A Robust [Pd(BIAN-IPr#)Cl2(H2O)] Catalyst Employing Water as a Disposable Ligand for C–S Cross Coupling of Aryl Chlorides and Thiols
Quan, Ziyi; Wang, Zheng; Liu, Yaxu; Sun, Yuanchao; Wang, Bo; Dalton Transactions  (2026) –; doi:10.1039/D6DT00623J

data_7720849
_publ_section_title
;
 A robust [Pd(BIAN-IPr<sup>#</sup>)Cl<sub>2</sub>(H<sub>2</sub>O)]
 catalyst employing water as a disposable ligand for C-S cross coupling of
 aryl chlorides and thiols.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6934
_journal_page_last               6943
_journal_paper_doi               10.1039/d6dt00623j
_journal_volume                  55
_journal_year                    2026
_chemical_formula_moiety         'C103 H78 Cl2 N2 O Pd, 2(H2 O)'
_chemical_formula_sum            'C103 H82 Cl2 N2 O3 Pd'
_chemical_formula_weight         1573.00
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2qgx6b
_audit_creation_date             2025-08-17
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2025-12-17 deposited with the CCDC.	2026-04-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.3042(2)
_cell_length_b                   25.7788(2)
_cell_length_c                   29.4625(3)
_cell_measurement_reflns_used    23986
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      76.3270
_cell_measurement_theta_min      2.2600
_cell_volume                     16180.7(3)
_computing_cell_refinement       'CrysAlisPro 1.171.43.144a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.144a (release 23-01-2025))'
_computing_data_reduction        'CrysAlisPro 1.171.43.144a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.956
_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   -162.00 -91.00   0.50    1.50    -- -103.57-116.00 -75.00  142
  2  \w   -155.00 -94.00   0.50    1.50    -- -103.57 -12.00  80.00  122
  3  \w    -68.00 -41.00   0.50    1.50    -- -103.57  61.00 -30.00   54
  4  \w    -18.00  25.00   0.50    0.38    --  -45.61  12.00-107.00   86
  5  \w    -22.00  22.00   0.50    0.38    --   45.61 -12.00  80.00   88
  6  \w    -20.00  27.00   0.50    0.38    --   45.61 -19.00   0.00   94
  7  \w     36.00  70.00   0.50    1.50    --  103.57 -61.00  60.00   68
  8  \w    145.00 172.00   0.50    1.50    --  103.57  45.00 -90.00   54
  9  \w     80.00 105.00   0.50    1.50    --  103.57 -95.00 -30.00   50
 10  \w     39.00 106.00   0.50    1.50    --  103.57-125.00  60.00  134
 11  \w     32.00 116.00   0.50    1.50    --  103.57-142.00-149.00  168
 12  \w     51.00  99.00   0.50    0.38    --   45.61-142.00-149.00   96
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0112857000
_diffrn_orient_matrix_UB_12      0.0502291000
_diffrn_orient_matrix_UB_13      -0.0268895000
_diffrn_orient_matrix_UB_21      0.0028794000
_diffrn_orient_matrix_UB_22      -0.0309003000
_diffrn_orient_matrix_UB_23      -0.0447217000
_diffrn_orient_matrix_UB_31      -0.0715117000
_diffrn_orient_matrix_UB_32      -0.0092435000
_diffrn_orient_matrix_UB_33      0.0025489000
_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  0.0887
_diffrn_reflns_av_unetI/netI     0.0587
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            58098
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.521
_diffrn_reflns_theta_min         3.000
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.880
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.06585
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.144a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.291
_exptl_crystal_description       block
_exptl_crystal_F_000             6544
_refine_diff_density_max         2.042
_refine_diff_density_min         -2.141
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1007
_refine_ls_number_reflns         16268
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0973
_refine_ls_R_factor_gt           0.0861
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1856P)^2^+15.1308P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2434
_refine_ls_wR_factor_ref         0.2563
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13284
_reflns_number_total             16268
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6dt00623j2.cif
_cod_data_source_block           195_auto
_cod_depositor_comments
'Adding full bibliography for 7720849--7720851.cif.'
_cod_database_code               7720849
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Free rotating group:
 O1(H1A,H1B), O2(H2A,H2B)
2.b Rotating group:
 O005(H00A,H00B)
2.c Ternary CH refined with riding coordinates:
 C00I(H00I), C00J(H00J), C00R(H00R), C00Z(H00Z), C012(H012), C016(H016)
2.d Aromatic/amide H refined with riding coordinates:
 C00F(H00F), C00L(H00L), C00M(H00M), C00O(H00O), C00X(H00X), C013(H013),
 C014(H014), C015(H015), C017(H017), C01C(H01C), C01E(H01E), C01F(H01F),
 C01H(H01H), C01I(H01I), C01J(H01J), C01K(H01K), C01L(H01L), C01M(H01M),
 C01N(H01N), C01O(H01O), C01P(H01P), C01Q(H01Q), C01R(H01R), C01S(H01S),
 C01T(H01T), C01U(H01U), C01V(H01V), C01W(H01W), C01X(H01X), C01Y(H01Y),
 C01Z(H01Z), C020(H020), C021(H021), C022(H022), C023(H023), C024(H024),
 C025(H025), C026(H026), C027(H027), C028(H028), C029(H029), C02A(H02A),
 C02B(H02B), C02D(H02D), C02E(H02E), C02F(H02F), C02G(H02G), C02H(H02H),
 C02I(H02I), C02J(H02J), C02K(H02K), C02L(H02L), C02M(H02M), C02N(H02N),
 C02O(H02O), C02P(H02P), C02Q(H02Q), C02R(H02R), C02S(H02S), C02T(H02T),
 C02U(H02U), C02V(H02V), C02W(H02W), C02X(H02X), C02Y(H02Y), C02Z(H02Z),
 C030(H030), C031(H031), C032(H032), C033(H033)
;
_shelx_res_checksum              9633
_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 4.756
_oxdiff_exptl_absorpt_empirical_full_min 0.386