Phosphine-catalyzed annulation of ethyl (arylimino)acetates: synthesis of highly functionalized oxoimidazolidines.
Ma, Guang-Ning; Wang, Fei-Jun; Gao, Jun; Shi, Min; Chemical communications (Cambridge, England)  (2008) 4998–5000; doi:10.1039/b811167g

data_7103432
_publ_section_title
;
 Phosphine-catalyzed annulation of ethyl (arylimino)acetates: synthesis
 of highly functionalized oxoimidazolidines.
;
_journal_issue                   40
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              4998
_journal_page_last               5000
_journal_paper_doi               10.1039/b811167g
_journal_year                    2008
_chemical_formula_sum            'C24.25 H20.5 Br3 Cl0.5 N3 O3'
_chemical_formula_weight         659.39
_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-97
_cell_angle_alpha                90.901(3)
_cell_angle_beta                 98.503(2)
_cell_angle_gamma                90.942(2)
_cell_formula_units_Z            8
_cell_length_a                   13.9165(14)
_cell_length_b                   19.129(2)
_cell_length_c                   19.595(2)
_cell_measurement_reflns_used    1949
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.637
_cell_measurement_theta_min      4.377
_cell_volume                     5157.5(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0779
_diffrn_reflns_av_sigmaI/netI    0.3395
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            27508
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    4.776
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78936
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.698
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2596
_exptl_crystal_size_max          0.291
_exptl_crystal_size_mid          0.126
_exptl_crystal_size_min          0.044
_refine_diff_density_max         0.825
_refine_diff_density_min         -0.564
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.862
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1205
_refine_ls_number_reflns         18902
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.862
_refine_ls_R_factor_all          0.2301
_refine_ls_R_factor_gt           0.0521
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0495P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1005
_refine_ls_wR_factor_ref         0.1505
_reflns_number_gt                5177
_reflns_number_total             17002
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b811167g.txt
_cod_data_source_block           cd26131
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C24.25 H20.50 Br3 Cl0.50 N3 O3'
_cod_database_code               7103432