Bimetallic Pd/Cu complexes of pyridylchalcogenolates and their catalytic activity in the Sonogashira reaction
Pal, M. K.; Wadawale, A. P.; Dey, S.; New Journal of Chemistry 48 (2024) 15823–15829; doi:10.1039/D4NJ02694B

data_7063404
_publ_section_title
;
 Bimetallic Pd/Cu complexes of pyridylchalcogenolates and their catalytic
 activity in the Sonogashira reaction
;
_journal_issue                   36
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              15823
_journal_page_last               15829
_journal_paper_doi               10.1039/D4NJ02694B
_journal_volume                  48
_journal_year                    2024
_chemical_formula_sum            'C118 H98 Cl2 Cu2 N2 P6 Pd S2'
_chemical_formula_weight         2098.30
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2024-04-11 deposited with the CCDC.	2024-08-14 downloaded from the CCDC.
;
_cell_angle_alpha                69.4180(10)
_cell_angle_beta                 78.0530(10)
_cell_angle_gamma                83.5570(10)
_cell_formula_units_Z            1
_cell_length_a                   11.68270(10)
_cell_length_b                   14.22020(10)
_cell_length_c                   16.74980(10)
_cell_measurement_reflns_used    24515
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      76.8090
_cell_measurement_theta_min      2.8840
_cell_volume                     2546.24(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'OLEX 1.2'
_diffrn_ambient_temperature      298(2)
_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 0.963
_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    -24.00  62.00   0.50    0.05    --   47.70 -56.00 100.00  172
  2  \w     34.00  95.00   0.50    0.05    --   47.70-125.00 120.00  122
  3  \w     35.00  62.00   0.50    0.20    --  107.74 -56.00 100.00   54
  4  \w     39.00  64.00   0.50    0.20    --  107.74 -57.00 120.00   50
  5  \w     62.00  88.00   0.50    0.20    --  107.74 -99.00 150.00   52
  6  \w     49.00  91.00   0.50    0.20    --  107.74 -99.00 120.00   84
  7  \w     39.00  98.00   0.50    0.20    --  107.74 -99.00  90.00  118
  8  \w     76.00 103.00   0.50    0.20    --  107.74 -99.00  30.00   54
  9  \w     47.00  81.00   0.50    0.20    --  107.74 -77.00 -60.00   68
 10  \w     81.00 106.00   0.50    0.20    --  107.74 -99.00 -90.00   50
 11  \w     91.00 116.00   0.50    0.20    --  107.74-131.00-114.81   50
 12  \w     73.00 108.00   0.50    0.20    --  107.74-125.00-150.00   70
 13  \w     81.00 111.00   0.50    0.20    --  107.74-125.00-120.00   60
 14  \w     79.00 105.00   0.50    0.20    --  107.74 -77.00-180.00   52
 15  \w     76.00 106.00   0.50    0.20    --  107.74 -77.00-120.00   60
 16  \w     45.00  71.00   0.50    0.20    --  107.74-131.00-114.81   52
 17  \w     35.00 110.00   0.50    0.20    --  107.74-125.00 -30.00  150
 18  \w     46.00 107.00   0.50    0.20    --  107.74-104.00  20.41  122
 19  \w     43.00 108.00   0.50    0.20    --  107.74-125.00  90.00  130
 20  \w     96.00 177.00   0.50    0.20    --  107.74  19.00  30.00  162
 21  \w    151.00 177.00   0.50    0.20    --  107.74  57.00  30.00   52
 22  \w    147.00 177.00   0.50    0.20    --  107.74 125.00  90.00   60
 23  \w    133.00 175.00   0.50    0.20    --  107.74  37.00 120.00   84
 24  \w    116.00 178.00   0.50    0.20    --  107.74  19.00   0.00  124
 25  \w    129.00 155.00   0.50    0.20    --  107.74  56.00-116.00   52
 26  \w     72.00 119.00   0.50    0.05    --   47.70  56.00-116.00   94
 27  \w     96.00 176.00   0.50    0.20    --  107.74 125.00  30.00  160
 28  \w     95.00 175.00   0.50    0.20    --  107.74  37.00  90.00  160
 29  \w     96.00 125.00   0.50    0.20    --  107.74 125.00  90.00   58
