Self-Assembly of <i>N</i>-Terminal Aryl Amino Acids into Adaptive Single- and Double-Strand Helices.
Zong, Zhaohui; Li, Peizhou; Hao, Aiyou; Xing, Pengyao; The journal of physical chemistry letters 11 (2020) 4147–4155; doi:10.1021/acs.jpclett.0c00997

data_8000432
_publ_section_title
;
 Self-Assembly of <i>N</i>-Terminal Aryl Amino Acids into Adaptive Single-
 and Double-Strand Helices.
;
_journal_issue                   10
_journal_name_full               'The journal of physical chemistry letters'
_journal_page_first              4147
_journal_page_last               4155
_journal_paper_doi               10.1021/acs.jpclett.0c00997
_journal_volume                  11
_journal_year                    2020
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C20 H19 Fe N O3, C H2 Cl2'
_chemical_formula_sum            'C21 H21 Cl2 Fe N O3'
_chemical_formula_weight         462.14
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-10-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.66820(10)
_cell_length_b                   15.8378(2)
_cell_length_c                   26.3801(3)
_cell_measurement_reflns_used    15460
_cell_measurement_temperature    172.99(10)
_cell_measurement_theta_max      76.1930
_cell_measurement_theta_min      3.3170
_cell_volume                     4039.40(8)
_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_environment      N~2~
_diffrn_ambient_temperature      172.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.997
_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  24.00   1.00    0.45    --  -48.45  57.00 140.00   44
  2  \w    -62.00 -31.00   1.00    0.45    --  -48.45  57.00 140.00   31
  3  \w   -119.00 -61.00   1.00    0.45    --  -48.45 -57.00  -0.00   58
  4  \w   -117.00 -91.00   1.00    3.00    --  -86.25 -57.00  -0.00   26
  5  \w    -66.00 -14.00   1.00    3.00    --  -86.25  57.00 140.00   52
  6  \w    -97.00 -69.00   1.00    3.00    --  -86.25  57.00 140.00   28
  7  \w     35.00  69.00   1.00    3.00    --  106.49 -57.00  -0.00   34
  8  \w     77.00 121.00   1.00    3.00    --  106.49 -57.00  -0.00   44
  9  \w   -120.00 -72.00   1.00    0.45    --  -48.45-125.00-180.00   48
 10  \w   -119.00 -86.00   1.00    0.45    --  -48.45-125.00 -30.00   33
 11  \w    -11.00  63.00   1.00    0.45    --   48.45 -57.00  -0.00   74
 12  \w     67.00 115.00   1.00    0.45    --   48.45  57.00 140.00   48
 13  \w   -126.00 -73.00   1.00    3.00    --  -86.25 -38.00 -90.00   53
 14  \w   -159.00 -77.00   1.00    3.00    --  -86.25 -38.00-150.00   82
 15  \w   -152.00 -75.00   1.00    3.00    --  -86.25 -19.00 -60.00   77
 16  \w    -94.00 -63.00   1.00    3.00    --  -86.25 -77.00 -90.00   31
 17  \w   -147.00-117.00   1.00    3.00    --  -86.25 -77.00 -90.00   30
 18  \w   -159.00-129.00   1.00    3.00    --  -86.25 -38.00 -90.00   30
 19  \w   -159.00 -90.00   1.00    3.00    --  -86.25 -99.00  90.00   69
 20  \w     84.00 177.00   1.00    3.00    --  106.49  77.00-150.00   93
 21  \w     34.00 126.00   1.00    3.00    --  106.49 -77.00 -60.00   92
 22  \w     97.00 178.00   1.00    3.00    --  106.49  19.00  90.00   81
 23  \w     98.00 177.00   1.00    3.00    --  106.49  57.00 -90.00   79
 24  \w     34.00 109.00   1.00    3.00    --  106.49 -99.00-150.00   75
 25  \w     93.00 173.00   1.00    3.00    --  106.49  57.00 140.00   80
;
_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      -0.1549910000
_diffrn_orient_matrix_UB_12      -0.0227072000
_diffrn_orient_matrix_UB_13      0.0003276000
_diffrn_orient_matrix_UB_21      0.0252751000
_diffrn_orient_matrix_UB_22      -0.0625593000
_diffrn_orient_matrix_UB_23      0.0437798000
_diffrn_orient_matrix_UB_31      -0.0273232000
_diffrn_orient_matrix_UB_32      0.0708959000
_diffrn_orient_matrix_UB_33      0.0386464000
_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  0.0317
_diffrn_reflns_av_unetI/netI     0.0201
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            20085
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.059
_diffrn_reflns_theta_min         5.360
_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    8.609
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52195
_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 orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_description       block
_exptl_crystal_F_000             1904
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.333
_refine_diff_density_min         -0.658
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details
;
 Flack x determined using 1482 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.002(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         3605
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0382
_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^)+(0.0769P)^2^+4.2061P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1115
_refine_ls_wR_factor_ref         0.1146
_reflns_Friedel_coverage         0.781
_reflns_Friedel_fraction_full    0.988
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                3490
_reflns_number_total             3605
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jz0c00997_si_004.cif
_cod_data_source_block           191025f
_cod_depositor_comments
'Adding full bibliography for 8000429--8000432.cif.'
_cod_database_code               8000432
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         FeCNO
_shelx_estimated_absorpt_t_max   0.725
_shelx_estimated_absorpt_t_min   0.673
_reflns_odcompleteness_completeness 99.85
_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:
 C2(H2)
2.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C21(H21A,H21B)
2.c Aromatic/amide H refined with riding coordinates:
 N1(H1), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C13(H13),
 C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20)
2.d Idealised tetrahedral OH refined as rotating group:
 O3(H3)
;
_shelx_res_checksum              999
_shelx_hkl_checksum              79267
_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 1.560
_oxdiff_exptl_absorpt_empirical_full_min 0.721