7,14-Bis(4-methoxyphenyl)-11,11-dimethyl-1,4,10,12-tetraoxadispiro[4.2.5.2]pentadecane-9,13-dione
Zhang, Jinpeng; Yan, Shu; Ding, Jie; Acta Crystallographica Section E 65 (2009) o1076–; doi:10.1107/S1600536809013658

data_2221724
_publ_section_title
7,14-Bis(4-methoxyphenyl)-11,11-dimethyl-1,4,10,12-tetraoxadispiro[4.2.5.2]pentadecane-9,13-dione
_journal_coeditor_code           HK2665
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1076
_journal_paper_doi               10.1107/S1600536809013658
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C27 H30 O8'
_chemical_formula_moiety         'C27 H30 O8'
_chemical_formula_sum            'C27 H30 O8'
_chemical_formula_weight         482.51
_chemical_melting_point          479
_chemical_name_systematic
;
7,14-Bis(4-methoxyphenyl)-11,11-dimethyl-1,4,10,12-
tetraoxadispiro[4.2.5.2]pentadecane-9,13-dione
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 94.934(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.977(5)
_cell_length_b                   20.162(9)
_cell_length_c                   12.508(6)
_cell_measurement_reflns_used    1366
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      19.535
_cell_measurement_theta_min      2.285
_cell_volume                     2507(2)
_computing_cell_refinement       'SAINT (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_molecular_graphics
'ORTEP-3 for Windows (Farrugia, 1997) and PLATON (Spek, 2009)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.935
_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  0.1044
_diffrn_reflns_av_sigmaI/netI    0.1633
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11754
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.28
_exptl_absorpt_coefficient_mu    0.094
_exptl_absorpt_correction_T_max  0.9888
_exptl_absorpt_correction_T_min  0.9607
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.279
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.460
_refine_diff_density_min         -0.213
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         4126
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.2361
_refine_ls_R_factor_gt           0.0747
_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^)+(0.055P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1392
_refine_ls_wR_factor_ref         0.1874
_reflns_number_gt                1349
_reflns_number_total             4126
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hk2665.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2221724
_cod_database_fobs_code          2221724