Transfer of chirality in N-triphenylacetylamino acids and chiral derivatives of N-triphenylacetyl Gly–Gly dipeptide and control of their assembly with steric constraints
Bendzińska-Berus, Wioletta; Jelecki, Maciej; Kwit, Marcin; Rychlewska, Urszula; CrystEngComm 21 (2019) 3420–; doi:10.1039/C9CE00429G

data_7232694
_publ_section_title
;
 Transfer of chirality in N-triphenylacetylamino acids and chiral
 derivatives of N-triphenylacetyl Gly--Gly dipeptide and control of their
 assembly with steric constraints
;
_journal_issue                   22
_journal_name_full               CrystEngComm
_journal_page_first              3420
_journal_paper_doi               10.1039/C9CE00429G
_journal_volume                  21
_journal_year                    2019
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C28 H32 N2 O2'
_chemical_formula_sum            'C28 H32 N2 O2'
_chemical_formula_weight         428.55
_chemical_name_systematic
N-(triphenylacetyl)glycylamino(1-tert-butyl)ethane
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_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-2014/7
_audit_update_record
;
2019-03-05 deposited with the CCDC.    2019-04-23 downloaded from the CCDC.
;
_cell_angle_alpha                104.385(2)
_cell_angle_beta                 99.112(2)
_cell_angle_gamma                92.482(2)
_cell_formula_units_Z            2
_cell_length_a                   9.8268(2)
_cell_length_b                   10.7524(2)
_cell_length_c                   12.3034(3)
_cell_measurement_reflns_used    21616
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      76.3190
_cell_measurement_theta_min      3.7480
_cell_volume                     1238.70(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies (2014)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies (2014)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies (2014)
;
_computing_molecular_graphics    'Mercury (Bruno, et al. 2002)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      130(2)
_diffrn_detector_area_resol_mean 10.5357
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'SuperNova, Atlas detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0177
_diffrn_reflns_av_unetI/netI     0.0172
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            24231
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.930
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         76.551
_diffrn_reflns_theta_min         3.767
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.564
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89162
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm, 2014.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.149
_exptl_crystal_description       plate
_exptl_crystal_F_000             460
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.235
_refine_diff_density_min         -0.205
_refine_diff_density_rms         0.030
_refine_ls_abs_structure_details
;
 Flack x determined using 4452 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.00(7)
_refine_ls_extinction_coef       0.0085(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     586
_refine_ls_number_reflns         9684
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0319
_refine_ls_R_factor_gt           0.0316
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0415P)^2^+0.2575P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0852
_refine_ls_wR_factor_ref         0.0855
_reflns_Friedel_coverage         0.900
_reflns_Friedel_fraction_full    0.936
_reflns_Friedel_fraction_max     0.880
_reflns_number_gt                9586
_reflns_number_total             9684
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce00429g2.cif
_cod_data_source_block           15
_cod_depositor_comments
'Adding full bibliography for 7232683--7232694.cif.'
_cod_database_code               7232694
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.946
_shelx_estimated_absorpt_t_max   0.972
_shelx_res_checksum              35994