Absolute Structure of (Thian-5-one 1,1-dioxide)-3-spiro-3'-(5'-<i>O</i>-<i>tert</i>-butyldimethylsilyl-3'-deoxy-1',2'-<i>O</i>-isopropylidene-α-<small>D</small>-<i>xylo</i>-pentofuranose), a Novel Type of Spirosugar
Bernardinelli, G.; Tronchet, J. M. J.; Kovacs, I.; Acta Crystallographica Section C 53 (1997) 511–513; doi:10.1107/S010827019601445X

data_2006082
_publ_section_title
;Absolute Structure of (Thian-5-one
 1,1-dioxide)-3-spiro-3'-(5'-<i>O</i>-<i>tert</i>-butyldimethylsilyl-3'-deoxy-1',2'-<i>O</i>-isopropylidene-\a-<small>D</small>-<i>xylo</i>-pentofuranose),
 a Novel Type of Spirosugar
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              511
_journal_page_last               513
_journal_paper_doi               10.1107/S010827019601445X
_journal_volume                  53
_journal_year                    1997
_chemical_formula_moiety         'C18 H32 O7 S Si'
_chemical_formula_structural     'C18 H32 O7 S Si'
_chemical_formula_sum            'C18 H32 O7 S Si'
_chemical_formula_weight         420.6
_chemical_melting_point          161.0(2)
_chemical_name_systematic
; (thian-5-one-1,1-dioxide)-3-spiro-3'-(5'-O-tert-butyldimethylsilyl-3'-
  deoxy-1',2'-O-isopropylidene-alpha-D-xylo-pentofuranose)
;
_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           from_xtal_archive_file_using_CIFIO
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.6446(5)
_cell_length_b                   9.4721(8)
_cell_length_c                   35.046(2)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    293
_cell_measurement_theta_max      30.5
_cell_measurement_theta_min      14.5
_cell_volume                     2205.7(3)
_computing_cell_refinement       'Xtal LATCON (Hall, Flack & Stewart, 1992)'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction        Xtal_REFCAL_LSABS__SORTRF
_computing_molecular_graphics    Xtal_ORTEP
_computing_publication_material  Xtal_BONDLA_CIFIO
_computing_structure_refinement  Xtal_CRYLSQ
_computing_structure_solution    'MULTAN87 (Main et al., 1987)'
_diffrn_ambient_temperature      293
_diffrn_measurement_device       'Nonius CAD-4'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         Sealed-off_tube
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.031
_diffrn_reflns_av_sigmaI/netI    0.048
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3412
_diffrn_reflns_theta_max         54.96
_diffrn_reflns_theta_min         2.53
_diffrn_standards_decay_%        6.5
_diffrn_standards_interval_count 100
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    2.123
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.78
_exptl_absorpt_correction_type
'analytical by integration (Blanc, Schwarzenbach & Flack, 1991)'
_exptl_absorpt_process_details
;Analytical integration, xtal_lsabs program (Blanc, Schwarzenbach & Flack,
 1991)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.266
_exptl_crystal_density_meas      ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.026
_refine_diff_density_max         0.738
_refine_diff_density_min         -0.314
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   '\c = 0.02(5)'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   3.432
_refine_ls_goodness_of_fit_obs   3.101
_refine_ls_hydrogen_treatment
;
All non-methyl H atoms observed and refined (with fixed U~iso~);
all coordinates of methyl H atoms calculated
;
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     278
_refine_ls_number_reflns         2501
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.068
_refine_ls_R_factor_obs          0.059
_refine_ls_shift/esd_max         0.000182
_refine_ls_shift/esd_mean        0.0000176
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/\s^2^(F~o~)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.048
_refine_ls_wR_factor_obs         0.041
_reflns_number_observed          2501
_reflns_number_total             2746
_reflns_observed_criterion       F>4\s(F)
_cod_data_source_file            pa1244.cif
_cod_data_source_block           KOVA
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '160.8-161.2' was changed to
'161.0(2)' - the average value was taken and precision was estimated.

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 'w = 1/\s^2^(F~o~)' 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^(F~o~)'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2205.7(2)
_cod_original_sg_symbol_Hall     P_2ac_2ab
_cod_original_formula_sum        'C18 H32 O7 Si S'
_cod_database_code               2006082