Generation of 3-(1H-pyrrol-3-yl)-1H-inden-1-ones via a tandem reaction of 1-(2-alkynylphenyl)-2-enone, 2-isocyanoacetate, and water
Danqing Zheng; Shaoyu Li; Jie Wu; Chem.Commun. 48 (2012) 8568–; doi:10.1039/c2cc34509a

data_7108196
_publ_section_title
;
 Generation of 3-(1H-pyrrol-3-yl)-1H-inden-1-ones via a tandem reaction of
 1-(2-alkynylphenyl)-2-enone, 2-isocyanoacetate, and water
;
_journal_name_full               Chem.Commun.
_journal_page_first              8568
_journal_paper_doi               10.1039/c2cc34509a
_journal_volume                  48
_journal_year                    2012
_chemical_formula_sum            'C30 H24 Cl3 N O3'
_chemical_formula_weight         552.86
_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                91.983(6)
_cell_angle_beta                 103.980(6)
_cell_angle_gamma                93.387(7)
_cell_formula_units_Z            2
_cell_length_a                   11.125(5)
_cell_length_b                   11.134(5)
_cell_length_c                   11.495(5)
_cell_measurement_reflns_used    828
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.201
_cell_measurement_theta_min      2.542
_cell_volume                     1377.5(11)
_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, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_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  0.0341
_diffrn_reflns_av_sigmaI/netI    0.0666
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5797
_diffrn_reflns_theta_full        25.10
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    0.365
_exptl_absorpt_correction_T_max  0.9714
_exptl_absorpt_correction_T_min  0.9373
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             572
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.007
_refine_diff_density_min         -0.867
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         4813
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.1574
_refine_ls_R_factor_gt           0.1074
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+1.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3084
_refine_ls_wR_factor_ref         0.3429
_reflns_number_gt                2604
_reflns_number_total             4813
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc34509a.txt
_cod_data_source_block           a20410a
_cod_original_cell_volume        1377.4(10)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C15 H12 Cl1.50 N0.50 O1.50'
_cod_database_code               7108196