2,3:4,5-Di-<i>O</i>-isopropylidenefructos-1-yl <i>p</i>-toluenesulfonate
Huo, Shiyong; Li, Yueqing; Liang, Chaoyan; Liu, Jihong; Zhao, Weijie; Acta Crystallographica Section E 66 (2010) o3097–; doi:10.1107/S1600536810044582

data_2228529
_publ_section_title
;
 2,3:4,5-Di-<i>O</i>-isopropylidenefructos-1-yl
 <i>p</i>-toluenesulfonate
;
_journal_coeditor_code           RK2243
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3097
_journal_paper_doi               10.1107/S1600536810044582
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C19 H26 O8 S'
_chemical_formula_moiety         'C19 H26 O8 S'
_chemical_formula_sum            'C19 H26 O8 S'
_chemical_formula_weight         414.47
_chemical_melting_point          357
_chemical_name_systematic
;
2,3:4,5-Di-<i>O</i>-isopropylidenefructos-1-yl <i>p</i>-toluenesulfonate
;
_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           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 106.831(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.870(5)
_cell_length_b                   10.153(4)
_cell_length_c                   15.715(6)
_cell_measurement_reflns_used    4356
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      23.0
_cell_measurement_theta_min      2.4
_cell_volume                     2118.2(14)
_computing_cell_refinement       '<i>SAINT-Plus</i> (Bruker, 2001)'
_computing_data_collection       '<i>APEX2</i> (Bruker, 2005)'
_computing_data_reduction        '<i>SAINT-Plus</i> (Bruker, 2001)'
_computing_molecular_graphics    '<i>SHELXTL</i> (Sheldrick, 2008)'
_computing_publication_material  '<i>SHELXTL</i> (Sheldrick, 2008)'
_computing_structure_refinement  '<i>SHELXL97</i> (Sheldrick, 2008)'
_computing_structure_solution    '<i>SHELXS97</i> (Sheldrick, 2008)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       '\f- and \w-scans'
_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  0.0184
_diffrn_reflns_av_sigmaI/netI    0.0332
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10503
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.32
_exptl_absorpt_coefficient_mu    0.194
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.27
_refine_diff_density_max         0.148
_refine_diff_density_min         -0.187
_refine_ls_abs_structure_details 'Flack (1983), 3010 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.02(5)
_refine_ls_extinction_coef       0.0092(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     '<i>SHELXL97</i> (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         6948
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0342
_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^)+(0.0498P)^2^+0.0150P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0833
_refine_ls_wR_factor_ref         0.0884
_reflns_number_gt                6040
_reflns_number_total             6948
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            rk2243.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2228529
_cod_database_fobs_code          2228529