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_4113542
_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         'C15 H18 O3 S '
_chemical_formula_sum            'C15 H18 O3 S'
_chemical_formula_weight         278.37
_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'
_cell_angle_alpha                90
_cell_angle_beta                 107.374(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.1956(4)
_cell_length_b                   9.8812(6)
_cell_length_c                   10.0669(5)
_cell_measurement_reflns_used    6265
_cell_measurement_temperature    93.1
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.1
_cell_volume                     683.11(7)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure Ver. 2.00'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    SIR92
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.9988
_diffrn_measured_fraction_theta_max 0.9988
_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  0.040
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_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            6346
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_exptl_absorpt_coefficient_mu    0.238
_exptl_absorpt_correction_T_max  0.976
_exptl_absorpt_correction_T_min  0.592
_exptl_absorpt_correction_type
;
\y scans (North,Phillips & Matthews, 1968)
;
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_description       prism
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.29
_refine_diff_density_min         -0.39
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  0 Friedel Pairs'
_refine_ls_abs_structure_Flack   -0.0(2)
_refine_ls_extinction_coef       -98.9(3)
_refine_ls_extinction_method
'Larson (1970) Crystallographic Computing eq. 22'
_refine_ls_goodness_of_fit_ref   1.491
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     192
_refine_ls_number_reflns         1619
_refine_ls_R_factor_gt           0.0320
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w = 1/[0.001Fo^2^ + 1.000\s^2^(Fo)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0940
_reflns_number_gt                1619
_reflns_number_total             1651
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja029534lsi20030117_035028_2.cif
_cod_data_source_block           '_cpw______________________'
_cod_original_cell_volume        683.11(6)
_cod_original_formula_sum        'C15 H18 O3 S '
_cod_database_code               4113542