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_7108926
_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_formula_moiety         'C19 H10 Br2 F6 O2'
_chemical_formula_sum            'C19 H10 Br2 F6 O2'
_chemical_formula_weight         544.09
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                115.201(10)
_cell_angle_beta                 90.957(10)
_cell_angle_gamma                98.891(9)
_cell_formula_units_Z            2
_cell_length_a                   5.512(2)
_cell_length_b                   13.104(7)
_cell_length_c                   14.668(8)
_cell_measurement_reflns_used    2851
_cell_measurement_temperature    93
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      1.54
_cell_volume                     943.1(8)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 rc13'
_computing_data_collection
'CrystalClear-SM Expert 2.0 rc13 (Rigaku, 2009)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 rc13'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'DIRDIF99-PATTY (Gould, et al., 1999)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 14.629
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Rigaku Mercury70'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0541
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6092
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.36
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.381
_exptl_absorpt_correction_T_max  0.916
_exptl_absorpt_correction_T_min  0.488
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.916
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             528.00
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.670
_refine_diff_density_min         -0.650
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.971
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     262
_refine_ls_number_reflns         3342
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0539
_refine_ls_shift/su_max          0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0423P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1210
_reflns_number_gt                2201
_reflns_number_total             3342
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c3cc39066g.txt
_cod_data_source_block           4b
_cod_original_cell_volume        943.0(8)
_cod_database_code               7108926