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

data_7244035
_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 Cd0.5 Cl N3 O2'
_chemical_formula_sum            'C26 H21 Cd0.5 Cl N3 O2'
_chemical_formula_weight         499.11
_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             2021-07-09
_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                86.501(3)
_cell_angle_beta                 89.897(3)
_cell_angle_gamma                83.117(3)
_cell_formula_units_Z            2
_cell_length_a                   7.2058(2)
_cell_length_b                   7.7740(3)
_cell_length_c                   20.4876(7)
_cell_measurement_reflns_used    5785
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      75.5840
_cell_measurement_theta_min      4.3490
_cell_volume                     1137.26(7)
_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      100(1)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.931
_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    -20.00  14.00   0.50    0.16    --  -46.45  19.00   0.00   68
  2  \w    -24.00   3.00   0.50    0.16    --  -46.45 106.00 103.00   54
  3  \w    -59.00 -34.00   0.50    0.65    -- -102.00  61.00 -30.00   50
  4  \w    -70.00 -30.00   0.50    0.65    -- -102.00  77.00 -60.00   80
  5  \w    -78.00 -30.00   0.50    0.65    -- -102.00 125.00  30.00   96
  6  \w    -78.00 -26.00   0.50    0.16    --  -46.45 106.00 103.00  104
  7  \w    -80.00 -53.00   0.50    0.65    -- -102.00 106.00 103.00   54
  8  \w    -69.00 -42.00   0.50    0.65    -- -102.00  61.00  60.00   54
  9  \w   -112.00 -32.00   0.50    0.65    -- -102.00 125.00 -60.00  160
 10  \w    -69.00 -44.00   0.50    0.65    -- -102.00  61.00-180.00   50
 11  \w   -116.00 -58.00   0.50    0.65    -- -102.00 125.00-150.00  116
 12  \w   -116.00 -82.00   0.50    0.65    -- -102.00 125.00  30.00   68
 13  \w   -135.00 -97.00   0.50    0.65    -- -102.00 -30.00  30.00   76
 14  \w   -121.00 -85.00   0.50    0.65    -- -102.00 -61.00  90.00   72
 15  \w   -140.00 -88.00   0.50    0.65    -- -102.00-106.00   4.00  104
 16  \w   -118.00 -93.00   0.50    0.16    --  -46.45-125.00   0.00   50
 17  \w   -117.00 -72.00   0.50    0.16    --  -46.45-125.00  60.00   90
 18  \w   -118.00 -93.00   0.50    0.16    --  -46.45-125.00 150.00   50
 19  \w   -175.00-140.00   0.50    0.65    -- -102.00 -30.00  30.00   70
 20  \w   -167.00-140.00   0.50    0.65    -- -102.00 -61.00  90.00   54
 21  \w     15.00  52.00   0.50    0.16    --   46.45-106.00   4.00   74
 22  \w     42.00  68.00   0.50    0.65    --  104.75 -61.00 -90.00   52
 23  \w     55.00 103.00   0.50    0.65    --  104.75 -94.00-120.00   96
 24  \w     66.00  97.00   0.50    0.65    --  104.75-106.00   4.00   62
 25  \w     74.00 109.00   0.50    0.65    --  104.75 -94.00  30.00   70
 26  \w     44.00 107.00   0.50    0.65    --  104.75 -94.00 150.00  126
 27  \w     37.00 117.00   0.50    0.65    --  104.75-125.00 150.00  160
 28  \w     35.00  64.00   0.50    0.65    --  104.75 -77.00   0.00   58
 29  \w     34.00  61.00   0.50    0.65    --  104.75 -61.00-120.00   54
 30  \w     36.00  73.00   0.50    0.65    --  104.75 -61.00-180.00   74
 31  \w    136.00 176.00   0.50    0.65    --  104.75  30.00 -90.00   80
 32  \w    108.00 134.00   0.50    0.65    --  104.75  30.00 -90.00   52
 33  \w     95.00 174.00   0.50    0.65    --  104.75  45.00-120.00  158
 34  \w    104.00 175.00   0.50    0.65    --  104.75  30.00-180.00  142
 35  \w     86.00 153.00   0.50    0.65    --  104.75 106.00 103.00  134
 36  \w     40.00  73.00   0.50    0.65    --  104.75 -61.00 150.00   66
 37  \w    -19.00  25.00   0.50    0.16    --   46.45 -19.00 120.00   88
 38  \w    -22.00  67.00   0.50    0.16    --   46.45 -77.00 -90.00  178
 39  \w    -27.00  28.00   0.50    0.16    --   46.45 -19.00-180.00  110
;
_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      -0.0524535000
_diffrn_orient_matrix_UB_12      -0.1449947000
_diffrn_orient_matrix_UB_13      -0.0419418000
_diffrn_orient_matrix_UB_21      0.0927792000
_diffrn_orient_matrix_UB_22      0.0834047000
_diffrn_orient_matrix_UB_23      -0.0598200000
_diffrn_orient_matrix_UB_31      0.1871271000
_diffrn_orient_matrix_UB_32      -0.1096027000
_diffrn_orient_matrix_UB_33      0.0183849000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0738
_diffrn_reflns_av_unetI/netI     0.0623
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.931
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            11748
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.931
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.583
_diffrn_reflns_theta_min         4.324
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.358
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59197
_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 dark yellow'
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_description       block
_exptl_crystal_F_000             510
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.925
_refine_diff_density_min         -1.213
_refine_diff_density_rms         0.122
_refine_ls_extinction_coef       0.0008(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.158
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     297
_refine_ls_number_reflns         4460
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.162
_refine_ls_R_factor_all          0.0551
_refine_ls_R_factor_gt           0.0481
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0370P)^2^+4.6975P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1288
_refine_ls_wR_factor_ref         0.1306
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4155
_reflns_number_total             4460
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01349a1.cif
_cod_data_source_block           20210429e-complex1
_cod_depositor_comments
'Adding full bibliography for 7244034--7244035.cif.'
_cod_original_cell_volume        1137.27(7)
_cod_original_formula_sum        'C26 H21 Cd0.50 Cl N3 O2'
_cod_database_code               7244035
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H O N Cl Cd'
_diffrn_oxdiff_digest_frames
;
018387cb789d7701db88fcd0be0e1364a500068a0c4
;
_diffrn_oxdiff_digest_hkl
;
01c0420f0bfd8984f4452f5de9e82f5b62cec3
;
_reflns_odcompleteness_completeness 99.04
_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 O(H) groups
2. Rigid bond restraints
 O1
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.02
3. Uiso/Uaniso restraints and constraints
O1: within 2A with sigma of 0.002 and sigma for terminal atoms of 0.02
Uanis(O1) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.02
4.a Aromatic/amide H refined with riding coordinates:
 N1(H1), C11(H11), C5(H5), C6(H6), C3(H3), C2(H2a), C13(H13), C8(H8), C10(H10),
  C14(H14), C25(H25), C22(H22), C16(H16), C26(H26), C24(H24), C19(H19),
 C20(H20), C17(H17), C23(H23), C18(H18)
4.b Idealised tetrahedral OH refined as rotating group:
 O2(H2)
;
_shelx_res_checksum              34363
_shelx_hkl_checksum              18878
_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 2.303
_oxdiff_exptl_absorpt_empirical_full_min 0.515