Room-temperature Suzuki–Miyaura polycondensation of aryl dichloride monomers enabled by “large-but-flexible” Pd-NHC precatalysts
Feng, Juan-Juan; Guo, Yuman; Song, Qian; Guo, Ze-Cheng; Liu, Feng-Shou; Polymer Chemistry 17 (2026) 539–550; doi:10.1039/D5PY01111F

data_1576553
_publ_section_title
;
 Room-temperature Suzuki--Miyaura polycondensation of aryl dichloride
 monomers enabled by &#x201C;large-but-flexible&#x201D; Pd-NHC
 precatalysts
;
_journal_issue                   5
_journal_name_full               'Polymer Chemistry'
_journal_page_first              539
_journal_page_last               550
_journal_paper_doi               10.1039/D5PY01111F
_journal_volume                  17
_journal_year                    2026
_chemical_formula_moiety         'C40 H36 Cl3 N3 Pd'
_chemical_formula_sum            'C40 H36 Cl3 N3 Pd'
_chemical_formula_weight         771.47
_space_group_crystal_system      tetragonal
_space_group_IT_number           85
_space_group_name_Hall           '-P 4a'
_space_group_name_H-M_alt        'P 4/n :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-12-28
_audit_creation_method
;
Olex2 1.5-beta
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2025-07-09 deposited with the CCDC.	2025-12-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   30.4347(4)
_cell_length_b                   30.4347(4)
_cell_length_c                   8.9629(2)
_cell_measurement_reflns_used    7884
_cell_measurement_temperature    292.99(10)
_cell_measurement_theta_max      73.5030
_cell_measurement_theta_min      3.2640
_cell_volume                     8302.1(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      292.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2684
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.969
_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      7.00  82.00   1.00    1.25    --   40.92 -99.00 -90.00   75
  2  \w     23.00  50.00   1.00    1.25    --   40.92-125.00-120.00   27
  3  \w     55.00 102.00   1.00    3.00    --  107.58 -45.00-150.00   47
  4  \w     27.00 160.00   1.00    3.00    --  107.58 -15.00 -60.00  133
  5  \w     99.00 150.00   1.00    3.00    --  107.58 125.00 -30.00   51
  6  \w   -107.00 -64.00   1.00    1.25    --  -40.92 -57.00-120.00   43
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0413851000
_diffrn_orient_matrix_UB_12      -0.0058139000
_diffrn_orient_matrix_UB_13      0.0969996000
_diffrn_orient_matrix_UB_21      -0.0129722000
_diffrn_orient_matrix_UB_22      -0.0406966000
_diffrn_orient_matrix_UB_23      -0.0921096000
_diffrn_orient_matrix_UB_31      0.0261067000
_diffrn_orient_matrix_UB_32      -0.0295214000
_diffrn_orient_matrix_UB_33      0.1079588000
_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  0.0420
_diffrn_reflns_av_unetI/netI     0.0517
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            17609
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.028
_diffrn_reflns_theta_min         2.053
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.595
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.31346
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_description       block
_exptl_crystal_F_000             3152
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.349
_refine_diff_density_min         -2.173
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     430
_refine_ls_number_reflns         8169
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0622
_refine_ls_R_factor_gt           0.0556
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0887P)^2^+6.4992P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1474
_refine_ls_wR_factor_ref         0.1549
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7024
_reflns_number_total             8169
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5py01111f2.cif
_cod_data_source_block           pdcl4
_cod_original_cell_volume        8302.1(3)
_cod_original_sg_symbol_H-M      'P 4/n'
_cod_database_code               1576553
_shelx_shelxl_version_number     2018/3
_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.a Ternary CH refined with riding coordinates:
 C7(H7), C8(H8)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C11(H11), C12(H12), C13(H13), C14(H14),
 C20(H20), C22(H22), C29(H29), C31(H31), C36(H36), C37(H37), C38(H38), C40(H40)
2.c Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C33(H33A,H33B,
 H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              15546
_shelx_hkl_checksum              24093
_shelx_fab_checksum              75515
_olex2_date_sample_data_collection 2022-12-27
_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 1.593
_oxdiff_exptl_absorpt_empirical_full_min 0.559