Rh-catalyzed intramolecular sp2 C-H bond difluoromethylenation
Yajun Li; Jiangtao Zhu; Haibo Xie; Shan Li; Dongjie Peng; Zhengke Li; Yongming Wu; Yuefa Gong; Chem.Commun. 48 (2012) 3136–; doi:10.1039/c2cc30207a

data_7107473
_publ_section_title
;
 Rh-catalyzed intramolecular sp2 C-H bond difluoromethylenation
;
_journal_name_full               Chem.Commun.
_journal_page_first              3136
_journal_paper_doi               10.1039/c2cc30207a
_journal_volume                  48
_journal_year                    2012
_chemical_formula_sum            'C23 H16 F2 N2 O'
_chemical_formula_weight         374.38
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 94.973(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.1029(11)
_cell_length_b                   12.9419(13)
_cell_length_c                   12.5303(12)
_cell_measurement_reflns_used    4038
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      54.523
_cell_measurement_theta_min      4.534
_cell_volume                     1793.7(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0228
_diffrn_reflns_av_sigmaI/netI    0.0258
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9435
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         1.84
_exptl_absorpt_coefficient_mu    0.100
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77178
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.386
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             776
_exptl_crystal_size_max          0.318
_exptl_crystal_size_mid          0.167
_exptl_crystal_size_min          0.151
_refine_diff_density_max         0.437
_refine_diff_density_min         -0.239
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         3509
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0730
_refine_ls_R_factor_gt           0.0636
_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^)+(0.0995P)^2^+0.2931P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1545
_refine_ls_wR_factor_ref         0.1625
_reflns_number_gt                2890
_reflns_number_total             3509
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc30207a.txt
_cod_data_source_block           cd211312
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7107473