Atomic insight into short helical peptide comprised of consecutive multiple aromatic residues
Misra, Rajkumar; Vijayakanth, Thangavel; Shimon, Linda J. W.; Adler-Abramovich, Lihi; Chemical Communications  (2022) –; doi:10.1039/D2CC01038K

data_7130076
_publ_section_title
;
 Atomic insight into short helical peptide comprised of consecutive
 multiple aromatic residues
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC01038K
_journal_year                    2022
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C60 H66 N8 O8'
_chemical_formula_sum            'C60 H66 N8 O8'
_chemical_formula_weight         1027.20
_space_group_crystal_system      hexagonal
_space_group_IT_number           169
_space_group_name_Hall           'P 61'
_space_group_name_H-M_alt        'P 61'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/4
_audit_update_record
;
2022-01-04 deposited with the CCDC.	2022-05-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   11.9093(2)
_cell_length_b                   11.9093(2)
_cell_length_c                   68.9715(10)
_cell_measurement_reflns_used    18827
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.6890
_cell_measurement_theta_min      3.8570
_cell_volume                     8471.7(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.111a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.111a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.111a (Rigaku OD, 2021)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT-2016/4 (Sheldrick, 2016)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy R, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_unetI/netI     0.0396
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       67
_diffrn_reflns_limit_l_min       -81
_diffrn_reflns_number            45992
_diffrn_reflns_point_group_measured_fraction_full 0.868
_diffrn_reflns_point_group_measured_fraction_max 0.835
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.890
_diffrn_reflns_theta_min         3.845
_diffrn_source                   'Rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    0.655
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80037
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.111a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.208
_exptl_crystal_description       needle
_exptl_crystal_F_000             3276
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.727
_refine_diff_density_min         -0.552
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details
;
 Flack x determined using 2694 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.09(13)
_refine_ls_extinction_coef       0.00055(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/4 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     683
_refine_ls_number_reflns         9676
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0772
_refine_ls_R_factor_gt           0.0626
_refine_ls_shift/su_max          0.064
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0972P)^2^+4.0523P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1627
_refine_ls_wR_factor_ref         0.1751
_reflns_Friedel_coverage         0.686
_reflns_Friedel_fraction_full    0.737
_reflns_Friedel_fraction_max     0.685
_reflns_number_gt                7985
_reflns_number_total             9676
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc01038k2.cif
_cod_data_source_block           lihi20
_cod_original_cell_volume        8471.7(3)
_cod_database_code               7130076
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_min   0.880
_shelx_estimated_absorpt_t_max   0.987
_oxdiff_exptl_absorpt_empirical_full_min 0.475
_oxdiff_exptl_absorpt_empirical_full_max 1.440
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              55761
_shelx_hkl_checksum              88672