Palladium-Catalyzed Intermolecular Ditrifluoromethoxylation of Unactivated Alkenes: CF3O-Palladation Initiated by Pd(IV).
Chen, Chaohuang; Luo, Yixin; Fu, Liang; Chen, Pinhong; Lan, Yu; Liu, Guosheng; Journal of the American Chemical Society  (2018) –; doi:10.1021/jacs.7b11470

data_4127054
_publ_section_title
;
 Palladium-Catalyzed Intermolecular Ditrifluoromethoxylation of
 Unactivated Alkenes: CF3O-Palladation Initiated by Pd(IV).
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b11470
_journal_year                    2018
_chemical_formula_sum            'C22 H19 F6 N O6 S'
_chemical_formula_weight         539.44
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
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_cell_angle_gamma                90
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_cell_length_b                   13.2109(4)
_cell_length_c                   25.5413(8)
_cell_measurement_reflns_used    9806
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_cell_measurement_theta_min      4.815
_cell_volume                     4795.1(3)
_computing_cell_refinement       'Bruker SAINT'
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_computing_data_reduction        'Bruker SAINT'
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_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0457
_diffrn_reflns_av_unetI/netI     0.0144
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
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_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.998
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_diffrn_reflns_theta_max         24.997
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_exptl_absorpt_coefficient_mu    0.220
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7144
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
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_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2208
_exptl_crystal_size_max          0.160
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_refine_ls_extinction_coef       0.0028(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
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_refine_ls_restrained_S_all      1.126
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_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1111P)^2^+10.1972P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_refine_ls_wR_factor_ref         0.2135
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_reflns_number_gt                3666
_reflns_number_total             4219
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b11470_si_001.cif
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_cod_database_code               4127054
_shelx_estimated_absorpt_t_min   0.966
_shelx_estimated_absorpt_t_max   0.987
_shelxl_version_number           2013-4
_shelx_res_checksum              6786
_shelx_hkl_checksum              33157