Enantioselective total synthesis of (-)-erinacine B.
Watanabe, Hideaki; Takano, Masashi; Umino, Akinori; Ito, Toshiya; Ishikawa, Hiroyuki; Nakada, Masahisa; Organic letters 9 (2007) 359–362; doi:10.1021/ol0628816

data_1505283
_publ_section_title
;
 Enantioselective total synthesis of (-)-erinacine B.
;
_journal_issue                   2
_journal_name_full               'Organic letters'
_journal_page_first              359
_journal_page_last               362
_journal_paper_doi               10.1021/ol0628816
_journal_volume                  9
_journal_year                    2007
_chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk'
_chemical_formula_moiety         'C22 H26 N2 O7 '
_chemical_formula_sum            'C22 H26 N2 O7'
_chemical_formula_weight         430.46
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      5
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_cell_angle_alpha                90
_cell_angle_beta                 121.35(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.80(1)
_cell_length_b                   6.428(3)
_cell_length_c                   15.690(8)
_cell_measurement_reflns_used    10901
_cell_measurement_temperature    93.1
_cell_measurement_theta_max      29.6
_cell_measurement_theta_min      3.0
_cell_volume                     2049.9(17)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.6.0'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    SHELXS97
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.9949
_diffrn_measured_fraction_theta_max 0.9949
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.026
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9998
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    0.104
_exptl_absorpt_correction_T_max  0.979
_exptl_absorpt_correction_T_min  0.920
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
    Higashi, T. (1999). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             912.00
_exptl_crystal_size_max          1.00
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.44
_refine_diff_density_min         -0.31
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  1811 Friedel Pairs'
_refine_ls_abs_structure_Flack   -0.7(9)
_refine_ls_extinction_coef       -108(16)
_refine_ls_extinction_method
'Larson (1970) Crystallographic Computing eq. 22'
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     308
_refine_ls_number_reflns         3713
_refine_ls_R_factor_gt           0.0320
_refine_ls_shift/su_max          0.0030
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[0.0012Fo^2^ + 1.0000\s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0890
_reflns_number_gt                3713
_reflns_number_total             4356
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ol0628816si20061128_014820.cif
_cod_data_source_block           '_takano0125'
_cod_original_cell_volume        2050(1)
_cod_original_formula_sum        'C22 H26 N2 O7 '
_cod_database_code               1505283