Hydroxy group interactions in stannylated carbohydrates. Structures and thermal stabilities of 5-deoxy-5-C-(Ph3Sn)-1,2-O-isopropylidene-??-D-xylofuranose, 5-deoxy-5-C-(IPh2Sn)-1,2-O-isopropylidene-??-D- and -L-xylofuranose, and 5-deoxy-5-C-(I2PhSn)-1,2-O-isopropylidene-??-D- and -L-xylofuranose
Burnett, Lynne A.; Ferreira, Vitor F.; Alan Howie, R.; Rufino, Helena; Skakle, Janet M. S.; Wardell, James L.; Wardell, Solange M. S. V.; Journal of the Chemical Society, Perkin Transactions 1  (2002) 2288–; doi:10.1039/b204675j

data_7204458
_publ_section_title
;
 Hydroxy group interactions in stannylated carbohydrates. Structures
 and thermal stabilities of
 5-deoxy-5-C-(Ph3Sn)-1,2-O-isopropylidene-??-D-xylofuranose,
 5-deoxy-5-C-(IPh2Sn)-1,2-O-isopropylidene-??-D- and -L-xylofuranose,
 and 5-deoxy-5-C-(I2PhSn)-1,2-O-isopropylidene-??-D- and
 -L-xylofuranose
;
_journal_issue                   20
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 1'
_journal_page_first              2288
_journal_paper_doi               10.1039/b204675j
_journal_year                    2002
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C31 H36 O6 Sn'
_chemical_formula_sum            'C31 H36 O6 Sn'
_chemical_formula_weight         623.29
_chemical_melting_point          395.0(10)
_chemical_name_systematic
; 
3-C-(Triphenylstannyl)methyl-1,2:5,6-di-O-isopropylidene-alpha-D-
allofuranose
;
_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     heavy
_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                   6.070(4)
_cell_length_b                   13.074(12)
_cell_length_c                   37.69(3)
_cell_measurement_reflns_used    14
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      5.05
_cell_measurement_theta_min      4.6
_cell_volume                     2991(4)
_computing_cell_refinement       'Nicolet P3 software (Nicolet, 1980)'
_computing_data_collection       'Nicolet P3 software (Nicolet, 1980)'
_computing_data_reduction        'RDNIC (Howie, 1980)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Nicolet P3'
_diffrn_measurement_method       \w-scan
_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  0.0213
_diffrn_reflns_av_sigmaI/netI    0.5258
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3077
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.08
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 50
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.894
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1280
_exptl_crystal_preparation       'from hexane as solvent'
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.481
_refine_diff_density_min         -0.786
_refine_diff_density_rms         0.105
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.05(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         3063
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.1312
_refine_ls_R_factor_gt           0.0560
_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^)+(0.0325P)^2^+4.6114P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0940
_refine_ls_wR_factor_ref         0.1116
_reflns_number_gt                1862
_reflns_number_total             3063
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            b204675j.txt
_cod_data_source_block           (D)-6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '394-396' was changed to '395.0(10)'
- the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 
;
_cod_database_code               7204458