PdII and PtII complexes bearing acetamide and thioacetamide functionalized heteroscorpionates and their application in the hydrosilylation of terminal alkynes
Ortiz-Hernández, M.; Noguez-Maldonado, V. I.; Salazar-Pereda, V.; Gonzalez-Montiel, S.; Mendoza-Espinosa, D.; Suárez, A.; Cristobal, C.; New Journal of Chemistry 50 (2026) 4415–4424; doi:10.1039/D5NJ04709A

data_7064226
_publ_section_title
;
 PdII and PtII complexes bearing acetamide and thioacetamide
 functionalized heteroscorpionates and their application in the
 hydrosilylation of terminal alkynes
;
_journal_issue                   10
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              4415
_journal_page_last               4424
_journal_paper_doi               10.1039/D5NJ04709A
_journal_volume                  50
_journal_year                    2026
_chemical_formula_moiety         'C36 H40 N10 Pd S2'
_chemical_formula_sum            'C36 H40 N10 Pd S2'
_chemical_formula_weight         783.30
_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     dual
_audit_creation_date             2024-12-02
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2026-01-16 deposited with the CCDC.	2026-02-09 downloaded from the CCDC.
;
_cell_angle_alpha                94.7911(18)
_cell_angle_beta                 90.678(2)
_cell_angle_gamma                111.144(2)
_cell_formula_units_Z            2
_cell_length_a                   10.7568(3)
_cell_length_b                   10.9438(2)
_cell_length_c                   16.5867(4)
_cell_measurement_reflns_used    22127
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.9610
_cell_measurement_theta_min      3.4220
_cell_volume                     1812.92(8)
_computing_cell_refinement       'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET))'
_computing_data_reduction        'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_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      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3659
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -39.00  48.00   1.00   12.50    --   11.37 -88.00 140.28   87
  2  \w    -13.00  86.00   1.00   12.50    --   11.37  37.00-180.00   99
  3  \w    -21.00  88.00   1.00   12.50    --   11.37  77.00 -90.00  109
  4  \w    -17.00  85.00   1.00   12.50    --   11.37  57.00  60.00  102
  5  \w    -65.00  44.00   1.00   12.50    --   11.37 -77.00-120.00  109
  6  \w    -25.00  52.00   1.00   12.50    --   11.37 -99.00 -30.00   77
  7  \w    -39.00  48.00   1.00   12.50    --   11.37 -88.00  47.86   87
  8  \w    -67.00 -19.00   1.00   12.50    --   -9.96 126.00 -73.42   48
  9  \w    -67.00 -19.00   1.00   12.50    --   -9.96 126.00  30.52   48
 10  \w    -79.00 -31.00   1.00   12.50    --   -9.96 145.00-163.99   48
 11  \w    -84.00  14.00   1.00   12.50    --   -9.96 -37.00  90.00   98
 12  \w    -10.00  63.00   1.00   12.50    --   11.37-117.00-155.00   73
 13  \w    -25.00  52.00   1.00   12.50    --   11.37 -99.00   0.00   77
 14  \w    -77.00 100.00   1.00   12.50    --   11.37   0.00-180.00  177
 15  \w    -77.00 100.00   1.00   12.50    --   11.37   0.00-150.00  177
 16  \w    -77.00 100.00   1.00   12.50    --   11.37   0.00-120.00  177
 17  \w    -77.00 100.00   1.00   12.50    --   11.37   0.00 -90.00  177
 18  \w    -77.00 100.00   1.00   12.50    --   11.37   0.00 -60.00  177
 19  \w    -25.00  52.00   1.00   12.50    --   11.37 -99.00-120.00   77
 20  \w    -77.00 100.00   1.00   12.50    --   11.37   0.00   0.00  177
 21  \w    -77.00  -8.00   1.00   12.50    --   11.37   0.00  30.00   69
 22  \w    -77.00  -2.00   1.00   12.50    --   11.37   0.00 -30.00   75
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0663481000
_diffrn_orient_matrix_UB_12      0.0149872000
_diffrn_orient_matrix_UB_13      0.0150540000
_diffrn_orient_matrix_UB_21      -0.0192169000
_diffrn_orient_matrix_UB_22      0.0121921000
_diffrn_orient_matrix_UB_23      0.0397243000
_diffrn_orient_matrix_UB_31      -0.0154015000
_diffrn_orient_matrix_UB_32      -0.0670742000
_diffrn_orient_matrix_UB_33      0.0063764000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0673
_diffrn_reflns_av_unetI/netI     0.0262
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            107729
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         3.125
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.668
_exptl_absorpt_correction_T_max  0.945
_exptl_absorpt_correction_T_min  0.894
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.90 (Rigaku Oxford Diffraction, 2023)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_description       block
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.186
_exptl_crystal_size_mid          0.126
_exptl_crystal_size_min          0.072
_refine_diff_density_max         0.509
_refine_diff_density_min         -0.246
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     459
_refine_ls_number_reflns         6611
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0425
_refine_ls_R_factor_gt           0.0292
_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^)+(0.0257P)^2^+1.1114P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0610
_refine_ls_wR_factor_ref         0.0666
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5468
_reflns_number_total             6611
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj04709a2.cif
_cod_data_source_block           sgm_05_2022_dmo
_cod_depositor_comments
'Adding full bibliography for 7064225--7064228.cif.'
_cod_database_code               7064226
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C36 H42 N10 S2 Pd1 Cl2'
_shelx_estimated_absorpt_t_max   0.955
_shelx_estimated_absorpt_t_min   0.884
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C28-C30 \\sim C28-C30A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C30 \\sim C30A: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
4. Rigid body (RIGU) restrains
 C30, C30A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C30A)=Sof(H30D)=Sof(H30E)=Sof(H30F)=1-FVAR(1)
 Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(H30C)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C1(H1), C19(H19)
6.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C9(H9), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C22(H22),
 C27(H27), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36)
6.c Idealised Me refined with riding coordinates:
 C30(H30A,H30B,H30C), C30A(H30D,H30E,H30F)
6.d Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C29(H29A,H29B,H29C)
;
_shelx_res_checksum              171
_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 1.200
_oxdiff_exptl_absorpt_empirical_full_min 0.852