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

data_1576131
_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         '2(F6 P), C16 H20 N4 O2'
_chemical_formula_sum            'C16 H20 F12 N4 O2 P2'
_chemical_formula_weight         590.3
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-10-12T19:14:18-00:00
_audit_update_record
;
2025-04-02 deposited with the CCDC.	2025-10-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.0825(11)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.13858(7)
_cell_length_b                   21.77525(16)
_cell_length_c                   7.76094(8)
_cell_measurement_reflns_used    21719
_cell_measurement_temperature    173.1(5)
_cell_measurement_theta_max      79.464
_cell_measurement_theta_min      2.04
_cell_volume                     1146.81(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      173.1(5)
_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    -72.00 -14.00   0.50    0.10    --  -23.00 128.00 148.00  116
  2  \w    -80.00 -21.00   0.50    0.10    --  -23.00 142.00 -40.00  118
  3  \w    -95.00 -10.00   0.50    0.10    --  -23.00 -45.00 120.00  170
  4  \w    -95.00   0.00   0.50    0.10    --  -23.00 -77.00  90.00  190
  5  \w    -94.00  -8.00   0.50    0.10    --  -23.00 -57.00-120.00  172
  6  \w    -70.00 -12.00   0.50    0.10    --  -23.00 125.00   0.00  116
  7  \w    -26.00  23.00   0.50    0.10    --   47.95 -19.00 -30.00   98
  8  \w    -26.00  23.00   0.50    0.10    --   47.95 -19.00  90.00   98
  9  \w     33.00 119.00   0.50    0.10    --   47.95  57.00  60.00  172
 10  \w    -26.00  23.00   0.50    0.10    --   47.95 -19.00 120.00   98
 11  \w     42.00 106.00   0.50    0.50    --  113.25 -94.00   0.00  128
 12  \w     42.00 106.00   0.50    0.50    --  113.25 -94.00-150.00  128
 13  \w     42.00 106.00   0.50    0.50    --  113.25 -94.00 150.00  128
 14  \w    101.00 177.00   0.50    0.50    --  113.25  45.00 -60.00  152
 15  \w     97.00 177.00   0.50    0.50    --  113.25  61.00  60.00  160
 16  \w     42.00  68.00   0.50    0.50    --  113.25 -61.00  30.00   52
 17  \w     42.00 106.00   0.50    0.50    --  113.25 -94.00 -60.00  128
 18  \w    101.00 177.00   0.50    0.50    --  113.25  45.00   0.00  152
 19  \w     42.00 106.00   0.50    0.50    --  113.25 -94.00  60.00  128
 20  \w    101.00 177.00   0.50    0.50    --  113.25  45.00 -30.00  152
 21  \w    101.00 177.00   0.50    0.50    --  113.25  45.00  60.00  152
 22  \w     42.00  68.00   0.50    0.50    --  113.25 -61.00 -60.00   52
 23  \w     42.00  68.00   0.50    0.50    --  113.25 -61.00 -30.00   52
 24  \w     42.00 108.00   0.50    0.50    --  113.25-111.00 -31.75  132
 25  \w     91.00 177.00   0.50    0.50    --  113.25  75.00 -71.07  172
 26  \w     42.00 106.00   0.50    0.50    --  113.25 -94.00-120.00  128
 27  \w    101.00 177.00   0.50    0.50    --  113.25  45.00-180.00  152
 28  \w     42.00  68.00   0.50    0.50    --  113.25 -61.00-120.00   52
 29  \w     42.00 102.00   0.50    0.50    --  113.25 -77.00 -60.00  120
 30  \w     42.00  68.00   0.50    0.50    --  113.25 -61.00   0.00   52
 31  \w    100.00 177.00   0.50    0.50    --  113.25  15.00 150.00  154
 32  \w    101.00 177.00   0.50    0.50    --  113.25  30.00 -60.00  152
 33  \w     42.00 106.00   0.50    0.50    --  113.25 -94.00  30.00  128
 34  \w     42.00 106.00   0.50    0.50    --  113.25 -94.00  90.00  128
 35  \w     42.00  68.00   0.50    0.50    --  113.25 -61.00 150.00   52
 36  \w     42.00 102.00   0.50    0.50    --  113.25 -77.00-180.00  120
 37  \w     42.00 106.00   0.50    0.50    --  113.25 -94.00 120.00  128
 38  \w     91.00 177.00   0.50    0.50    --  113.25  75.00  38.48  172
 39  \w     93.00 177.00   0.50    0.50    --  113.25  70.00-138.15  168
 40  \w    -70.00 -12.00   0.50    0.10    --  -23.00 125.00-150.00  116
 41  \w     25.00 120.00   0.50    0.10    --   47.95  77.00  60.00  190
 42  \w     25.00 120.00   0.50    0.10    --   47.95  77.00 120.00  190
 43  \w     25.00 120.00   0.50    0.10    --   47.95  77.00-150.00  190
 44  \w     25.00 120.00   0.50    0.10    --   47.95  77.00 -90.00  190
 45  \w     25.00 120.00   0.50    0.10    --   47.95  77.00 -30.00  190
 46  \w     25.00 120.00   0.50    0.10    --   47.95  77.00-120.00  190
 47  \w     36.00 121.00   0.50    0.10    --   47.95  38.00 150.00  170
