Rapid assembly of highly-functionalised difluorinated cyclooctenones via ring-closing metathesis
Kariuki, Benson M.; Owton, W. Martin; Percy, Jonathan M.; Pintat, Stéphane; Smith, Clive A.; Spencer, Neil S.; Thomas, Andrew C.; Watson, Martin; Chemical Communications  (2002) 228–; doi:10.1039/b109651f

data_7111186
_publ_section_title
;
 Rapid assembly of highly-functionalised difluorinated cyclooctenones via
 ring-closing metathesis
;
_journal_issue                   3
_journal_name_full               'Chemical Communications'
_journal_page_first              228
_journal_paper_doi               10.1039/b109651f
_journal_year                    2002
_chemical_formula_moiety         'C15 H23 F2 N O4'
_chemical_formula_sum            'C15 H23 F2 N O4'
_chemical_formula_weight         319.34
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 100.353(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.9117(12)
_cell_length_b                   7.5944(6)
_cell_length_c                   14.8779(11)
_cell_measurement_reflns_used    2052
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.43
_cell_measurement_theta_min      1.39
_cell_volume                     1657.4(2)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measurement_device       'Rigaku R-axis II'
_diffrn_measurement_method       'Image plate scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0852
_diffrn_reflns_av_sigmaI/netI    0.0771
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7335
_diffrn_reflns_theta_max         25.43
_diffrn_reflns_theta_min         1.39
_exptl_absorpt_coefficient_mu    0.106
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_description       'Hexagonal blocks'
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.367
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.047
_refine_ls_extinction_coef       0.0486(108)
_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_all   1.081
_refine_ls_goodness_of_fit_obs   1.139
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         2881
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.113
_refine_ls_restrained_S_obs      1.139
_refine_ls_R_factor_all          0.0984
_refine_ls_R_factor_obs          0.0658
_refine_ls_shift/esd_max         0.053
_refine_ls_shift/esd_mean        0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0996P)^2^+0.1072P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2034
_refine_ls_wR_factor_obs         0.1742
_reflns_number_observed          2052
_reflns_number_total             2882
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b109651fsup1.cif
_cod_data_source_block           act1b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0996P)^2^+0.1072P] 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^)+(0.0996P)^2^+0.1072P] 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/a
_cod_database_code               7111186