3,9-Bis(2,4-dichlorophenyl)-2,4,8,10-tetraoxaspiro[5.5]undecane
Li, Zhengyi; Tang, Qiuzheng; Wu, Kang; Yu, Shuling; Sun, Xiaoqiang; Acta Crystallographica Section E 66 (2010) o1864–; doi:10.1107/S1600536810024712

data_2226426
_publ_section_title
;
 3,9-Bis(2,4-dichlorophenyl)-2,4,8,10-tetraoxaspiro[5.5]undecane
;
_journal_coeditor_code           EZ2218
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1864
_journal_paper_doi               10.1107/S1600536810024712
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C19 H16 Cl4 O4'
_chemical_formula_moiety         'C19 H16 Cl4 O4'
_chemical_formula_sum            'C19 H16 Cl4 O4'
_chemical_formula_weight         450.12
_chemical_name_systematic
;
3,9-Bis(2,4-dichlorophenyl)-2,4,8,10-tetraoxaspiro[5.5]undecane
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 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                 93.275(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.365(2)
_cell_length_b                   5.7397(9)
_cell_length_c                   11.7464(19)
_cell_measurement_reflns_used    2876
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      29.48
_cell_measurement_theta_min      2.84
_cell_volume                     966.9(3)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w 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  0.0219
_diffrn_reflns_av_sigmaI/netI    0.0260
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5044
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.42
_exptl_absorpt_coefficient_mu    0.635
_exptl_absorpt_correction_T_max  0.9052
_exptl_absorpt_correction_T_min  0.8782
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.546
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             460
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.345
_refine_diff_density_min         -0.404
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     123
_refine_ls_number_reflns         1686
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0349
_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^)+(0.1330P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1409
_refine_ls_wR_factor_ref         0.1597
_reflns_number_gt                1444
_reflns_number_total             1686
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ez2218.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 2/c'
_cod_database_code               2226426
_cod_database_fobs_code          2226426