(2<i>R</i>,3<i>S</i>,4<i>R</i>)-3,4-Isopropylidenedioxy-2-(phenylsulfonylmethyl)pyrrolidin-1-ol
Flores, Mari Fe; Garcia, Pilar; M. Garrido, Narciso; Sanz, Francisca; Diez, David; Acta Crystallographica Section E 68 (2012) o2560–; doi:10.1107/S1600536812033028

data_2235759
_publ_section_title
;
 (2<i>R</i>,3<i>S</i>,4<i>R</i>)-3,4-Isopropylidenedioxy-2-(phenylsulfonylmethyl)pyrrolidin-1-ol
;
_journal_coeditor_code           BT5981
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2560
_journal_paper_doi               10.1107/S1600536812033028
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C14 H19 N O5 S'
_chemical_formula_moiety         'C14 H19 N O5 S'
_chemical_formula_sum            'C14 H19 N O5 S'
_chemical_formula_weight         313.36
_chemical_name_systematic
;
(2<i>R</i>,3<i>S</i>,4<i>R</i>)-3,4-Isopropylidenedioxy-2-
(phenylsulfonylmethyl)pyrrolidin-1-ol
;
_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                 102.658(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   9.1876(2)
_cell_length_b                   19.5284(5)
_cell_length_c                   17.9187(5)
_cell_measurement_reflns_used    9406
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      63.58
_cell_measurement_theta_min      4.93
_cell_volume                     3136.82(14)
_computing_cell_refinement       'SAINT (Bruker, 2006)'
_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_data_reduction        'SAINT (Bruker, 2006)'
_computing_molecular_graphics    'MERCURY (Macrae <i>et al.</i>, 2006)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.947
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0363
_diffrn_reflns_av_sigmaI/netI    0.0377
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            46376
_diffrn_reflns_theta_full        67.27
_diffrn_reflns_theta_max         67.27
_diffrn_reflns_theta_min         4.53
_exptl_absorpt_coefficient_mu    2.023
_exptl_absorpt_correction_T_max  0.817
_exptl_absorpt_correction_T_min  0.730
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2006)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.327
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Monoclinic
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.339
_refine_diff_density_min         -0.375
_refine_ls_abs_structure_details 'Flack (1983), 4863 Friedel pairs'
_refine_ls_abs_structure_Flack   0.040(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     769
_refine_ls_number_reflns         10345
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0519
_refine_ls_R_factor_gt           0.0484
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0765P)^2^+1.1560P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1314
_refine_ls_wR_factor_ref         0.1347
_reflns_number_gt                9616
_reflns_number_total             10345
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bt5981.cif
_cod_data_source_block           I
_cod_original_sg_symbol_Hall     'P 2yb '
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2235759
_cod_database_fobs_code          2235759