Tunable bis(pyridinium amidate) ligands efficiently promote palladium-catalyzed ethylene polymerization
Reusser, Esaïe; Albrecht, Martin; Catalysis Science & Technology  (2025) –; doi:10.1039/D5CY01102G

data_1576132
_publ_section_title
;
 Tunable bis(pyridinium amidate) ligands efficiently promote
 palladium-catalyzed ethylene polymerization
;
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_paper_doi               10.1039/D5CY01102G
_journal_year                    2025
_chemical_formula_moiety         'C14 H14 N4 O2'
_chemical_formula_sum            'C14 H14 N4 O2'
_chemical_formula_weight         270.29
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2022-01-10T17:58:45-00:00
_audit_update_record
;
2025-04-02 deposited with the CCDC.	2025-10-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.3237(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.29001(8)
_cell_length_b                   24.7363(2)
_cell_length_c                   7.53443(8)
_cell_measurement_reflns_used    21307
_cell_measurement_temperature    173.01(10)
_cell_measurement_theta_max      79.922
_cell_measurement_theta_min      3.554
_cell_volume                     1247.64(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_details
;
        List of Runs (angles in degrees, time in seconds):
  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -84.00 -25.00   0.50    0.10    --  -23.00 149.00  88.00  118
  2  \w    -69.00 -11.00   0.50    0.10    --  -23.00 123.00 -75.00  116
  3  \w    -95.00   0.00   0.50    0.10    --  -23.00 -77.00 -90.00  190
  4  \w    -25.00  40.00   0.50    0.10    --   47.88 -38.00-180.00  130
  5  \w    -26.00  23.00   0.50    0.10    --   47.88 -19.00 -60.00   98
  6  \w     25.00 120.00   0.50    0.10    --   47.88  77.00-150.00  190
  7  \w    -23.00  63.00   0.50    0.10    --   47.88 -57.00-120.00  172
  8  \w     25.00 120.00   0.50    0.10    --   47.88  77.00   0.00  190
  9  \w     42.00  68.00   0.50    0.50    --  113.25 -61.00 -30.00   52
 10  \w     42.00  68.00   0.50    0.50    --  113.25 -61.00 120.00   52
 11  \w     42.00 102.00   0.50    0.50    --  113.25 -77.00-120.00  120
 12  \w    100.00 177.00   0.50    0.50    --  113.25  15.00 -30.00  154
 13  \w    101.00 177.00   0.50    0.50    --  113.25  45.00-150.00  152
 14  \w    101.00 177.00   0.50    0.50    --  113.25  45.00  30.00  152
 15  \w     42.00  68.00   0.50    0.50    --  113.25 -61.00-150.00   52
 16  \w     42.00 106.00   0.50    0.50    --  113.25 -94.00-180.00  128
 17  \w     42.00 102.00   0.50    0.50    --  113.25 -77.00  30.00  120
 18  \w     42.00 106.00   0.50    0.50    --  113.25 -94.00  90.00  128
 19  \w     42.00 106.00   0.50    0.50    --  113.25 -94.00  30.00  128
 20  \w     42.00  68.00   0.50    0.50    --  113.25 -61.00-120.00   52
 21  \w     42.00  68.00   0.50    0.50    --  113.25 -61.00-180.00   52
 22  \w     42.00 106.00   0.50    0.50    --  113.25 -94.00-120.00  128
 23  \w     42.00  68.00   0.50    0.50    --  113.25 -61.00   0.00   52
 24  \w     42.00 106.00   0.50    0.50    --  113.25 -94.00 -30.00  128
 25  \w     42.00  68.00   0.50    0.50    --  113.25 -61.00 -90.00   52
 26  \w     42.00 106.00   0.50    0.50    --  113.25 -94.00  60.00  128
 27  \w     97.00 177.00   0.50    0.50    --  113.25  61.00  30.00  160
 28  \w     42.00 106.00   0.50    0.50    --  113.25 -94.00-150.00  128
 29  \w    101.00 177.00   0.50    0.50    --  113.25  45.00-120.00  152
 30  \w     42.00 106.00   0.50    0.50    --  113.25 -94.00   0.00  128
 31  \w     97.00 177.00   0.50    0.50    --  113.25  61.00 120.00  160
