Further studies on silatropic carbonyl ene cyclisations: β-crotyl(diphenyl)silyloxy aldehyde substrates; synthesis of 2-deoxy-2-C-phenylhexoses
Robertson, Jeremy; Green, Stuart P.; Hall, Michael J.; Tyrrell, Andrew J.; Unsworth, William P.; Organic & Biomolecular Chemistry 6 (2008) 2628–2635; doi:10.1039/b804752a

data_7150936
_publ_section_title
;
 Further studies on silatropic carbonyl ene cyclisations:
 \b-crotyl(diphenyl)silyloxy aldehyde substrates; synthesis of
 2-deoxy-2-C-phenylhexoses
;
_journal_issue                   14
_journal_name_full               'Organic &amp; Biomolecular Chemistry'
_journal_page_first              2628
_journal_page_last               2635
_journal_paper_doi               10.1039/b804752a
_journal_volume                  6
_journal_year                    2008
_chemical_compound_source
;
?
;
_chemical_formula_moiety         ' C20 H24 O2 Si1 '
_chemical_formula_sum            'C20 H24 O2 Si'
_chemical_formula_weight         324.50
_chemical_melting_point          ?
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             02-17-04
_audit_creation_method           CRYSTALS_ver_12-03-99
_cell_angle_alpha                90
_cell_angle_beta                 97.145(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.8918(3)
_cell_length_b                   15.1623(7)
_cell_length_c                   13.7021(5)
_cell_measurement_reflns_used    3867
_cell_measurement_temperature    120
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     1832.97(12)
_computing_cell_refinement
;
Denzo/Scalepack (Otwinowski & Minor, 1996)
;
_computing_data_collection
;
COLLECT (Nonius BV, 1997)
;
_computing_data_reduction
;
Denzo/Scalepack (Otwinowski & Minor, 1996)
;
_computing_molecular_graphics
;
CAMERON (Watkin et al 1996)
;
_computing_publication_material
;
CRYSTALS (Watkin et al 2001)
;
_computing_structure_refinement
;
CRYSTALS (Watkin et al 2001)
;
_computing_structure_solution
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SIR92 (Altomare et al, 1994)
;
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type
;
Enraf Nonius Kappa CCD
;
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.01
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6513
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         5.19
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.135
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.97
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            ' colourless '
_exptl_crystal_density_diffrn    1.176
_exptl_crystal_density_meas      ?
_exptl_crystal_description       ' plate '
_exptl_crystal_F_000             696.554
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_refine_ls_hydrogen_treatment    noref
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_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Chebychev polynomial with 3 parameters, Carruthers & Watkin , 1979,
1.64 0.392 1.18
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0584
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              19
_reflns_limit_k_min              0
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_gt                2996
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_reflns_threshold_expression     >3.00\s(I)
_cod_data_source_file            b804752a.txt
_cod_data_source_block           CRYSTALS_cif
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic ' changed to 'monoclinic'
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:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        1833.0
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        ' C20 H24 O2 Si1 '
_cod_database_code               7150936