Studies toward the Total Synthesis of Garsubellin A: A Concise Synthesis of the 18-epi-Tricyclic Core
Usuda, Hiroyuki; Kanai, Motomu; Shibasaki, Masakatsu; Organic Letters 4 (2002) 859–; doi:10.1021/ol0255965

data_1507446
_publ_section_title
;
 Studies toward the Total Synthesis of Garsubellin A:&#x2009; A Concise
 Synthesis of the 18-epi-Tricyclic Core
;
_journal_issue                   5
_journal_name_full               'Organic Letters'
_journal_page_first              859
_journal_paper_doi               10.1021/ol0255965
_journal_volume                  4
_journal_year                    2002
_chemical_formula_sum            'C20 H27 I O5'
_chemical_formula_weight         474.33
_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'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.2206(7)
_cell_length_b                   22.134(1)
_cell_length_c                   11.6664(4)
_cell_measurement_reflns_used    46903
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.7
_cell_volume                     4188.5(3)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        'teXsan Ver. 1.10'
_computing_publication_material  'teXsan Ver. 1.10'
_computing_structure_refinement  'teXsan Ver. 1.10'
_computing_structure_solution    SIR97
_diffrn_measured_fraction_theta_full 0.2746
_diffrn_measured_fraction_theta_max 0.2746
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.022
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            17504
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    0.778
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.752
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.50
_refine_diff_density_min         -0.56
_refine_ls_abs_structure_Flack   0.00000
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     1041
_refine_ls_number_reflns         5242
_refine_ls_R_factor_gt           0.0494
_refine_ls_shift/su_max          0.8710
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^) + (0.05000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1332
_reflns_number_gt                3296
_reflns_number_total             1753
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ol0255965_s2.cif
_cod_data_source_block           020118HU
_cod_original_cell_volume        4188.6(3)
_cod_original_sg_symbol_H-M      'P -1         '
_cod_original_formula_sum        'C20 H27 I O5 '
_cod_database_code               1507446