3-(4-Fluorobenzylidene)-1,5-dioxaspiro[5.5]undecane-2,4-dione
Zeng, Wu-Lan; Acta Crystallographica Section E 67 (2011) o276–; doi:10.1107/S1600536810054395

data_2229006
_publ_section_title
;
 3-(4-Fluorobenzylidene)-1,5-dioxaspiro[5.5]undecane-2,4-dione
;
_journal_coeditor_code           CV5023
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o276
_journal_paper_doi               10.1107/S1600536810054395
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C16 H15 F O4'
_chemical_formula_moiety         'C16 H15 F O4'
_chemical_formula_sum            'C16 H15 F O4'
_chemical_formula_weight         290.28
_chemical_name_systematic
;
3-(4-Fluorobenzylidene)-1,5-dioxaspiro[5.5]undecane-2,4-dione
;
_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
_cell_angle_alpha                100.68(3)
_cell_angle_beta                 90.73(3)
_cell_angle_gamma                91.20(3)
_cell_formula_units_Z            2
_cell_length_a                   5.6690(11)
_cell_length_b                   10.130(2)
_cell_length_c                   12.160(2)
_cell_measurement_reflns_used    2481
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.41
_cell_volume                     686.0(2)
_computing_cell_refinement       'SAINT (Bruker, 1997)'
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        'SAINT (Bruker, 1997)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       'phi and omega 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  0.0285
_diffrn_reflns_av_sigmaI/netI    0.0331
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6753
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.41
_exptl_absorpt_coefficient_mu    0.109
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             304
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.221
_refine_diff_density_min         -0.219
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         3124
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0397
_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 w=1/[\s^2^(Fo^2^)+(0.0750P)^2^+0.0414P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1122
_refine_ls_wR_factor_ref         0.1267
_reflns_number_gt                2481
_reflns_number_total             3124
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            cv5023.cif
_cod_data_source_block           I
_cod_database_code               2229006
_cod_database_fobs_code          2229006