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

data_1576130
_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), C18 H24 N4 O2'
_chemical_formula_sum            'C18 H24 F12 N4 O2 P2'
_chemical_formula_weight         618.35
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-02-03
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2025-04-02 deposited with the CCDC.	2025-10-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.5921(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   5.83359(4)
_cell_length_b                   11.41940(9)
_cell_length_c                   18.48940(14)
_cell_measurement_reflns_used    10869
_cell_measurement_temperature    173.01(10)
_cell_measurement_theta_max      79.4750
_cell_measurement_theta_min      2.3370
_cell_volume                     1229.272(16)
_computing_cell_refinement       'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.105a (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 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_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    -56.00   7.00   0.50    0.25    --  -23.00 103.00  -0.00  126
  2  \w     15.00  83.00   0.50    0.25    --   49.64-103.00-102.00  136
  3  \w    106.00 177.00   0.50    0.80    --  111.50 103.00  -0.00  142
  4  \w     41.00 107.00   0.50    0.80    --  111.50-103.00-102.00  132
  5  \w    -68.00 -12.00   0.50    0.25    --  -23.00 125.00 150.00  112
  6  \w    -68.00 -12.00   0.50    0.25    --  -23.00 125.00  90.00  112
  7  \w    -23.00  23.00   0.50    0.25    --   49.64 -19.00   0.00   92
  8  \w    -23.00  23.00   0.50    0.25    --   49.64 -19.00 -90.00   92
  9  \w    -22.00  40.00   0.50    0.25    --   49.64 -38.00 150.00  124
 10  \w     41.00  68.00   0.50    0.80    --  111.50 -61.00   0.00   54
 11  \w     41.00 102.00   0.50    0.80    --  111.50 -77.00 -90.00  122
 12  \w    104.00 177.00   0.50    0.80    --  111.50  15.00-180.00  146
 13  \w     41.00 102.00   0.50    0.80    --  111.50 -77.00-120.00  122
 14  \w    104.00 177.00   0.50    0.80    --  111.50  30.00-150.00  146
 15  \w    104.00 177.00   0.50    0.80    --  111.50  30.00 -90.00  146
 16  \w     41.00 102.00   0.50    0.80    --  111.50 -77.00  30.00  122
 17  \w     41.00  68.00   0.50    0.80    --  111.50 -61.00-180.00   54
 18  \w    104.00 177.00   0.50    0.80    --  111.50  15.00 120.00  146
 19  \w     41.00 102.00   0.50    0.80    --  111.50 -77.00 -60.00  122
 20  \w     41.00 105.00   0.50    0.80    --  111.50 -94.00 -30.00  128
 21  \w     41.00 102.00   0.50    0.80    --  111.50 -77.00 -30.00  122
 22  \w     41.00  68.00   0.50    0.80    --  111.50 -61.00 -90.00   54
 23  \w     41.00  68.00   0.50    0.80    --  111.50 -61.00  30.00   54
 24  \w     41.00  68.00   0.50    0.80    --  111.50 -61.00  90.00   54
 25  \w     37.00 122.00   0.50    0.25    --   49.64  57.00 -60.00  170
 26  \w     29.00 122.00   0.50    0.25    --   49.64  77.00 150.00  186
 27  \w     37.00 122.00   0.50    0.25    --   49.64  57.00  60.00  170
;
_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      0.0678512000
_diffrn_orient_matrix_UB_12      0.0803562000
_diffrn_orient_matrix_UB_13      0.0647809000
_diffrn_orient_matrix_UB_21      -0.0415355000
_diffrn_orient_matrix_UB_22      -0.1013666000
_diffrn_orient_matrix_UB_23      0.0525451000
_diffrn_orient_matrix_UB_31      0.2524499000
_diffrn_orient_matrix_UB_32      -0.0381980000
_diffrn_orient_matrix_UB_33      -0.0033050000
_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  0.0247
_diffrn_reflns_av_unetI/netI     0.0154
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            12824
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.228
_diffrn_reflns_theta_min         4.554
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.712
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49015
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.105a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.671
_exptl_crystal_description       block
_exptl_crystal_F_000             628
_exptl_crystal_size_max          0.254
_exptl_crystal_size_mid          0.211
_exptl_crystal_size_min          0.131
_refine_diff_density_max         0.905
_refine_diff_density_min         -0.783
_refine_diff_density_rms         0.069
_refine_ls_extinction_coef       0.0029(5)
_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   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     213
_refine_ls_number_reflns         2503
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0563
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0758P)^2^+1.6053P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1492
_refine_ls_wR_factor_ref         0.1501
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2418
_reflns_number_total             2503
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cy01102g2.cif
_cod_data_source_block           22ma006_Er-0341
_cod_database_code               1576130
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C18H24F12N4O2P2
_shelx_estimated_absorpt_t_max   0.718
_shelx_estimated_absorpt_t_min   0.546
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(F2A) \\sim Ueq, Uanis(F3B) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.005
Uanis(F3B) \\sim Ueq, Uanis(F2A) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.005
3. Others
 Sof(F1A)=Sof(F4A)=Sof(F3A)=Sof(F2A)=1-FVAR(1)
 Sof(F3B)=Sof(F2B)=Sof(F1B)=Sof(F4B)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 N2(H2), C6(H6), C3(H3)
4.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C8(H8A,H8B,H8C), C7(H7A,H7B,H7C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              71540
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.537
_oxdiff_exptl_absorpt_empirical_full_min 0.816