Inverse Evolution of Helicity from the Molecular to the Macroscopic Level Based on N-Terminal Aromatic Amino Acids
Liang, Juncong; Hao, Aiyou; Xing, Pengyao; Zhao, Yanli; ACS Nano  (2021) –; doi:10.1021/acsnano.0c10876

data_4518542
_publ_section_title
;
 Inverse Evolution of Helicity from the Molecular to the Macroscopic Level
 Based on N-Terminal Aromatic Amino Acids
;
_journal_name_full               'ACS Nano'
_journal_paper_doi               10.1021/acsnano.0c10876
_journal_year                    2021
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C19 H17 N O6'
_chemical_formula_sum            'C19 H17 N O6'
_chemical_formula_weight         355.33
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-01-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 106.621(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.6539(2)
_cell_length_b                   7.8453(2)
_cell_length_c                   13.4413(4)
_cell_measurement_reflns_used    6169
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      75.9580
_cell_measurement_theta_min      3.4230
_cell_volume                     874.43(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.999
_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    -37.00 -12.00   1.00    0.10    --  -48.45   4.00 -30.00   25
  2  \w   -119.00 -61.00   1.00    0.10    --  -48.45  -4.00 151.00   58
  3  \w     25.00  66.00   1.00    0.10    --   48.45   4.00 -30.00   41
  4  \w   -104.00 -72.00   1.00    0.40    --  -86.25   4.00 -30.00   32
  5  \w     41.00  87.00   1.00    0.40    --  106.49  -4.00 151.00   46
  6  \w    105.00 140.00   1.00    0.40    --  106.49   4.00 -30.00   35
  7  \w    -69.00 -36.00   1.00    0.10    --  -48.45 -19.00   0.00   33
  8  \w    -74.00 -44.00   1.00    0.10    --  -48.45 -29.00  92.81   30
  9  \w    -52.00 -26.00   1.00    0.10    --  -48.45 -77.00 150.00   26
 10  \w    -55.00 -28.00   1.00    0.10    --  -48.45 -77.00  30.00   27
 11  \w    -53.00 -27.00   1.00    0.10    --  -48.45 -77.00 -90.00   26
 12  \w    -53.00 -28.00   1.00    0.10    --  -48.45 -77.00  60.00   25
 13  \w    -51.00 -26.00   1.00    0.10    --  -48.45 -77.00 120.00   25
 14  \w    -54.00 -26.00   1.00    0.10    --  -48.45 -77.00-180.00   28
 15  \w     43.00  69.00   1.00    0.10    --   48.45  38.00  60.00   26
 16  \w     38.00  72.00   1.00    0.10    --   48.45  38.00   0.00   34
 17  \w     37.00  71.00   1.00    0.10    --   48.45  57.00 -30.00   34
 18  \w    -21.00  61.00   1.00    0.10    --   48.45 -38.00   0.00   82
 19  \w     41.00  83.00   1.00    0.10    --   48.45  38.00  90.00   42
 20  \w    -99.00 -65.00   1.00    0.40    --  -86.25 -72.00  72.73   34
 21  \w    -89.00 -63.00   1.00    0.40    --  -86.25 -77.00   0.00   26
 22  \w    -88.00 -63.00   1.00    0.40    --  -86.25 -77.00  30.00   25
 23  \w    -96.00 -66.00   1.00    0.40    --  -86.25 -72.00  63.75   30
 24  \w   -155.00-130.00   1.00    0.40    --  -86.25 -77.00  30.00   25
 25  \w    -86.00 -61.00   1.00    0.40    --  -86.25 -83.00   1.17   25
 26  \w    -91.00 -65.00   1.00    0.40    --  -86.25 -75.00 -43.90   26
 27  \w    -88.00 -63.00   1.00    0.40    --  -86.25 -77.00 120.00   25
 28  \w   -145.00 -93.00   1.00    0.40    --  -86.25 -77.00 120.00   52
 29  \w    -92.00 -66.00   1.00    0.40    --  -86.25 -77.00 150.00   26
 30  \w   -159.00-102.00   1.00    0.40    --  -86.25 -83.00   1.17   57
 31  \w    -91.00 -65.00   1.00    0.40    --  -86.25 -73.00  13.29   26
 32  \w   -101.00 -64.00   1.00    0.40    --  -86.25 -77.00-180.00   37
 33  \w    -96.00 -64.00   1.00    0.40    --  -86.25 -82.00  55.48   32
 34  \w    -87.00 -62.00   1.00    0.40    --  -86.25 -80.00  56.27   25
 35  \w   -105.00 -65.00   1.00    0.40    --  -86.25 -72.00  55.26   40
