Experimental and Theoretical Studies on the Mechanism of the C‒S Bond Activation of PdII Thiolate/Thioether Complexes
Kumar, Sushil; Guyon, Fabrice; Knorr, Michael; Labat, Stéphane; Miqueu, Karinne; Golz, Christopher; Strohmann, Carsten; Organometallics 36 (2017) 1303–; doi:10.1021/acs.organomet.7b00039

data_4087310
_publ_section_title
;
 Experimental and Theoretical Studies on the Mechanism of the C--S Bond
 Activation of PdII Thiolate/Thioether Complexes
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1303
_journal_paper_doi               10.1021/acs.organomet.7b00039
_journal_volume                  36
_journal_year                    2017
_chemical_formula_moiety         'C14 H21 P Pd S10'
_chemical_formula_sum            'C14 H21 P Pd S10'
_chemical_formula_weight         647.28
_chemical_name_systematic
;
 ? 
;
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-07-01
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 98.541(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.8179(8)
_cell_length_b                   29.265(2)
_cell_length_c                   7.6040(6)
_cell_measurement_reflns_used    5461
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.4370
_cell_measurement_theta_min      2.3740
_cell_volume                     2380.6(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.15
_diffrn_detector_area_resol_mean 16.0560
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega   57.00  100.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       26.1808  156.0000  -20.0000 43

  2 omega   45.00   74.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       26.1808   57.0000  -30.0000 29

  3 omega  -41.00   58.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       26.1808  -57.0000  120.0000 99

  4 omega   -3.00   92.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       26.1808   77.0000  150.0000 95

  5 omega   31.00   85.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       26.1808   57.0000  150.0000 54

  6 omega  -17.00   24.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.4308  -99.0000   30.0000 41

  7 omega  -25.00    9.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.4308  -99.0000 -180.0000 34

  8 omega  -24.00    4.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.4308  -99.0000    0.0000 28

  9 omega  -92.00   51.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.4308  -19.0000  -30.0000 143

 10 omega -118.00  -93.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.4308 -179.0000  -90.0000 25
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0069503000
_diffrn_orient_matrix_UB_12      -0.0172054000
_diffrn_orient_matrix_UB_13      -0.0634495000
_diffrn_orient_matrix_UB_21      0.0228049000
_diffrn_orient_matrix_UB_22      0.0165736000
_diffrn_orient_matrix_UB_23      -0.0551817000
_diffrn_orient_matrix_UB_31      0.0618801000
_diffrn_orient_matrix_UB_32      -0.0041860000
_diffrn_orient_matrix_UB_33      0.0425778000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0789
_diffrn_reflns_av_unetI/netI     0.0637
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            20358
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.997
_diffrn_reflns_theta_min         2.358
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.725
_exptl_absorpt_correction_T_max  0.8461
_exptl_absorpt_correction_T_min  0.6251
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.806
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.170
_refine_diff_density_min         -0.715
_refine_diff_density_rms         0.172
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.144
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         4679
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.144
_refine_ls_R_factor_all          0.0633
_refine_ls_R_factor_gt           0.0471
_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^)+(0.0518P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1116
_refine_ls_wR_factor_ref         0.1229
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3703
_reflns_number_total             4679
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om7b00039_si_002.cif
_cod_data_source_block           compound1
_cod_database_code               4087310
_chemical_oxdiff_formula         'C5 H12 S6 Pd'
_shelx_estimated_absorpt_t_max   0.846
_shelx_estimated_absorpt_t_min   0.626
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.01
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C11(H11A,H11B), C13(H13A,H13B)
2.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C),
 C14(H14A,H14B,H14C)
;
_shelx_res_checksum              10168
_shelx_hkl_checksum              9557
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'