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_7130075
_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         'C55 H63 N8 O8, 0.5(H2 O)'
_chemical_formula_sum            'C55 H64 N8 O8.5'
_chemical_formula_weight         973.14
_space_group_crystal_system      orthorhombic
_space_group_IT_number           20
_space_group_name_Hall           'C 2c 2'
_space_group_name_H-M_alt        'C 2 2 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2021-11-20 deposited with the CCDC.	2022-05-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.93847(11)
_cell_length_b                   29.7180(3)
_cell_length_c                   27.4444(2)
_cell_measurement_reflns_used    36684
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      79.6120
_cell_measurement_theta_min      4.6300
_cell_volume                     12183.71(18)
_computing_cell_refinement       'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 (Dolomanov 2016)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXT-2016/4 (Sheldrick, 2016)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual home/near'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0213
_diffrn_reflns_av_unetI/netI     0.0184
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            52855
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.272
_diffrn_reflns_theta_min         3.683
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.588
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.406
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.69a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.061
_exptl_crystal_description       plate
_exptl_crystal_F_000             4144
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.040
_platon_squeeze_details
;
;
_refine_diff_density_max         0.401
_refine_diff_density_min         -0.271
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details
;
 Flack x determined using 5321 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.04(4)
_refine_ls_extinction_coef       0.00039(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     608
_refine_ls_number_reflns         13016
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.161
_refine_ls_R_factor_all          0.0875
_refine_ls_R_factor_gt           0.0848
_refine_ls_shift/su_max          0.024
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1625P)^2^+6.3241P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2528
_refine_ls_wR_factor_ref         0.2574
_reflns_Friedel_coverage         0.833
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.963
_reflns_number_gt                12202
_reflns_number_total             13016
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc01038k2.cif
_cod_data_source_block           lihi10-sr
_cod_depositor_comments
;

2025-03-31
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C110 H128 N16 O17'
_cod_original_formula_weight         1946.28
_cod_original_formula_moiety         '2(C55 H63 N8 O8), H2 O'
_cod_original_formula_units_Z            4
_cod_database_code               7130075
_shelx_estimated_absorpt_t_min   0.891
_shelx_estimated_absorpt_t_max   0.977
_oxdiff_exptl_absorpt_empirical_full_min 0.755
_oxdiff_exptl_absorpt_empirical_full_max 1.971
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelxl_version_number           2013-4
_shelx_res_checksum              68426
_shelx_hkl_checksum              28116