3,3,9,9-Tetraphenyl-2,4,8,10-tetraoxaspiro[5.5]undecane
Sun, Xiaoqiang; Chen, Liang; Jiang, Yan; Li, Zhengyi; Acta Crystallographica Section E 66 (2010) o3035–; doi:10.1107/S1600536810043795

data_2227186
_publ_section_title
;
 3,3,9,9-Tetraphenyl-2,4,8,10-tetraoxaspiro[5.5]undecane
;
_journal_coeditor_code           BQ2239
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3035
_journal_paper_doi               10.1107/S1600536810043795
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C31 H28 O4'
_chemical_formula_moiety         'C31 H28 O4'
_chemical_formula_sum            'C31 H28 O4'
_chemical_formula_weight         464.53
_chemical_melting_point_gt       436
_chemical_melting_point_lt       437
_chemical_name_systematic
;
3,3,9,9-Tetraphenyl-2,4,8,10-tetraoxaspiro[5.5]undecane
;
_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
_audit_creation_method           SHELXL97
_cell_angle_alpha                102.327(7)
_cell_angle_beta                 104.199(6)
_cell_angle_gamma                112.170(4)
_cell_formula_units_Z            4
_cell_length_a                   13.509(3)
_cell_length_b                   13.790(3)
_cell_length_c                   15.626(5)
_cell_measurement_reflns_used    13730
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      24.84
_cell_measurement_theta_min      2.56
_cell_volume                     2456.8(11)
_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 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_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  0.0257
_diffrn_reflns_av_sigmaI/netI    0.0545
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13730
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.43
_exptl_absorpt_coefficient_mu    0.082
_exptl_absorpt_correction_T_max  0.9838
_exptl_absorpt_correction_T_min  0.9790
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.256
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.230
_refine_diff_density_min         -0.278
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         8545
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0936
_refine_ls_R_factor_gt           0.0527
_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^)+(0.1020P)^2^+0.5251P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1432
_refine_ls_wR_factor_ref         0.1955
_reflns_number_gt                5355
_reflns_number_total             8545
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bq2239.cif
_cod_data_source_block           I
_cod_database_code               2227186
_cod_database_fobs_code          2227186