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_4105580
_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            'C42 H46 F6 O6 Pd2'
_chemical_formula_weight         973.59
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
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_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_cell_length_b                   12.781(5)
_cell_length_c                   15.300(5)
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_cell_measurement_temperature    291(2)
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_cell_measurement_theta_min      3.0497
_cell_volume                     2200.3(14)
_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 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Gemini S Ultra, Oxford Diffraction'
_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
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_diffrn_reflns_av_sigmaI/netI    0.1251
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
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_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            14841
_diffrn_reflns_theta_full        62.39
_diffrn_reflns_theta_max         62.39
_diffrn_reflns_theta_min         3.04
_exptl_absorpt_coefficient_mu    7.182
_exptl_absorpt_correction_T_max  0.2775
_exptl_absorpt_correction_T_min  0.2218
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.30
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_platon_squeeze_details
;
;
_refine_diff_density_max         1.497
_refine_diff_density_min         -0.747
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     509
_refine_ls_number_reflns         6879
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.1200
_refine_ls_R_factor_gt           0.0632
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0549P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1458
_refine_ls_wR_factor_ref         0.1563
_reflns_number_gt                3180
_reflns_number_total             6879
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja108450m_si_004.cif
_cod_data_source_block           100323
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