<i>rac</i>-(3a<i>R</i>,6a<i>R</i>)-(<i>E</i>)-Methyl 2-(3a-methylperhydrofuro[3,2-<i>b</i>]furan-2-ylidene)acetate
Bellovičová, Lenka; Kožíšek, Jozef; Doháňošová, Jana; Lásiková, Angelika; Gracza, Tibor; Acta Crystallographica Section E 66 (2010) o2381–; doi:10.1107/S1600536810032101

data_2227276
_publ_section_title
;
 <i>rac</i>-(3a<i>R</i>,6a<i>R</i>)-(<i>E</i>)-Methyl
 2-(3a-methylperhydrofuro[3,2-<i>b</i>]furan-2-ylidene)acetate
;
_journal_coeditor_code           BV2142
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2381
_journal_paper_doi               10.1107/S1600536810032101
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C10 H14 O4'
_chemical_formula_moiety         'C10 H14 O4'
_chemical_formula_sum            'C10 H14 O4'
_chemical_formula_weight         198.21
_chemical_name_systematic
;
<i>rac</i>-(3a<i>R</i>,6a<i>R</i>)-(<i>E</i>)-methyl
2-(3a-methylperhydrofuro[3,2-<i>b</i>]furan-2-ylidene)acetate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 101.510(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.1590(10)
_cell_length_b                   5.8100(3)
_cell_length_c                   28.5090(10)
_cell_measurement_reflns_used    35551
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.5349
_cell_measurement_theta_min      3.5743
_cell_volume                     1973.5(2)
_computing_cell_refinement       'CrysAlis CCD (Oxford Diffraction, 2009)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2009)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2009)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1998)'
_computing_publication_material  'enCIFer (Allen <i>et al.</i>, 2004)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.4340
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Oxford Diffraction Gemini R CCD'
_diffrn_measurement_method
;
Rotation method data acquisition using \w and \f scans
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0237
_diffrn_reflns_av_sigmaI/netI    0.0087
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            59312
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.58
_exptl_absorpt_coefficient_mu    0.10268
_exptl_absorpt_correction_T_max  0.988
_exptl_absorpt_correction_T_min  0.941
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
[CrysAlis Pro (Oxford Diffraction, 2010); analytical numeric absorption
correction using a multi-faceted crystal model based on expressions derived
by Clark & Reid (1995)]
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.835
_exptl_crystal_size_mid          0.360
_exptl_crystal_size_min          0.124
_refine_diff_density_max         0.321
_refine_diff_density_min         -0.221
_refine_ls_extinction_coef       0.0031(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         4025
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0362
_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^)+(0.0375P)^2^+1.2579P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0867
_refine_ls_wR_factor_ref         0.0911
_reflns_number_gt                3571
_reflns_number_total             4033
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            bv2142.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2227276
_cod_database_fobs_code          2227276