A Synthetic Strategy for the Preparation of Cyclic Peptide Mimetics Based on SET-Promoted Photocyclization Processes
Ung Chan Yoon; Ying Xue Jin; Sun Wha Oh; Chan Hyo Park; Jong Hoon Park; Charles F. Campana; Xiaolu Cai; Eileen N. Duesler; Patrick S. Mariano; Journal of the American Chemical Society 125 (2003) 10664–10671; doi:10.1021/ja030297b

data_4114104
_publ_section_title
;
 A Synthetic Strategy for the Preparation of Cyclic Peptide Mimetics Based
 on SET-Promoted Photocyclization Processes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10664
_journal_page_last               10671
_journal_paper_doi               10.1021/ja030297b
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C36 H36 N4 O6'
_chemical_formula_weight         620.69
_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                111.772(6)
_cell_angle_beta                 97.092(13)
_cell_angle_gamma                93.043(14)
_cell_formula_units_Z            2
_cell_length_a                   6.6763(14)
_cell_length_b                   15.329(3)
_cell_length_c                   16.572(4)
_cell_measurement_reflns_used    35
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.48
_cell_measurement_theta_min      2.69
_cell_volume                     1553.9(6)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_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, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.864
_diffrn_measured_fraction_theta_max 0.864
_diffrn_measurement_device_type  'Siemens-Bruker P4'
_diffrn_measurement_method       '\w 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  0.0303
_diffrn_reflns_av_sigmaI/netI    0.0390
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9986
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         23.97
_diffrn_reflns_theta_min         1.55
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.091
_exptl_absorpt_correction_T_max  0.9868
_exptl_absorpt_correction_T_min  0.9795
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
 data processed with psi scan corrections and
 also face-indexed gaussian correction. results
 for both about the same with slightly better
 R's for gaussian which was used in final
 refinements.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.327
_exptl_crystal_description       prism
_exptl_crystal_F_000             656
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.249
_refine_diff_density_min         -0.233
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment
;
 all hydrogen positions observed in difference map after going anisotropic
 on all non-H atoms. riding model used to position H atoms on C's. H atoms
 on O's were initially positioned as seen in difference maps and these
 positions were allowed to vary; all H's have fixed isotropic U's set to
 1.25U[equiv] of parent atom
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         4713
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0387
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0626P)^2^+0.0759P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1025
_refine_ls_wR_factor_ref         0.1154
_reflns_number_gt                3509
_reflns_number_total             4713
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja030297b_2.cif
_cod_data_source_block           Compd-41a/pm022
_cod_database_code               4114104