A Catalytic Reaction of Alkynes via Multiple-Site Functionalization
Subramanian Karur; S. R. S. Saibabu Kotti; Xin Xu; John F. Cannon; Allan Headley; Guigen Li; Journal of the American Chemical Society 125 (2003) 13340–13341; doi:10.1021/ja0304188

data_4114304
_publ_section_title
;
 A Catalytic Reaction of Alkynes via Multiple-Site Functionalization
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13340
_journal_page_last               13341
_journal_paper_doi               10.1021/ja0304188
_journal_volume                  125
_journal_year                    2003
_chemical_formula_moiety         'C15 H13 Cl2 N O2 S'
_chemical_formula_sum            'C15 H13 Cl2 N O2 S'
_chemical_formula_weight         342.22
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.4042(13)
_cell_length_b                   9.1502(11)
_cell_length_c                   21.1802(15)
_cell_measurement_reflns_used    92
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      11.94
_cell_measurement_theta_min      5.43
_cell_volume                     3179.2(5)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_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      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '2\q/\w 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  0.0318
_diffrn_reflns_av_sigmaI/netI    0.0593
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            3585
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.29
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.542
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            COLORLESS
_exptl_crystal_density_diffrn    1.430
_exptl_crystal_density_meas      0
_exptl_crystal_description       PLATE
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.328
_refine_diff_density_min         -0.368
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     194
_refine_ls_number_reflns         2796
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0939
_refine_ls_R_factor_gt           0.0511
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0532P)^2^+1.1477P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1132
_refine_ls_wR_factor_ref         0.1330
_reflns_number_gt                1766
_reflns_number_total             2796
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0304188.cif
_cod_data_source_block           li403a
_cod_database_code               4114304