3-(2,4-Dichlorobenzylidene)-1,5-dioxaspiro[5.5]undecane-2,4-dione
Zeng, Wu-Lan; Acta Crystallographica Section E 67 (2011) o1362–; doi:10.1107/S1600536811016813

data_2230373
_publ_section_title
;
 3-(2,4-Dichlorobenzylidene)-1,5-dioxaspiro[5.5]undecane-2,4-dione
;
_journal_coeditor_code           IS2706
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1362
_journal_paper_doi               10.1107/S1600536811016813
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C16 H14 Cl2 O4'
_chemical_formula_moiety         'C16 H14 Cl2 O4'
_chemical_formula_sum            'C16 H14 Cl2 O4'
_chemical_formula_weight         341.17
_chemical_name_systematic
;
3-(2,4-Dichlorobenzylidene)-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                100.569(2)
_cell_angle_beta                 100.870(2)
_cell_angle_gamma                99.0500(10)
_cell_formula_units_Z            2
_cell_length_a                   7.2378(6)
_cell_length_b                   7.6496(7)
_cell_length_c                   14.8099(13)
_cell_measurement_reflns_used    1133
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.279
_cell_measurement_theta_min      2.955
_cell_volume                     775.80(12)
_computing_cell_refinement       'SAINT (Bruker, 1997)'
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        'SAINT (Bruker, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_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  0.0231
_diffrn_reflns_av_sigmaI/netI    0.0521
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4085
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.76
_exptl_absorpt_coefficient_mu    0.433
_exptl_absorpt_correction_T_max  0.9340
_exptl_absorpt_correction_T_min  0.9033
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>SADABS</i>; Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.461
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             352
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.185
_refine_diff_density_min         -0.208
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         2697
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0759
_refine_ls_R_factor_gt           0.0398
_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^)+(0.0188P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0652
_refine_ls_wR_factor_ref         0.0731
_reflns_number_gt                1596
_reflns_number_total             2697
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            is2706.cif
_cod_data_source_block           I
_cod_database_code               2230373
_cod_database_fobs_code          2230373