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_4028031
_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_moiety         'C18 H20 O4'
_chemical_formula_sum            'C18 H20 O4'
_chemical_formula_weight         300.34
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                100.02(3)
_cell_angle_beta                 97.28(3)
_cell_angle_gamma                116.291(18)
_cell_formula_units_Z            2
_cell_length_a                   8.681(5)
_cell_length_b                   9.419(5)
_cell_length_c                   11.422(10)
_cell_measurement_temperature    293(2)
_cell_volume                     802.3(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0519
_diffrn_reflns_av_sigmaI/netI    0.0546
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9381
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.86
_exptl_absorpt_coefficient_mu    0.087
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.243
_exptl_crystal_F_000             320
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.143
_refine_diff_density_min         -0.146
_refine_diff_density_rms         0.037
_refine_ls_extinction_coef       0.021(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.929
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         2804
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.929
_refine_ls_R_factor_all          0.1230
_refine_ls_R_factor_gt           0.0508
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0622P)^2^+0.2331P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1208
_refine_ls_wR_factor_ref         0.1551
_reflns_number_gt                1361
_reflns_number_total             2804
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            jo302643v_si_002.cif
_cod_data_source_block           ddout
_cod_original_cell_volume        802.3(9)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4028031