Induction of chirality: experimental evidence of atropisomerism in azapeptides
Philipp A. Ottersbach; Gregor Schnakenburg; Michael Gutschow; Chem.Commun. 48 (2012) 5772–; doi:10.1039/c2cc31161e

data_7107769
_publ_section_title
;
 Induction of chirality: experimental evidence of atropisomerism in
 azapeptides
;
_journal_name_full               Chem.Commun.
_journal_page_first              5772
_journal_paper_doi               10.1039/c2cc31161e
_journal_volume                  48
_journal_year                    2012
_chemical_formula_moiety         'C12 H16 N4 O4'
_chemical_formula_sum            'C12 H16 N4 O4'
_chemical_formula_weight         280.29
_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                99.755(7)
_cell_angle_beta                 94.085(7)
_cell_angle_gamma                90.661(8)
_cell_formula_units_Z            2
_cell_length_a                   4.8613(5)
_cell_length_b                   11.6939(16)
_cell_length_c                   11.7674(16)
_cell_measurement_reflns_used    905
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.33
_cell_measurement_theta_min      2.70
_cell_volume                     657.41(14)
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.33333
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker X8-KappaApexII'
_diffrn_measurement_method       'fine slicing \f and \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  0.0465
_diffrn_reflns_av_sigmaI/netI    0.0804
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4690
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         25.24
_diffrn_reflns_theta_min         3.52
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.108
_exptl_absorpt_correction_T_max  0.9978
_exptl_absorpt_correction_T_min  0.9378
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS 2008/1'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.416
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             296
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.309
_refine_diff_density_min         -0.325
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         2358
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0990
_refine_ls_R_factor_gt           0.0573
_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^)+(0.0799P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1342
_refine_ls_wR_factor_ref         0.1538
_reflns_number_gt                1551
_reflns_number_total             2358
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc31161e.txt
_cod_data_source_block           Greg1588f
_cod_database_code               7107769