Synthesis of Conformationally Constrained Peptidomimetics using Multicomponent Reactions
Scheffelaar, Rachel; Nijenhuis, Roel A. Klein; Paravidino, Monica; Lutz, Martin; Spek, Anthony L.; Ehlers, Andreas W.; de Kanter, Frans J. J.; Groen, Marinus B.; Orru, Romano V. A.; Ruijter, Eelco; The Journal of Organic Chemistry 74 (2009) 660–668; doi:10.1021/jo802052j

data_4028927
_publ_section_title
;
 Synthesis of Conformationally Constrained Peptidomimetics using
 Multicomponent Reactions
;
_journal_issue                   2
_journal_name_full               'The Journal of Organic Chemistry'
_journal_page_first              660
_journal_page_last               668
_journal_paper_doi               10.1021/jo802052j
_journal_volume                  74
_journal_year                    2009
_chemical_formula_moiety         'C33 H34 N4 O6'
_chemical_formula_sum            'C33 H34 N4 O6'
_chemical_formula_weight         582.64
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.7278(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.3373(1)
_cell_length_b                   19.3871(3)
_cell_length_c                   16.8614(3)
_cell_measurement_reflns_used    49709
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.02
_cell_volume                     2965.11(8)
_computing_cell_refinement       HKL2000
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        'HKL2000, denzox, Sadabs'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-97 (Altomare et al., 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0553
_diffrn_reflns_av_sigmaI/netI    0.0395
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            50586
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.63
_exptl_absorpt_coefficient_mu    0.091
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.83
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.305
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.302
_refine_diff_density_min         -0.217
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     410
_refine_ls_number_reflns         6794
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0740
_refine_ls_R_factor_gt           0.0455
_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^)+(0.0416P)^2^+1.0844P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0959
_refine_ls_wR_factor_ref         0.1068
_reflns_number_gt                4887
_reflns_number_total             6794
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            jo802052jsup1.cif
_cod_data_source_block           s3974a
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4028927