Highly diastereo- and enantioselective construction of both central and axial chiralities by Rh-catalyzed [2 + 2 + 2] cycloaddition
Shibata, Takanori; Otomo, Mayumi; Tahara, Yu-ki; Endo, Kohei; Organic & Biomolecular Chemistry 6 (2008) 4296–4298; doi:10.1039/b814014f

data_7151031
_publ_section_title
;
 Highly diastereo- and enantioselective construction of both central
 and axial chiralities by Rh-catalyzed [2 + 2 + 2] cycloaddition
;
_journal_issue                   23
_journal_name_full               'Organic &amp; Biomolecular Chemistry'
_journal_page_first              4296
_journal_page_last               4298
_journal_paper_doi               10.1039/b814014f
_journal_volume                  6
_journal_year                    2008
_chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk'
_chemical_formula_moiety         'C37 H41 N O6 S '
_chemical_formula_sum            'C37 H41 N O6 S'
_chemical_formula_weight         627.79
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_audit_creation_date             2008-07-17
_audit_creation_method           'by CrystalStructure 3.8'
_cell_angle_alpha                90.0000
_cell_angle_beta                 97.4949(15)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            2
_cell_length_a                   11.0147(3)
_cell_length_b                   10.9320(3)
_cell_length_c                   14.7938(4)
_cell_measurement_reflns_used    15273
_cell_measurement_temperature    296.1
_cell_measurement_theta_max      68.2
_cell_measurement_theta_min      3.0
_cell_volume                     1766.14(8)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    SIR92
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.048
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19781
_diffrn_reflns_theta_full        68.24
_diffrn_reflns_theta_max         68.24
_exptl_absorpt_coefficient_mu    1.169
_exptl_absorpt_correction_T_max  0.890
_exptl_absorpt_correction_T_min  0.684
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Higashi, T. (1995). Program for Absorption Correction.
Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.180
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             668.00
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.31
_refine_diff_density_min         -0.37
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881. 2719 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.035(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     448
_refine_ls_number_reflns         4843
_refine_ls_R_factor_gt           0.0432
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[0.0002Fo^2^ + 1.0000\s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1059
_reflns_number_gt                4807
_reflns_number_total             6131
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            b814014f.txt
_cod_data_source_block           '_otomo'
_cod_original_cell_volume        1766.15(9)
_cod_original_formula_sum        'C37 H41 N O6 S '
_cod_database_code               7151031