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_7129952
_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, 2[C4H8O2]'
_chemical_formula_sum            'C68 H108 N12 O24'
_chemical_formula_weight         1477.66
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2022-02-28
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-03-16 deposited with the CCDC.	2022-03-28 downloaded from the CCDC.
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_cell_angle_alpha                90
_cell_angle_beta                 100.5630(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.7433(3)
_cell_length_b                   24.2497(7)
_cell_length_c                   13.9071(4)
_cell_measurement_reflns_used    9886
_cell_measurement_temperature    296.00
_cell_measurement_theta_max      74.60
_cell_measurement_theta_min      3.71
_cell_volume                     3893.23(19)
_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      296.00
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.912
_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  0.0619
_diffrn_reflns_av_unetI/netI     0.0377
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.912
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            45155
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.912
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.598
_diffrn_reflns_theta_min         3.711
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.799
_exptl_absorpt_correction_T_max  0.7538
_exptl_absorpt_correction_T_min  0.5327
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0959 before and 0.0665 after correction.
The Ratio of minimum to maximum transmission is 0.7067.
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    1.260
_exptl_crystal_description       prism
_exptl_crystal_F_000             1584
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: ethyl acetate/toluene'
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.312
_refine_diff_density_min         -0.261
_refine_diff_density_rms         0.036
_refine_ls_extinction_coef       0.0019(3)
_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   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     430
_refine_ls_number_reflns         7289
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0810
_refine_ls_R_factor_gt           0.0557
_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^)+(0.0841P)^2^+0.7139P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1535
_refine_ls_wR_factor_ref         0.1688
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4919
_reflns_number_total             7289
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc00682k2.cif
_cod_data_source_block           res59_e5_cap3_sir_90_squeeze
_cod_database_code               7129952
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.932
_shelx_estimated_absorpt_t_min   0.756
_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 C(H,H,H,H,H,H) groups
2. Others
 Sof(H14C)=Sof(H14D)=Sof(H15D)=Sof(H15E)=Sof(H15F)=Sof(O7B)=1-FVAR(1)
 Sof(O7A)=Sof(H14A)=Sof(H14B)=Sof(H15A)=Sof(H15B)=Sof(H15C)=FVAR(1)
3.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), C14(H14A,H14B), C14(H14C,H14D), C16(H16A,H16B),
 C17(H17A,H17B), C19(H19A,H19B), C22(H22A,H22B), C25(H25A,H25B), C26(H26A,H26B),
  C28(H28A,H28B), C29(H29A,H29B)
3.b Idealised Me refined as rotating group:
 C15(H15D,H15E,H15F), C15(H15A,H15B,H15C), C18(H18A,H18B,H18C), C27(H27A,H27B,
 H27C), C30(H30A,H30B,H30C)
3.c :
 C21(H21), C24(H24)
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_smtbx_masks_special_details
;
A solvent mask was calculated and 188 electrons were 
found in a volume of 700\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
2[C4H8O2] per Formula Unit 
which account for 192 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              82264
_shelx_fab_checksum              50363
_olex2_submission_special_instructions 'No special instructions were received'