Synthesis of a Novel, Highly Symmetric Bis-Oxa-Bridged Compound
Faiz Ahmed Khan; Jyotirmayee Dash; Journal of the American Chemical Society 124 (2002) 2424–2425; doi:10.1021/ja017371f

data_4114681
_publ_section_title
;
 Synthesis of a Novel, Highly Symmetric Bis-Oxa-Bridged Compound
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2424
_journal_page_last               2425
_journal_paper_doi               10.1021/ja017371f
_journal_volume                  124
_journal_year                    2002
_chemical_formula_sum            'C24 H32 O14'
_chemical_formula_weight         544.50
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 109.169(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            4
_cell_length_a                   14.043(5)
_cell_length_b                   13.819(5)
_cell_length_c                   14.067(5)
_cell_measurement_temperature    293(2)
_cell_volume                     2578.5(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.1031
_diffrn_reflns_av_sigmaI/netI    0.3111
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8681
_diffrn_reflns_theta_full        24.96
_diffrn_reflns_theta_max         24.96
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    0.116
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.219
_refine_diff_density_min         -0.238
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.739
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     351
_refine_ls_number_reflns         4357
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.739
_refine_ls_R_factor_all          0.2385
_refine_ls_R_factor_gt           0.0674
_refine_ls_shift/su_max          2.760
_refine_ls_shift/su_mean         0.549
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1463
_refine_ls_wR_factor_ref         0.2015
_reflns_number_gt                1246
_reflns_number_total             4357
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja017371f_s2.cif
_cod_data_source_block           14feb
_cod_database_code               4114681