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_8000509
_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_formula_moiety         'C48 H46 Fe N4 O8, 2(C4 H8 O), 2(H2 O)'
_chemical_formula_sum            'C56 H66 Fe N4 O12'
_chemical_formula_weight         1043.01
_chemical_name_systematic        1
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2020-07-20
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_cell_angle_alpha                62.882(6)
_cell_angle_beta                 85.647(5)
_cell_angle_gamma                61.341(6)
_cell_formula_units_Z            1
_cell_length_a                   12.1314(7)
_cell_length_b                   12.1865(8)
_cell_length_c                   12.2183(7)
_cell_measurement_reflns_used    6340
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      76.0680
_cell_measurement_theta_min      4.0790
_cell_volume                     1387.1(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_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    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.933
_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    -13.00  73.00   1.00    0.14    --   48.45 -83.00 104.00   86
  2  \w    -68.00  24.00   1.00    0.14    --  -48.45  83.00-134.00   92
  3  \w    -25.00  22.00   1.00    0.14    --  -48.45  19.00 -60.00   47
  4  \w    -37.00  25.00   1.00    0.14    --  -48.45  38.00 150.00   62
  5  \w   -117.00 -74.00   1.00    0.14    --  -48.45-125.00 -90.00   43
  6  \w   -116.00 -75.00   1.00    0.14    --  -48.45-125.00-120.00   41
  7  \w   -106.00 -81.00   1.00    1.00    --  -86.25  83.00-134.00   25
  8  \w    -54.00 -16.00   1.00    1.00    --  -86.25  83.00-134.00   38
  9  \w    -43.00 -13.00   1.00    1.00    --  -86.25  38.00  30.00   30
 10  \w    -43.00 -16.00   1.00    1.00    --  -86.25  38.00  60.00   27
 11  \w   -156.00 -78.00   1.00    1.00    --  -86.25 -38.00 120.00   78
 12  \w   -146.00 -89.00   1.00    1.00    --  -86.25 -83.00 104.00   57
 13  \w    101.00 171.00   1.00    1.00    --  106.49  38.00 -60.00   70
 14  \w    103.00 164.00   1.00    1.00    --  106.49  83.00-134.00   61
 15  \w     95.00 121.00   1.00    1.00    --  106.49  19.00-150.00   26
 16  \w    123.00 178.00   1.00    1.00    --  106.49  19.00-150.00   55
 17  \w     95.00 178.00   1.00    1.00    --  106.49  19.00-180.00   83
 18  \w     37.00 104.00   1.00    1.00    --  106.49-125.00 -30.00   67
 19  \w     55.00 111.00   1.00    1.00    --  106.49-125.00 -60.00   56
 20  \w     36.00 111.00   1.00    1.00    --  106.49-125.00 -90.00   75
 21  \w     34.00 111.00   1.00    1.00    --  106.49-125.00   0.00   77
 22  \w     34.00 103.00   1.00    1.00    --  106.49 -99.00  60.00   69
 23  \w     34.00 106.00   1.00    1.00    --  106.49 -99.00  90.00   72
 24  \w     49.00 132.00   1.00    1.00    --  106.49 -83.00 104.00   83
 25  \w     39.00  64.00   1.00    1.00    --  106.49 -57.00 150.00   25
 26  \w     34.00 102.00   1.00    1.00    --  106.49 -77.00 -30.00   68
;
_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      -0.0123708000
_diffrn_orient_matrix_UB_12      0.0102007000
_diffrn_orient_matrix_UB_13      0.1219017000
_diffrn_orient_matrix_UB_21      -0.1464960000
_diffrn_orient_matrix_UB_22      0.0746164000
_diffrn_orient_matrix_UB_23      -0.0333195000
_diffrn_orient_matrix_UB_31      0.0072537000
_diffrn_orient_matrix_UB_32      -0.1458597000
_diffrn_orient_matrix_UB_33      0.0692137000
_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  0.0775
_diffrn_reflns_av_unetI/netI     0.0830
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.933
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14423
_diffrn_reflns_point_group_measured_fraction_full 0.637
_diffrn_reflns_point_group_measured_fraction_max 0.595
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.245
_diffrn_reflns_theta_min         4.135
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.698
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85542
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.68a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.247
_exptl_crystal_description       needle
_exptl_crystal_F_000             551
_exptl_crystal_preparation       THF
_exptl_crystal_recrystallization_method 1
_exptl_crystal_size_max          1
_exptl_crystal_size_mid          1
_exptl_crystal_size_min          1
_refine_diff_density_max         1.688
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.116
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.027(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     658
_refine_ls_number_reflns         6932
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0900
_refine_ls_R_factor_gt           0.0827
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2308
_refine_ls_wR_factor_ref         0.2408
_reflns_Friedel_coverage         0.277
_reflns_Friedel_fraction_full    0.291
_reflns_Friedel_fraction_max     0.258
_reflns_number_gt                6160
_reflns_number_total             6932
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jz1c01231_si_004.cif
_cod_data_source_block           200604a
_cod_depositor_comments
;

2025-04-27
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_weight         40.08
_cod_original_formula_moiety
'0.038(C48 H46 Fe N4 O8), 0.038(N), 0.038(C4 H8 O), 0.038(C4 H5 O), 0.038(H2 O)'
_cod_original_formula_units_Z            26
_cod_original_cell_volume        1387.05(18)
_cod_original_formula_sum        'C2.15 H2.50 Fe0.04 N0.15 O0.46'
_cod_database_code               8000509
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CNO
_reflns_odcompleteness_completeness 98.55
_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, All O(H,H) groups
2.a Free rotating group:
 O22(H22A,H22B)
2.b Ternary CH refined with riding coordinates:
 C22(H22), C20(H20), C15(H15), C19(H19)
2.c Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C23(H23A,H23B), C1(H1A,H1B), C1C(H1CA,H1CB), C2AA(H2AA,H2AB),
 C1AA(H1AA,H1AB), C0AA(H0AA,H0AB), C21(H21A,H21B), C27(H27A,H27B)
2.d Aromatic/amide H refined with riding coordinates:
 N(H), N8(H8), N9(H9), C(HA), C3(H3A), C4(H4), C6AA(H6AA), C5(H5), C8(H8A),
 C26(H26), C14(H14), C16(H16), C17(H17), C18(H18), C1D(H1D), C1F(H1F), C24(H24),
  C10(H10), C1I(H1I), C1J(H1J), C12(H12), C1M(H1M), C1N(H1N), C1O(H1O),
 C13(H13), C1T(H1T), N1L(H1L), C3AA(H3AA), C4AA(H4AA), C5AA(H5AA), C8AA(H8AA),
 C9AA(H9AA), C0BA(H0BA), C29(H29), C28(H28)
2.e Idealised tetrahedral OH refined as rotating group:
 O1(H1), O3(H3)
;
_shelx_res_checksum              95556
_shelx_hkl_checksum              12180
_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 1.889
_oxdiff_exptl_absorpt_empirical_full_min 0.619