3,9-Di-<i>tert</i>-butyl-2,4,8,10-tetraoxaspiro[5.5]undecane
Li, Zhengyi; Chen, Liang; Tang, Qiuzheng; Sun, Xiaoqiang; Acta Crystallographica Section E 66 (2010) o3368–; doi:10.1107/S1600536810049524

data_2228557
_publ_section_title
;
 3,9-Di-<i>tert</i>-butyl-2,4,8,10-tetraoxaspiro[5.5]undecane
;
_journal_coeditor_code           SI2313
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3368
_journal_paper_doi               10.1107/S1600536810049524
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C15 H28 O4'
_chemical_formula_moiety         'C15 H28 O4'
_chemical_formula_sum            'C15 H28 O4'
_chemical_formula_weight         272.37
_chemical_melting_point_gt       451
_chemical_melting_point_lt       452
_chemical_name_systematic
;
3,9-Di-<i>tert</i>-butyl-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                 113.846(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   26.726(4)
_cell_length_b                   5.7894(8)
_cell_length_c                   11.2635(15)
_cell_measurement_reflns_used    3133
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      25.78
_cell_measurement_theta_min      3.11
_cell_volume                     1594.0(4)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'APEX2 (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0192
_diffrn_reflns_av_sigmaI/netI    0.0213
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4400
_diffrn_reflns_theta_full        25.78
_diffrn_reflns_theta_max         25.78
_diffrn_reflns_theta_min         3.33
_exptl_absorpt_coefficient_mu    0.080
_exptl_absorpt_correction_T_max  0.9881
_exptl_absorpt_correction_T_min  0.9724
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.135
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             600
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.213
_refine_diff_density_min         -0.252
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     90
_refine_ls_number_reflns         1513
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0416
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.4000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1356
_refine_ls_wR_factor_ref         0.1448
_reflns_number_gt                1347
_reflns_number_total             1513
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            si2313.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2228557
_cod_database_fobs_code          2228557