Synthesis of new fluorinated proline analogues from polyfluoroalkyl β-ketoacetals and ethyl isocyanoacetate.
Tolmachova, Nataliya A.; Kondratov, Ivan S.; Dolovanyuk, Violetta G.; Pridma, Stanislav O.; Chernykh, Anton V.; Daniliuc, Constantin G.; Haufe, Günter; Chemical communications (Cambridge, England) 54 (2018) 9683–9686; doi:10.1039/c8cc05912h

data_7122082
_publ_section_title
;
 Synthesis of new fluorinated proline analogues from polyfluoroalkyl
 \b-ketoacetals and ethyl isocyanoacetate.
;
_journal_issue                   69
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              9683
_journal_page_last               9686
_journal_paper_doi               10.1039/c8cc05912h
_journal_volume                  54
_journal_year                    2018
_chemical_formula_structural     'Y[2-(mesN=CH)6-ButC6H3O]3 0.5 n-hexane'
_chemical_formula_sum            'C63 H79 N3 O3 Y'
_chemical_formula_weight         1015.20
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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_block_doi                 10.5517/cc6742m
_audit_creation_method           SHELXL
_audit_update_record
;
2002-05-13 deposited with the CCDC.
2018-08-02 downloaded from the CCDC.
;
_cell_angle_alpha                87.84(3)
_cell_angle_beta                 77.96(3)
_cell_angle_gamma                76.14(3)
_cell_formula_units_Z            2
_cell_length_a                   10.266(2)
_cell_length_b                   12.111(2)
_cell_length_c                   23.973(5)
_cell_measurement_temperature    140(1)
_cell_volume                     2829.9(11)
_computing_cell_refinement       'DENZO (Otwinowski and Minor, 1985)'
_computing_data_collection       'MSC R-Axis-II control software'
_computing_data_reduction        'DENZO, Scalepack (Otwinowski and Minor, 1985)'
_computing_molecular_graphics    'XP (SHELXTL, v.5, 1994)'
_computing_publication_material  'XL (SHELXTL, v.5, 1994)'
_computing_structure_refinement  'XL (SHELXTL, v.5, 1994)'
_computing_structure_solution    'XS (SHELXTL, v.5, 1994)'
_diffrn_ambient_temperature      140(1)
_diffrn_measurement_device       'Rigaku R-Axis-IIc'
_diffrn_measurement_method       'image-plate oscillation photos'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0816
_diffrn_reflns_av_sigmaI/netI    0.1001
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            14412
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.09
_exptl_absorpt_coefficient_mu    1.076
_exptl_absorpt_correction_type   'none applied'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.191
_exptl_crystal_description       block
_exptl_crystal_F_000             1082
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.423
_refine_diff_density_min         -0.898
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.975
_refine_ls_goodness_of_fit_obs   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     640
_refine_ls_number_reflns         9052
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.975
_refine_ls_restrained_S_obs      1.061
_refine_ls_R_factor_all          0.0810
_refine_ls_R_factor_obs          0.0573
_refine_ls_shift/esd_max         0.010
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0897P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1539
_refine_ls_wR_factor_obs         0.1415
_reflns_number_observed          6595
_reflns_number_total             9052
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            c8cc05912h2.cif
_cod_data_source_block           a21
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0897P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. A new data item '_refine_ls_weighting_details' was
created with the value set to
'w=1/[\s^2^(Fo^2^)+(0.0897P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7122082--7122083.cif.
;
_cod_original_cell_volume        2829.9(10)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7122082