Chain-Walking Strategy for Organic Synthesis: Catalytic Cycloisomerization of 1,n-Dienes
Takuya Kochi; Taro Hamasaki; Yuka Aoyama; Junichi Kawasaki; Fumitoshi Kakiuchi; Journal of the American Chemical Society 134 (2012) 16544–16547; doi:10.1021/ja308377u

data_4118748
_publ_section_title
;
 Chain-Walking Strategy for Organic Synthesis: Catalytic
 Cycloisomerization of 1,n-Dienes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16544
_journal_page_last               16547
_journal_paper_doi               10.1021/ja308377u
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'C17 H26 O4'
_chemical_formula_weight         294.38
_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                83.478(3)
_cell_angle_beta                 77.578(2)
_cell_angle_gamma                60.886(3)
_cell_formula_units_Z            4
_cell_length_a                   11.0933(10)
_cell_length_b                   11.5651(12)
_cell_length_c                   14.6276(13)
_cell_measurement_temperature    93(2)
_cell_volume                     1601.1(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      93(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.1003
_diffrn_reflns_av_sigmaI/netI    0.1438
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15750
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.21
_exptl_absorpt_coefficient_mu    0.085
_exptl_absorpt_correction_T_max  0.9915
_exptl_absorpt_correction_T_min  0.9586
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Jacobson, R. (1998). Private communication to the Rigaku Corporation'
_exptl_crystal_density_diffrn    1.221
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.400
_refine_diff_density_min         -0.452
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     385
_refine_ls_number_reflns         7235
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.1829
_refine_ls_R_factor_gt           0.0787
_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^)+(0.0279P)^2^+3.7703P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1513
_refine_ls_wR_factor_ref         0.2011
_reflns_number_gt                3449
_reflns_number_total             7235
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja308377u_si_002.cif
_cod_data_source_block           5i
_cod_database_code               4118748