 32  \w     42.00 102.00   0.50    0.50    --  113.25 -77.00 -60.00  120
 33  \w     42.00 102.00   0.50    0.50    --  113.25 -77.00  90.00  120
 34  \w     97.00 177.00   0.50    0.50    --  113.25  61.00   0.00  160
 35  \w     42.00 109.00   0.50    0.50    --  113.25-113.00-166.65  134
 36  \w    101.00 177.00   0.50    0.50    --  113.25  45.00  60.00  152
 37  \w     42.00 141.00   0.50    0.50    --  113.25 -88.00 127.74  198
 38  \w    101.00 177.00   0.50    0.50    --  113.25  30.00-180.00  152
 39  \w    -96.00 -10.00   0.50    0.10    --  -23.00 -38.00  90.00  172
 40  \w    -70.00 -12.00   0.50    0.10    --  -23.00 125.00  60.00  116
 41  \w     25.00 120.00   0.50    0.10    --   47.88  77.00 150.00  190
 42  \w     33.00 119.00   0.50    0.10    --   47.88  57.00 -30.00  172
 43  \w     25.00 120.00   0.50    0.10    --   47.88  77.00  60.00  190
 44  \w     -1.00  81.00   0.50    0.10    --   47.88 -99.00 120.00  164
 45  \w     25.00 120.00   0.50    0.10    --   47.88  77.00 -90.00  190
 46  \w     25.00 120.00   0.50    0.10    --   47.88  77.00  90.00  190
 47  \w     33.00 119.00   0.50    0.10    --   47.88  57.00 -90.00  172
 48  \w    101.00 156.00   0.50    0.50    --  113.25  45.00 -90.00  110
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0964245
_diffrn_orient_matrix_UB_12      0.0266805
_diffrn_orient_matrix_UB_13      0.1267433
_diffrn_orient_matrix_UB_21      0.0675534
_diffrn_orient_matrix_UB_22      0.0559268
_diffrn_orient_matrix_UB_23      -0.0410466
_diffrn_orient_matrix_UB_31      -0.1977648
_diffrn_orient_matrix_UB_32      0.0060977
_diffrn_orient_matrix_UB_33      -0.1784593
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0272
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 1
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            24882
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 1
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.855
_diffrn_reflns_theta_min         3.574
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.823
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.73189
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro 1.171.41.112a (Rigaku Oxford Diffraction, 2021)
        Empirical absorption correction using spherical harmonics,
        implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_description       block
_exptl_crystal_F_000             568
_exptl_crystal_size_max          0.193
_exptl_crystal_size_mid          0.148
_exptl_crystal_size_min          0.147
_refine_diff_density_max         0.252
_refine_diff_density_min         -0.17
_refine_diff_density_rms         0.034
_refine_ls_extinction_coef       0.0042(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         2399
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.032
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0420P)^2^+0.4085P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0845
_refine_ls_wR_factor_ref         0.0851
_reflns_Friedel_coverage         0
_reflns_number_gt                2321
_reflns_number_total             2399
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cy01102g2.cif
_cod_data_source_block           21MA212_ER-390
_cod_database_code               1576132
_shelx_estimated_absorpt_t_min   0.857
_shelx_estimated_absorpt_t_max   0.889
_oxdiff_exptl_absorpt_empirical_details
;
        Empirical correction (ABSPACK) includes:
        - Absorption correction using spherical harmonics
        - Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.657
_oxdiff_exptl_absorpt_empirical_full_min 0.79
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
;
_shelx_res_checksum              12710