Reactions of polyfluorinated cyclohexadienones with diazoalkanes. Part 1. Formation of cyclopropanes from polyfluorinated cyclohexa-2,4-dienones with diazomethane and phenyldiazomethane
Kovtonyuk, Vladimir N.; Kobrina, Ljubov S.; Gatilov, Yurij V.; Bagryanskaya, Irina Yu.; Fröhlich, Roland; Haufe, Günter; Journal of the Chemical Society, Perkin Transactions 1  (2000) 1929–; doi:10.1039/b001618g

data_7213290
_publ_section_title
;
 Reactions of polyfluorinated cyclohexadienones with diazoalkanes. Part 1.
 Formation of cyclopropanes from polyfluorinated cyclohexa-2,4-dienones
 with diazomethane and phenyldiazomethane
;
_journal_issue                   12
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 1'
_journal_page_first              1929
_journal_paper_doi               10.1039/b001618g
_journal_year                    2000
_chemical_formula_sum            'C13 H6 Cl F5 O'
_chemical_formula_weight         308.63
_chemical_name_systematic
;
 7-endo-phenyl-1,2,3,4,6-pentafluoro-4-chloro-
 -bicyclo[4.1.0]hept-2-ene-5-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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.68(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.914(6)
_cell_length_b                   10.407(7)
_cell_length_c                   13.607(9)
_cell_measurement_reflns_used    9
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.4
_cell_measurement_theta_min      23.9
_cell_volume                     1256.1(15)
_computing_cell_refinement       'Syntex P21'
_computing_data_collection       'Syntex P21'
_computing_data_reduction        XTAPE
_computing_molecular_graphics    XP
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.815
_diffrn_measured_fraction_theta_max 0.816
_diffrn_measurement_device_type  'Syntex P21'
_diffrn_measurement_method       theta/2theta
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_sigmaI/netI    0.0609
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       2
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            2312
_diffrn_reflns_theta_full        70.05
_diffrn_reflns_theta_max         70.05
_diffrn_reflns_theta_min         4.99
_diffrn_standards_decay_%        23.65
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.250
_exptl_absorpt_correction_T_max  0.958
_exptl_absorpt_correction_T_min  0.488
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'unregular prism'
_exptl_crystal_F_000             616
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.192
_refine_diff_density_min         -0.272
_refine_diff_density_rms         0.053
_refine_ls_extinction_coef       0.0036(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     206
_refine_ls_number_reflns         2056
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.1177
_refine_ls_R_factor_gt           0.0608
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0756P)^2^+0.3502P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1399
_refine_ls_wR_factor_ref         0.1733
_reflns_number_gt                1152
_reflns_number_total             2056
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b001618gsup1.cif
_cod_data_source_block           Kovtonyuk_izomer_2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0756P)^2^+0.3502P] where P=(Fo^2^+2Fc^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^(Fo^2^)+(0.0756P)^2^+0.3502P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7213290