Palladium-Catalyzed Intermolecular directed C-H Amidation of Aromatic Ketones
Bin Xiao; Tian-Jun Gong; Jun Xu; Zhao-Jing Liu; Lei Liu; Journal of the American Chemical Society 133 (2011) 1466–1474; doi:10.1021/ja108450m

data_4105582
_publ_section_title
;
 Palladium-Catalyzed Intermolecular directed C-H Amidation of Aromatic
 Ketones
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1466
_journal_page_last               1474
_journal_paper_doi               10.1021/ja108450m
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C26 H25 Cl N2 O5 S2'
_chemical_formula_weight         545.05
_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
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_cell_angle_beta                 96.391(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            12
_cell_length_a                   10.7141(6)
_cell_length_b                   24.593(2)
_cell_length_c                   30.357(2)
_cell_measurement_reflns_used    3748
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      63.5179
_cell_measurement_theta_min      3.4344
_cell_volume                     7949.1(9)
_computing_cell_refinement       'CrysAlisPro (Oxford Diffraction Ltd.)'
_computing_data_collection       'CrysAlisPro (Oxford Diffraction Ltd.)'
_computing_data_reduction        'CrysAlisPro (Oxford Diffraction Ltd.)'
_computing_molecular_graphics    'Ortep-3 (L. J. Farrugia, 2001)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      291(2)
_diffrn_detector_area_resol_mean 15.9149
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0649
_diffrn_reflns_av_sigmaI/netI    0.0871
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            31135
_diffrn_reflns_theta_full        63.61
_diffrn_reflns_theta_max         63.61
_diffrn_reflns_theta_min         3.44
_exptl_absorpt_coefficient_mu    3.080
_exptl_absorpt_correction_T_max  0.7482
_exptl_absorpt_correction_T_min  0.4585
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_description       plate
_exptl_crystal_F_000             3408
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.410
_refine_diff_density_min         -0.384
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1010
_refine_ls_number_reflns         12655
_refine_ls_number_restraints     63
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.1288
_refine_ls_R_factor_gt           0.0729
_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^)+(0.0560P)^2^+7.2110P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1590
_refine_ls_wR_factor_ref         0.1972
_reflns_number_gt                7127
_reflns_number_total             12655
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja108450m_si_006.cif
_cod_data_source_block           101123
_cod_original_cell_volume        7949.0(10)
_cod_database_code               4105582