6-[Bis(ethoxycarbonyl)methyl]-6-deoxy-1,2;3,4-di-<i>O</i>-isopropylidene-<small>D</small>-galactopyranose
Doboszewski, Bogdan; da Silva, Paulo R.; Nazarenko, Alexander Y.; Nemykin, Victor N.; Acta Crystallographica Section E 66 (2010) o3217–o3218; doi:10.1107/S1600536810046921

data_2228626
_publ_section_title
;
 6-[Bis(ethoxycarbonyl)methyl]-6-deoxy-1,2;3,4-di-<i>O</i>-isopropylidene-<small>D</small>-galactopyranose
;
_journal_coeditor_code           ZL2327
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3217
_journal_page_last               o3218
_journal_paper_doi               10.1107/S1600536810046921
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C19 H30 O9'
_chemical_formula_moiety         'C19 H30 O9'
_chemical_formula_sum            'C19 H30 O9'
_chemical_formula_weight         402.43
_chemical_melting_point          322
_chemical_name_systematic
;
6-[Bis(ethoxycarbonyl)methyl]-6-deoxy-1,2;3,4-di-<i>O</i>-isopropylidene-
D-galactopyranose
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.3287(4)
_cell_length_b                   10.8895(4)
_cell_length_c                   23.7706(16)
_cell_measurement_reflns_used    9579
_cell_measurement_temperature    292(2)
_cell_measurement_theta_max      68.17
_cell_measurement_theta_min      6.69
_cell_volume                     2155.9(2)
_computing_cell_refinement       '<i>HKL-2000</i> (Otwinowski & Minor, 1997)'
_computing_data_collection       '<i>CrystalClear-SM Expert</i> (Rigaku, 2009)'
_computing_data_reduction        '<i>CrystalClear-SM Expert</i> (Rigaku, 2009)'
_computing_molecular_graphics    '<i>ORTEP-3 for Windows</i> (Farrugia, 1999)'
_computing_publication_material  '<i>PLATON</i> (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      292(2)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID II imaging plate'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0750
_diffrn_reflns_av_sigmaI/netI    0.0746
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            9353
_diffrn_reflns_theta_full        66.49
_diffrn_reflns_theta_max         66.49
_diffrn_reflns_theta_min         6.69
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  12
_diffrn_standards_number         9353
_exptl_absorpt_coefficient_mu    0.828
_exptl_absorpt_correction_T_max  0.840
_exptl_absorpt_correction_T_min  0.822
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>ABSCOR</i>; Higashi,1995)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.240
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.185
_refine_diff_density_min         -0.154
_refine_ls_abs_structure_details 'Flack (1983),  1607 Friedel pairs'
_refine_ls_abs_structure_Flack   0.06(18)
_refine_ls_extinction_coef       0.0057(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         3745
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0402
_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^)+(0.0285P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0875
_refine_ls_wR_factor_ref         0.0963
_reflns_number_gt                2824
_reflns_number_total             3745
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            zl2327.cif
_cod_data_source_block           I
_cod_database_code               2228626
_cod_database_fobs_code          2228626