Crystal structure analysis of helix–turn–helix type motifs in α,γ-hybrid peptides
Nalawade, Sachin A.; Kumar, Mothukuri Ganesh; Puneeth Kumar, DRGKoppalu R.; Singh, Manjeet; Dey, Sanjit; Gopi, Hosahudya N.; CrystEngComm 26 (2024) 913–917; doi:10.1039/D3CE01236K

data_7248266
_publ_section_title
;
 Crystal structure analysis of helix--turn--helix type motifs in
 \a,\g-hybrid peptides
;
_journal_issue                   7
_journal_name_full               CrystEngComm
_journal_page_first              913
_journal_page_last               917
_journal_paper_doi               10.1039/D3CE01236K
_journal_volume                  26
_journal_year                    2024
_chemical_absolute_configuration (7R,15R,20S,23S,28S,31R,39R)
_chemical_formula_moiety         'C64 H116 N12 O12, C H4 O'
_chemical_formula_sum            'C65 H120 N12 O13'
_chemical_formula_weight         1277.74
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2024-01-10 deposited with the CCDC.	2024-01-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.947(16)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.637(8)
_cell_length_b                   19.378(9)
_cell_length_c                   16.197(7)
_cell_measurement_reflns_used    21737
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.325
_cell_measurement_theta_min      2.472
_cell_volume                     4439(4)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  microfocus
_diffrn_measurement_method       APEXIII
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_av_unetI/netI     0.0725
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            43572
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.325
_diffrn_reflns_theta_min         2.472
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.067
_exptl_absorpt_correction_T_max  0.993
_exptl_absorpt_correction_T_min  0.990
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0891 before and 0.0494 after correction. The Ratio of minimum to maximum transmission is 0.9338. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.956
_exptl_crystal_description       plate
_exptl_crystal_F_000             1396
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.442
_refine_diff_density_min         -0.275
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.3(8)
_refine_ls_extinction_coef       0.0128(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     837
_refine_ls_number_reflns         21737
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0876
_refine_ls_R_factor_gt           0.0531
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0634P)^2^+0.0938P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1158
_refine_ls_wR_factor_ref         0.1277
_reflns_Friedel_coverage         0.916
_reflns_Friedel_fraction_full    0.975
_reflns_Friedel_fraction_max     0.966
_reflns_number_gt                15105
_reflns_number_total             21737
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce01236k2.cif
_cod_data_source_block           P2
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7248266
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.990
_shelx_estimated_absorpt_t_max   0.993
_exptl_absorpt_special_details   multi-scan
_shelx_res_checksum              33574
_shelx_fab_checksum              87859