Water-Mediated Folding Behaviors and Chiroptical Inversion of Ferrocene-Conjugated Dipeptides
Liu, Bingyu; Hao, Aiyou; Xing, Pengyao; The Journal of Physical Chemistry Letters  (2021) 6190–6196; doi:10.1021/acs.jpclett.1c01231

data_8000508
_publ_section_title
;
 Water-Mediated Folding Behaviors and Chiroptical Inversion of
 Ferrocene-Conjugated Dipeptides
;
_journal_name_full               'The Journal of Physical Chemistry Letters'
_journal_page_first              6190
_journal_page_last               6196
_journal_paper_doi               10.1021/acs.jpclett.1c01231
_journal_year                    2021
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C34 H34 Fe N4 O8'
_chemical_formula_sum            'C34 H34 Fe N4 O8'
_chemical_formula_weight         682.50
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-11-26
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_cell_angle_alpha                90
_cell_angle_beta                 113.733(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.6429(3)
_cell_length_b                   12.1175(2)
_cell_length_c                   11.3048(3)
_cell_measurement_reflns_used    5322
_cell_measurement_temperature    172.99(10)
_cell_measurement_theta_max      76.1530
_cell_measurement_theta_min      5.2550
_cell_volume                     1585.43(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 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      172.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_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     85.00 175.00   1.00    0.37    --  106.49  77.00  30.00   90
  2  \w    139.00 165.00   1.00    0.37    --  106.49  71.00 -85.00   26
  3  \w     93.00 178.00   1.00    0.37    --  106.49  38.00-120.00   85
  4  \w     86.00 122.00   1.00    0.37    --  106.49  71.00 -85.00   36
  5  \w     93.00 178.00   1.00    0.37    --  106.49  38.00   0.00   85
  6  \w    102.00 178.00   1.00    0.37    --  106.49  19.00 -30.00   76
  7  \w     51.00  86.00   1.00    0.10    --   48.45  71.00 -85.00   35
  8  \w     94.00 178.00   1.00    0.37    --  106.49  19.00-150.00   84
  9  \w     35.00  62.00   1.00    0.37    --  106.49 -57.00  60.00   27
 10  \w     -9.00  17.00   1.00    0.10    --   48.45 -71.00 144.00   26
 11  \w     22.00  49.00   1.00    0.10    --   48.45 -71.00 144.00   27
 12  \w     37.00  89.00   1.00    0.37    --  106.49 -71.00 144.00   52
 13  \w     36.00  66.00   1.00    0.37    --  106.49 -57.00 150.00   30
 14  \w     40.00 111.00   1.00    0.37    --  106.49-125.00 150.00   71
 15  \w     69.00 102.00   1.00    0.37    --  106.49 -99.00 150.00   33
 16  \w     38.00  64.00   1.00    0.37    --  106.49 -99.00 150.00   26
 17  \w     34.00 102.00   1.00    0.37    --  106.49 -99.00  60.00   68
 18  \w     35.00 103.00   1.00    0.37    --  106.49 -99.00-120.00   68
 19  \w   -120.00 -73.00   1.00    0.10    --  -48.45-125.00 -60.00   47
 20  \w   -148.00 -85.00   1.00    0.37    --  -86.25 -71.00 144.00   63
 21  \w   -115.00 -50.00   1.00    0.10    --  -48.45 -71.00 144.00   65
 22  \w   -158.00 -75.00   1.00    0.37    --  -86.25 -19.00  30.00   83
 23  \w   -158.00-133.00   1.00    0.37    --  -86.25 -38.00   0.00   25
 24  \w   -103.00 -76.00   1.00    0.37    --  -86.25 -38.00   0.00   27
 25  \w    -16.00  27.00   1.00    0.10    --  -48.45  19.00 -90.00   43
 26  \w    -67.00  16.00   1.00    0.10    --  -48.45  71.00 -85.00   83
 27  \w    -89.00 -24.00   1.00    0.37    --  -86.25  71.00 -85.00   65
 28  \w    -43.00 -13.00   1.00    0.37    --  -86.25  38.00  60.00   30
 29  \w    -42.00 -13.00   1.00    0.37    --  -86.25  38.00  90.00   29
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0943414000
_diffrn_orient_matrix_UB_12      -0.0882869000
_diffrn_orient_matrix_UB_13      0.0257569000
_diffrn_orient_matrix_UB_21      -0.0311151000
_diffrn_orient_matrix_UB_22      -0.0503433000
_diffrn_orient_matrix_UB_23      0.1070122000
_diffrn_orient_matrix_UB_31      -0.0885988000
_diffrn_orient_matrix_UB_32      -0.0762932000
_diffrn_orient_matrix_UB_33      -0.1003952000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_av_unetI/netI     0.0351
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8116
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.077
_diffrn_reflns_theta_max         67.077
_diffrn_reflns_theta_min         4.272
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.315
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88160
_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 light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.430
_exptl_crystal_description       plate
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.248
_refine_diff_density_min         -0.223
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details
;
 Flack x determined using 1223 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.001(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         2819
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0319
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0309P)^2^+1.7257P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0777
_refine_ls_wR_factor_ref         0.0779
_reflns_Friedel_coverage         0.886
_reflns_Friedel_fraction_full    0.979
_reflns_Friedel_fraction_max     0.979
_reflns_number_gt                2777
_reflns_number_total             2819
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jz1c01231_si_003.cif
_cod_data_source_block           201123b
_cod_database_code               8000508
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.958
_shelx_estimated_absorpt_t_min   0.813
_reflns_odcompleteness_completeness 99.73
_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:
 C12(H12)
2.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C16(H16A,H16B)
2.c Aromatic/amide H refined with riding coordinates:
 N8(H8), N11(H11), C2(H2), C5(H5), C24(H24), C6(H6), C23(H23), C20(H20),
 C21(H21), C4(H4), C22(H22)
2.d Idealised tetrahedral OH refined as rotating group:
 O15(H15)
;
_shelx_res_checksum              29045
_shelx_hkl_checksum              6903
_shelx_fab_checksum              3236
_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 1.553
_oxdiff_exptl_absorpt_empirical_full_min 0.813