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_7064227
_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 Pt S2'
_chemical_formula_sum            'C36 H40 N10 Pt S2'
_chemical_formula_weight         871.99
_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             2025-10-29
_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                94.8680(10)
_cell_angle_beta                 90.7820(10)
_cell_angle_gamma                110.887(2)
_cell_formula_units_Z            2
_cell_length_a                   10.8601(2)
_cell_length_b                   10.8921(2)
_cell_length_c                   16.3934(2)
_cell_measurement_reflns_used    54981
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.2450
_cell_measurement_theta_min      3.2480
_cell_volume                     1803.19(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_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 0.974
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -10.00   86.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       11.4454   37.0000   90.0000 96

  2 omega  -18.00   80.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       11.4454   77.0000 -180.0000 98

  3 omega  -63.00   44.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       11.4454  -77.0000  -60.0000 107

  4 omega  -25.00   31.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.9610  -99.0000  -90.0000 56

  5 omega  -34.00   65.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.9610   37.0000 -180.0000 99

  6 omega  -17.00   85.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       11.4454   57.0000  -90.0000 102

  7 omega  -25.00   52.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       11.4454  -99.0000  -90.0000 77

  8 omega  -25.00   52.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       11.4454  -99.0000  -30.0000 77

  9 omega  -25.00   52.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       11.4454  -99.0000   90.0000 77

 10 omega  -84.00   14.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.9610  -37.0000   90.0000 98

 11 omega  -25.00   52.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       11.4454  -99.0000   30.0000 77

 12 omega  -25.00   52.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       11.4454  -99.0000 -150.0000 77

 13 omega  -13.00   86.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       11.4454   37.0000  -30.0000 99

 14 omega  -25.00   52.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       11.4454  -99.0000  120.0000 77

 15 omega  -65.00   44.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       11.4454  -77.0000  150.0000 109

 16 omega  -65.00   44.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       11.4454  -77.0000 -180.0000 109

 17 omega  -77.00  100.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       11.4454    0.0000 -180.0000 177

 18 omega  -77.00  100.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       11.4454    0.0000 -150.0000 177

 19 omega  -77.00  100.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       11.4454    0.0000 -120.0000 177

 20 omega  -77.00  100.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       11.4454    0.0000  -90.0000 177

 21 omega  -25.00   52.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       11.4454  -99.0000   60.0000 77

 22 omega  -77.00  100.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       11.4454    0.0000  -30.0000 177

 23 omega  -77.00  100.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       11.4454    0.0000    0.0000 177

 24 omega  -77.00    0.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       11.4454    0.0000   30.0000 77

 25 omega  -77.00  100.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       11.4454    0.0000  -60.0000 177
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0603123000
_diffrn_orient_matrix_UB_12      -0.0532432000
_diffrn_orient_matrix_UB_13      0.0031380000
_diffrn_orient_matrix_UB_21      -0.0252677000
_diffrn_orient_matrix_UB_22      0.0430904000
_diffrn_orient_matrix_UB_23      0.0230654000
_diffrn_orient_matrix_UB_31      -0.0249362000
_diffrn_orient_matrix_UB_32      0.0145565000
_diffrn_orient_matrix_UB_33      -0.0367150000
_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  0.0466
_diffrn_reflns_av_unetI/netI     0.0141
_diffrn_reflns_Laue_measured_fraction_full 0.974
_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       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            125812
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         3.052
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.048
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38259
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.606
_exptl_crystal_description       Block
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.637
_refine_diff_density_min         -0.493
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     450
_refine_ls_number_reflns         6347
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0184
_refine_ls_R_factor_gt           0.0161
_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^)+(0.0190P)^2^+1.2487P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0395
_refine_ls_wR_factor_ref         0.0410
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6016
_reflns_number_total             6347
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj04709a2.cif
_cod_data_source_block           dme-218
_cod_depositor_comments
'Adding full bibliography for 7064225--7064228.cif.'
_cod_database_code               7064227
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'C12 H26 N6 Pt1 Cl2'
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.a Ternary CH refined with riding coordinates:
 C8(H8), C19(H19)
2.b Aromatic/amide H refined with riding coordinates:
 C34(H34), C7(H7), C16(H16), C11(H11), C29(H29), C6(H6), C22(H22), C26(H26),
 C3(H3), C5(H5), C24(H24), C23(H23), C25(H25), C4(H4)
2.c Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C18(H18A,H18B,H18C), C36(H36A,H36B,H36C), C15(H15A,H15B,
 H15C), C31(H31A,H31B,H31C), C10(H10A,H10B,H10C), C28(H28A,H28B,H28C), C13(H13A,
 H13B,H13C)
;
_olex2_date_sample_data_collection 2025-10-16
_olex2_submission_special_instructions 'No special instructions were received'