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_1576556
_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         'C37 H38 Cl2 N2 O Pd'
_chemical_formula_sum            'C37 H38 Cl2 N2 O Pd'
_chemical_formula_weight         704.05
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_symmetry_Int_Tables_number      60
_audit_creation_date             2025-04-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_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            16
_cell_length_a                   27.28920(10)
_cell_length_b                   27.5522(2)
_cell_length_c                   17.85610(10)
_cell_measurement_reflns_used    34973
_cell_measurement_temperature    298.61(10)
_cell_measurement_theta_max      74.6670
_cell_measurement_theta_min      3.1800
_cell_volume                     13425.60(13)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      298.61(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.9996
_diffrn_measured_fraction_theta_max 0.9996
_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    115.00 146.00   0.50    0.10    --  107.48  77.00 150.00   62
  2  \w    102.00 139.00   0.50    0.10    --  107.48  15.00  60.00   74
  3  \w     98.00 139.00   0.50    0.10    --  107.48  15.00 -60.00   82
  4  \w     46.00  72.00   0.50    0.10    --  107.48 -95.00 -90.00   52
  5  \w     36.00  71.00   0.50    0.10    --  107.48-134.00 -66.00   70
  6  \w     75.00 104.00   0.50    0.10    --  107.48-134.00 -66.00   58
  7  \w     24.00  90.00   0.50    0.05    --   43.21-136.00 115.00  132
  8  \w     57.00  92.00   0.50    0.10    --  107.48 -95.00 120.00   70
  9  \w     42.00  84.00   0.50    0.10    --  107.48 -95.00   0.00   84
 10  \w     48.00  75.00   0.50    0.10    --  107.48 -77.00-150.00   54
 11  \w     44.00  70.00   0.50    0.10    --  107.48 -77.00-180.00   52
 12  \w     39.00  71.00   0.50    0.10    --  107.48 -77.00  60.00   64
 13  \w     33.00  58.00   0.50    0.10    --  107.48 -77.00 -30.00   50
 14  \w    -30.00  48.00   0.50    0.05    --   43.21 -57.00-180.00  156
 15  \w   -126.00-100.00   0.50    0.10    -- -103.00 -15.00-180.00   52
 16  \w   -104.00 -70.00   0.50    0.10    -- -103.00 134.00   0.00   68
 17  \w    -83.00 -58.00   0.50    0.10    -- -103.00  89.00 -65.00   50
 18  \w    -63.00 -30.00   0.50    0.05    --  -43.21 -33.00 -21.00   66
 19  \w   -117.00 -68.00   0.50    0.05    --  -43.21 -33.00 -21.00   98
 20  \w   -165.00 -94.00   0.50    0.10    -- -103.00 -33.00 -21.00  142
 21  \w   -123.00 -90.00   0.50    0.10    -- -103.00 -15.00  60.00   66
 22  \w   -174.00-131.00   0.50    0.10    -- -103.00 -89.00 179.00   86
 23  \w    -55.00 -29.00   0.50    0.10    -- -103.00  77.00  60.00   52
 24  \w      6.00  32.00   0.50    0.05    --  -43.21  38.00  60.00   52
 25  \w    -16.00  10.00   0.50    0.05    --  -43.21  38.00 -90.00   52
 26  \w     -9.00  23.00   0.50    0.05    --  -43.21  38.00-150.00   64
 27  \w    -72.00 -39.00   0.50    0.10    -- -103.00  77.00-120.00   66
;
_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      0.0129117000
_diffrn_orient_matrix_UB_12      -0.0467050000
_diffrn_orient_matrix_UB_13      0.0430808000
_diffrn_orient_matrix_UB_21      0.0205710000
_diffrn_orient_matrix_UB_22      0.0307140000
_diffrn_orient_matrix_UB_23      0.0649167000
_diffrn_orient_matrix_UB_31      -0.0509707000
_diffrn_orient_matrix_UB_32      0.0005508000
_diffrn_orient_matrix_UB_33      0.0370767000
_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  0.0424
