Structural Aspects of the Transposition Reaction of Oxatricyclo[6.5.0.0^2,7^]tridecane-6,7-diol Monomesylate
Ianelli, S.; Nardelli, M.; Belletti, D.; Jamart-Grégoire, B.; Mercier-Girardot, S.; Caubère, P.; Acta Crystallographica Section C 52 (1996) 1243–1248; doi:10.1107/S0108270195014417

data_2004847
_publ_section_title
;
 Structural Aspects of the Transposition Reaction of
 Oxatricyclo[6.5.0.0^2,7^]tridecane-6,7-diol Monomesylate
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1243
_journal_page_last               1248
_journal_paper_doi               10.1107/S0108270195014417
_journal_volume                  52
_journal_year                    1996
_chemical_formula_analytical     'C14 H22 O5'
_chemical_formula_sum            'C14 H22 O5'
_chemical_formula_weight         270.33
_chemical_name_systematic
;
(1RS,2SR,6SR,7SR,8SR)1-acetoxy-3-oxatricyclo[6.5.0.0^2,7^]tridecan-6,7-diol
;
_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                112.13(4)
_cell_angle_beta                 104.58(5)
_cell_angle_gamma                91.52(4)
_cell_formula_units_Z            4
_cell_length_a                   7.909(3)
_cell_length_b                   12.608(9)
_cell_length_c                   15.303(11)
_cell_measurement_reflns_used    29
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      37.24
_cell_measurement_theta_min      18.92
_cell_volume                     1355.4(16)
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens AED diffractometer'
_diffrn_measurement_method       '\q-2\q scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_sigmaI/netI    0.039
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5167
_diffrn_reflns_reduction_process
;
standard
;
_diffrn_reflns_theta_max         70.25
_diffrn_reflns_theta_min         3.25
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 50
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    0.825
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_description       prism
_exptl_crystal_F_000             584
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.16
_refine_diff_density_min         -0.15
_refine_ls_extinction_coef       0.034(3)
_refine_ls_extinction_method     'SHELXL93 (Sheldrick, 1993)'
_refine_ls_goodness_of_fit_all   0.932
_refine_ls_goodness_of_fit_obs   1.050
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     520
_refine_ls_number_reflns         5167
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.932
_refine_ls_restrained_S_obs      1.050
_refine_ls_R_factor_all          0.0714
_refine_ls_R_factor_obs          0.0343
_refine_ls_shift/esd_max         -0.004
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef F^2^
_refine_ls_weighting_details
'w = 1/[\s^2^(F~o~^2^)+(0.05P)^2^]  where  P=(F~o~^2^+2F~c~^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0980
_refine_ls_wR_factor_obs         0.0845
_reflns_number_observed          3235
_reflns_number_total             5167
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            bm1024.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w =
1/[\s^2^(F~o~^2^)+(0.05P)^2^] where P=(F~o~^2^+2F~c~^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to 'w =
1/[\s^2^(F~o~^2^)+(0.05P)^2^] where P=(F~o~^2^+2F~c~^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1355(2)
_cod_database_code               2004847