Gold-catalyzed synthesis of tetrahydrocarbazole derivatives through an intermolecular cycloaddition of vinyl indoles and N-allenamides
Valentina Pirovano; Laura Decataldo; Elisabetta Rossi; Ruben Vicente; Chem.Commun. 49 (2013) 3594–; doi:10.1039/c3cc41514g

data_7109141
_publ_section_title
;
 Gold-catalyzed synthesis of tetrahydrocarbazole derivatives through an
 intermolecular cycloaddition of vinyl indoles and N-allenamides
;
_journal_name_full               Chem.Commun.
_journal_page_first              3594
_journal_paper_doi               10.1039/c3cc41514g
_journal_volume                  49
_journal_year                    2013
_chemical_formula_moiety         'C26 H22 N2 O4'
_chemical_formula_sum            'C26 H22 N2 O4'
_chemical_formula_weight         426.45
_chemical_name_systematic
;
?
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 101.018(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   27.7207(19)
_cell_length_b                   5.8026(2)
_cell_length_c                   28.3766(16)
_cell_measurement_reflns_used    4931
_cell_measurement_temperature    123.0(3)
_cell_measurement_theta_max      74.5999
_cell_measurement_theta_min      3.2242
_cell_volume                     4480.3(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_molecular_graphics    'PLATON (Spek, 2006)'
_computing_publication_material  'SHELXL-97(Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-2004 (Altomare, 2004)'
_diffrn_ambient_temperature      123.0(3)
_diffrn_detector_area_resol_mean 8.2640
_diffrn_measured_fraction_theta_full 0.946
_diffrn_measured_fraction_theta_max 0.833
_diffrn_measurement_device_type  'Xcalibur, Onyx, Nova'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'Nova (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0551
_diffrn_reflns_av_sigmaI/netI    0.0386
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            17465
_diffrn_reflns_theta_full        70.00
_diffrn_reflns_theta_max         88.49
_diffrn_reflns_theta_min         3.17
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.699
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79819
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.264
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.2028
_exptl_crystal_size_mid          0.0460
_exptl_crystal_size_min          0.0157
_refine_diff_density_max         0.713
_refine_diff_density_min         -0.304
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         4272
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0777
_refine_ls_R_factor_gt           0.0648
_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^)+(0.1239P)^2^+3.4169P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1809
_refine_ls_wR_factor_ref         0.1972
_reflns_number_gt                3449
_reflns_number_total             4272
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c3cc41514g.txt
_cod_data_source_block           7a'
_cod_depositor_comments
;

2018-03-11
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C52 H44 N4 O8'
_cod_original_formula_weight         852.91
_cod_original_formula_moiety         'C52 H44 N4 O8'
_cod_original_formula_units_Z            4
_cod_original_sg_symbol_Hall     'C 2yc'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7109141