 48  \w     -1.00  81.00   0.50    0.10    --   47.95 -99.00 150.00  164
 49  \w     25.00 120.00   0.50    0.10    --   47.95  77.00-180.00  190
 50  \w     91.00 177.00   0.50    0.50    --  113.25  77.00   0.00  172
 51  \w    101.00 177.00   0.50    0.50    --  113.25  45.00 -90.00  152
 52  \w     97.00 177.00   0.50    0.50    --  113.25  61.00  90.00  160
 53  \w    101.00 177.00   0.50    0.50    --  113.25  45.00 150.00  152
 54  \w    101.00 177.00   0.50    0.50    --  113.25  45.00-150.00  152
 55  \w     97.00 150.00   0.50    0.50    --  113.25  61.00 120.00  106
 56  \w     97.00 177.00   0.50    0.50    --  113.25  61.00  30.00  160
;
_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      -0.2105602
_diffrn_orient_matrix_UB_12      0.0263714
_diffrn_orient_matrix_UB_13      -0.05644
_diffrn_orient_matrix_UB_21      -0.0842485
_diffrn_orient_matrix_UB_22      -0.0655606
_diffrn_orient_matrix_UB_23      -0.0122177
_diffrn_orient_matrix_UB_31      0.0088588
_diffrn_orient_matrix_UB_32      0.0034662
_diffrn_orient_matrix_UB_33      0.200688
_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  0.0525
_diffrn_reflns_av_unetI/netI     0.0334
_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       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            27914
_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         74.486
_diffrn_reflns_theta_min         4.06
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.875
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.82999
_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            colourless
_exptl_crystal_density_diffrn    1.709
_exptl_crystal_description       block
_exptl_crystal_F_000             596
_exptl_crystal_size_max          0.282
_exptl_crystal_size_mid          0.121
_exptl_crystal_size_min          0.081
_refine_diff_density_max         0.362
_refine_diff_density_min         -0.242
_refine_diff_density_rms         0.041
_refine_ls_extinction_coef       0.0017(3)
_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   1.078
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         2336
_refine_ls_number_restraints     76
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0364
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0438P)^2^+0.5790P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0958
_refine_ls_wR_factor_ref         0.0962
_reflns_Friedel_coverage         0
_reflns_number_gt                2290
_reflns_number_total             2336
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cy01102g2.cif
_cod_data_source_block           21MA185_ER-0300
_cod_original_cell_volume        1146.811(19)
_cod_database_code               1576131
_shelx_estimated_absorpt_t_min   0.498
_shelx_estimated_absorpt_t_max   0.8
_oxdiff_exptl_absorpt_empirical_details
;
        Empirical correction (ABSPACK) includes:
        - Absorption correction using spherical harmonics
        - Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.466
_oxdiff_exptl_absorpt_empirical_full_min 0.732
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
        1. Fixed Uiso
 At 1.2 times of:
  All N(H) groups
        2. Restrained distances
 P1-F5A \\sim P1-F5 \\sim P1-F6A \\sim P1-F6 \\sim P1-F3A \\sim P1-F3 \\sim
        P1-F4A \\sim P1-F4
 with sigma of 0.0002
        3. Uiso/Uaniso restraints and constraints
F6 \\sim F4: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
        0.004 within 1.7A
F5A \\sim F3A: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
        0.004 within 1.7A
F3 \\sim F5: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
        0.004 within 1.7A
F6A \\sim F4A: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
        0.004 within 1.7A
Uanis(F6A) \\sim Ueq, Uanis(F3A) \\sim Ueq, Uanis(F4A) \\sim Ueq, Uanis(F4)
\\sim Ueq, Uanis(F5) \\sim Ueq, Uanis(F6) \\sim Ueq, Uanis(F3) \\sim Ueq: with
        sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(F5A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
        4. Others
 Sof(F3A)=Sof(F6A)=Sof(F5A)=Sof(F4A)=Sof(O1A)=1-FVAR(1)
 Sof(F4)=Sof(F5)=Sof(F3)=Sof(F6)=Sof(O1)=FVAR(1)
 Sof(C3A)=Sof(N2A)=1-FVAR(2)
 Sof(C3)=Sof(N2)=FVAR(2)
        5.a Aromatic/amide H refined with riding coordinates:
 N1(H1)
;
_shelx_res_checksum              28864