Rh/Cu-catalyzed multiple C-H, C-C, and C-N bond cleavage: facile synthesis of pyrido[2,1-a]indoles from 1-(pyridin-2-yl)-1H-indoles and gamma-substituted propargyl alcohols
Ting Li; Zhen Wang; Mingliang Zhang; Hui-Jun Zhang; Ting-Bin Wen; Chem.Commun. 51 (2015) 6777–; doi:10.1039/C5cc01412C

data_7116936
_publ_section_title
;
 Rh/Cu-catalyzed multiple C-H, C-C, and C-N bond cleavage: facile
 synthesis of pyrido[2,1-a]indoles from 1-(pyridin-2-yl)-1H-indoles and
 gamma-substituted propargyl alcohols
;
_journal_name_full               Chem.Commun.
_journal_page_first              6777
_journal_paper_doi               10.1039/C5cc01412C
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety         'C30.30 H25.60 Cl0.60 N4 O2 Rh'
_chemical_formula_sum            'C30.3 H25.6 Cl0.6 N4 O2 Rh'
_chemical_formula_weight         601.93
_chemical_name_systematic
; 
 ? 
;
_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_block_doi                 10.5517/cc13n9cf
_audit_creation_method           SHELXL-97
_audit_update_record
;
2014-11-03 deposited with the CCDC.
2015-03-09 downloaded from the CCDC.
;
_cell_angle_alpha                82.69(3)
_cell_angle_beta                 77.98(3)
_cell_angle_gamma                83.72(3)
_cell_formula_units_Z            2
_cell_length_a                   9.6401(19)
_cell_length_b                   11.069(2)
_cell_length_c                   12.562(3)
_cell_measurement_temperature    173(2)
_cell_volume                     1295.6(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0616
_diffrn_reflns_av_sigmaI/netI    0.0566
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            16782
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.30
_exptl_absorpt_coefficient_mu    0.757
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             613
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.901
_refine_diff_density_min         -0.964
_refine_diff_density_rms         0.141
_refine_ls_extinction_coef       0.0042(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         4565
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0727
_refine_ls_R_factor_gt           0.0505
_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^)+(0.0774P)^2^+5.5233P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1225
_refine_ls_wR_factor_ref         0.1693
_reflns_number_gt                3527
_reflns_number_total             4565
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5cc01412c2.cif
_cod_data_source_block           p1
_cod_original_cell_volume        1295.6(4)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C30.30 H25.60 Cl0.60 N4 O2 Rh'
_cod_database_code               7116936