Investigation of the base promoted tandem syn-elimination–Favorskii rearrangement of levoglucosan sulfonates
Muldgaard, Lene; Thomsen, Ib B.; Hazell, Rita G.; Bols, Mikael; Journal of the Chemical Society, Perkin Transactions 1  (2002) 1297–; doi:10.1039/b200064b

data_7204347
_publ_section_title
;
 Investigation of the base promoted tandem syn-elimination--Favorskii
 rearrangement of levoglucosan sulfonates
;
_journal_issue                   10
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 1'
_journal_page_first              1297
_journal_paper_doi               10.1039/b200064b
_journal_year                    2002
_chemical_formula_sum            'C14 H20 O8'
_chemical_formula_weight         316.31
_chemical_name_systematic
;
Di-(2,3-dideoxy-3-methoxycarbonyl-beta-D-erythro-pentofuranose)-
1,5':1',5-dianhydride
;
_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_type_scat_source           IntTabIV
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_cell_angle_beta                 92.386(3)
_cell_angle_gamma                90.000
_cell_formula_units_Z            2
_cell_length_a                   16.975(2)
_cell_length_b                   5.1909(6)
_cell_length_c                   8.569(1)
_cell_measurement_reflns_used    605
_cell_measurement_temperature    298
_cell_measurement_theta_max      21.3
_cell_measurement_theta_min      2.4
_cell_volume                     754.41(15)
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        'SAINT (Siemens, 1995)'
_computing_molecular_graphics
;
ORTEP-III (Burnett & Johnson,  1996), KRYSTAL
;
_computing_publication_material  KRYSTAL
_computing_structure_refinement  'modified ORFLS(1962), KRYSTAL'
_computing_structure_solution
;
SIR97 (Altomare et al., 1997 ), KRYSTAL
;
_diffrn_ambient_temperature      298
_diffrn_measurement_device       'Siemens SMART CCD diffractometer'
_diffrn_measurement_method       '\w rotation scans with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'x-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.081
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            2433
_diffrn_reflns_reduction_process 2433
_diffrn_reflns_theta_max         29.2
_diffrn_reflns_theta_min         2.4
_exptl_absorpt_coefficient_mu    0.115
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.39
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       needle
_exptl_crystal_F_000             336
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.36(7)
_refine_diff_density_min         -0.37(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.72
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    1
_refine_ls_number_parameters     99
_refine_ls_number_reflns         932
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.078
_refine_ls_shift/su_max          0.0014
_refine_ls_shift/su_mean         0.0003
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
w= 1/{[\s~cs~(F^2^)+1.02F^2^]^1/2^- |F|}^2^
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.100
_reflns_number_gt                934
_reflns_number_total             1210
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            b200064b.txt
_cod_data_source_block           ib30
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_site_thermal_displace_type' tag value 'Uij' was replaced with
'Uani' value 11 times.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        754.4(2)
_cod_original_sg_symbol_H-M      C2
_cod_original_formula_sum        C14H20O8
_cod_database_code               7204347