Synthetic Studies on Polymaxenolides: Synthesis and Structure Elucidation of Nominal Epoxyafricanane and Other Africane-Type Sesquiterpenoids
Yutaka Matsuda; Yusuke Endo; Yoko Saikawa; Masaya Nakata; Journal of Organic Chemistry 76 (2011) 6258–6263; doi:10.1021/jo2010186

data_4026497
_publ_section_title
;
 Synthetic Studies on Polymaxenolides: Synthesis and Structure Elucidation
 of Nominal Epoxyafricanane and Other Africane-Type Sesquiterpenoids
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              6258
_journal_page_last               6263
_journal_paper_doi               10.1021/jo2010186
_journal_volume                  76
_journal_year                    2011
_chemical_formula_sum            'C15 H26 O2'
_chemical_formula_weight         238.36
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 87.537(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.377(3)
_cell_length_b                   5.927(2)
_cell_length_c                   29.072(7)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      11.3
_cell_measurement_theta_min      10.0
_cell_volume                     2819.3(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku AFC7R'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0505
_diffrn_reflns_av_sigmaI/netI    0.0414
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       2
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            4871
_diffrn_reflns_theta_full        23.99
_diffrn_reflns_theta_max         23.99
_diffrn_reflns_theta_min         2.80
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.072
_exptl_absorpt_correction_T_max  0.9649
_exptl_absorpt_correction_T_min  0.9380
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.123
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.90
_exptl_crystal_size_mid          0.80
_exptl_crystal_size_min          0.50
_refine_diff_density_max         0.939
_refine_diff_density_min         -0.282
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.627
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     332
_refine_ls_number_reflns         4415
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.627
_refine_ls_R_factor_all          0.1726
_refine_ls_R_factor_gt           0.1146
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3713
_refine_ls_wR_factor_ref         0.4324
_reflns_number_gt                2517
_reflns_number_total             4415
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo2010186_si_001.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        2819.5(13)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4026497