A trans-palladium dichloride complex with a bulky organosulfur ligand: syntheses, structure, and applications in catalytic alkylation of acetophenone and secondary alcohols using alcohols
K., Gaatha; Kumar, Sunil; Sharma, Ashutosh; Bhuvanesh, Nattamai; Roy, Partha; Joshi, Hemant; New Journal of Chemistry 49 (2025) 3956–3968; doi:10.1039/D4NJ04901B

data_7063634
_publ_section_title
;
 A trans-palladium dichloride complex with a bulky organosulfur ligand:
 syntheses, structure, and applications in catalytic alkylation of
 acetophenone and secondary alcohols using alcohols
;
_journal_issue                   10
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              3956
_journal_page_last               3968
_journal_paper_doi               10.1039/D4NJ04901B
_journal_volume                  49
_journal_year                    2025
_chemical_formula_moiety         'C44 H36 Cl2 Pd S2'
_chemical_formula_sum            'C44 H36 Cl2 Pd S2'
_chemical_formula_weight         806.15
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2023-03-28
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-11-12 deposited with the CCDC.	2025-02-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.928(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.9194(7)
_cell_length_b                   6.1161(2)
_cell_length_c                   26.6465(9)
_cell_measurement_reflns_used    9936
_cell_measurement_temperature    110.00
_cell_measurement_theta_max      70.064
_cell_measurement_theta_min      3.316
_cell_volume                     3571.8(2)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       'APEX 3 (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_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    'XT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      110.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Venture (PHOTON III)'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0467
_diffrn_reflns_av_unetI/netI     0.0256
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            30433
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.115
_diffrn_reflns_theta_min         3.317
_diffrn_source                   'Bruker Venture Cu-IuS'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.898
_exptl_absorpt_correction_T_max  0.3841
_exptl_absorpt_correction_T_min  0.1984
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1389 before and 0.0778 after correction.
The Ratio of minimum to maximum transmission is 0.5165.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_description       plate
_exptl_crystal_F_000             1648
_exptl_crystal_size_max          0.362
_exptl_crystal_size_mid          0.132
_exptl_crystal_size_min          0.014
_refine_diff_density_max         0.363
_refine_diff_density_min         -0.459
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         3400
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0251
_refine_ls_R_factor_gt           0.0247
_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^)+(0.0360P)^2^+5.3313P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0672
_refine_ls_wR_factor_ref         0.0676
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3314
_reflns_number_total             3400
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj04901b2.cif
_cod_data_source_block           hj_sk386b
_cod_depositor_comments
'Adding full bibliography for 7063633--7063634.cif.'
_cod_database_code               7063634
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.910
_shelx_estimated_absorpt_t_min   0.189
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C12(H12A,H12B)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C16(H16),
 C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22)
;
_shelx_res_checksum              97833
_shelx_hkl_checksum              80336
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder'
_olex2_submission_original_sample_id HJB_230327_V_SK386B
_olex2_submission_special_instructions 'No special instructions were received'