Intramolecular cyclohexadienone annulations of Fischer carbene complexes: model studies for the synthesis of Phomactins.
Huang, Jie; Wang, Huan; Wu, Chunrui; Wulff, William D.; Organic letters 9 (2007) 2799–2802; doi:10.1021/ol070904q

data_1505429
_publ_section_title
;
 Intramolecular cyclohexadienone annulations of Fischer carbene complexes:
 model studies for the synthesis of Phomactins.
;
_journal_issue                   15
_journal_name_full               'Organic letters'
_journal_page_first              2799
_journal_page_last               2802
_journal_paper_doi               10.1021/ol070904q
_journal_volume                  9
_journal_year                    2007
_chemical_formula_sum            'C27 H48 O3 Si'
_chemical_formula_weight         448.74
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_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                117.10(3)
_cell_angle_beta                 112.07(3)
_cell_angle_gamma                95.88(3)
_cell_formula_units_Z            2
_cell_length_a                   11.714(2)
_cell_length_b                   12.064(2)
_cell_length_c                   12.691(3)
_cell_measurement_temperature    173(2)
_cell_volume                     1395.8(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.901
_diffrn_measured_fraction_theta_max 0.901
_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  0.0141
_diffrn_reflns_av_sigmaI/netI    0.0361
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8784
_diffrn_reflns_theta_full        28.14
_diffrn_reflns_theta_max         28.14
_diffrn_reflns_theta_min         1.96
_exptl_absorpt_coefficient_mu    0.107
_exptl_crystal_density_diffrn    1.068
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.496
_refine_diff_density_min         -0.255
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.921
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         6147
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.921
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0436
_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          0.1271
_refine_ls_wR_factor_ref         0.1364
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_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol070904qsi20070531_074520.cif
_cod_data_source_block           wulff06
_cod_original_cell_volume        1395.9(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1505429