Stabilization of beta-peptide helices by direct attachment of trifluoromethyl groups to peptide backbones
Joonil Cho; Kyohei Sawaki; Shinya Hanashima; Yoshiki Yamaguchi; Motoo Shiro; Kazuhiko Saigo; Yasuhiro Ishida; Chem.Commun. 50 (2014) 9855–; doi:10.1039/C4cc02136C

data_7115493
_publ_section_title
;
 Stabilization of beta-peptide helices by direct attachment of
 trifluoromethyl groups to peptide backbones
;
_journal_name_full               Chem.Commun.
_journal_page_first              9855
_journal_paper_doi               10.1039/C4cc02136C
_journal_volume                  50
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C48 H68 F6 N6 O9, C H Cl3'
_chemical_formula_sum            'C49 H69 Cl3 F6 N6 O9'
_chemical_formula_weight         1106.47
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            8
_cell_length_a                   19.7038(4)
_cell_length_b                   23.9063(4)
_cell_length_c                   24.8954(7)
_cell_measurement_reflns_used    89944
_cell_measurement_temperature    93.1
_cell_measurement_theta_max      68.2
_cell_measurement_theta_min      3.5
_cell_volume                     11726.9(5)
_computing_cell_refinement       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction        'CrystalStructure (Rigaku & RAC 2007)'
_computing_molecular_graphics    'ORTEP (Johnson, 1976)'
_computing_publication_material  'CrystalStructure (Rigaku & RAC 2007)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR2004 (Burla, 2005)'
_diffrn_ambient_temperature      93.1
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.048
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            128107
_diffrn_reflns_theta_full        68.25
_diffrn_reflns_theta_max         68.25
_exptl_absorpt_coefficient_mu    2.043
_exptl_absorpt_correction_T_max  0.849
_exptl_absorpt_correction_T_min  0.608
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.253
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4656.00
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_platon_squeeze_details
;
;
_refine_diff_density_max         2.25
_refine_diff_density_min         -1.07
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  9786 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.13(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.197
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     1292
_refine_ls_number_reflns         21305
_refine_ls_R_factor_gt           0.1065
_refine_ls_shift/su_max          0.0010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.3023
_reflns_number_gt                15988
_reflns_number_total             21305
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c4cc02136c2.cif
_cod_data_source_block           '_pep-FF'
_cod_original_cell_volume        11726.9(4)
_cod_original_formula_sum        'C49 H69 Cl3 F6 N6 O9 '
_cod_database_code               7115493