(+)-(1<i>S</i>,5<i>R</i>,6<i>R</i>)-6-[(<i>S</i>)-1-Hydroxy-2-(methoxymethyloxy)ethyl]-1-methyl-3-trichloromethyl-2-aza-4,7-dioxabicyclo[3.3.0]oct-2-en-8-one
Oishi, Takeshi; Oishi, Hiroki; Tsuzaki, Syun; Sato, Takaaki; Chida, Noritaka; Acta Crystallographica Section E 68 (2012) o3185–; doi:10.1107/S1600536812042912

data_2236404
_publ_section_title
;
 (+)-(1<i>S</i>,5<i>R</i>,6<i>R</i>)-6-[(<i>S</i>)-1-Hydroxy-2-(methoxymethyloxy)ethyl]-1-methyl-3-trichloromethyl-2-aza-4,7-dioxabicyclo[3.3.0]oct-2-en-8-one
;
_journal_coeditor_code           IS5207
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3185
_journal_paper_doi               10.1107/S1600536812042912
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C11 H14 Cl3 N O6'
_chemical_formula_moiety         'C11 H14 Cl3 N O6'
_chemical_formula_sum            'C11 H14 Cl3 N O6'
_chemical_formula_weight         362.58
_chemical_melting_point          409.7
_chemical_name_systematic
(+)-(1<i>S</i>,5<i>R</i>,6<i>R</i>)-6-[(<i>S</i>)-1-Hydroxy-2-(methoxymethyloxy)ethyl]-1-methyl-3-trichloromethyl-2-aza-4,7-dioxabicyclo[3.3.0]oct-2-en-8-one
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 99.699(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.9311(7)
_cell_length_b                   6.0283(4)
_cell_length_c                   13.8694(10)
_cell_measurement_reflns_used    5778
_cell_measurement_temperature    90
_cell_measurement_theta_max      25.1150
_cell_measurement_theta_min      2.3135
_cell_volume                     736.05(9)
_computing_cell_refinement       'SAINT (Bruker, 2012)'
_computing_data_collection       'APEX2 (Bruker, 2012)'
_computing_data_reduction        'SAINT (Bruker, 2012)'
_computing_molecular_graphics    '<i>Mercury</i> (Macrae <i>et al.</i>, 2006)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker D8 goniometer'
_diffrn_measurement_method       '\w scans'
_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  0.0279
_diffrn_reflns_av_sigmaI/netI    0.0301
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6662
_diffrn_reflns_theta_full        25.12
_diffrn_reflns_theta_max         25.12
_diffrn_reflns_theta_min         2.31
_exptl_absorpt_coefficient_mu    0.648
_exptl_absorpt_correction_T_max  0.9035
_exptl_absorpt_correction_T_min  0.7377
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2012)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.636
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             372
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.160
_refine_diff_density_max         0.369
_refine_diff_density_min         -0.215
_refine_ls_abs_structure_details 'Flack (1983), 947 Friedel pairs'
_refine_ls_abs_structure_Flack   0.01(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.341
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         2364
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.341
_refine_ls_R_factor_all          0.0278
_refine_ls_R_factor_gt           0.0266
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0338P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0671
_refine_ls_wR_factor_ref         0.0687
_reflns_number_gt                2291
_reflns_number_total             2364
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            is5207.cif
_cod_data_source_block           I
_cod_database_code               2236404
_cod_database_fobs_code          2236404