5,7,13,14-Tetraoxatrispiro[2.2.2.2^9^.2^6^.2^3^]pentadecane
Betz, Richard; Klüfers, Peter; Reichvilser, Moritz M.; Acta Crystallographica Section E 63 (2007) o3558–o3558; doi:10.1107/S1600536807034915

data_2214558
_publ_section_title
;
 5,7,13,14-Tetraoxatrispiro[2.2.2.2^9^.2^6^.2^3^]pentadecane
;
_journal_coeditor_code           BT2444
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3558
_journal_page_last               o3558
_journal_paper_doi               10.1107/S1600536807034915
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C11 H16 O4'
_chemical_formula_moiety         'C11 H16 O4'
_chemical_formula_sum            'C11 H16 O4'
_chemical_formula_weight         212.242
_chemical_name_systematic
;
5,7,13,14-Tetraoxatrispiro[2.2.2.2^9^.2^6^.2^3^]pentadecane
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.2980(8)
_cell_length_b                   7.1520(8)
_cell_length_c                   23.508(3)
_cell_measurement_temperature    200(3)
_cell_measurement_theta_max      27.4984
_cell_measurement_theta_min      4.3875
_cell_volume                     1058.9(2)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2005)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2005)'
_computing_data_reduction        'CrysAlis RED'
_computing_molecular_graphics    'ORTEPIII (Burnett & Johnson, 1996)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>,  1999)'
_diffrn_ambient_temperature      200(3)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Oxford XCalibur3'
_diffrn_measurement_method       \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  0.0438
_diffrn_reflns_av_sigmaI/netI    0.0340
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            6256
_diffrn_reflns_theta_full        27.56
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         4.40
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.101
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.3314(3)
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             456
_exptl_crystal_size_max          0.259
_exptl_crystal_size_mid          0.185
_exptl_crystal_size_min          0.098
_refine_diff_density_max         0.158
_refine_diff_density_min         -0.172
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     137
_refine_ls_number_reflns         1442
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0414
_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^)+(0.0525P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0927
_refine_ls_wR_factor_ref         0.0983
_reflns_number_gt                1237
_reflns_number_total             1442
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bt2444.cif
_cod_data_source_block           I
_cod_database_code               2214558
_cod_database_fobs_code          2214558