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_8000429
_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             2019-11-25
_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                   9.6818(2)
_cell_length_b                   15.8107(3)
_cell_length_c                   26.3785(4)
_cell_measurement_reflns_used    4131
_cell_measurement_temperature    172.99(10)
_cell_measurement_theta_max      75.5480
_cell_measurement_theta_min      3.2880
_cell_volume                     4037.92(13)
_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 0.975
_diffrn_measured_fraction_theta_max 0.987
_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    -59.00  20.00   1.00    2.50    --  -48.45  80.00 134.00   79
  2  \w   -120.00 -80.00   1.00    2.50    --  -48.45-125.00-180.00   40
  3  \w   -154.00 -71.00   1.00   15.50    --  -86.25 -75.00-105.00   83
  4  \w     91.00 124.00   1.00   15.50    --  106.49 -67.00 126.00   33
  5  \w     35.00  76.00   1.00   15.50    --  106.49 -67.00 126.00   41
  6  \w     32.00 118.00   1.00   15.50    --  106.49 -19.00   0.00   86
  7  \w     83.00 178.00   1.00   15.50    --  106.49  80.00 134.00   95
;
_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      0.1184845000
_diffrn_orient_matrix_UB_12      -0.0251519000
_diffrn_orient_matrix_UB_13      0.0359299000
_diffrn_orient_matrix_UB_21      0.0273425000
_diffrn_orient_matrix_UB_22      -0.0795254000
_diffrn_orient_matrix_UB_23      -0.0322434000
_diffrn_orient_matrix_UB_31      0.1026098000
_diffrn_orient_matrix_UB_32      0.0503726000
_diffrn_orient_matrix_UB_33      -0.0328715000
_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  0.0371
_diffrn_reflns_av_unetI/netI     0.0455
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            6556
_diffrn_reflns_point_group_measured_fraction_full 0.911
_diffrn_reflns_point_group_measured_fraction_max 0.922
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.050
_diffrn_reflns_theta_min         5.596
_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    8.612
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70280
_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 yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_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          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.444
_refine_diff_density_min         -0.942
_refine_diff_density_rms         0.120
_refine_ls_abs_structure_details
;
 Flack x determined using 1154 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.005(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         3328
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.142
_refine_ls_R_factor_all          0.0632
_refine_ls_R_factor_gt           0.0569
_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^)+(0.1046P)^2^+10.7363P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1594
_refine_ls_wR_factor_ref         0.1754
_reflns_Friedel_coverage         0.663
_reflns_Friedel_fraction_full    0.828
_reflns_Friedel_fraction_max     0.838
_reflns_number_gt                3085
_reflns_number_total             3328
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jz0c00997_si_002.cif
_cod_data_source_block           191125a
_cod_depositor_comments
'Adding full bibliography for 8000429--8000432.cif.'
_cod_database_code               8000429
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         FeCO
_shelx_estimated_absorpt_t_max   0.782
_shelx_estimated_absorpt_t_min   0.673
_reflns_odcompleteness_completeness 98.73
_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:
 C4(H4)
2.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C21(H21A,H21B)
2.c Aromatic/amide H refined with riding coordinates:
 N1(H1), C3(H3A), 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              70408
_shelx_hkl_checksum              8397
_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 1.519
_oxdiff_exptl_absorpt_empirical_full_min 0.590