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_2009633
_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     'C15 H22 O3'
_chemical_formula_sum            'C15 H22 O3'
_chemical_formula_weight         250.34
_chemical_name_systematic
;
trans,syn,cis-1-acetoxytricyclo[7.4.0.0^2,7^]tridecan-8-one
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P -2n 2a'
_symmetry_space_group_name_H-M   'P 21 c n'
_atom_sites_solution_hydrogens   'difmap excepting C14 methyl'
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.902(6)
_cell_length_b                   11.952(5)
_cell_length_c                   9.380(6)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17.6
_cell_measurement_theta_min      10.2
_cell_volume                     1334.0(10)
_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, 1986)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-Nonius CAD4 diffractometer'
_diffrn_measurement_method       '\q-2\q scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine focus X-ray sealed tube'
_diffrn_radiation_type           'Mo K\a~1~'
_diffrn_radiation_wavelength     0.709300
_diffrn_reflns_av_R_equivalents  0.0230
_diffrn_reflns_av_sigmaI/netI    0.0408
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -2
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4421
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         3.25
_diffrn_standards_interval_time  150
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    0.0795
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_description       'small prisms'
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.61
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.29
_refine_diff_density_max         0.085
_refine_diff_density_min         -0.076
_refine_ls_goodness_of_fit_all   0.852
_refine_ls_goodness_of_fit_obs   0.976
_refine_ls_hydrogen_treatment
;
 refall excepting those of C14 Me that were placed in calculated positions
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         1368
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_obs          0.0245
_refine_ls_shift/esd_max         -0.286
_refine_ls_shift/esd_mean        0.012
_refine_ls_structure_factor_coef F^2^
_refine_ls_weighting_details
'w = 1/[\s^2^(F~o~^2^) + (0.0211P)^2^]  where  P = (F~o~^2^ + 2F~c~^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.0471
_reflns_number_observed          999
_reflns_number_total             1368
_reflns_observed_criterion       'I > 2\s(I)'
_cod_data_source_file            li1073.cif
_cod_data_source_block           2a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w = 1/[\s^2^(F~o~^2^) +
(0.0211P)^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^) + (0.0211P)^2^]
where P = (F~o~^2^ + 2F~c~^2^)/3'.

Automatic conversion script
Id: cif_fix_values 4586 2016-02-24 11:40:35Z andrius 
;
_cod_database_code               2009633