 36  \w    -98.00 -66.00   1.00    0.40    --  -86.25 -73.00  31.32   32
 37  \w    -92.00 -65.00   1.00    0.40    --  -86.25 -77.00  90.00   27
 38  \w   -155.00 -63.00   1.00    0.40    --  -86.25 -81.00 106.14   92
 39  \w    -90.00 -65.00   1.00    0.40    --  -86.25 -77.00  60.00   25
 40  \w    -89.00 -64.00   1.00    0.40    --  -86.25 -77.00 -30.00   25
 41  \w     34.00 121.00   1.00    0.40    --  106.49 -57.00 -30.00   87
 42  \w    110.00 175.00   1.00    0.40    --  106.49  57.00   0.00   65
 43  \w     41.00 108.00   1.00    0.40    --  106.49-125.00 150.00   67
 44  \w     93.00 147.00   1.00    0.40    --  106.49  38.00 150.00   54
 45  \w     84.00 109.00   1.00    0.40    --  106.49 -99.00-180.00   25
 46  \w    130.00 156.00   1.00    0.40    --  106.49  38.00   0.00   26
 47  \w     34.00  73.00   1.00    0.40    --  106.49 -99.00-180.00   39
 48  \w     76.00 104.00   1.00    0.40    --  106.49 -99.00 -30.00   28
 49  \w     34.00  67.00   1.00    0.40    --  106.49 -99.00 -30.00   33
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1417590000
_diffrn_orient_matrix_UB_12      0.0051986000
_diffrn_orient_matrix_UB_13      -0.1001657000
_diffrn_orient_matrix_UB_21      -0.1198274000
_diffrn_orient_matrix_UB_22      0.0093003000
_diffrn_orient_matrix_UB_23      0.0653216000
_diffrn_orient_matrix_UB_31      0.0095522000
_diffrn_orient_matrix_UB_32      0.1960666000
_diffrn_orient_matrix_UB_33      -0.0004194000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0718
_diffrn_reflns_av_unetI/netI     0.0521
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10596
_diffrn_reflns_point_group_measured_fraction_full 0.951
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.033
_diffrn_reflns_theta_min         3.432
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.850
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85133
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.25a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_description       block
_exptl_crystal_F_000             372
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.148
_refine_diff_density_min         -0.233
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details
;
 Flack x determined using 1051 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.28(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         3004
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0542
_refine_ls_R_factor_gt           0.0430
_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^)+(0.0645P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1025
_refine_ls_wR_factor_ref         0.1105
_reflns_Friedel_coverage         0.786
_reflns_Friedel_fraction_full    0.910
_reflns_Friedel_fraction_max     0.923
_reflns_number_gt                2625
_reflns_number_total             3004
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            nn0c10876_si_002.cif
_cod_data_source_block           200117c
_cod_database_code               4518542
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         CNO
_shelx_estimated_absorpt_t_max   0.983
_shelx_estimated_absorpt_t_min   0.959
_reflns_odcompleteness_completeness 99.94
_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 C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C3(H3A), C4(H4)
2.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C10(H10A,H10B)
2.c Aromatic/amide H refined with riding coordinates:
 N1(H1), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18),
 C19(H19)
2.d Idealised tetrahedral OH refined as rotating group:
 O3(H3), O5(H5)
;
_shelx_res_checksum              78281
_shelx_hkl_checksum              97533
_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 3.132
_oxdiff_exptl_absorpt_empirical_full_min 0.482