Pd-Catalyzed C-S Activation/Isocyanide Insertion/Hydrogenation Enables a Selective Aerobic Oxidation/Cyclization.
Chang, Jian; Liu, Bangyu; Yang, Yang; Wang, Mang; Organic letters 18 (2016) 3984–3987; doi:10.1021/acs.orglett.6b01780

data_1555651
_publ_section_title
;
 Pd-Catalyzed C-S Activation/Isocyanide Insertion/Hydrogenation Enables a
 Selective Aerobic Oxidation/Cyclization.
;
_journal_issue                   16
_journal_name_full               'Organic letters'
_journal_page_first              3984
_journal_page_last               3987
_journal_paper_doi               10.1021/acs.orglett.6b01780
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'C17 H20 F N O4 S'
_chemical_formula_sum            'C17 H20 F N O4 S'
_chemical_formula_weight         353.40
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_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                75.804(10)
_cell_angle_beta                 70.345(11)
_cell_angle_gamma                81.631(9)
_cell_formula_units_Z            2
_cell_length_a                   8.5007(9)
_cell_length_b                   10.2500(12)
_cell_length_c                   11.2985(15)
_cell_measurement_reflns_used    1893
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.0379
_cell_measurement_theta_min      2.9960
_cell_volume                     896.6(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans'
_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  0.0203
_diffrn_reflns_av_sigmaI/netI    0.0369
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5666
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    0.210
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94220
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             372
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.38
_refine_diff_density_max         0.392
_refine_diff_density_min         -0.327
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     258
_refine_ls_number_reflns         3499
_refine_ls_number_restraints     216
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0749
_refine_ls_R_factor_gt           0.0532
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0681P)^2^+0.3174P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1305
_refine_ls_wR_factor_ref         0.1505
_reflns_number_gt                2563
_reflns_number_total             3499
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol6b01780_si_002.cif
_cod_data_source_block           y
_cod_original_cell_volume        896.65(18)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1555651