Heterobimetallic Pd-Sn Catalysis: Michael Addition Reaction with C-, N-, O-, and S-Nucleophiles and in Situ Diagnostics
Debjit Das; Sanjay Pratihar; Sujit Roy; Journal of Organic Chemistry 78 (2013) 2430–2442; doi:10.1021/jo302643v

data_4028032
_publ_section_title
;
 Heterobimetallic Pd-Sn Catalysis: Michael Addition Reaction with C-, N-,
 O-, and S-Nucleophiles and in Situ Diagnostics
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              2430
_journal_page_last               2442
_journal_paper_doi               10.1021/jo302643v
_journal_volume                  78
_journal_year                    2013
_chemical_formula_sum            'C15 H14 O S'
_chemical_formula_weight         242.32
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.565(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.6935(7)
_cell_length_b                   7.4544(9)
_cell_length_c                   29.487(4)
_cell_measurement_temperature    293(2)
_cell_volume                     1249.1(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0452
_diffrn_reflns_av_sigmaI/netI    0.0285
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            13761
_diffrn_reflns_theta_full        24.85
_diffrn_reflns_theta_max         24.85
_diffrn_reflns_theta_min         2.77
_exptl_absorpt_coefficient_mu    0.239
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_F_000             512
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.192
_refine_diff_density_min         -0.195
_refine_diff_density_rms         0.034
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         2135
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0612
_refine_ls_R_factor_gt           0.0396
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0377P)^2^+0.4804P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0871
_refine_ls_wR_factor_ref         0.0971
_reflns_number_gt                1602
_reflns_number_total             2135
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            jo302643v_si_003.cif
_cod_data_source_block           rn140out
_cod_original_cell_volume        1249.0(3)
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_database_code               4028032