Efficient Control of π-Alkyne and Vinylidene Complex Pathways for the W(CO)5(L)-Catalyzed Synthesis of Two Types of Nitrogen-Containing Bicyclic Compounds
Yuji Onizawa; Hiroyuki Kusama; Nobuharu Iwasawa; Journal of the American Chemical Society 130 (2008) 802–803; doi:10.1021/ja0782605

data_4107331
_publ_section_title
;
 Efficient Control of \p-Alkyne and Vinylidene Complex Pathways for the
 W(CO)5(L)-Catalyzed Synthesis of Two Types of Nitrogen-Containing
 Bicyclic Compounds
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              802
_journal_page_last               803
_journal_paper_doi               10.1021/ja0782605
_journal_volume                  130
_journal_year                    2008
_chemical_formula_sum            'C28 H36 N2 O5 S Si'
_chemical_formula_weight         540.74
_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                 114.11(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.510(11)
_cell_length_b                   25.71(3)
_cell_length_c                   11.552(17)
_cell_measurement_temperature    223(2)
_cell_volume                     2849(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0257
_diffrn_reflns_av_sigmaI/netI    0.0185
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            41757
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.06
_exptl_absorpt_coefficient_mu    0.195
_exptl_absorpt_correction_T_max  0.9808
_exptl_absorpt_correction_T_min  0.0848
_exptl_crystal_density_diffrn    1.261
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          25.00
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.548
_refine_diff_density_min         -0.531
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.327
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         6495
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.327
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0485
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1644
_refine_ls_wR_factor_ref         0.1731
_reflns_number_gt                5299
_reflns_number_total             6495
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0782605-file001.cif
_cod_data_source_block           shelxl
_cod_database_code               4107331