Ruthenium porphyrin catalyzed diimination of indoles with aryl azides as the nitrene source
Jinhu Wei; Wenbo Xiao; Cong-Ying Zhou; Chi-Ming Che; Chem.Commun. 50 (2014) 3373–; doi:10.1039/c3cc49052a

data_7112098
_publ_section_title
;
 Ruthenium porphyrin catalyzed diimination of indoles with aryl azides as
 the nitrene source
;
_journal_name_full               Chem.Commun.
_journal_page_first              3373
_journal_paper_doi               10.1039/c3cc49052a
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C21 H15 N5 O4, 0.5(C4 H8 O2)'
_chemical_formula_sum            'C23 H19 N5 O5'
_chemical_formula_weight         445.43
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                73.1170(10)
_cell_angle_beta                 73.449(2)
_cell_angle_gamma                79.959(2)
_cell_formula_units_Z            2
_cell_length_a                   8.0842(9)
_cell_length_b                   12.2092(13)
_cell_length_c                   12.7761(14)
_cell_measurement_reflns_used    6480
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      2.64
_cell_volume                     1150.9(2)
_computing_cell_refinement       'SAINT v7.34A (Bruker AXS Inc, 2006)'
_computing_data_collection       'SMART (Bruker AXS Inc, 1998)'
_computing_data_reduction        'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics    'MERCURY (Macrae et al., 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker SMASRT 1000 CCD'
_diffrn_measurement_method       \w
_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  0.0134
_diffrn_reflns_av_sigmaI/netI    0.0214
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6480
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.64
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.093
_exptl_absorpt_correction_T_max  0.9852
_exptl_absorpt_correction_T_min  0.9592
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2004)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             464
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.381
_refine_diff_density_min         -0.289
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     297
_refine_ls_number_reflns         3989
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0767
_refine_ls_R_factor_gt           0.0579
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1242P)^2^+0.2333P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1738
_refine_ls_wR_factor_ref         0.1956
_reflns_number_gt                2955
_reflns_number_total             3989
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c3cc49052a2.cif
_cod_data_source_block           wt1999w-shelxl
_cod_database_code               7112098