An unexpected silver triflate-catalyzed tandem reaction of N'-(2-alkynylbenzylidene)hydrazide with ketene
Gang Liu; Hongliang Liu; Guanyinsheng Qiu; Shouzhi Pu; Jie Wu; Chem.Commun. 48 (2012) 7049–; doi:10.1039/c2cc33375a

data_7107966
_publ_section_title
;
 An unexpected silver triflate-catalyzed tandem reaction of
 N'-(2-alkynylbenzylidene)hydrazide with ketene
;
_journal_name_full               Chem.Commun.
_journal_page_first              7049
_journal_paper_doi               10.1039/c2cc33375a
_journal_volume                  48
_journal_year                    2012
_chemical_formula_sum            'C30 H24 N2 O3 S'
_chemical_formula_weight         492.57
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 116.046(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.328(7)
_cell_length_b                   11.798(6)
_cell_length_c                   16.315(8)
_cell_measurement_reflns_used    976
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.851
_cell_measurement_theta_min      2.779
_cell_volume                     2478(2)
_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, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.1113
_diffrn_reflns_av_sigmaI/netI    0.1004
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10356
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.58
_exptl_absorpt_coefficient_mu    0.166
_exptl_absorpt_correction_T_max  0.9803
_exptl_absorpt_correction_T_min  0.9675
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.401
_refine_diff_density_min         -0.623
_refine_diff_density_rms         0.135
_refine_ls_extinction_coef       0.048(4)
_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   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         4593
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0900
_refine_ls_R_factor_gt           0.0742
_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^)+(0.1110P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1679
_refine_ls_wR_factor_ref         0.1825
_reflns_number_gt                3440
_reflns_number_total             4593
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc33375a.txt
_cod_data_source_block           a20309a
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7107966