(5<i>S</i>)-3-Phenyl-5-[(6<i>R</i>,7<i>R</i>,14<i>R</i>)-1,8,13,16-tetraoxadispiro[5.0.5.4]hexadecan-14-yl]-4,5-dihydroisoxazole: the Major Adduct Resulting from Cycloaddition of Benzonitrile Oxide to (6<i>R</i>,7<i>R</i>,14<i>S</i>)-14-Vinyl-1,8,13,16-tetraoxadispiro[5.0.5.4]hexadecane
Blake, A. J.; Gould, R. O.; Paton, R. M.; Todd, C. J.; Acta Crystallographica Section C 53 (1997) 116–117; doi:10.1107/S0108270196012243

data_2005868
_publ_section_title
;(5<i>S</i>)-3-Phenyl-5-[(6<i>R</i>,7<i>R</i>,14<i>R</i>)-1,8,13,16-tetraoxadispiro[5.0.5.4]hexadecan-14-yl]-4,5-dihydroisoxazole:
 the Major Adduct Resulting from Cycloaddition of Benzonitrile Oxide to
 (6<i>R</i>,7<i>R</i>,14<i>S</i>)-14-Vinyl-1,8,13,16-tetraoxadispiro[5.0.5.4]hexadecane
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              116
_journal_page_last               117
_journal_paper_doi               10.1107/S0108270196012243
_journal_volume                  53
_journal_year                    1997
_chemical_formula_sum            'C21 H27 N O5'
_chemical_formula_weight         373.44
_chemical_name_systematic
;
5S-3-Phenyl-5-(6'R,7R,14'R-1',8',13',16'-tetraoxadispiro[5.0.5.4]
hexadecan-14'-yl)-4,5-dihydrooxisoxazole
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 95.04(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.3561(14)
_cell_length_b                   9.892(2)
_cell_length_c                   14.937(3)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      16
_cell_measurement_theta_min      15
_cell_volume                     935.5(3)
_computing_cell_refinement       DIF4
_computing_data_collection       'DIF4 (Stoe & Cie, 1990a)'
_computing_data_reduction        'REDU4 (Stoe & Cie, 1990b)'
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 1992)'
_computing_publication_material  SHELXL93
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       Stoe
_diffrn_measurement_method       \w/2\q
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0162
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1308
_diffrn_reflns_theta_max         22.53
_diffrn_reflns_theta_min         2.74
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.094
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_density_meas      ?
_exptl_crystal_description       Column
_exptl_crystal_F_000             400
_exptl_crystal_size_max          0.78
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.156
_refine_diff_density_min         -0.140
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   -0.6(13)
_refine_ls_extinction_coef       0.040(5)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.095
_refine_ls_goodness_of_fit_obs   1.096
_refine_ls_hydrogen_treatment    'H-atom U's refined'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         1304
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.136
_refine_ls_restrained_S_obs      1.096
_refine_ls_R_factor_all          0.0305
_refine_ls_R_factor_obs          0.0276
_refine_ls_shift/esd_max         -0.043
_refine_ls_shift/esd_mean        0.010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0504P)^2^+0.1692P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0766
_refine_ls_wR_factor_obs         0.0714
_reflns_number_observed          1237
_reflns_number_total             1308
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ha1176.cif
_cod_data_source_block           phistc
_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:

'_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.

'_exptl_absorpt_correction_type' value 'None' changed to
'none' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

'_geom_bond_publ_flag'
value 'Y' changed to 'y' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (26
times).

'_geom_torsion_publ_flag' value 'Y' changed to 'y' according
to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29 (4 times).

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 'calc w =
1/[\s^2^(Fo^2^)+(0.0504P)^2^+0.1692P] 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^)+(0.0504P)^2^+0.1692P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        935.6(3)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2005868