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_1576555
_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         'C42 H40 Cl3 N3 Pd'
_chemical_formula_sum            'C42 H40 Cl3 N3 Pd'
_chemical_formula_weight         799.52
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-12-22
_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                 104.135(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.8191(7)
_cell_length_b                   23.1145(9)
_cell_length_c                   18.5583(9)
_cell_measurement_reflns_used    12365
_cell_measurement_temperature    260.03(10)
_cell_measurement_theta_max      27.2500
_cell_measurement_theta_min      2.4230
_cell_volume                     8244.3(6)
_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      N~2~
_diffrn_ambient_temperature      260.03(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2684
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -35.00  62.00   1.00    3.50    --  -11.27  38.00 -60.00   97
  2  \w    -84.00   3.00   1.00    3.50    --  -11.27 -57.00 150.00   87
  3  \w     34.00  75.00   1.00    3.50    --   11.90-178.00 120.00   41
;
_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      -0.0069590000
_diffrn_orient_matrix_UB_12      0.0274780000
_diffrn_orient_matrix_UB_13      0.0135968000
_diffrn_orient_matrix_UB_21      0.0319818000
_diffrn_orient_matrix_UB_22      -0.0013072000
_diffrn_orient_matrix_UB_23      0.0273593000
_diffrn_orient_matrix_UB_31      0.0170400000
_diffrn_orient_matrix_UB_32      0.0136361000
_diffrn_orient_matrix_UB_33      -0.0248883000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0334
_diffrn_reflns_av_unetI/netI     0.0436
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            41502
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.940
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.675
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91016
_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    1.288
_exptl_crystal_description       block
_exptl_crystal_F_000             3280
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.034
_refine_diff_density_min         -1.731
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     931
_refine_ls_number_reflns         14515
_refine_ls_number_restraints     114
_refine_ls_restrained_S_all      0.991
_refine_ls_R_factor_all          0.0736
_refine_ls_R_factor_gt           0.0515
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0382P)^2^+18.2026P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1089
_refine_ls_wR_factor_ref         0.1225
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10859
_reflns_number_total             14515
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5py01111f2.cif
_cod_data_source_block           pdcl
_cod_database_code               1576555
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Pd2-N43 \\sim Pd2-N43A
 with sigma of 0.02
 Cl7-C47 \\sim Cl7A-C47A
 with sigma of 0.02
 C48-C47 \\sim C48A-C47A
 with sigma of 0.02
 C48-N43 \\sim C48A-N43A
 with sigma of 0.02
 C47-C45 \\sim C47A-C45A
 with sigma of 0.04
 C47-C46 \\sim C47A-C46A
 with sigma of 0.02
 C46-C45 \\sim C46A-C45A
 with sigma of 0.02
 C45-C44 \\sim C45A-C44A
 with sigma of 0.02
 C48-C44 \\sim C48A-C44A
 with sigma of 0.04
 C44-N43 \\sim C44A-N43A
 with sigma of 0.02
 C47-N43 \\sim C47A-N43A
 with sigma of 0.04
 C46-C44 \\sim C46A-C44A
 with sigma of 0.04
 C45-N43 \\sim C45A-N43A
 with sigma of 0.04
 Pd2-C48 \\sim Pd2-C48A
 with sigma of 0.04
 Pd2-C44 \\sim Pd2-C44A
 with sigma of 0.04
 Cl7-C48 \\sim Cl7A-C48A
 with sigma of 0.04
 Cl7-C46 \\sim Cl7A-C46A
 with sigma of 0.04
 C48-C46 \\sim C48A-C46A
 with sigma of 0.04
3. Rigid body (RIGU) restrains
 C48, N43, C44, C45, C46, C47
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C48A, C44A, Cl7A, C47A, N43A, C46A, C45A, Pd2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 Cl7, C45, N43, C48, C44, C47, C46, Pd2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
4. Others
 Sof(C48A)=Sof(H48A)=Sof(C47A)=Sof(C46A)=Sof(H46A)=Sof(C45A)=Sof(H45A)=
 Sof(C44A)=Sof(H44A)=Sof(N43A)=Sof(Cl7A)=1-FVAR(1)
 Sof(Cl7)=Sof(C48)=Sof(H48)=Sof(C47)=Sof(C46)=Sof(H46)=Sof(C45)=Sof(H45)=
 Sof(C44)=Sof(H44)=Sof(N43)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C7(H7), C61(H61), C69(H69), C10(H10)
5.b Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C25(H25A,H25B), C33(H33A,H33B), C35(H35A,H35B), C82(H82A,
 H82B), C57(H57A,H57B), C55(H55A,H55B), C84(H84A,H84B)
5.c Aromatic/amide H refined with riding coordinates:
 C38(H38), C62(H62), C42(H42), C40(H40), C19(H19), C41(H41), C75(H75),
 C21(H21), C74(H74), C15(H15), C12(H12), C64(H64), C72(H72), C31(H31), C67(H67),
  C73(H73), C29(H29), C51(H51), C2(H2), C5(H5), C53(H53), C30(H30), C65(H65),
 C52(H52), C66(H66), C78(H78), C79(H79), C13(H13), C80(H80), C14(H14), C48(H48),
  C46(H46), C45(H45), C44(H44), C4(H4), C3(H3), C48A(H48A), C46A(H46A),
 C45A(H45A), C44A(H44A)
5.d Fitted hexagon refined as free rotating group:
 C48(C47,C46,C45,C44,N43), C48A(C47A,C46A,C45A,C44A,N43A)
5.e Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C36(H36A,H36B,H36C), C26(H26A,H26B,H26C), C83(H83A,H83B,
 H83C), C34(H34A,H34B,H34C), C56(H56A,H56B,H56C), C85(H85A,H85B,H85C), C58(H58A,
 H58B,H58C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              39780
_shelx_hkl_checksum              74718
_shelx_fab_checksum              23185
_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 1.102
_oxdiff_exptl_absorpt_empirical_full_min 0.906