_diffrn_reflns_av_unetI/netI     0.0272
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            74577
_diffrn_reflns_theta_full        66.5914
_diffrn_reflns_theta_max         66.59
_diffrn_reflns_theta_min         2.28
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.159
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43491
_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 yellow'
_exptl_crystal_density_diffrn    1.3932
_exptl_crystal_description       block
_exptl_crystal_F_000             5819.9173
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.6049
_refine_diff_density_min         -0.8510
_refine_diff_density_rms         0.0863
_refine_ls_d_res_high            0.8401
_refine_ls_d_res_low             19.3887
_refine_ls_goodness_of_fit_ref   1.0350
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    144
_refine_ls_number_parameters     808
_refine_ls_number_reflns         11858
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.0349
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0487
_refine_ls_shift/su_max          0.1210
_refine_ls_shift/su_mean         0.0065
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0898P)^2^+13.3792P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1423
_refine_ls_wR_factor_ref         0.1478
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              32
_reflns_limit_h_min              0
_reflns_limit_k_max              32
_reflns_limit_k_min              0
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                10528
_reflns_number_total             11858
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d5py01111f2.cif
_cod_data_source_block           y_5
_cod_database_code               1576556
_chemical_oxdiff_formula         'C H O N Pd Cl P I'
_diffrn_oxdiff_digest_frames
;
01a8338e9d15b35cb9c8a2ce04252041940197470df
;
_diffrn_oxdiff_digest_hkl
;
0157c05978691ba113829c66d60f3874d257b9
;
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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, All O(H,H) groups
2. Restrained distances
 C24-C25 \\sim C24A-C25
 with sigma of 0.02
3. Others
 Sof(H65c)=Sof(H65d)=Sof(C67)=Sof(H67a)=Sof(H67b)=Sof(H67c)=1-FVAR(1)
 Sof(H65a)=Sof(H65b)=Sof(C66)=Sof(H66a)=Sof(H66b)=Sof(H66c)=FVAR(1)
 Fixed Sof: H0aa(0.5) H0ab(0.5) C24(0.5) H24a(0.5) H24b(0.5) H24c(0.5)
 H25a(0.5) H25b(0.5) H25c(0.5) H25d(0.5) H3a(0.5) H3b(0.5) C24A(0.5) H24d(0.5)
 H24e(0.5) H24f(0.5)
4.a Rotating group:
 O0aa(H0aa,H0ab), O1(H1a,H1b), O3(H3a,H3b)
4.b Ternary CH refined with riding coordinates:
 C2(H2), C30(H30), C33(H33), C82(H82)
4.c Secondary CH2 refined with riding coordinates:
 C11(H11a,H11b), C13(H13a,H13b), C25(H25a,H25b), C25(H25c,H25d), C47(H47a,
 H47b), C49(H49a,H49b), C65(H65c,H65d), C65(H65a,H65b), C69(H69a,H69b),
 C89(H89a,H89b)
4.d Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C19(H19), C20(H20), C21(H21), C22(H22), C43(H43),
 C44(H44), C45(H45), C53(H53), C54(H54), C55(H55), C56(H56), C57(H57), C58(H58),
  C59(H59), C60(H60), C62(H62), C63(H63), C64(H64), C71(H71), C72(H72),
 C73(H73), C85(H85), C86(H86), C87(H87), C88(H88)
4.e Idealised Me refined as rotating group:
 C12(H12a,H12b,H12c), C14(H14a,H14b,H14c), C24(H24a,H24b,H24c), C48(H48a,H48b,
 H48c), C50(H50a,H50b,H50c), C66(H66a,H66b,H66c), C67(H67a,H67b,H67c), C68(H68a,
 H68b,H68c), C90(H90a,H90b,H90c), C24A(H24d,H24e,H24f)
;
_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 1.659
_oxdiff_exptl_absorpt_empirical_full_min 0.609