Design, Synthesis, and Conformational Analysis of Trispyrimidonamides as α-Helix Mimetics.
Spanier, Lukas; Ciglia, Emanuele; Hansen, Finn K.; Kuna, Krystina; Frank, Walter; Gohlke, Holger; Kurz, Thomas; The Journal of organic chemistry 79 (2014) 1582–1593; doi:10.1021/jo402353z

data_4028997
_publ_section_title
;
 Design, Synthesis, and Conformational Analysis of Trispyrimidonamides as
 \a-Helix Mimetics.
;
_journal_issue                   4
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              1582
_journal_page_last               1593
_journal_paper_doi               10.1021/jo402353z
_journal_volume                  79
_journal_year                    2014
_chemical_formula_moiety         'C34 H40 N10 O7'
_chemical_formula_sum            'C34 H40 N10 O7'
_chemical_formula_weight         700.76
_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                 93.845(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.6997(6)
_cell_length_b                   26.578(2)
_cell_length_c                   23.461(2)
_cell_measurement_reflns_used    13178
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      29.94
_cell_measurement_theta_min      1.54
_cell_volume                     3546.0(6)
_computing_cell_refinement       'IPDS Software (Stoe & Cie, 2000)'
_computing_data_collection       'IPDS Software (Stoe & Cie, 2000)'
_computing_data_reduction        'IPDS Software (Stoe & Cie, 2000)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       \f-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  0.3560
_diffrn_reflns_av_sigmaI/netI    0.2091
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            26011
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.53
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.095
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1480
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.553
_refine_diff_density_min         -0.474
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.307
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     485
_refine_ls_number_reflns         6244
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.307
_refine_ls_R_factor_all          0.2415
_refine_ls_R_factor_gt           0.1627
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+15.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3242
_refine_ls_wR_factor_ref         0.3654
_reflns_number_gt                3569
_reflns_number_total             6244
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo402353z_si_001.cif
_cod_data_source_block           no_224
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4028997