(1'<i>S</i>,2<i>R</i>,3<i>R</i>)-3-(1'-<i>tert</i>-Butyldimethylsilyloxy-1'-phenylmethyl)-2-(4''-methylphenylthio)-2-nitrooxirane
Clegg, William; .; Elsegood, Mark R. J.; Acta Crystallographica Section E 59 (2003) o1070–o1072; doi:10.1107/S1600536803014326

data_2202328
_publ_section_title
(1'<i>S</i>,2<i>R</i>,3<i>R</i>)-3-(1'-<i>tert</i>-Butyldimethylsilyloxy-1'-phenylmethyl)-2-(4''-methylphenylthio)-2-nitrooxirane
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1070
_journal_page_last               o1072
_journal_paper_doi               10.1107/S1600536803014326
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          'C22 H29 N O4 S Si'
_chemical_formula_moiety         'C22 H29 N O4 S Si'
_chemical_formula_sum            'C22 H29 N O4 S Si'
_chemical_formula_weight         431.61
_chemical_name_systematic
;
(1'S,2R,3R)-3-(1'-tert-Butyldimethylsilyloxy-1'-phenylmethyl)-
2-(4''-methylphenylthio)-2-nitrooxirane
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_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                 95.531(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.0904(12)
_cell_length_b                   8.9428(11)
_cell_length_c                   13.1503(16)
_cell_measurement_reflns_used    5503
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.6
_cell_measurement_theta_min      2.4
_cell_volume                     1181.1(2)
_computing_cell_refinement       'local programs'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 2001)'
_diffrn_ambient_temperature      160(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.904
_diffrn_measurement_device_type  'Bruker SMART 1K CCD'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0200
_diffrn_reflns_av_sigmaI/netI    0.0453
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7705
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.91
_diffrn_reflns_theta_min         2.43
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.214
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.90
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2002)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.214
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             460
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.242
_refine_diff_density_min         -0.219
_refine_ls_abs_structure_details 'Flack (1983), 2251 Friedel pairs'
_refine_ls_abs_structure_Flack   0.05(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.976
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         5239
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.976
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0362
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0461P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0818
_refine_ls_wR_factor_ref         0.0849
_reflns_number_gt                4405
_reflns_number_total             5239
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bt6296.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2202328
_cod_database_fobs_code          2202328