The Major Isoxazoline Cycloadduct from Reaction of a Xylopyranosylnitrile Oxide with a Hex-5-enopyranoside
Ferguson, W. J.; Parsons, S.; Paton, R. M.; Acta Crystallographica Section C 52 (1996) 3067–3069; doi:10.1107/S010827019601178X

data_2005741
_publ_section_title
;
 The Major Isoxazoline Cycloadduct from Reaction of a
 Xylopyranosylnitrile Oxide with a Hex-5-enopyranoside
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              3067
_journal_page_last               3069
_journal_paper_doi               10.1107/S010827019601178X
_journal_volume                  52
_journal_year                    1996
_chemical_formula_sum            'C22 H31 N O12'
_chemical_formula_weight         501.48
_chemical_melting_point          466.5
_chemical_name_systematic
;
5R-(2,3,4-Tri-O-acetyl-\b-D-xylopyranosyl)-5-(2,3-O-isopropylidene-
1-O-methyl-\a-D-lyxo-tetrafuranos-4-yl)-4,5-dihydroisoxazole
;
_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'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.518(2)
_cell_length_b                   16.514(3)
_cell_length_c                   17.250(3)
_cell_measurement_reflns_used    40
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      22
_cell_measurement_theta_min      20
_cell_volume                     2426.5(8)
_computing_cell_refinement       DIF4
_computing_data_collection       'DIF4 (Stoe & Cie, 1992a)'
_computing_data_reduction        'REDU4 (Stoe & Cie, 1992b)'
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  SHELXTL/PC
_computing_structure_refinement  'SHELXTL/PC (Sheldrick, 1995)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150.0(2)
_diffrn_measurement_device
;
Stoe Stadi-4 four-circle diffractometer equipped with an Oxford
Cryosystems variable-temperature device (Cosier & Glazer, 1986)
;
_diffrn_measurement_method
;
\w-\q scans with on-line profile learning (Clegg, 1981)
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0359
_diffrn_reflns_av_sigmaI/netI    0.0764
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3897
_diffrn_reflns_theta_max         59.99
_diffrn_reflns_theta_min         3.71
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.959
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_density_meas      ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.62
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.22
_refine_diff_density_min         -0.21
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   0.2(4)
_refine_ls_extinction_coef       0.00035(6)
_refine_ls_extinction_method     'SHELXL93 (Sheldrick, 1993)'
_refine_ls_goodness_of_fit_all   1.065
_refine_ls_goodness_of_fit_obs   1.076
_refine_ls_hydrogen_treatment    'H atoms: see text'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     323
_refine_ls_number_reflns         3485
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_restrained_S_obs      1.076
_refine_ls_R_factor_all          0.0827
_refine_ls_R_factor_obs          0.0569
_refine_ls_shift/esd_max         -0.04
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0335P)^2^+1.847P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1226
_refine_ls_wR_factor_obs         0.1073
_reflns_number_observed          2713
_reflns_number_total             3493
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            bm1111.cif
_cod_data_source_block           everst
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'Not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0335P)^2^+1.847P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to 'w =
1/[\s^2^(Fo^2^)+(0.0335P)^2^+1.847P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               2005741