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_7063402
_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_moiety         'C41 H34 Cl N P2 Pd S, 0.5 O'
_chemical_formula_sum            'C41 H34 Cl N O0.5 P2 Pd S'
_chemical_formula_weight         784.54
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_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                90
_cell_angle_beta                 96.7350(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.93610(10)
_cell_length_b                   16.70070(10)
_cell_length_c                   40.8473(4)
_cell_measurement_reflns_used    17675
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      76.7390
_cell_measurement_theta_min      4.3410
_cell_volume                     7408.89(11)
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_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 0.986
_diffrn_measured_fraction_theta_max 0.017
_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    -26.00  26.00   0.50    0.54    --  -47.82  19.00  60.00  104
  2  \w     -9.00  25.00   0.50    0.54    --  -47.82  98.00 -28.00   68
  3  \w    -42.00 -16.00   0.50    4.16    --  -86.25  37.00 -60.00   52
  4  \w    -41.00 -14.00   0.50    4.16    --  -86.25  37.00-120.00   54
  5  \w    -42.00 -16.00   0.50    4.16    --  -86.25  37.00 -90.00   52
  6  \w    -42.00 -15.00   0.50    4.16    --  -86.25  37.00 -30.00   54
  7  \w    -80.00 -16.00   0.50    0.54    --  -47.82  98.00 -28.00  128
  8  \w    -42.00 -17.00   0.50    4.16    --  -86.25  37.00 120.00   50
  9  \w    -42.00 -17.00   0.50    4.16    --  -86.25  37.00 150.00   50
 10  \w    -76.00 -50.00   0.50    4.16    --  -86.25  98.00 -28.00   52
 11  \w    -24.00  25.00   0.50    0.54    --   47.82 -19.00-120.00   98
 12  \w     14.00  45.00   0.50    0.54    --   47.82 -98.00-135.00   62
 13  \w     62.00  88.00   0.50    4.16    --  107.74 -98.00-135.00   52
 14  \w     72.00 106.00   0.50    4.16    --  107.74 -77.00-120.00   68
 15  \w     65.00 106.00   0.50    4.16    --  107.74 -77.00 -30.00   82
 16  \w     37.00  62.00   0.50    4.16    --  107.74 -57.00  60.00   50
 17  \w     35.00  61.00   0.50    4.16    --  107.74 -57.00  90.00   52
 18  \w     36.00  62.00   0.50    4.16    --  107.74 -57.00 120.00   52
 19  \w     35.00  60.00   0.50    4.16    --  107.74 -57.00  30.00   50
 20  \w     37.00  66.00   0.50    4.16    --  107.74 -57.00 -60.00   58
 21  \w     37.00 104.00   0.50    4.16    --  107.74 -99.00 -90.00  134
 22  \w     35.00  65.00   0.50    4.16    --  107.74 -77.00-120.00   60
 23  \w    100.00 169.00   0.50    4.16    --  107.74  37.00 -60.00  138
 24  \w    112.00 170.00   0.50    4.16    --  107.74  98.00 -28.00  116
 25  \w     95.00 177.00   0.50    4.16    --  107.74  37.00  30.00  164
 26  \w   -119.00 -82.00   0.50    0.54    --  -47.82-125.00  30.00   74
 27  \w   -157.00-112.00   0.50    4.16    --  -86.25 -98.00-135.00   90
;
_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      -0.0190961000
_diffrn_orient_matrix_UB_12      -0.0119345000
_diffrn_orient_matrix_UB_13      -0.0376557000
_diffrn_orient_matrix_UB_21      -0.0483002000
_diffrn_orient_matrix_UB_22      0.0864265000
_diffrn_orient_matrix_UB_23      -0.0044147000
_diffrn_orient_matrix_UB_31      0.1320103000
_diffrn_orient_matrix_UB_32      0.0299049000
_diffrn_orient_matrix_UB_33      -0.0022673000
_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  0.0611
_diffrn_reflns_av_unetI/netI     0.0423
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.017
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            25202
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.017
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.332
_diffrn_reflns_theta_min         3.268
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.285
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70274
_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            red
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_description       block
_exptl_crystal_F_000             3200
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.164
_refine_diff_density_min         -1.929
_refine_diff_density_rms         0.168
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     465
_refine_ls_number_reflns         7339
_refine_ls_number_restraints     114
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0631
_refine_ls_R_factor_gt           0.0341
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0593P)^2^+10.5902P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0928
_refine_ls_wR_factor_ref         0.1107
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6657
_reflns_number_total             7339
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj02694b2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7063402--7063405.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C41 H34 Cl1 N1 O0.5 P2 Pd1 S1'
_cod_database_code               7063402
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.744
_shelx_estimated_absorpt_t_max   0.744
_oxdiff_exptl_absorpt_empirical_full_min 0.744
_oxdiff_exptl_absorpt_empirical_full_max 1.571
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_oxdiff_digest_frames
;
010cea9c348ec788b4a57cd0b91e95d23100031d107
;
_diffrn_oxdiff_digest_hkl
;
013618f97ba0b45090930e1f479f385b2d2f41
;
_shelx_res_checksum              96488