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_4111311
_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         'C30 H42 O5 Si'
_chemical_formula_sum            'C30 H42 O5 Si'
_chemical_formula_weight         510.73
_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                79.19(5)
_cell_angle_beta                 81.02(6)
_cell_angle_gamma                77.41(6)
_cell_formula_units_Z            4
_cell_length_a                   11.173(16)
_cell_length_b                   12.582(18)
_cell_length_c                   21.63(3)
_cell_measurement_temperature    296(2)
_cell_volume                     2894(7)
_computing_cell_refinement       'Rapid Scale, Rigaku'
_computing_data_collection       'Rapid Auto, Rigaku'
_computing_data_reduction        'Rapid Scale, Rigaku'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 10.0
_diffrn_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku UX-18'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_av_sigmaI/netI    0.0379
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            27459
_diffrn_reflns_theta_full        27.42
_diffrn_reflns_theta_max         27.42
_diffrn_reflns_theta_min         3.11
_exptl_absorpt_coefficient_mu    0.117
_exptl_absorpt_correction_T_max  0.9793
_exptl_absorpt_correction_T_min  0.8044
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR, Rigaku'
_exptl_crystal_colour            transparent
_exptl_crystal_density_diffrn    1.172
_exptl_crystal_description       block
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.447
_refine_diff_density_min         -0.432
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     667
_refine_ls_number_reflns         12605
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.0531
_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^)+(0.0732P)^2^+1.4220P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1562
_refine_ls_wR_factor_ref         0.1645
_reflns_number_gt                10394
_reflns_number_total             12605
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0671924si20061120_012033.cif
_cod_data_source_block           onizawa6
_cod_database_code               4111311