Fluorous Mixture Synthesis of Fused-Tricyclic Hydantoins. Use of a Redundant Tagging Strategy on Fluorinated Substrates
Manku, Sukhdev; Curran, Dennis P.; The Journal of Organic Chemistry 70 (2005) 4470–4473; doi:10.1021/jo0502596

data_4028893
_publ_section_title
;
 Fluorous Mixture Synthesis of Fused-Tricyclic Hydantoins. Use of a
 Redundant Tagging Strategy on Fluorinated Substrates
;
_journal_issue                   11
_journal_name_full               'The Journal of Organic Chemistry'
_journal_page_first              4470
_journal_page_last               4473
_journal_paper_doi               10.1021/jo0502596
_journal_volume                  70
_journal_year                    2005
_chemical_formula_sum            'C132 H120 N8 O12'
_chemical_formula_weight         2010.36
_chemical_name_systematic
;
  ?
;
_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                101.088(2)
_cell_angle_beta                 90.658(2)
_cell_angle_gamma                104.314(2)
_cell_formula_units_Z            1
_cell_length_a                   10.6129(8)
_cell_length_b                   12.1178(9)
_cell_length_c                   22.3579(17)
_cell_measurement_temperature    293(2)
_cell_volume                     2728.8(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Smart Apex CCD'
_diffrn_measurement_method       '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  0.1340
_diffrn_reflns_av_sigmaI/netI    0.2119
_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       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            22181
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    0.078
_exptl_absorpt_correction_T_max  0.9938
_exptl_absorpt_correction_T_min  0.9799
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker Saint Sadabs'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.223
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.288
_refine_diff_density_min         -0.213
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     685
_refine_ls_number_reflns         9622
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.2720
_refine_ls_R_factor_gt           0.1239
_refine_ls_shift/su_max          0.024
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s2^(Fo2^)+(0.0879P)2^+0.0000P] where P=(Fo2^+2Fc2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2188
_refine_ls_wR_factor_ref         0.2678
_reflns_number_gt                3614
_reflns_number_total             9622
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo0502596sup1.cif
_cod_data_source_block           dm810
_cod_database_code               4028893
_cod_duplicate_entry 4020271