Stereochemistry of transposition reactions involving polycyclic methylenecyclobutanol derivatives
Ianelli, S.; Nardelli, M.; Belletti, D.; Brosse, N.; Jamart-Grégoire, B.; Caubère, P.; Acta Crystallographica, Section C: Crystal Structure Communications 50 (1994) 569–574; doi:10.1107/s0108270193010601

data_2009634
_publ_section_title
;
 Stereochemistry of transposition reactions involving polycyclic
 methylenecyclobutanol derivatives
;
_journal_coden_ASTM              ACSCEE
_journal_coeditor_code           LI1073
_journal_issue                   4
_journal_name_full
;
 Acta Crystallographica, Section C: Crystal Structure Communications
;
_journal_page_first              569
_journal_page_last               574
_journal_paper_doi               10.1107/s0108270193010601
_journal_volume                  50
_journal_year                    1994
_chemical_formula_analytical     'C14 H20 O4'
_chemical_formula_sum            'C14 H20 O4'
_chemical_formula_weight         252.31
_chemical_name_systematic
;
cis,anti,cis-1-acetoxy-7-hydroxytricyclo[7.3.0.0^2,7^]dodecan-8-one
;
_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   difmap
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90.060(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.769(2)
_cell_length_b                   15.185(2)
_cell_length_c                   15.849(2)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      36
_cell_measurement_theta_min      25
_cell_volume                     2591.7(7)
_computing_cell_refinement       'LQPARM (Nardelli & Mangia, 1984)'
_computing_data_collection       'local programs'
_computing_data_reduction        'local programs'
_computing_molecular_graphics    'ORTEP (Johnson, 1965)'
_computing_publication_material
;
 PARST (Nardelli, 1983); PARSTCIF (Nardelli, 1991)
;
_computing_structure_refinement  'SHELXL92 (Sheldrick, 1992)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1985)'
_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         'fine focus sealed X-ray tube'
_diffrn_radiation_type           'Cu K\a~1~'
_diffrn_radiation_wavelength     1.5405620
_diffrn_reflns_av_R_equivalents  0.0869
_diffrn_reflns_av_sigmaI/netI    0.0787
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5218
_diffrn_reflns_theta_max         70.1
_diffrn_reflns_theta_min         4.0
_diffrn_standards_interval_count 50
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    0.730
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_description       'small prisms'
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.33
_refine_diff_density_max         0.268
_refine_diff_density_min         -0.223
_refine_ls_extinction_coef       0.0053(3)
_refine_ls_extinction_expression
'F~c~^*^ = kF~c~[1 + 0.001\cF~c~^2^\l^3^/sin(2\q)]^-1/4^'
_refine_ls_extinction_method
'F~c~^*^ = kF~c~[1 + 0.001\cF~c~^2^\l^3^/sin(2\q)]^-1/4^'
_refine_ls_goodness_of_fit_all   0.817
_refine_ls_goodness_of_fit_obs   0.989
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     486
_refine_ls_number_reflns         4946
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0966
_refine_ls_R_factor_obs          0.0472
_refine_ls_shift/esd_max         0.492
_refine_ls_shift/esd_mean        0.013
_refine_ls_structure_factor_coef F^2^
_refine_ls_weighting_details
'w = 1/[\s^2^(F~o~^2^) + (0.0686P)^2^]  where  P = (F~o~^2^ + 2F~c~^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1265
_refine_ls_wR_factor_obs         0.1238
_reflns_number_observed          2782
_reflns_number_total             4947
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            li1073.cif
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w = 1/[\s^2^(F~o~^2^) +
(0.0686P)^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^) + (0.0686P)^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_sg_symbol_H-M      'P 21/c'
_cod_database_code               2009634