Rhodium-catalyzed direct coupling of biaryl pyridine derivatives with internal alkynes
Jun Zheng; Shu-Li You; Chem.Commun. 50 (2014) 8204–; doi:10.1039/C4cc02822H

data_7115309
_publ_section_title
;
 Rhodium-catalyzed direct coupling of biaryl pyridine derivatives with
 internal alkynes
;
_journal_name_full               Chem.Commun.
_journal_page_first              8204
_journal_paper_doi               10.1039/C4cc02822H
_journal_volume                  50
_journal_year                    2014
_chemical_formula_sum            'C47 H32 Cl N'
_chemical_formula_weight         646.19
_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                96.760(2)
_cell_angle_beta                 99.441(3)
_cell_angle_gamma                90.583(2)
_cell_formula_units_Z            2
_cell_length_a                   8.7922(9)
_cell_length_b                   9.5339(10)
_cell_length_c                   21.234(2)
_cell_measurement_reflns_used    1918
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      46.603
_cell_measurement_theta_min      4.699
_cell_volume                     1742.8(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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0275
_diffrn_reflns_av_sigmaI/netI    0.0590
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            10628
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.96
_exptl_absorpt_coefficient_mu    0.144
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.37002
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.231
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             676
_exptl_crystal_size_max          0.211
_exptl_crystal_size_mid          0.148
_exptl_crystal_size_min          0.112
_refine_diff_density_max         0.213
_refine_diff_density_min         -0.177
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     446
_refine_ls_number_reflns         6824
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0842
_refine_ls_R_factor_gt           0.0511
_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^)+(0.0627P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1238
_refine_ls_wR_factor_ref         0.1402
_reflns_number_gt                4369
_reflns_number_total             6824
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc02822h2.cif
_cod_data_source_block           cd213199
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7115309