2 Pd'
_chemical_formula_weight         727.63
_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   mixed
_audit_creation_date             2022-11-17
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-11-20 deposited with the CCDC.	2023-03-30 downloaded from the CCDC.
;
_cell_angle_alpha                73.502(11)
_cell_angle_beta                 80.941(11)
_cell_angle_gamma                78.858(12)
_cell_formula_units_Z            2
_cell_length_a                   11.2154(16)
_cell_length_b                   11.8439(18)
_cell_length_c                   14.4771(19)
_cell_measurement_reflns_used    9624
_cell_measurement_temperature    295
_cell_measurement_theta_max      69.49
_cell_measurement_theta_min      3.20
_cell_volume                     1798.3(5)
_computing_cell_refinement
;
X-Area Recipe 1.37.0.0 (STOE, 2021)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.175.0 (STOE, 2021)
;
_computing_data_reduction
;
X-Area Integrate 2.5.1.0 (STOE, 2021)
X-Area LANA 2.6.2.0 (STOE, 2021)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 2.0, Darmstadt 2021
;
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      295
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 300K'
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_details
;
 1273 frames, detector distance = 40 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '1.2 mm, 0.6 diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0478
_diffrn_reflns_av_unetI/netI     0.0443
_diffrn_reflns_Laue_measured_fraction_full 0.960
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12917
_diffrn_reflns_point_group_measured_fraction_full 0.960
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        66.599
_diffrn_reflns_theta_max         66.599
_diffrn_reflns_theta_min         3.203
_diffrn_source                   'GeniX 3D HF Cu'
_diffrn_source_current           0.600
_diffrn_source_power             0.030
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    5.080
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  1.0000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.080
_refine_diff_density_min         -1.397
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     431
_refine_ls_number_reflns         6098
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0937
_refine_ls_R_factor_gt           0.0765
_refine_ls_shift/su_max          0.109
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1739P)^2^+0.0733P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2127
_refine_ls_wR_factor_ref         0.2369
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4992
_reflns_number_total             6098
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3py00146f2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 1568725--1568726.cif.'
_cod_database_code               1568726
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.863
_shelx_estimated_absorpt_t_min   0.581
_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. Rigid bond restraints
 H28
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
3.a Ternary CH refined with riding coordinates:
 C15(H15), C41(H41)
3.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C13(H13), C40(H40), C38(H38), C17(H17), C34(H34), C30(H30),
 C39(H39), C5(H5), C36(H36), C27(H27), C18(H18), C26(H26), C37(H37), C21(H21),
 C8(H8), C25(H25), C6(H6), C19(H19), C33(H33), C20(H20), C32(H32), C7(H7),
 C31(H31), C24(H24), C23(H23)
3.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C)
;
_shelx_res_checksum              25621
_olex2_submission_special_instructions 'No special instructions were received'
_stoe_detector_distance          '40.0 mm'
_stoe_detector_pixelsize_x       '0.172 mm'
_stoe_detector_pixelsize_y       '0.172 mm'
_stoe_detector_size_x            '8.4 cm'
_stoe_detector_size_y            '10.6 cm'
_stoe_evaluation_integration_a   6.0
_stoe_evaluation_integration_b   0.5
_stoe_evaluation_integration_ems 0.020
_stoe_evaluation_lana_bis_l_even_max -
_stoe_evaluation_lana_bis_l_odd_max -
_stoe_evaluation_lana_bos_l_even_max 4
_stoe_evaluation_lana_bos_l_odd_max 1
_stoe_evaluation_lana_completeness 92.7
_stoe_evaluation_lana_dxs_max_order 3
_stoe_evaluation_lana_dys_max_order 3
_stoe_evaluation_lana_fs_max_order 3
_stoe_evaluation_lana_max_2theta_available 139.7
_stoe_evaluation_lana_max_2theta_desired 139.7
_stoe_evaluation_lana_mean_redundancy 2.1
_stoe_evaluation_lana_number_refls_after_or 13216
_stoe_evaluation_lana_number_refls_outliers 2584
_stoe_evaluation_lana_number_refls_total 15800
_stoe_evaluation_lana_number_refls_unique 6314
_stoe_evaluation_lana_number_refls_written 13216
_stoe_evaluation_lana_or_c1      0.035
_stoe_evaluation_lana_or_c2      0
_stoe_evaluation_lana_or_c3      0
_stoe_evaluation_lana_or_c4      0.7
_stoe_evaluation_lana_point_group -1
_stoe_evaluation_lana_table
;
2Theta          13.1   28.1   43.1   58.1   73.1   88.1  103.1  118.1  133.1
<Resolution>    5.78   3.04   2.02   1.57   1.29   1.11   0.99   0.90   0.85
N(total)          79    189    510   2489   3252   3043   2845   2344   1049
<Redundancy>     1.7    1.1    1.4    2.7    2.7    2.2    2.1    1.8    1.5
Complet. [%%]    93.8   86.4   86.5   99.7   99.8   99.6   98.3   96.2   66.8
<I/sigma>      167.2   89.0   49.8   24.9   14.5    9.9    6.9    5.3    4.5
R(int)         0.019  0.021  0.045  0.035  0.050  0.059  0.084  0.101  0.125
;
_stoe_measurement_identifier     2
_stoe_measurement_max_exposure_per_frame '1.5 s'
_stoe_measurement_mean_exposure_per_frame '1.3 s'
_stoe_measurement_min_exposure_per_frame '0.5 s'
_stoe_measurement_total_exposure_time '28 min'
_stoe_measurement_total_frame_number 1273
_stoe_measurement_total_run_number 28
_stoe_measurement_tube_power     '30.0 W'