Asymmetric Catalysis on the Intramolecular Cyclopropanation of α-Diazo-β-keto Sulfones
Masahiro Honma; Takashi Sawada; Yuri Fujisawa; Masayuki Utsugi; Hideaki Watanabe; Akinori Umino; Takehiko Matsumura; Takayuki Hagihara; Masashi Takano; Masahisa Nakada; Journal of the American Chemical Society 125 (2003) 2860–2861; doi:10.1021/ja029534l

data_4113547
_publ_section_title
;
 Asymmetric Catalysis on the Intramolecular Cyclopropanation of
 \a-Diazo-\b-keto Sulfones
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2860
_journal_page_last               2861
_journal_paper_doi               10.1021/ja029534l
_journal_volume                  125
_journal_year                    2003
_chemical_formula_moiety         'C16 H16 O3 S '
_chemical_formula_sum            'C16 H16 O3 S'
_chemical_formula_weight         288.36
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_audit_creation_date             2002-10-29
_audit_creation_method           'by CrystalStructure v3.00'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.823(1)
_cell_length_b                   11.023(2)
_cell_length_c                   12.542(2)
_cell_measurement_reflns_used    10916
_cell_measurement_temperature    296.1
_cell_measurement_theta_max      23.2
_cell_measurement_theta_min      3.2
_cell_volume                     1358.0(4)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure Ver. 3.00'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    SIR92
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.9948
_diffrn_measured_fraction_theta_max 0.9948
_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  0.070
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9320
_diffrn_reflns_theta_full        23.25
_diffrn_reflns_theta_max         23.25
_exptl_absorpt_coefficient_mu    0.242
_exptl_absorpt_correction_T_max  0.953
_exptl_absorpt_correction_T_min  0.233
_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    1.410
_exptl_crystal_description       block
_exptl_crystal_F_000             608.00
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.28
_refine_diff_density_min         -0.32
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  652 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.10(9)
_refine_ls_extinction_coef       -20.5(2)
_refine_ls_extinction_method
'Larson (1970) Crystallographic Computing eq. 22'
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     247
_refine_ls_number_reflns         1794
_refine_ls_R_factor_gt           0.0260
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[0.0001Fo^2^ + 1.0000\s^2^(Fo) + 0.4000]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0620
_reflns_number_gt                1794
_reflns_number_total             1948
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja029534lsi20030117_035028_7.cif
_cod_data_source_block           '_cpp56____________________'
_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_original_formula_sum        'C16 H16 O3 S '
_cod_database_code               4113547