(3<i>R</i>,3a<i>S</i>,6<i>R</i>,6a<i>R</i>)-<i>tert</i>-Butyl <i>N</i>-(6-chloro-2-oxo-6a-phenylperhydrofuro[3,2-<i>b</i>]furan-3-yl)carbamate
Erdsack, Jörg; Schürmann, Markus; Preut, Hans; Krause, Norbert; Acta Crystallographica Section E 63 (2007) o3371–o3371; doi:10.1107/S1600536807031388

data_2214673
_publ_section_title
;(3<i>R</i>,3a<i>S</i>,6<i>R</i>,6a<i>R</i>)-<i>tert</i>-Butyl
 <i>N</i>-(6-chloro-2-oxo-6a-phenylperhydrofuro[3,2-<i>b</i>]furan-3-yl)carbamate
;
_journal_coeditor_code           HB2449
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3371
_journal_page_last               o3371
_journal_paper_doi               10.1107/S1600536807031388
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C17 H20 Cl N O5'
_chemical_formula_moiety         'C17 H20 Cl N O5'
_chemical_formula_sum            'C17 H20 Cl N O5'
_chemical_formula_weight         353.79
_chemical_name_systematic
;
(3R,3aS,6R,6aR)-tert-Butyl
N-(6-chloro-2-oxo-6a-phenylperhydrofuro[3,2-b]furan-3-yl)carbamate
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.1519(7)
_cell_length_b                   12.029(2)
_cell_length_c                   23.655(4)
_cell_measurement_reflns_used    14042
_cell_measurement_temperature    291.0(10)
_cell_measurement_theta_max      25.82
_cell_measurement_theta_min      3.09
_cell_volume                     1750.5(5)
_computing_cell_refinement
;
DENZO and SCALEPACK (Otwinowski & Minor, 1997)
;
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction
;
DENZO and SCALEPACK
;
_computing_molecular_graphics    'SHELXTL-Plus (Sheldrick, 1991)'
_computing_publication_material
;
SHELXL97 and PLATON (Spek, 2003)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      291.0(10)
_diffrn_detector_area_resol_mean '19 vertical, 18 horizontal'
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method
;
309 frames via \w-rotation (\D\w=1%) and two times 120 s per frame
(three sets at different \k-angles)
;
_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  0.036
_diffrn_reflns_av_sigmaI/netI    0.2241
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            14042
_diffrn_reflns_theta_full        25.79
_diffrn_reflns_theta_max         25.79
_diffrn_reflns_theta_min         3.09
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.244
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.101
_refine_diff_density_min         -0.106
_refine_ls_abs_structure_details 'Flack (1983), 1313 Friedel pairs'
_refine_ls_abs_structure_Flack   0.08(10)
_refine_ls_extinction_coef       0.0215(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         3280
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.1433
_refine_ls_R_factor_gt           0.0285
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; calc
 [1.0exp(7.10(sin\q/\l)^2^)]/[\s^2^(Fo^2^)]
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0552
_refine_ls_wR_factor_ref         0.0785
_reflns_number_gt                1085
_reflns_number_total             3280
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb2449.cif
_cod_data_source_block           I
_cod_database_code               2214673
_cod_database_fobs_code          2214673