Crystal structure of <i>rac</i>-3,9-bis(2,6-difluorophenyl)-2,4,8,10-tetraoxaspiro[5.5]undecane
Chen, Liang; Li, Zhengyi; Jin, Linlin; Sun, Xiaoqiang; Wang, Zhiming; Acta Crystallographica Section E 71 (2015) o127–o128; doi:10.1107/S2056989015001206

data_2240417
_publ_section_title
;
 Crystal structure of
 <i>rac</i>-3,9-bis(2,6-difluorophenyl)-2,4,8,10-tetraoxaspiro[5.5]undecane
;
_journal_coeditor_code           SU5070
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o127
_journal_page_last               o128
_journal_paper_doi               10.1107/S2056989015001206
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C19 H16 F4 O4'
_chemical_formula_moiety         'C19 H16 F4 O4'
_chemical_formula_sum            'C19 H16 F4 O4'
_chemical_formula_weight         384.32
_chemical_name_systematic
;
3,9-Bis(2,6-difluorophenyl)-2,4,8,10-tetraoxaspiro[5.5]undecane
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 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                 95.442(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   28.960(5)
_cell_length_b                   5.5627(11)
_cell_length_c                   11.205(2)
_cell_measurement_reflns_used    2905
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      29.65
_cell_measurement_theta_min      2.83
_cell_volume                     1796.9(6)
_computing_cell_refinement
;
SAINT (Bruker, 2009)
;
_computing_data_collection
;
APEX2 (Bruker, 2009)
;
_computing_data_reduction
;
SAINT (Bruker, 2009)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEXII 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  0.0307
_diffrn_reflns_av_sigmaI/netI    0.0333
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4856
_diffrn_reflns_theta_full        25.49
_diffrn_reflns_theta_max         25.49
_diffrn_reflns_theta_min         1.41
_exptl_absorpt_coefficient_mu    0.126
_exptl_absorpt_correction_T_max  0.9814
_exptl_absorpt_correction_T_min  0.9753
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2009)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.421
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.260
_refine_diff_density_min         -0.340
_refine_ls_extinction_coef       0.057(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     124
_refine_ls_number_reflns         1671
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0501
_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^)+(0.0997P)^2^+0.5847P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1423
_refine_ls_wR_factor_ref         0.1483
_reflns_number_gt                1444
_reflns_number_total             1671
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            su5070sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        1797.0(6)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2240417
_cod_database_fobs_code          2240417