Fluorinated 5- and 7-membered carbacycle motifs by reaction of difluorocarbene with acetylene ethers
Poh Wai Chia; Davide Bello; Alexandra M. Z. Slawin; David O'Hagan; Chemical communications (Cambridge, England) 49 (2013) 2189–2191; doi:10.1039/c3cc39066g

data_7108925
_publ_section_title
;
 Fluorinated 5- and 7-membered carbacycle motifs by reaction of
 difluorocarbene with acetylene ethers
;
_journal_issue                   22
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              2189
_journal_page_last               2191
_journal_paper_doi               10.1039/c3cc39066g
_journal_volume                  49
_journal_year                    2013
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C11 H12 F6 O2'
_chemical_formula_sum            'C11 H12 F6 O2'
_chemical_formula_weight         290.20
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      33
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   9.4508(11)
_cell_length_b                   26.424(3)
_cell_length_c                   5.0500(6)
_cell_measurement_reflns_used    11417
_cell_measurement_temperature    173
_cell_measurement_theta_max      68.09
_cell_measurement_theta_min      3.33
_cell_volume                     1261.1(3)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r2'
_computing_data_collection       'CrystalClear-SM Expert 2.0 r2 (Rigaku, 2009)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r2'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla, et al., 2005)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 29.257
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Rigaku Saturn70'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0881
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            14894
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         68.13
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.459
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             592.00
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.230
_refine_diff_density_min         -0.230
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881. 938 Friedel Pairs'
_refine_ls_abs_structure_Flack   -0.0(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     172
_refine_ls_number_reflns         2197
_refine_ls_number_restraints     1
_refine_ls_R_factor_gt           0.0452
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0540P)^2^+0.6180P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1206
_reflns_number_gt                2122
_reflns_number_total             2197
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c3cc39066g.txt
_cod_data_source_block           4a
_cod_database_code               7108925