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_1576554
_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         'C41 H42 Cl2 N4 Pd, C H2 Cl2'
_chemical_formula_sum            'C42 H44 Cl4 N4 Pd'
_chemical_formula_weight         853.01
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2025-04-16
_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                 101.7640(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.01670(10)
_cell_length_b                   20.6583(2)
_cell_length_c                   17.1121(2)
_cell_measurement_reflns_used    18202
_cell_measurement_temperature    300.03(10)
_cell_measurement_theta_max      74.6460
_cell_measurement_theta_min      3.3760
_cell_volume                     4158.76(7)
_computing_cell_refinement       'CrysAlisPro 1.171.43.121a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.121a 64-bit (release 24-04-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.121a (Rigaku OD, 2024)'
_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    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      300.03(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.962
_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     32.00 121.00   0.50    0.05    --   43.21  26.00-158.00  178
  2  \w     93.00 127.00   0.50    0.05    --  107.48  15.00-180.00   68
  3  \w     94.00 143.00   0.50    0.05    --  107.48  26.00-158.00   98
  4  \w     95.00 139.00   0.50    0.05    --  107.48  15.00 -90.00   88
  5  \w     94.00 139.00   0.50    0.05    --  107.48  15.00 120.00   90
  6  \w    100.00 125.00   0.50    0.05    --  107.48  15.00 150.00   50
  7  \w      5.00  30.00   0.50    0.05    --  -43.21  26.00-158.00   50
  8  \w    -15.00  31.00   0.50    0.05    --  -43.21  38.00 -30.00   92
  9  \w     35.00  76.00   0.50    0.05    --   43.21-126.00-180.00   82
 10  \w     60.00  87.00   0.50    0.05    --  107.48 -95.00 -60.00   54
 11  \w     43.00  68.00   0.50    0.05    --  107.48 -77.00-120.00   50
 12  \w     37.00  67.00   0.50    0.05    --  107.48 -77.00 -60.00   60
 13  \w     40.00  77.00   0.50    0.05    --  107.48 -77.00   0.00   74
 14  \w     51.00  76.00   0.50    0.05    --  107.48 -77.00  90.00   50
 15  \w    -36.00   1.00   0.50    0.05    --   43.21 -26.00  38.00   74
 16  \w    -34.00  11.00   0.50    0.05    --   43.21 -38.00-120.00   90
 17  \w    -18.00  42.00   0.50    0.05    --   43.21 -57.00 -90.00  120
 18  \w    115.00 174.00   0.50    0.05    --  107.48 126.00  90.00  118
 19  \w    -71.00 -36.00   0.50    0.05    -- -103.00  77.00 120.00   70
 20  \w    -71.00 -37.00   0.50    0.05    -- -103.00  77.00 150.00   68
 21  \w    -61.00 -35.00   0.50    0.05    -- -103.00  77.00  90.00   52
 22  \w    -65.00 -39.00   0.50    0.05    -- -103.00  77.00   0.00   52
 23  \w    -68.00 -37.00   0.50    0.05    -- -103.00  77.00 -60.00   62
 24  \w    -69.00 -31.00   0.50    0.05    -- -103.00  77.00 -90.00   76
 25  \w    -71.00 -36.00   0.50    0.05    -- -103.00  77.00-120.00   70
 26  \w   -101.00 -66.00   0.50    0.05    -- -103.00 126.00-120.00   70
 27  \w    -63.00 -37.00   0.50    0.05    -- -103.00 126.00-120.00   52
 28  \w   -133.00 -95.00   0.50    0.05    -- -103.00 -15.00 -60.00   76
 29  \w   -129.00 -89.00   0.50    0.05    -- -103.00 -15.00 -30.00   80
 30  \w   -152.00 -93.00   0.50    0.05    -- -103.00 -26.00  38.00  118
 31  \w   -102.00 -76.00   0.50    0.05    --  -43.21 -26.00  38.00   52
 32  \w    -67.00 -30.00   0.50    0.05    --  -43.21 -26.00  38.00   74
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1192537000
_diffrn_orient_matrix_UB_12      -0.0123784000
_diffrn_orient_matrix_UB_13      -0.0511603000
_diffrn_orient_matrix_UB_21      0.0420400000
_diffrn_orient_matrix_UB_22      0.0218425000
_diffrn_orient_matrix_UB_23      -0.0750804000
_diffrn_orient_matrix_UB_31      0.0341485000
_diffrn_orient_matrix_UB_32      -0.0701962000
_diffrn_orient_matrix_UB_33      -0.0142889000
_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  0.0447
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            28526
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.953
_diffrn_reflns_theta_min         3.397
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.219
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.18054
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.121a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_description       block
_exptl_crystal_F_000             1752
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.802
_refine_diff_density_min         -0.803
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     479
_refine_ls_number_reflns         8236
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0520
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1075P)^2^+1.2819P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1528
_refine_ls_wR_factor_ref         0.1611
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6976
_reflns_number_total             8236
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5py01111f2.cif
_cod_data_source_block           y_7
_cod_database_code               1576554
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C  H O N Pd Cl Br'
_shelx_estimated_absorpt_t_max   0.548
_shelx_estimated_absorpt_t_min   0.456
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(Cl5)=Sof(H1SC)=Sof(H1SD)=1-FVAR(1)
 Sof(Cl3)=Sof(H1SA)=Sof(H1SB)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 C19(H19)
3.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C16(H16A,H16B), C41(H41A,H41B), C43(H43A,H43B), C1S(H1SA,
 H1SB), C1S(H1SC,H1SD)
3.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C12(H12), C22(H22), C23(H23), C24(H24), C25(H25),
 C28(H28), C30(H30), C31(H31), C37(H37), C38(H38), C39(H39), C45(H45), C46(H46),
  C47(H47), C48(H48)
3.d Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C32(H32A,H32B,H32C), C42(H42A,H42B,
 H42C), C44(H44A,H44B,H44C)
;
_shelx_res_checksum              23973
_shelx_hkl_checksum              52442
_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 3.937
_oxdiff_exptl_absorpt_empirical_full_min 0.320