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_4028727
_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         'C14 H21 Cl O6'
_chemical_formula_sum            'C14 H21 Cl O6'
_chemical_formula_weight         320.76
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                80.767(3)
_cell_angle_beta                 80.035(3)
_cell_angle_gamma                84.869(3)
_cell_formula_units_Z            2
_cell_length_a                   7.5473(13)
_cell_length_b                   8.2391(14)
_cell_length_c                   12.532(2)
_cell_measurement_reflns_used    3570
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.32
_cell_measurement_theta_min      2.51
_cell_volume                     756.1(2)
_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 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.0168
_diffrn_reflns_av_sigmaI/netI    0.0391
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5016
_diffrn_reflns_theta_full        28.32
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         2.51
_exptl_absorpt_coefficient_mu    0.277
_exptl_absorpt_correction_T_max  0.9649
_exptl_absorpt_correction_T_min  0.9518
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_description       prism
_exptl_crystal_F_000             340
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.647
_refine_diff_density_min         -0.768
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.193
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         3570
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.193
_refine_ls_R_factor_all          0.0801
_refine_ls_R_factor_gt           0.0575
_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^)+(0.0526P)^2^+2.4718P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1315
_refine_ls_wR_factor_ref         0.1899
_reflns_number_gt                2979
_reflns_number_total             3570
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo401870s_si_003.cif
_cod_data_source_block           Compound_3g
_cod_database_code               4028727