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_4113549
_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         'C17 H18 O3 S '
_chemical_formula_sum            'C17 H18 O3 S'
_chemical_formula_weight         302.39
_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             'Tue Nov 26 09:07:31 2002'
_audit_creation_method           'by teXsan'
_cell_angle_alpha                90
_cell_angle_beta                 110.062(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.4622(7)
_cell_length_b                   8.0474(6)
_cell_length_c                   11.547(1)
_cell_measurement_reflns_used    7354
_cell_measurement_temperature    123.2
_cell_measurement_theta_max      24.4
_cell_measurement_theta_min      2.6
_cell_volume                     738.62(11)
_computing_cell_refinement       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction        'teXsan (MSC & Rigaku, 1999)'
_computing_molecular_graphics    'ORTEP (Johnson, 1976)'
_computing_publication_material  'teXsan (MSC & Rigaku, 1999)'
_computing_structure_refinement  'teXsan (MSC & Rigaku, 1999)'
_computing_structure_solution    'SIR97 (Altomare, 1999)'
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.9965
_diffrn_measured_fraction_theta_max 0.9965
_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  0.027
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7914
_diffrn_reflns_theta_full        29.95
_diffrn_reflns_theta_max         29.95
_exptl_absorpt_coefficient_mu    0.226
_exptl_absorpt_correction_T_max  0.989
_exptl_absorpt_correction_T_min  0.854
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_description       platelet
_exptl_crystal_F_000             320.00
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.45
_refine_diff_density_min         -0.36
_refine_ls_abs_structure_details
;
Determined based on the Flack's parameter (Flack, 1983) refined using the 
reflection data including Friedel mates.
;
_refine_ls_abs_structure_Flack   0.00(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.198
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     191
_refine_ls_number_reflns         3724
_refine_ls_R_factor_gt           0.0346
_refine_ls_shift/su_max          0.0013
_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         0.0866
_reflns_number_gt                3436
_reflns_number_total             2277
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja029534lsi20030117_035028_9.cif
_cod_data_source_block           8a
_cod_original_cell_volume        738.6(1)
_cod_original_formula_sum        'C17 H18 O3 S '
_cod_database_code               4113549