Structural studies of the regioselectivity of bishydroxylation of polycyclic methylenecyclobutanol derivatives
Ianelli, S.; Nardelli, M.; Belletti, D.; Brosse, N.; Jamart-Grégoire, B.; Caubère, P.; Acta Crystallographica Section C 49 (1993) 2022–2027; doi:10.1107/S0108270193004718

data_2001260
_publ_section_title
;
 Structural studies of the regioselectivity of bishydroxylation of
 polycyclic methylenecyclobutanol derivatives
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              2022
_journal_page_last               2027
_journal_paper_doi               10.1107/S0108270193004718
_journal_volume                  49
_journal_year                    1993
_chemical_formula_analytical     'C16 H26 O4'
_chemical_formula_sum            'C16 H26 O4'
_chemical_formula_weight         282.38
_chemical_name_systematic
;
cis-transoid-cis-7,8-dihydroxytricyclo[7.5.0.0^2,8^]tetradec-1-yl acetate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                90.090(10)
_cell_angle_beta                 104.50(2)
_cell_angle_gamma                90.630(10)
_cell_formula_units_Z            2
_cell_length_a                   5.7300(10)
_cell_length_b                   15.767(6)
_cell_length_c                   8.3940(10)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      40.0
_cell_measurement_theta_min      25.6
_cell_volume                     734.1(3)
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens AED diffractometer'
_diffrn_measurement_method       '\q-2\q scan'
_diffrn_radiation_monochromator  Ni-filter
_diffrn_radiation_source         'standard Cu anode'
_diffrn_radiation_type           'Cu K\=\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_sigmaI/netI    0.0271
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            2779
_diffrn_reflns_reduction_process
;   All reflections were corrected for Lorentz and polarization effects
   but not for absorption.
;
_diffrn_reflns_theta_max         70.12
_diffrn_reflns_theta_min         5.44
_diffrn_standards_decay_%        'within statistical fluctuation'
_diffrn_standards_interval_count 50
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    .691
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.277
_exptl_crystal_description
;
small prisms
;
_exptl_crystal_F_000             308
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.39
_refine_diff_density_max         0.231
_refine_diff_density_min         -0.163
_refine_ls_extinction_coef       0.038(2)
_refine_ls_extinction_method     'SHELXL92 (Sheldrick, 1992)'
_refine_ls_goodness_of_fit_all   1.009
_refine_ls_goodness_of_fit_obs   1.128
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     189
_refine_ls_number_reflns         2777
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_restrained_S_obs      1.128
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_obs          0.0366
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef F^2^
_refine_ls_weighting_scheme
; calc w=1/[\s^2^(F~o~^2^) + ( 0.0592P)^2^ + 0.0184P]
  where P = (F~o~^2^ + 2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.1076
_refine_ls_wR_factor_obs         0.0998
_reflns_number_observed          2098
_reflns_number_total             2779
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            al1053.cif
_cod_data_source_block           2
_cod_original_cell_volume        734.2(3)
_cod_database_code               2001260