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_7129950
_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 H60 N12 O12, [+ solvents]'
_chemical_formula_sum            'C60 H60 N12 O12'
_chemical_formula_weight         1141.20
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2022-02-23
_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                 98.846(17)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.1468(17)
_cell_length_b                   19.626(4)
_cell_length_c                   18.398(5)
_cell_measurement_reflns_used    4298
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      74.03
_cell_measurement_theta_min      4.69
_cell_volume                     3620.2(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(2)
_diffrn_measured_fraction_theta_full 0.939
_diffrn_measured_fraction_theta_max 0.884
_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  0.0428
_diffrn_reflns_av_unetI/netI     0.0776
_diffrn_reflns_Laue_measured_fraction_full 0.939
_diffrn_reflns_Laue_measured_fraction_max 0.884
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            11770
_diffrn_reflns_point_group_measured_fraction_full 0.939
_diffrn_reflns_point_group_measured_fraction_max 0.884
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.694
_diffrn_reflns_theta_min         4.506
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.616
_exptl_absorpt_correction_T_max  0.7538
_exptl_absorpt_correction_T_min  0.5944
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1022 before and 0.0556 after correction.
The Ratio of minimum to maximum transmission is 0.7885.
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    1.047
_exptl_crystal_description       prism
_exptl_crystal_F_000             1200
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: methanol/toluene'
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.222
_refine_diff_density_min         -0.226
_refine_diff_density_rms         0.040
_refine_ls_extinction_coef       0.0029(6)
_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   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         6577
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0947
_refine_ls_R_factor_gt           0.0660
_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^)+(0.0908P)^2^+0.6687P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1796
_refine_ls_wR_factor_ref         0.1969
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4433
_reflns_number_total             6577
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc00682k2.cif
_cod_data_source_block           res84_tol_squeeze
_cod_original_cell_volume        3620.3(14)
_cod_database_code               7129950
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.913
_shelx_estimated_absorpt_t_min   0.732
_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
2. Others
 Sof(H16C)=Sof(H16D)=Sof(C17B)=Sof(C18B)=Sof(H18B)=1-FVAR(1)
 Sof(H16A)=Sof(H16B)=Sof(C17A)=Sof(C18A)=Sof(H18A)=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), C16(H16C,H16D), C16(H16A,H16B), C19(H19A,H19B),
 C22(H22A,H22B), C25(H25A,H25B), C28(H28A,H28B)
3.b :
 C15(H15), C18A(H18A), C21(H21), C24(H24), C27(H27), C30(H30), C18B(H18B)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 132 electrons were 
found in a volume of 740\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1[C5H12O2] per Formula Unit 
which account for 116 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              2041
_shelx_fab_checksum              544
_olex2_submission_special_instructions 'No special instructions were received'