6-(Acetoxymethyl)-5-chloro-2-[(2<i>R</i>,3<i>R</i>,4<i>R</i>,5<i>S</i>)-3,4-diacetoxy-2,5-bis(chloromethyl)-2,3,4,5-tetrahydrofuran-2-yloxy]-3,4,5,6-tetrahydro-2<i>H</i>-pyran-3,4-diyl diacetate toluene solvate
Hui-Liang Wen; Zhi-Jie Fang; Zi-Sheng Wu; Ming-Yong Xie; Acta Crystallographica Section E 62 (2006) o1157–o1159; doi:10.1107/S1600536806006167

data_2208377
_publ_section_title
;6-(Acetoxymethyl)-5-chloro-2-[(2<i>R</i>,3<i>R</i>,4<i>R</i>,5<i>S</i>)-3,4-diacetoxy-2,5-bis(chloromethyl)-2,3,4,5-tetrahydrofuran-2-yloxy]-3,4,5,6-tetrahydro-2<i>H</i>-pyran-3,4-diyl
 diacetate toluene solvate
;
_journal_coeditor_code           LH6586
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1157
_journal_page_last               o1159
_journal_paper_doi               10.1107/S1600536806006167
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          'C22 H29 Cl3 O13, C7 H8'
_chemical_formula_moiety         'C22 H29 Cl3 O13, C7 H8'
_chemical_formula_sum            'C29 H37 Cl3 O13'
_chemical_formula_weight         699.94
_chemical_name_systematic
;6-(Acetoxymethyl)-2-[(2R,3R,4R,5S)-3,4-diacetoxy-2,5-bis(chloromethyl)-
2,3,4,5-tetrahydrofuran-2-yloxy]-5-chloro-3,4,5,6-tetrahydro-2H-pyran-3,4-diyl
diacetate
 toluene solvate
;
_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                   8.3693(13)
_cell_length_b                   13.072(2)
_cell_length_c                   31.603(5)
_cell_measurement_reflns_used    4347
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      26.09
_cell_measurement_theta_min      2.48
_cell_volume                     3457.5(9)
_computing_cell_refinement       'SAINT (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Bruker, 1998) and PLATON (Spek,2003)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART-CCD area detector'
_diffrn_measurement_method       '\f and \w'
_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  0.0565
_diffrn_reflns_av_sigmaI/netI    0.0767
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            18609
_diffrn_reflns_theta_full        26.32
_diffrn_reflns_theta_max         26.32
_diffrn_reflns_theta_min         1.29
_exptl_absorpt_coefficient_mu    0.325
_exptl_absorpt_correction_T_max  0.960
_exptl_absorpt_correction_T_min  0.756
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.536
_refine_diff_density_min         -0.533
_refine_ls_abs_structure_details 'Flack (1983) 3019 Friedels'
_refine_ls_abs_structure_Flack   0.00(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     411
_refine_ls_number_reflns         7000
_refine_ls_number_restraints     85
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.1380
_refine_ls_R_factor_gt           0.0628
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0387P)^2^+3.6447P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1216
_refine_ls_wR_factor_ref         0.1530
_reflns_number_gt                3951
_reflns_number_total             7000
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh6586.cif
_cod_data_source_block           I
_cod_original_cell_volume        3457.4(9)
_cod_database_code               2208377
_cod_database_fobs_code          2208377