Sulfur oxidation in supercritical carbon dioxide: dramatic pressure dependant enhancement of diastereoselectivity for sulfoxidation of cysteine derivatives
Scott Oakes, R.; Clifford, Anthony A.; Bartle, Keith D.; Pett, Mark Thornton; Rayner, Christopher M.; Chemical Communications  (1999) 247–; doi:10.1039/a809434i

data_7110431
_publ_section_title
;
 Sulfur oxidation in supercritical carbon dioxide: dramatic pressure
 dependant enhancement of diastereoselectivity for sulfoxidation of
 cysteine derivatives
;
_journal_issue                   3
_journal_name_full               'Chemical Communications'
_journal_page_first              247
_journal_paper_doi               10.1039/a809434i
_journal_year                    1999
_chemical_formula_sum            'C13 H17 N O5 S'
_chemical_formula_weight         299.34
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.87930(10)
_cell_length_b                   8.19550(10)
_cell_length_c                   22.0906(4)
_cell_measurement_reflns_used    24188
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.2
_cell_measurement_theta_min      2.02
_cell_volume                     1426.50(4)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'KCCD (Nonius, 1997)'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'ORTEX (McArdle, 1995)'
_computing_publication_material  'local program'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Nonius KappaCCD area-detector diffractometer'
_diffrn_measurement_method
;
   Detector set at 25mm from sample
   'head-on' data - 360 * 1 degree phi exposures for chi=0 and 2theta = 
0
   'cusp' data' - 55 * 1 degree omega exposures for chi=90 at 2theta = 
40 at
                  4 different settings of phi
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_sigmaI/netI    0.0181
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            27208
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.65
_exptl_absorpt_coefficient_mu    0.245
_exptl_absorpt_correction_T_max  0.9526
_exptl_absorpt_correction_T_min  0.8831
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
 Using multiple and symmetry-related data measurements via the program 
SORTAV
 See R.H. Blessing, Acta Cryst (1995), A51, 33-38
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.171
_refine_diff_density_min         -0.263
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(6)
_refine_ls_extinction_coef       0.046(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     184
_refine_ls_number_reflns         2747
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0258
_refine_ls_R_factor_gt           0.0256
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0430P)^2^+0.3491P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0706
_refine_ls_wR_factor_ref         0.0707
_reflns_number_gt                2724
_reflns_number_total             2747
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            809434isup1.cif
_cod_data_source_block           CR5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P212121
_cod_database_code               7110431