Supramolecular helical self-assembly of small peptides
Giri, Rajat Subhra; Mandal, Bhubaneswar; CrystEngComm 24 (2022) 10–32; doi:10.1039/D1CE01349A

data_7244034
_publ_section_title
;
 Supramolecular helical self-assembly of small peptides
;
_journal_issue                   1
_journal_name_full               CrystEngComm
_journal_page_first              10
_journal_page_last               32
_journal_paper_doi               10.1039/D1CE01349A
_journal_volume                  24
_journal_year                    2022
_chemical_formula_moiety         'C26 H21 N3 O2, 2(C2 H3 N)'
_chemical_formula_sum            'C30 H25 N5 O2'
_chemical_formula_weight         487.55
_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   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-07-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-07-27 deposited with the CCDC.	2021-11-26 downloaded from the CCDC.
;
_cell_angle_alpha                75.824(3)
_cell_angle_beta                 85.556(3)
_cell_angle_gamma                89.480(3)
_cell_formula_units_Z            4
_cell_length_a                   11.5136(5)
_cell_length_b                   14.4562(5)
_cell_length_c                   16.3680(6)
_cell_measurement_reflns_used    13077
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      75.4570
_cell_measurement_theta_min      3.8170
_cell_volume                     2633.30(18)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -26.00   0.00   0.50    1.12    --  -46.95  77.00 -90.00   52
  2  \w    -19.00  12.00   0.50    1.12    --  -46.95  19.00-120.00   62
  3  \w     -9.00  25.00   0.50    1.12    --  -46.95  37.00-180.00   68
  4  \w    -21.00  29.00   0.50    1.12    --  -46.95  19.00 -30.00  100
  5  \w     38.00  66.00   0.50    1.12    --   46.95-111.00  92.00   56
  6  \w     83.00 109.00   0.50    4.49    --  104.75-111.00  92.00   52
  7  \w     77.00 116.00   0.50    4.49    --  104.75-125.00  60.00   78
  8  \w     42.00 109.00   0.50    4.49    --  104.75 -94.00  90.00  134
  9  \w     41.00  70.00   0.50    4.49    --  104.75 -61.00 -30.00   58
 10  \w     36.00  72.00   0.50    4.49    --  104.75 -61.00 -90.00   72
 11  \w     32.00  71.00   0.50    4.49    --  104.75 -61.00 -60.00   78
 12  \w     32.00  57.00   0.50    4.49    --  104.75 -61.00-120.00   50
 13  \w     32.00 114.00   0.50    4.49    --  104.75-125.00-120.00  164
 14  \w     32.00  60.00   0.50    4.49    --  104.75-125.00  60.00   56
 15  \w     -7.00  40.00   0.50    1.12    --   46.95 -37.00  60.00   94
 16  \w    -26.00  44.00   0.50    1.12    --   46.95 -37.00   0.00  140
 17  \w     90.00 146.00   0.50    4.49    --  104.75  77.00 150.00  112
 18  \w    149.00 175.00   0.50    4.49    --  104.75  77.00 150.00   52
 19  \w    135.00 161.00   0.50    4.49    --  104.75 125.00 150.00   52
 20  \w     77.00 111.00   0.50    4.49    --  104.75 125.00 150.00   68
 21  \w     76.00 174.00   0.50    4.49    --  104.75 125.00  30.00  196
 22  \w     96.00 149.00   0.50    4.49    --  104.75 125.00-120.00  106
 23  \w    109.00 168.00   0.50    4.49    --  104.75 111.00-173.00  118
 24  \w    -55.00 -30.00   0.50    4.49    -- -102.00 125.00 -60.00   50
 25  \w    -86.00   0.00   0.50    1.12    --  -46.95 111.00-173.00  172
 26  \w    -69.00 -40.00   0.50    1.12    --  -46.95  77.00 -90.00   58
 27  \w    -63.00 -33.00   0.50    4.49    -- -102.00  61.00 -30.00   60
 28  \w   -100.00 -29.00   0.50    4.49    -- -102.00  77.00  60.00  142
 29  \w    -67.00 -29.00   0.50    4.49    -- -102.00  61.00 120.00   76
 30  \w    -67.00 -34.00   0.50    4.49    -- -102.00  61.00 150.00   66
 31  \w   -116.00 -89.00   0.50    4.49    -- -102.00 -30.00 150.00   54
 32  \w   -147.00 -79.00   0.50    4.49    -- -102.00-111.00  92.00  136
 33  \w   -115.00 -71.00   0.50    1.12    --  -46.95-125.00 120.00   88
 34  \w   -152.00-107.00   0.50    4.49    -- -102.00 -30.00 -60.00   90
