Solid-Phase Synthesis of Multiple Classes of Peptidomimetics from Versatile Resin-Bound Aldehyde Intermediates
William L. Scott; Jacek G. Martynow; John C. Huffman; Martin J. O'Donnell; Journal of the American Chemical Society 129 (2007) 7077–7088; doi:10.1021/ja069188y

data_4109470
_publ_section_title
;
 Solid-Phase Synthesis of Multiple Classes of Peptidomimetics from
 Versatile Resin-Bound Aldehyde Intermediates
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7077
_journal_page_last               7088
_journal_paper_doi               10.1021/ja069188y
_journal_volume                  129
_journal_year                    2007
_chemical_formula_moiety         'C31 H30 N2 O6, C2.84'
_chemical_formula_sum            'C31 H30 N2 O6'
_chemical_formula_weight         526.57
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.300(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.9652(9)
_cell_length_b                   8.1963(6)
_cell_length_c                   26.6271(18)
_cell_measurement_reflns_used    1958
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      21.32
_cell_measurement_theta_min      2.60
_cell_volume                     2824.9(3)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        'SAINT (Bruker, 1999), XTEL (local package)'
_computing_molecular_graphics    'Reciprocal Net (http://recipnet.org)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      130(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 44.52
_diffrn_detector_type            'Bruker SMART 6000'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
'   0.30 degree frames measured for 5.16 seconds each'
_diffrn_measurement_device       'three-circle goniometer with fixed chi'
_diffrn_measurement_device_type  'Bruker Platform goniometer'
_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  0.1020
_diffrn_reflns_av_sigmaI/netI    0.1075
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            41349
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         2.60
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.238
_exptl_crystal_description       triangular
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.256
_refine_diff_density_min         -0.200
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.803
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         6489
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.803
_refine_ls_R_factor_all          0.1360
_refine_ls_R_factor_gt           0.0505
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0377P)^2^+0.3000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0978
_refine_ls_wR_factor_ref         0.1172
_reflns_number_gt                2457
_reflns_number_total             6489
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja069188ysi20061221_040214.cif
_cod_data_source_block           06904
_cod_original_sg_symbol_Hall     '-P 2yn   '
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_database_code               4109470