Right- and left-handed PPI helices in cyclic dodecapeptoids.
Pierri, Giovanni; Schettini, Rosaria; Summa, Francesco F.; De Riccardis, Francesco; Monaco, Guglielmo; Izzo, Irene; Tedesco, Consiglia; Chemical communications (Cambridge, England)  (2022) –; doi:10.1039/d2cc00682k

data_7129951
_publ_section_title
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 Right- and left-handed PPI helices in cyclic dodecapeptoids.
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_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_paper_doi               10.1039/d2cc00682k
_journal_year                    2022
_chemical_formula_moiety         'C60 H92 N12 O20, 0.556(H2 O), 2[C3H8O]'
_chemical_formula_sum            'C66 H109.11 N12 O22.56'
_chemical_formula_weight         1431.72
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2022-03-25
_audit_creation_method
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Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
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_audit_update_record
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2022-03-25 deposited with the CCDC.	2022-03-28 downloaded from the CCDC.
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_cell_angle_alpha                105.2750(10)
_cell_angle_beta                 108.615(2)
_cell_angle_gamma                99.629(2)
_cell_formula_units_Z            1
_cell_length_a                   11.5603(5)
_cell_length_b                   13.0290(5)
_cell_length_c                   14.4868(6)
_cell_measurement_reflns_used    9903
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      72.92
_cell_measurement_theta_min      3.66
_cell_volume                     1917.90(14)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.920
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0518
_diffrn_reflns_av_unetI/netI     0.0519
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.920
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            23947
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.920
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.310
_diffrn_reflns_theta_min         3.658
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.779
_exptl_absorpt_correction_T_max  0.7538
_exptl_absorpt_correction_T_min  0.4442
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1448 before and 0.0653 after correction.
The Ratio of minimum to maximum transmission is 0.5893.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.240
_exptl_crystal_description       prism
_exptl_crystal_F_000             770
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: isopropyl alcohol'
_exptl_crystal_size_max          0.59
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.249
_refine_diff_density_min         -0.248
_refine_diff_density_rms         0.034
_refine_ls_extinction_coef       0.0047(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   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     470
_refine_ls_number_reflns         7207
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0680
_refine_ls_R_factor_gt           0.0521
_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^)+(0.0804P)^2^+0.2685P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1440
_refine_ls_wR_factor_ref         0.1561
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5414
_reflns_number_total             7207
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc00682k2.cif
_cod_data_source_block           res55_a4__28_squeeze_h_water
_cod_database_code               7129951
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.947
_shelx_estimated_absorpt_t_min   0.656
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 O1W-H1WA = O1W-H1WB
 0.85 with sigma of 0.02
 H1WA-H1WB
 1.34 with sigma of 0.04
3. Others
 Sof(H19C)=Sof(H19D)=Sof(C20B)=Sof(H20C)=Sof(H20D)=1-FVAR(1)
 Sof(H19A)=Sof(H19B)=Sof(C20A)=Sof(H20A)=Sof(H20B)=FVAR(1)
 Sof(O7B)=Sof(H16C)=Sof(H16D)=Sof(C17B)=Sof(H17C)=Sof(H17D)=Sof(C18B)=
 Sof(H18D)=Sof(H18E)=Sof(H18F)=1-FVAR(2)
 Sof(O7A)=Sof(H16A)=Sof(H16B)=Sof(C17A)=Sof(H17A)=Sof(H17B)=Sof(C18A)=
 Sof(H18A)=Sof(H18B)=Sof(H18C)=FVAR(2)
 Sof(O1W)=Sof(H1WA)=Sof(H1WB)=FVAR(3)
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3A,H3B), C5(H5A,H5B), C7(H7A,H7B), C9(H9A,H9B), C11(H11A,
 H11B), C13(H13A,H13B), C16(H16A,H16B), C16(H16C,H16D), C17A(H17A,H17B),
 C17B(H17C,H17D), C19A(H19A,H19B), C19A(H19C,H19D), C20A(H20A,H20B), C20B(H20C,
 H20D), C22(H22A,H22B), C25(H25A,H25B), C26(H26A,H26B), C28(H28A,H28B),
 C29(H29A,H29B)
4.b Idealised Me refined as rotating group:
 C18A(H18A,H18B,H18C), C18B(H18D,H18E,H18F), C21(H21A,H21B,H21C), C27(H27A,
 H27B,H27C), C30(H30A,H30B,H30C)
4.c :
 C15(H15), C24(H24)
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_smtbx_masks_special_details
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A solvent mask was calculated and 65 electrons were 
found in a volume of 321\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
2[C3H8O] per Formula Unit 
which account for 68 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              5362
_shelx_fab_checksum              79138
_olex2_submission_special_instructions 'No special instructions were received'