Facile carbon-sulfur bond cleavage in diarylsulfonium ylides: a catalytic sulfur-to-silicon group transfer
Xueliang Huang; Richard Goddard; Nuno Maulide; Chem.Commun. 49 (2013) 4292–; doi:10.1039/c2cc35762c

data_7109194
_publ_section_title
;
 Facile carbon-sulfur bond cleavage in diarylsulfonium ylides: a catalytic
 sulfur-to-silicon group transfer
;
_journal_name_full               Chem.Commun.
_journal_page_first              4292
_journal_paper_doi               10.1039/c2cc35762c
_journal_volume                  49
_journal_year                    2013
_chemical_compound_source        'dichloromethane, diethylether'
_chemical_formula_moiety         'C46 H38 Cl2 N2 O4 Pd S2, 3(C H2 Cl2)'
_chemical_formula_sum            'C49 H44 Cl8 N2 O4 Pd S2'
_chemical_formula_weight         1178.98
_chemical_name_systematic
;
Bis(2-(ethoxycarbonyl)-3-(diphenylsulfanylidene)-3H-indole)-palladium-
dicarbonyl tri-dichloromethane solute
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_code                HUG-HA-392-01
_audit_creation_date             2012-07-20
_cell_angle_alpha                90.00
_cell_angle_beta                 105.211(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   28.301(2)
_cell_length_b                   20.495(2)
_cell_length_c                   18.0924(13)
_cell_measurement_reflns_used    137711
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.9999
_cell_measurement_theta_min      2.8017
_cell_volume                     10126.5(15)
_computing_cell_refinement       'DENZO (Bruker AXS, 2006)'
_computing_data_collection       'DATCOL (Bruker AXS, 2006)'
_computing_data_reduction        'DENZO (Bruker AXS, 2006)'
_computing_molecular_graphics    'DIAMOND (Crystal Impact GbR, 2005)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 18.02
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker AXS Enraf-Nonius KappaCCD'
_diffrn_measurement_method       'CCD \f- and \w-scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         '0.2 x 2mm^2^ focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1041
_diffrn_reflns_av_sigmaI/netI    0.0552
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            100126
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         2.81
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.917
_exptl_absorpt_correction_T_max  0.95945
_exptl_absorpt_correction_T_min  0.88566
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2008)'
_exptl_crystal_colour            yellow-orange
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_description       plate
_exptl_crystal_F_000             4784
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.776
_refine_diff_density_min         -1.515
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.530
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     590
_refine_ls_number_reflns         11175
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.530
_refine_ls_R_factor_all          0.1162
_refine_ls_R_factor_gt           0.0799
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0949P)^2^+4.5000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2120
_refine_ls_wR_factor_ref         0.2300
_reflns_number_gt                7729
_reflns_number_total             11175
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc35762c.txt
_cod_data_source_block           7095
_cod_original_cell_volume        10126.3(15)
_cod_original_sg_symbol_Hall     '-c 2yc'
_cod_original_sg_symbol_H-M      'c 2/c'
_cod_database_code               7109194