W(CO)5(L)-Catalyzed Tandem Intramolecular Cyclopropanation/Cope Rearrangement for the Stereoselective Construction of Bicyclo[5.3.0]decane Framework
Hiroyuki Kusama; Yuji Onizawa; Nobuharu Iwasawa; Journal of the American Chemical Society 128 (2006) 16500–16501; doi:10.1021/ja0671924

data_4111309
_publ_section_title
;
 W(CO)5(L)-Catalyzed Tandem Intramolecular Cyclopropanation/Cope
 Rearrangement for the Stereoselective Construction of
 Bicyclo[5.3.0]decane Framework
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16500
_journal_page_last               16501
_journal_paper_doi               10.1021/ja0671924
_journal_volume                  128
_journal_year                    2006
_chemical_formula_moiety         'C32 H46 O7 Si'
_chemical_formula_sum            'C32 H46 O7 Si'
_chemical_formula_weight         570.78
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                74.020(7)
_cell_angle_beta                 88.427(5)
_cell_angle_gamma                71.392(5)
_cell_formula_units_Z            2
_cell_length_a                   10.3570(10)
_cell_length_b                   11.4750(16)
_cell_length_c                   14.484(2)
_cell_measurement_reflns_used    14837
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      0.0262
_cell_measurement_theta_min      0.0172
_cell_volume                     1564.9(4)
_computing_cell_refinement       'HKL-2000 '
_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction        'HKL-2000 '
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       '\w scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0172
_diffrn_reflns_av_sigmaI/netI    0.0262
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14837
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.47
_diffrn_source                   'Rigaku rotating anode Ultrax18'
_exptl_absorpt_coefficient_mu    0.119
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.211
_exptl_crystal_description       plate
_exptl_crystal_F_000             616
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.355
_refine_diff_density_min         -0.189
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         6937
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0361
_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^)+(0.0469P)^2^+0.5614P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0961
_refine_ls_wR_factor_ref         0.1007
_reflns_number_gt                6297
_reflns_number_total             6937
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0671924si20061007_073616.cif
_cod_data_source_block           shelxl
_cod_database_code               4111309