Product of a Paterno‒Büchi reaction of pentafluorobenzaldehyde and 1-acetoxycyclododecene
Brock, Carolyn Pratt; Watt, David S.; Hiroyuki Morita; Acta Crystallographica Section C 50 (1994) 1805–1807; doi:10.1107/S0108270194003525

data_2010162
_publ_contact_author
;
                                 Prof. Carolyn P. Brock
                                 Department of Chemistry
                                 University of Kentucky
                                 Lexington, KY  40506-0055
                                 USA
;
_publ_section_title
;
 Product of a Paterno--B\"uchi reaction of pentafluorobenzaldehyde and
 1-acetoxycyclododecene
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1805
_journal_page_last               1807
_journal_paper_doi               10.1107/S0108270194003525
_journal_volume                  50
_journal_year                    1994
_chemical_formula_moiety         'C21 H25 F5 O3'
_chemical_formula_sum            'C21 H25 F5 O3'
_chemical_formula_weight         420.42
_chemical_melting_point          349.6(5)
_chemical_name_systematic
;
1-acetoxy-14-pentafluorophenyl-13-oxa-bicyclo[10.2.0]tetradecane
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_method           'created by SHELXL-93 and C P Brock'
_cell_angle_alpha                90.
_cell_angle_beta                 94.338(5)
_cell_angle_gamma                90.
_cell_formula_units_Z            4
_cell_length_a                   8.6548(4)
_cell_length_b                   15.8640(7)
_cell_length_c                   14.9305(12)
_cell_measurement_reflns_used    22
_cell_measurement_temperature    296.0(10)
_cell_measurement_theta_max      13.1
_cell_measurement_theta_min      12.2
_cell_volume                     2044.1(2)
_computing_cell_refinement       CAD4-VAX
_computing_data_collection       'CAD4-VAX (Enraf-Nonius, 1988)'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXTL/PC (Sheldrick, 1990)'
_diffrn_measurement_device       'ENRAF-Nonius CAD4-VAX diffractometer'
_diffrn_measurement_method       '\w/2\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_sigmaI/netI    0.0691
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            4682
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         2.0
_diffrn_standards_decay_%        <0.1
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.114
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_description
;
Rhomboidal tablets
;
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.127
_refine_diff_density_min         -0.183
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.827
_refine_ls_goodness_of_fit_obs   1.130
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         4681
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.829
_refine_ls_restrained_S_obs      1.130
_refine_ls_R_factor_all          0.2083
_refine_ls_R_factor_obs          0.0432
_refine_ls_shift/esd_max         0.048
_refine_ls_shift/esd_mean        0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;calc w = 1/[\s^2^(F~o~^2^) + (0.1000P)^2^]
where P = (F~o~^2^ + 2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.1627
_refine_ls_wR_factor_obs         0.1321
_reflns_number_observed          1823
_reflns_number_total             4682
_reflns_observed_criterion       >2\s(I)
_cod_data_source_file            cr1120.cif
_cod_data_source_block           MORITA02
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '76-77_C' was changed to '349.6(5)' -
it was converted from degrees Celsius(C) to Kelvins(K), the average
value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_chemical_melting_point' value '76-77_C' was changed to '349.6(5)' -
it was converted from degrees Celsius(C) to Kelvins(K), the average
value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2010162