Rhodium(III)-Catalyzed N-Nitroso-Directed C-H Olefination of Arenes. High-Yield, Versatile Coupling under Mild Conditions
Baoqing Liu; Yang Fan; Yang Gao; Chao Sun; Cheng Xu; Jin Zhu; Journal of the American Chemical Society 135 (2013) 468–473; doi:10.1021/ja3099245

data_4119159
_publ_section_title
;
 Rhodium(III)-Catalyzed N-Nitroso-Directed C-H Olefination of Arenes.
 High-Yield, Versatile Coupling under Mild Conditions
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              468
_journal_page_last               473
_journal_paper_doi               10.1021/ja3099245
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C34 H42 Cl2 F2 N4 O2 Rh2'
_chemical_formula_weight         853.44
_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                77.900(7)
_cell_angle_beta                 78.893(7)
_cell_angle_gamma                68.444(8)
_cell_formula_units_Z            1
_cell_length_a                   7.889(5)
_cell_length_b                   8.303(5)
_cell_length_c                   14.135(8)
_cell_measurement_reflns_used    4421
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.41
_cell_measurement_theta_min      2.67
_cell_volume                     835.2(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and 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  0.0372
_diffrn_reflns_av_sigmaI/netI    0.0551
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5575
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         1.49
_exptl_absorpt_coefficient_mu    1.197
_exptl_absorpt_correction_T_max  0.7957
_exptl_absorpt_correction_T_min  0.7152
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_density_diffrn    1.697
_exptl_crystal_F_000             432
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.109
_refine_diff_density_min         -1.153
_refine_diff_density_rms         0.219
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.177
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         2799
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.180
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0432
_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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1361
_refine_ls_wR_factor_ref         0.1527
_reflns_number_gt                2471
_reflns_number_total             2799
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja3099245_si_003.cif
_cod_data_source_block           wpp2
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4119159