An Unusual Fragmentation of Oxetane-Embedded Tetracyclic Ketal Systems
G. Hari Mangeswara Rao; Faiz Ahmed Khan; Journal of Organic Chemistry 78 (2013) 11092–11095; doi:10.1021/jo401870s

data_4028726
_publ_section_title
;
 An Unusual Fragmentation of Oxetane-Embedded Tetracyclic Ketal Systems
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              11092
_journal_page_last               11095
_journal_paper_doi               10.1021/jo401870s
_journal_volume                  78
_journal_year                    2013
_chemical_formula_moiety         'C13 H18 O6'
_chemical_formula_sum            'C13 H18 O6'
_chemical_formula_weight         270.27
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 90.309(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   11.8699(12)
_cell_length_b                   27.928(3)
_cell_length_c                   7.6424(7)
_cell_measurement_reflns_used    6258
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.33
_cell_measurement_theta_min      2.25
_cell_volume                     2533.4(4)
_computing_cell_refinement       'SMART 5.628 (Bruker, 2003)'
_computing_data_collection       'SMART 5.628 (Bruker, 2003)'
_computing_data_reduction        'SAINT+ 6.45  (Bruker, 2003)'
_computing_molecular_graphics    'diamond 3.1d'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    Sir92
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker smart Apex'
_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  0.0664
_diffrn_reflns_av_sigmaI/netI    0.0911
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            16801
_diffrn_reflns_theta_full        28.33
_diffrn_reflns_theta_max         28.33
_diffrn_reflns_theta_min         2.25
_diffrn_standards_decay_%        0.5
_diffrn_standards_interval_time  60
_exptl_absorpt_coefficient_mu    0.112
_exptl_absorpt_correction_T_max  0.9855
_exptl_absorpt_correction_T_min  0.9801
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_description       prism
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.477
_refine_diff_density_min         -0.514
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         6258
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.1359
_refine_ls_R_factor_gt           0.0826
_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^)+(0.0000P)^2^+9.8524P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1329
_refine_ls_wR_factor_ref         0.1679
_reflns_number_gt                4091
_reflns_number_total             6258
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo401870s_si_002.cif
_cod_data_source_block           Compound_2c
_cod_original_cell_volume        2533.5(4)
_cod_database_code               4028726