(3a<i>R</i>,5<i>R</i>,7<i>S</i>,7a<i>S</i>)-5-[(<i>tert</i>-Butyldimethylsilyloxy)methyl]-7-ethoxy-3-methyl-7,7a-dihydro-3a<i>H</i>-pyrano[4,3-<i>d</i>]isoxazol-4(5<i>H</i>)-one
Cottier, Louis; Srivastava, Rajendra M.; Sinou, Denis; Freitas Filho, Joao R.; Jeanneau, Erwann; Acta Crystallographica Section E 62 (2006) o540–o541; doi:10.1107/S1600536805034392

data_2208057
_publ_section_title
(3a<i>R</i>,5<i>R</i>,7<i>S</i>,7a<i>S</i>)-5-[(<i>tert</i>-Butyldimethylsilyloxy)methyl]-7-ethoxy-3-methyl-7,7a-dihydro-3a<i>H</i>-pyrano[4,3-<i>d</i>]isoxazol-4(5<i>H</i>)-one
_journal_coeditor_code           FL6197
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o540
_journal_page_last               o541
_journal_paper_doi               10.1107/S1600536805034392
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          'C16 H29 N O5 Si'
_chemical_formula_moiety         'C16 H29 N O5 Si'
_chemical_formula_sum            'C16 H29 N O5 Si'
_chemical_formula_weight         343.49
_chemical_melting_point          90
_chemical_name_systematic
;
(3aR,5S,7S,7aS)-5-{[tert-Butyl(dimethyl)silyloxy]methyl}-7-ethoxy-3-methyl-
7,7a-dihydro-3aH-pyrano[4,3-d]isoxazol-4(5H)-one
;
_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
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.366(5)
_cell_length_b                   11.372(5)
_cell_length_c                   23.020(5)
_cell_measurement_reflns_used    2082
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     1928.3(16)
_computing_cell_refinement       DENZO/SCALEPACK
_computing_data_collection       'COLLECT (Nonius, 2001)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 1996)'
_computing_publication_material  CRYSTALS
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.049
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            3739
_diffrn_reflns_theta_full        25.232
_diffrn_reflns_theta_max         27.426
_diffrn_reflns_theta_min         1.769
_exptl_absorpt_coefficient_mu    0.144
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.78
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   '(DIFABS; Walker & Stuart, 1983)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_description       needle
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.26
_refine_diff_density_min         -0.24
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.0566
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         1647
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0749
_refine_ls_R_factor_gt           0.0463
_refine_ls_shift/su_max          0.000192
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Weighting scheme: Chebychev polynomial (Watkin, 1994; Prince,
1982):  w = 1/[1.31T~0~(x)-0.0224T~1~(x)+0.584T~2~(x)+0.0446T~3~(x)],
where x = F~calc~/F~max~;  robust weighting (Prince, 1982): W =
w[1-(\dF/6\sF)^2^]^2^
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0475
_refine_ls_wR_factor_ref         0.0475
_reflns_number_gt                1647
_reflns_number_total             2388
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fl6197.cif
_cod_data_source_block           III
_cod_database_code               2208057
_cod_database_fobs_code          2208057