(2<i>R</i>,5<i>S</i>)-2-Trichloromethyl-3-oxa-1-azabicyclo[3.3.0]octane-4,8-dione
Punzo, Francesco; Watkin, David J.; Pike, Richard; Moloney, Mark; Panchal, Terry; Acta Crystallographica Section E 61 (2005) o42–o44; doi:10.1107/S1600536804031605

data_2204968
_publ_section_title
(2<i>R</i>,5<i>S</i>)-2-Trichloromethyl-3-oxa-1-azabicyclo[3.3.0]octane-4,8-dione
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o42
_journal_page_last               o44
_journal_paper_doi               10.1107/S1600536804031605
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          'C7 H6 Cl3 N1 O3'
_chemical_formula_moiety         'C7 H6 Cl3 N1 O3'
_chemical_formula_sum            'C7 H6 Cl3 N O3'
_chemical_formula_weight         258.49
_chemical_name_systematic
;
(2R,5S)-2-Trichloromethyl-3-oxa-1-azabicyclo[3,3,0]octane-4,8-dione
;
_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
_audit_creation_method           CRYSTALS_ver_12.50
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.04800(10)
_cell_length_b                   10.1735(3)
_cell_length_c                   15.5791(4)
_cell_measurement_reflns_used    1485
_cell_measurement_temperature    190
_cell_measurement_theta_max      30
_cell_measurement_theta_min      5
_cell_volume                     958.57(4)
_computing_cell_refinement       DENZO/SCALEPACK
_computing_data_collection       'COLLECT (Nonius, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS '
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      190
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.028
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            2708
_diffrn_reflns_theta_full        28.801
_diffrn_reflns_theta_max         30.001
_diffrn_reflns_theta_min         5.175
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.933
_exptl_absorpt_correction_T_max  0.83
_exptl_absorpt_correction_T_min  0.83
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(DENZO/SCALEPACK; Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.791
_exptl_crystal_density_meas      ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.27
_refine_diff_density_min         -0.26
_refine_ls_abs_structure_details 'Flack, (1983), 1104 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.01(6)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9547
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         2692
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0297
_refine_ls_R_factor_gt           0.0269
_refine_ls_shift/su_max          0.000770
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[sigma^2^(F^2^) + 0.02 + 0.49p]
 where p=(max(Fo^2^,0) + 2Fc^2^)/3
 Method = SHELXL 97 (Sheldrick, 1997)
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0637
_refine_ls_wR_factor_gt          0.0618
_refine_ls_wR_factor_ref         0.0637
_reflns_number_gt                2545
_reflns_number_total             2692
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sj6035.cif
_cod_data_source_block           3
_cod_original_formula_sum        'C7 H6 Cl3 N1 O3'
_cod_database_code               2204968
_cod_database_fobs_code          2204968