 30  \w     93.00 140.00   0.50    0.20    --  107.74  57.00  30.00   94
 31  \w     95.00 127.00   0.50    0.20    --  107.74  37.00 120.00   64
 32  \w     35.00  67.00   0.50    0.20    --  107.74 -77.00-120.00   64
 33  \w     35.00  65.00   0.50    0.20    --  107.74 -57.00-180.00   60
 34  \w     35.00  71.00   0.50    0.20    --  107.74 -77.00-180.00   72
 35  \w     35.00  61.00   0.50    0.20    --  107.74-125.00-150.00   52
 36  \w    -20.00  15.00   0.50    0.05    --   47.70 -19.00-180.00   70
 37  \w    -57.00  23.00   0.50    0.05    --  -47.70  56.00-116.00  160
 38  \w    -42.00  14.00   0.50    0.05    --  -47.70  37.00 -30.00  112
 39  \w    -42.00 -13.00   0.50    0.20    --  -86.25  37.00-120.00   58
 40  \w    -51.00 -15.00   0.50    0.20    --  -86.25  56.00-116.00   72
 41  \w    -40.00 -15.00   0.50    0.20    --  -86.25  37.00 -30.00   50
 42  \w    -40.00 -15.00   0.50    0.20    --  -86.25  37.00   0.00   50
 43  \w    -39.00 -14.00   0.50    0.20    --  -86.25  37.00  90.00   50
 44  \w    -64.00 -23.00   0.50    0.20    --  -86.25  57.00  60.00   82
 45  \w   -119.00 -56.00   0.50    0.05    --  -47.70 -56.00 100.00  126
 46  \w   -108.00 -83.00   0.50    0.05    --  -47.70-125.00-150.00   50
 47  \w   -118.00 -93.00   0.50    0.05    --  -47.70-125.00-180.00   50
 48  \w   -113.00 -74.00   0.50    0.05    --  -47.70-125.00  30.00   78
 49  \w   -156.00-120.00   0.50    0.20    --  -86.25 -56.00 100.00   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0917046000
_diffrn_orient_matrix_UB_12      0.0329865000
_diffrn_orient_matrix_UB_13      0.0666213000
_diffrn_orient_matrix_UB_21      -0.0913977000
_diffrn_orient_matrix_UB_22      -0.0635190000
_diffrn_orient_matrix_UB_23      -0.0096779000
_diffrn_orient_matrix_UB_31      0.0379201000
_diffrn_orient_matrix_UB_32      -0.0910709000
_diffrn_orient_matrix_UB_33      0.0737826000
_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  0.0452
_diffrn_reflns_av_unetI/netI     0.0410
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            35587
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.076
_diffrn_reflns_theta_min         2.865
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.040
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55650
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.57a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_description       plate
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.673
_refine_diff_density_min         -0.962
_refine_diff_density_rms         0.059
_refine_ls_extinction_coef       0.00038(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     602
_refine_ls_number_reflns         10386
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0420
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0442P)^2^+1.9832P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1063
_refine_ls_wR_factor_ref         0.1075
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9789
_reflns_number_total             10386
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj02694b2.cif
_cod_data_source_block           shelx_CCDC2
_cod_depositor_comments
'Adding full bibliography for 7063402--7063405.cif.'
_cod_database_code               7063404
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.432
_shelx_estimated_absorpt_t_max   0.824
_oxdiff_exptl_absorpt_empirical_full_min 0.586
_oxdiff_exptl_absorpt_empirical_full_max 2.610
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_oxdiff_digest_frames
;
011699cc7111c7e2e8867e00777081f0c200101e38c
;
_diffrn_oxdiff_digest_hkl
;
01ad21d8fdcf128d1f03cbd2fb08b7e63999c8
;
_shelx_res_checksum              59121