Monoclinic polymorph of 2,5-dideoxy-2,5-epithio-1,3:4,6-bis-<i>O</i>-[(<i>R</i>)-phenylmethylene]-<small>L</small>-iditol
Gibson, Jerrell G.; Cho, Jung Young; Fronczek, Frank R.; Watkins, Steven F.; Acta Crystallographica Section E 68 (2012) o2668–o2669; doi:10.1107/S1600536812034514

data_2236486
_publ_section_title
;
 Monoclinic polymorph of
 2,5-dideoxy-2,5-epithio-1,3:4,6-bis-<i>O</i>-[(<i>R</i>)-phenylmethylene]-<small>L</small>-iditol
;
_journal_coeditor_code           MW2079
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2668
_journal_page_last               o2669
_journal_paper_doi               10.1107/S1600536812034514
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C20 H20 O4 S1'
_chemical_formula_moiety         'C20 H20 O4 S1'
_chemical_formula_sum            'C20 H20 O4 S'
_chemical_formula_weight         356.42
_chemical_melting_point          481.5(5)
_chemical_name_systematic
;
2,5-dideoxy-2,5-epithio-1,3:4,6-bis-<i>O</i>-[(<i>R</i>)-phenylmethylene]-
<i>L</i>-iditol
;
_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           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 95.785(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.1580(10)
_cell_length_b                   9.223(2)
_cell_length_c                   15.407(4)
_cell_measurement_pressure       101.3
_cell_measurement_reflns_used    3254
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      33.10
_cell_measurement_theta_min      2.50
_cell_volume                     870.6(3)
_computing_cell_refinement
'DENZO and SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2000)'
_computing_data_reduction
'DENZO and SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material
'WinGX (Farrugia, 1999) and IDEAL (Gould <i>et al.</i>, 1988)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0(5)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6225
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         33.14
_diffrn_reflns_theta_min         2.58
_exptl_absorpt_coefficient_mu    0.208
_exptl_absorpt_correction_T_max  0.9795
_exptl_absorpt_correction_T_min  0.9499
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SCALEPACK; Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.36
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             376
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.293
_refine_diff_density_min         -0.230
_refine_ls_abs_structure_details 'Flack (1983), 2730 Bijvoet pairs'
_refine_ls_abs_structure_Flack   0.02(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     227
_refine_ls_number_reflns         6225
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_gt           0.037
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0366P)^2^+0.1562P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0882
_reflns_number_gt                5648
_reflns_number_total             6225
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            mw2079.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21'
_cod_original_formula_sum        'C20 H20 O4 S1'
_cod_database_code               2236486
_cod_database_fobs_code          2236486