4,6-<i>O</i>-Benzylidene-1-<i>O</i>-methyl-2,3-deoxy-α-<small>D</small>-glucopyranose-2,3-diyl 1,2-phenylene orthocarbonate
Betz, Richard; Klüfers, Peter; Acta Crystallographica Section E 63 (2007) o4132–o4132; doi:10.1107/S1600536807045266

data_2215403
_publ_section_title
;4,6-<i>O</i>-Benzylidene-1-<i>O</i>-methyl-2,3-deoxy-\a-<small>D</small>-glucopyranose-2,3-diyl
 1,2-phenylene orthocarbonate
;
_journal_coeditor_code           CF2136
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o4132
_journal_page_last               o4132
_journal_paper_doi               10.1107/S1600536807045266
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C21 H20 O8'
_chemical_formula_moiety         'C21 H20 O8'
_chemical_formula_sum            'C21 H20 O8'
_chemical_formula_weight         400.37
_chemical_name_common
;
4,6-<i>O</i>-benzylidene-methyl-\a-D-glucopyranoside-2,3-diyl 1',2'-
phenylene orthocarbonate
;
_chemical_name_systematic
;4,6-<i>O</i>-Benzylidene-1-<i>O</i>-methyl-2,3-deoxy-\a-D-glucopyranos-2,3-diyl-
1',2'-phenylene
 orthocarbonate
;
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.710(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   27.8221(12)
_cell_length_b                   5.10820(10)
_cell_length_c                   13.0090(5)
_cell_measurement_reflns_used    11294
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      3.134
_cell_volume                     1827.53(11)
_computing_cell_refinement       'SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2004)'
_computing_data_reduction
'SCALEPACK and DENZO (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEPIII (Burnett & Johnson, 1996)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Nonius Kappa 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  0.0562
_diffrn_reflns_av_sigmaI/netI    0.0399
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17337
_diffrn_reflns_theta_full        27.59
_diffrn_reflns_theta_max         27.59
_diffrn_reflns_theta_min         3.14
_exptl_absorpt_coefficient_mu    0.112
_exptl_absorpt_correction_T_max  0.996
_exptl_absorpt_correction_T_min  0.985
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SCALEPACK; Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.455
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.167
_refine_diff_density_min         -0.246
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         2340
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0674
_refine_ls_R_factor_gt           0.0430
_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^)+(0.0524P)^2^+0.4733P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0893
_refine_ls_wR_factor_ref         0.1008
_reflns_number_gt                1770
_reflns_number_total             2340
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cf2136.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               2215403
_cod_database_fobs_code          2215403