3-<i>O</i>-<i>tert</i>-Butyldimethylsilyl-2,2':5,6-di-<i>O</i>-isopropylidene-2-<i>C</i>-hydroxymethyl-<small>D</small>-1,4-gluconolactone
Cowley, Andrew R.; Fleet, George W. J.; Iezzi Simone, Michela; Soengas, Raquel; Acta Crystallographica Section E 60 (2004) o2142–o2143; doi:10.1107/S1600536804025310

data_2204561
_publ_section_title
3-<i>O</i>-<i>tert</i>-Butyldimethylsilyl-2,2':5,6-di-<i>O</i>-isopropylidene-2-<i>C</i>-hydroxymethyl-<small>D</small>-1,4-gluconolactone
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2142
_journal_page_last               o2143
_journal_paper_doi               10.1107/S1600536804025310
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          'C19 H34 O7 Si1'
_chemical_formula_moiety         'C19 H34 O7 Si1'
_chemical_formula_sum            'C19 H34 O7 Si'
_chemical_formula_weight         402.56
_chemical_name_systematic
;
2,2:5,6-Di-O-isopropylidene-2-C-hydroxymethyl-D-glucono-1,4-lactone
;
_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
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.4765(2)
_cell_length_b                   13.2189(2)
_cell_length_c                   25.7075(6)
_cell_measurement_reflns_used    12716
_cell_measurement_temperature    150
_cell_measurement_theta_max      28
_cell_measurement_theta_min      5
_cell_volume                     2200.88(9)
_computing_cell_refinement       'COLLECT and DENZO'
_computing_data_collection       'COLLECT  (Nonius, 2000)'
_computing_data_reduction        'COLLECT and DENZO (Otwinowski & Minor, 1996)'
_computing_molecular_graphics    'ATOMS (Shape Software, 2002)'
_computing_publication_material  CRYSTALS
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.051
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            12716
_diffrn_reflns_theta_full        27.470
_diffrn_reflns_theta_max         27.470
_diffrn_reflns_theta_min         5.203
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.141
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.95
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(DENZO/SCALEPACK; Otwinowski & Minor, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.215
_exptl_crystal_density_meas      ?
_exptl_crystal_description       fragment
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.45
_refine_diff_density_min         -0.29
_refine_ls_abs_structure_details 'Flack (1983), 1960 Friedel pairs'
_refine_ls_abs_structure_Flack   0.04(12)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1144
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         4025
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0480
_refine_ls_R_factor_gt           0.0373
_refine_ls_shift/su_max          0.001951
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;Method, part 1, Chebychev polynomial (Watkin, 1994; Prince, 1982):
[weight] =
 1.0/[A~0~T~0~(x) + A~1~T~1~(x) ... + A~n-1~]T~n-1~(x)],
where A~i~ are the
 Chebychev coefficients listed below and x = F~calc~/F~max~;
Method = Robust
 Weighting (Prince, 1982); W =
[weight][1-(\dF/6*\sF)^2^]^2^, with A~i~ are
 0.682, 0.0517 and 0.322
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0446
_refine_ls_wR_factor_gt          0.0396
_refine_ls_wR_factor_ref         0.0396
_reflns_number_gt                4025
_reflns_number_total             4801
_reflns_threshold_expression     I>3s(I)
_cod_data_source_file            rz6004.cif
_cod_data_source_block           1
_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 'none' 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 
;
_cod_original_formula_sum        'C19 H34 O7 Si1'
_cod_database_code               2204561