(1<i>R</i>,4'<i>S</i>)-4-(<i>tert</i>-Butyldimethylsilanoxy)-1-[2,2-dimethyl-3-(<i>p</i>-tolylsulfonyl)-1,3-oxazolidin-4-yl]but-2-yn-1-ol
Erdsack, Jörg; Schürmann, Markus; Preut, Hans; Krause, Norbert; Acta Crystallographica Section E 64 (2008) o1171–; doi:10.1107/S1600536808014906

data_2218413
_publ_section_title
(1<i>R</i>,4'<i>S</i>)-4-(<i>tert</i>-Butyldimethylsilanoxy)-1-[2,2-dimethyl-3-(<i>p</i>-tolylsulfonyl)-1,3-oxazolidin-4-yl]but-2-yn-1-ol
_journal_coeditor_code           HB2724
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1171
_journal_paper_doi               10.1107/S1600536808014906
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          'C22 H35 N O5 S Si'
_chemical_formula_moiety         'C22 H35 N O5 S Si'
_chemical_formula_sum            'C22 H35 N O5 S Si'
_chemical_formula_weight         453.66
_chemical_name_systematic
;
(1<i>R</i>,4'<i>S</i>)-4-(<i>tert</i>-Butyldimethylsilanoxy)-
1-[2,2-dimethyl-3-(p-tolylsulfonyl)-1,3-oxazolidin-4-yl]but-2-yn-1-ol
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 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                 121.40(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   26.283(5)
_cell_length_b                   11.335(2)
_cell_length_c                   19.219(4)
_cell_measurement_reflns_used    20719
_cell_measurement_temperature    173.0(10)
_cell_measurement_theta_max      25.34
_cell_measurement_theta_min      2.60
_cell_volume                     4887(2)
_computing_cell_refinement
;
DENZO and SCALEPACK (Otwinowski & Minor, 1997)
;
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction
;
DENZO and SCALEPACK (Otwinowski & Minor, 1997)
;
_computing_molecular_graphics    'SHELXTL-Plus (Sheldrick, 2008)'
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008) and PLATON (Spek, 2003)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean '19 vertical, 18 horizontal'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method
;
286 frames via \w-rotation (\D\w=1\%) and two times 120 s per frame
(3 sets at different \k-angles)
;
_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  0.035
_diffrn_reflns_av_sigmaI/netI    0.2337
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            8353
_diffrn_reflns_theta_full        25.34
_diffrn_reflns_theta_max         25.34
_diffrn_reflns_theta_min         2.60
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.213
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.233
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1952
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.184
_refine_diff_density_min         -0.198
_refine_ls_abs_structure_details 'Flack (1983), 3636 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.09(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         8353
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.1140
_refine_ls_R_factor_gt           0.0346
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
calc [1.0exp(6.50(sin\q/\l)^2^)]/[\s^2^(Fo^2^)]
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0648
_refine_ls_wR_factor_ref         0.0870
_reflns_number_gt                3487
_reflns_number_total             8353
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb2724.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               2218413
_cod_database_fobs_code          2218413