(2<i>R</i>,3<i>R</i>,4<i>S</i>)-3-(<i>tert</i>-Butyldiphenylsiloxy)-4-hydroxy-3-methylhex-5-ene-1,2-diyl Diacetate
Lewinski, Krzysztof; Acta Crystallographica Section C 53 (1997) 753–755; doi:10.1107/S0108270197000498

data_2006236
_publ_contact_author
;    Dr Krzysztof Lewinski
 Faculty of Chemistry
 Jagiellonian University
 ul. Ingardena 3
 30-060 Krakow, Poland
;
_publ_section_title
;(2<i>R</i>,3<i>R</i>,4<i>S</i>)-3-(<i>tert</i>-Butyldiphenylsiloxy)-4-hydroxy-3-methylhex-5-ene-1,2-diyl
 Diacetate
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              753
_journal_page_last               755
_journal_paper_doi               10.1107/S0108270197000498
_journal_volume                  53
_journal_year                    1997
_chemical_formula_moiety         'C27 H36 O6 Si'
_chemical_formula_sum            'C27 H36 O6 Si'
_chemical_formula_weight         484.65
_chemical_name_systematic
;
(3S,4R,5R)-5,6-diacetoxy-4-(t-butyldiphenylsilyloxy)-3-hydroxy
-4-methylhex-1-en
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_audit_creation_method           'SHELXL and manual'
_cell_angle_alpha                90.00
_cell_angle_beta                 92.300(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.8380(10)
_cell_length_b                   9.3470(10)
_cell_length_c                   13.4560(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17.5
_cell_measurement_theta_min      14.0
_cell_volume                     1362.0(2)
_computing_cell_refinement       'CAD-4 Software'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction        'MOLEN (Fair, 1990)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  'PARST (Nardelli, 1983)'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       CAD-4
_diffrn_measurement_method       '\w/2\q scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0235
_diffrn_reflns_av_sigmaI/netI    0.0163
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4964
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.37
_diffrn_standards_decay_%        0.5
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.123
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.182
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.135
_refine_diff_density_min         -0.150
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   -0.05(10)
_refine_ls_extinction_coef       0.016(2)
_refine_ls_extinction_method     'SHELXL93 (Sheldrick, 1993)'
_refine_ls_goodness_of_fit_all   1.021
_refine_ls_goodness_of_fit_obs   1.037
_refine_ls_hydrogen_treatment    'H atoms: see text'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         4755
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_restrained_S_obs      1.037
_refine_ls_R_factor_all          0.0345
_refine_ls_R_factor_obs          .0317
_refine_ls_shift/esd_max         0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0596P)^2^+0.1165P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0869
_refine_ls_wR_factor_obs         .0856
_reflns_number_observed          4485
_reflns_number_total             4755
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            na1274.cif
_cod_data_source_block           MR13
_cod_depositor_comments
;
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^)+(0.0596P)^2^+0.1165P] 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^)+(0.0596P)^2^+0.1165P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2006236