Cobalt(II)/silver relay catalytic isocyanide insertion/cycloaddition cascades: a new access to pyrrolo[2,3-b]indoles
Qian Gao; Peng Zhou; Feng Liu; Wen-Juan Hao; Changsheng Yao; Bo Jiang; Shu-Jiang Tu; Chem.Commun. 51 (2015) 9519–; doi:10.1039/C5cc02754C

data_7117227
_publ_section_title
;
 Cobalt(II)/silver relay catalytic isocyanide insertion/cycloaddition
 cascades: a new access to pyrrolo[2,3-b]indoles
;
_journal_name_full               Chem.Commun.
_journal_page_first              9519
_journal_paper_doi               10.1039/C5cc02754C
_journal_volume                  51
_journal_year                    2015
_chemical_formula_sum            'C28 H31 N3'
_chemical_formula_weight         409.56
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-04-02 deposited with the CCDC.
2015-04-28 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 121.270(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   31.282(3)
_cell_length_b                   8.8017(7)
_cell_length_c                   19.4725(19)
_cell_measurement_reflns_used    1867
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.7270
_cell_measurement_theta_min      3.2270
_cell_volume                     4582.6(7)
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_collection       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.1087
_diffrn_reflns_av_sigmaI/netI    0.1003
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            15177
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.44
_exptl_absorpt_coefficient_mu    0.070
_exptl_absorpt_correction_T_max  0.9746
_exptl_absorpt_correction_T_min  0.9692
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.187
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.37
_refine_diff_density_max         0.233
_refine_diff_density_min         -0.188
_refine_diff_density_rms         0.045
_refine_ls_extinction_coef       0.0023(5)
_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   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         4054
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.1276
_refine_ls_R_factor_gt           0.0697
_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^)+(0.0876P)^2^+0.4143P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1612
_refine_ls_wR_factor_ref         0.2090
_reflns_number_gt                2203
_reflns_number_total             4054
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5cc02754c2.cif
_cod_data_source_block           141015e
_cod_original_cell_volume        4582.7(7)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7117227