 35  \w   -115.00 -86.00   0.50    1.12    --  -46.95-125.00-120.00   58
 36  \w   -115.00 -71.00   0.50    1.12    --  -46.95-125.00 -90.00   88
 37  \w   -172.00-106.00   0.50    4.49    -- -102.00 -30.00-180.00  132
 38  \w    -65.00 -33.00   0.50    4.49    -- -102.00  61.00-180.00   64
 39  \w   -100.00 -45.00   0.50    4.49    -- -102.00  77.00-150.00  110
 40  \w   -111.00 -69.00   0.50    4.49    -- -102.00 111.00-173.00   84
 41  \w   -116.00 -64.00   0.50    4.49    -- -102.00 125.00 -60.00  104
 42  \w   -169.00-126.00   0.50    4.49    -- -102.00 -30.00 150.00   86
 43  \w   -171.00 -86.00   0.50    4.49    -- -102.00-125.00 120.00  170
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0034111000
_diffrn_orient_matrix_UB_12      0.0515593000
_diffrn_orient_matrix_UB_13      0.0721089000
_diffrn_orient_matrix_UB_21      -0.0281361000
_diffrn_orient_matrix_UB_22      0.0943788000
_diffrn_orient_matrix_UB_23      -0.0625306000
_diffrn_orient_matrix_UB_31      -0.1311877000
_diffrn_orient_matrix_UB_32      -0.0227333000
_diffrn_orient_matrix_UB_33      0.0192687000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0666
_diffrn_reflns_av_unetI/netI     0.0553
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.933
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            32913
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.933
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.868
_diffrn_reflns_theta_min         3.665
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.636
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72432
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light red'
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_description       block
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.493
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.249
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     673
_refine_ls_number_reflns         10507
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.249
_refine_ls_R_factor_all          0.0949
_refine_ls_R_factor_gt           0.0727
_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^)+(0.0208P)^2^+5.3579P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1927
_refine_ls_wR_factor_ref         0.2035
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8339
_reflns_number_total             10507
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01349a1.cif
_cod_data_source_block           20210406f-HL
_cod_depositor_comments
;
Adding full bibliography for 7244034--7244035.cif.

2024-06-28
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C60 H50 N10 O4'
_cod_original_formula_weight         975.10
_cod_original_formula_moiety         '2(C26 H21 N3 O2), 4(C2 H3 N)'
_cod_original_formula_units_Z            2
_cod_database_code               7244034
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O N '
_diffrn_oxdiff_digest_frames
;
01fc29eb9f2bc47a75bd79b5c496a5d82e0003190df
;
_diffrn_oxdiff_digest_hkl
;
01d50ca6e6b86fc6d7192a6c6172bf2094c9f7
;
_reflns_odcompleteness_completeness 99.55
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N1(H1), N4(H4A), C28(H28), C32(H32), C31(H31), C13(H13), C29(H29), C40(H40),
 C8(H8), C14(H14), C5(H5), C3(H3), C34(H34), C2(H2A), C6(H6), C39(H39),
 C10(H10), C36(H36), C11(H11), C16(H16), C20(H20), C26(H26), C37(H37), C52(H52),
  C48(H48), C18(H18), C22(H22), C17(H17), C42(H42), C25(H25), C19(H19),
 C24(H24), C51(H51), C46(H46), C43(H43), C23(H23), C49(H49), C50(H50), C44(H44),
  C45(H45)
2.b Idealised Me refined as rotating group:
 C60(H60A,H60B,H60C), C54(H54A,H54B,H54C), C58(H58A,H58B,H58C), C56(H56A,H56B,
 H56C)
2.c Idealised tetrahedral OH refined as rotating group:
 O4(H4), O2(H2)
;
_shelx_res_checksum              41889
_shelx_hkl_checksum              48436
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.323
_oxdiff_exptl_absorpt_empirical_full_min 0.192