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_7111185
_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           2
_symmetry_cell_setting           triclinic
_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
_audit_creation_method           SHELXL
_cell_angle_alpha                94.581(15)
_cell_angle_beta                 103.053(15)
_cell_angle_gamma                88.349(8)
_cell_formula_units_Z            2
_cell_length_a                   10.063(5)
_cell_length_b                   11.594(5)
_cell_length_c                   7.484(3)
_cell_measurement_reflns_used    1914
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.18
_cell_measurement_theta_min      1.76
_cell_volume                     847.8(7)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan (MSC, 1995)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SIR92 (Altomare, et. al. 1993)'
_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  0.0445
_diffrn_reflns_av_sigmaI/netI    0.0575
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            4660
_diffrn_reflns_theta_max         25.18
_diffrn_reflns_theta_min         1.76
_exptl_absorpt_coefficient_mu    0.104
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.251
_exptl_crystal_description       block
_exptl_crystal_F_000             340
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.165
_refine_diff_density_min         -0.205
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.851
_refine_ls_goodness_of_fit_obs   0.890
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     204
_refine_ls_number_reflns         2674
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.947
_refine_ls_restrained_S_obs      0.890
_refine_ls_R_factor_all          0.0812
_refine_ls_R_factor_obs          0.0581
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1031P)^2^+0.2498P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1904
_refine_ls_wR_factor_obs         0.1498
_reflns_number_observed          1914
_reflns_number_total             2681
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b109651fsup1.cif
_cod_data_source_block           act1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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^)+(0.1031P)^2^+0.2498P] 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^)+(0.1031P)^2^+0.2498P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        847.7(7)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7111185