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_8000430
_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         'C30 H28 Fe N2 O6, C H2 Cl2'
_chemical_formula_sum            'C31 H30 Cl2 Fe N2 O6'
_chemical_formula_weight         653.32
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-12-12
_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            4
_cell_length_a                   11.0166(2)
_cell_length_b                   12.3581(3)
_cell_length_c                   22.5772(6)
_cell_measurement_reflns_used    8199
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      74.9460
_cell_measurement_theta_min      4.4380
_cell_volume                     3073.76(12)
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.996
_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    -83.00 -42.00   1.00    0.40    --  -48.45-169.00 -40.00   41
  2  \w    -86.00 -53.00   1.00    0.40    --  -48.45 115.00-167.00   33
  3  \w    -40.00  -3.00   1.00    0.40    --  -48.45 115.00-167.00   37
  4  \w     66.00  91.00   1.00    0.40    --   48.45-115.00 103.00   25
  5  \w    -40.00 -13.00   1.00    3.30    --  -86.25 115.00-167.00   27
  6  \w   -142.00-117.00   1.00    3.30    --  -86.25-115.00 103.00   25
  7  \w    -84.00 -33.00   1.00    3.30    --  -86.25 169.00 -23.00   51
  8  \w     74.00 149.00   1.00    3.30    --  106.49-169.00 -40.00   75
  9  \w     46.00 112.00   1.00    3.30    --  106.49-115.00 103.00   66
 10  \w   -120.00 -70.00   1.00    0.40    --  -48.45-125.00-150.00   50
 11  \w   -117.00 -35.00   1.00    0.40    --  -48.45 -57.00  30.00   82
 12  \w     34.00  81.00   1.00    3.30    --  106.49-125.00 -30.00   47
 13  \w     31.00 118.00   1.00    3.30    --  106.49 -19.00  30.00   87
 14  \w     90.00 116.00   1.00    3.30    --  106.49-125.00 -30.00   26
 15  \w     34.00 115.00   1.00    3.30    --  106.49 -38.00  60.00   81
 16  \w     92.00 171.00   1.00    3.30    --  106.49 125.00  60.00   79
 17  \w    114.00 139.00   1.00    3.30    --  106.49 115.00-167.00   25
;
_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      -0.0052969000
_diffrn_orient_matrix_UB_12      0.1044205000
_diffrn_orient_matrix_UB_13      0.0373387000
_diffrn_orient_matrix_UB_21      0.0332960000
_diffrn_orient_matrix_UB_22      -0.0649986000
_diffrn_orient_matrix_UB_23      0.0557662000
_diffrn_orient_matrix_UB_31      0.1357659000
_diffrn_orient_matrix_UB_32      0.0199948000
_diffrn_orient_matrix_UB_33      -0.0123650000
_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  0.0621
_diffrn_reflns_av_unetI/netI     0.0581
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            18061
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.075
_diffrn_reflns_theta_min         4.078
_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    5.915
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49642
_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    1.412
_exptl_crystal_description       block
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.883
_refine_diff_density_min         -1.445
_refine_diff_density_rms         0.177
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.12(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         5319
_refine_ls_number_restraints     276
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.1566
_refine_ls_R_factor_gt           0.1435
_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^)+74.6630P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3263
_refine_ls_wR_factor_ref         0.3350
_reflns_Friedel_coverage         0.772
_reflns_Friedel_fraction_full    0.984
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                5045
_reflns_number_total             5319
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jz0c00997_si_003.cif
_cod_data_source_block           191212b
_cod_depositor_comments
'Adding full bibliography for 8000429--8000432.cif.'
_cod_database_code               8000430
_shelxl_version_number           2013-4
_chemical_oxdiff_usercomment     FeCN
_shelx_estimated_absorpt_t_max   0.589
_shelx_estimated_absorpt_t_min   0.270
_reflns_odcompleteness_completeness 99.55
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.88(3)
 0.12(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups
3. Uiso/Uaniso restraints and constraints
Cl1 \\sim Cl1A \\sim Cl2 \\sim Cl2A \\sim C21: within 2A with sigma of 0.004
and sigma for terminal atoms of 0.008
Fe1 \\sim O1 \\sim O2 \\sim O3 \\sim O4 \\sim O5 \\sim O6 \\sim N1 \\sim N2
\\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim
C9 \\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim
C17 \\sim C18 \\sim C19 \\sim C20 \\sim C22 \\sim C23 \\sim C24 \\sim C25 \\sim
C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31: within 2A with sigma of
0.004 and sigma for terminal atoms of 0.008
4. Others
 Fixed Sof: Cl1(0.5) Cl1A(0.5) Cl2(0.5) Cl2A(0.5) H21C(0.5) H21D(0.5)
 H21A(0.5) H21B(0.5)
5.a Ternary CH refined with riding coordinates:
 C6(H6), C8(H8)
5.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C11(H11A,H11B), C21(H21C,H21D), C21(H21A,H21B)
5.c Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), C7(H7), C10(H10), C12(H12), C13(H13), C14(H14), C15(H15),
 C16(H16), C18(H18), C19(H19), C20(H20), C23(H23), C24(H24), C25(H25), C26(H26),
  C28(H28), C29(H29), C30(H30), C31(H31)
5.d Fitted hexagon refined as free rotating group:
 C15(C16,C17,C18,C19,C20)
5.e Idealised tetrahedral OH refined as rotating group:
 O4(H4), O5(H5)
;
_shelx_res_checksum              19774
_shelx_hkl_checksum              88148
_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 1.676
_oxdiff_exptl_absorpt_empirical_full_min 0.577