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_7063403
_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            'C48 H46 N2 O2 P2 Pd S2'
_chemical_formula_weight         915.33
_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     iter
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2024-04-11 deposited with the CCDC.	2024-08-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.4320(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.1283(2)
_cell_length_b                   19.3886(3)
_cell_length_c                   8.76560(10)
_cell_measurement_reflns_used    10523
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      76.5120
_cell_measurement_theta_min      3.3850
_cell_volume                     2230.49(5)
_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_molecular_graphics    'ORTEP 3 for Windows'
_computing_publication_material  'WinGX 2023.1'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_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 0.994
_diffrn_measured_fraction_theta_max 0.953
_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  26.00   0.50    0.08    --  -47.82  33.00-103.00  122
  2  \w    -38.00 -13.00   0.50    0.32    --  -86.25  33.00-103.00   50
  3  \w    -42.00 -17.00   0.50    0.32    --  -86.25  37.00-120.00   50
  4  \w    -39.00 -14.00   0.50    0.32    --  -86.25  37.00-180.00   50
  5  \w    -41.00 -16.00   0.50    0.32    --  -86.25  37.00-150.00   50
  6  \w    -65.00 -14.00   0.50    0.32    --  -86.25  57.00 -30.00  102
  7  \w    -23.00  26.00   0.50    0.08    --  -47.82  19.00  30.00   98
  8  \w    -52.00 -16.00   0.50    0.32    --  -86.25  57.00  60.00   72
  9  \w    -65.00 -40.00   0.50    0.32    --  -86.25  57.00  30.00   50
 10  \w   -100.00 -43.00   0.50    0.08    --  -47.82 -33.00  97.00  114
 11  \w     78.00 103.00   0.50    0.08    --   47.82  33.00-103.00   50
 12  \w     94.00 172.00   0.50    0.32    --  107.74  33.00-103.00  156
 13  \w    106.00 135.00   0.50    0.32    --  107.74 125.00  90.00   58
 14  \w    139.00 168.00   0.50    0.32    --  107.74 125.00  90.00   58
 15  \w     40.00  65.00   0.50    0.32    --  107.74 -57.00-150.00   50
 16  \w     36.00  61.00   0.50    0.32    --  107.74 -57.00-180.00   50
 17  \w     43.00 105.00   0.50    0.32    --  107.74 -77.00-180.00  124
 18  \w     35.00  60.00   0.50    0.32    --  107.74 -57.00 -60.00   50
 19  \w     56.00  99.00   0.50    0.32    --  107.74 -99.00 -60.00   86
 20  \w     37.00  66.00   0.50    0.32    --  107.74 -57.00  60.00   58
 21  \w     35.00  60.00   0.50    0.32    --  107.74 -57.00  90.00   50
 22  \w     35.00  94.00   0.50    0.32    --  107.74 -77.00 150.00  118
 23  \w     39.00  96.00   0.50    0.32    --  107.74-125.00  60.00  114
 24  \w     43.00  93.00   0.50    0.32    --  107.74 -99.00 150.00  100
 25  \w      2.00  27.00   0.50    0.08    --   47.82 -33.00  97.00   50
 26  \w     35.00  60.00   0.50    0.32    --  107.74 -57.00 -30.00   50
 27  \w     38.00  64.00   0.50    0.32    --  107.74 -57.00-120.00   52
 28  \w   -119.00 -76.00   0.50    0.08    --  -47.82-125.00-180.00   86
 29  \w   -116.00 -91.00   0.50    0.32    --  -86.25 -33.00  97.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1552368000
_diffrn_orient_matrix_UB_12      0.0337444000
_diffrn_orient_matrix_UB_13      0.0209308000
_diffrn_orient_matrix_UB_21      0.0369300000
_diffrn_orient_matrix_UB_22      -0.0019511000
_diffrn_orient_matrix_UB_23      0.1153081000
_diffrn_orient_matrix_UB_31      0.0738323000
_diffrn_orient_matrix_UB_32      0.0719019000
_diffrn_orient_matrix_UB_33      -0.0066672000
_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  0.0527
_diffrn_reflns_av_unetI/netI     0.0475
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            16240
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.205
_diffrn_reflns_theta_min         3.368
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.219
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53481
_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    1.363
_exptl_crystal_description       plate
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.912
_refine_diff_density_min         -1.148
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     261
_refine_ls_number_reflns         4504
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0353
_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^)+(0.0478P)^2^+1.9794P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0898
_refine_ls_wR_factor_ref         0.1109
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3911
_reflns_number_total             4504
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj02694b2.cif
_cod_data_source_block           shelx_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7063402--7063405.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7063403
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.623
_shelx_estimated_absorpt_t_max   0.903
_oxdiff_exptl_absorpt_empirical_full_min 0.556
_oxdiff_exptl_absorpt_empirical_full_max 2.421
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              30141