<i>rac</i>-<i>N</i>-(6a-Butyl-6-chloro-2-oxoperhydrofuro[3,2-<i>b</i>]furan-3-yl)-2,2,2-trifluoroacetamide
Erdsack, Jörg; Schürmann, Markus; Preut, Hans; Krause, Norbert; Acta Crystallographica Section E 63 (2007) o3372–o3372; doi:10.1107/S1600536807031376

data_2214674
_publ_section_title
<i>rac</i>-<i>N</i>-(6a-Butyl-6-chloro-2-oxoperhydrofuro[3,2-<i>b</i>]furan-3-yl)-2,2,2-trifluoroacetamide
_journal_coeditor_code           HB2450
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3372
_journal_page_last               o3372
_journal_paper_doi               10.1107/S1600536807031376
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C12 H15 Cl F3 N O4'
_chemical_formula_moiety         'C12 H15 Cl F3 N O4'
_chemical_formula_sum            'C12 H15 Cl F3 N O4'
_chemical_formula_weight         329.70
_chemical_name_systematic
;
rac-N-(6a-Butyl-6-chloro-2-oxoperhydrofuro[3,2-b]furan-3-yl)-2,2,2-
trifluoroacetamide
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                66.904(13)
_cell_angle_beta                 76.782(14)
_cell_angle_gamma                71.684(13)
_cell_formula_units_Z            2
_cell_length_a                   7.674(3)
_cell_length_b                   9.586(3)
_cell_length_c                   11.590(4)
_cell_measurement_reflns_used    8179
_cell_measurement_temperature    291.0(10)
_cell_measurement_theta_max      25.32
_cell_measurement_theta_min      3.08
_cell_volume                     739.1(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  'SHELXTL 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 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Nonius KappaCCD area-detector'
_diffrn_measurement_method
;
185 frames via \w-rotation (\D\w = 2\%) and two times 190 s per frame
(four 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  0.0310
_diffrn_reflns_av_sigmaI/netI    0.2022
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8179
_diffrn_reflns_theta_full        25.32
_diffrn_reflns_theta_max         25.32
_diffrn_reflns_theta_min         3.08
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.306
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             340
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.143
_refine_diff_density_min         -0.121
_refine_ls_extinction_coef       0.0297(18)
_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   0.905
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     219
_refine_ls_number_reflns         2680
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.905
_refine_ls_R_factor_all          0.1384
_refine_ls_R_factor_gt           0.0313
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
w = [1.0 exp(4.90(sin\q/\l)^2^)]/[\s^2^(Fo^2^)]
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0571
_refine_ls_wR_factor_ref         0.0790
_reflns_number_gt                959
_reflns_number_total             2680
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb2450.cif
_cod_data_source_block           I
_cod_original_cell_volume        739.1(4)
_cod_database_code               2214674
_cod_database_fobs_code          2214674