Design of an abiotic unimolecular three-helix bundle.
Wang, Shuhe; Sigl, Johannes; Allmendinger, Lars; Maurizot, Victor; Huc, Ivan; Chemical science 16 (2025) 1136–1146; doi:10.1039/d4sc07336c

data_1573401
_publ_section_title
;
 Design of an abiotic unimolecular three-helix bundle.
;
_journal_issue                   3
_journal_name_full               'Chemical science'
_journal_page_first              1136
_journal_page_last               1146
_journal_paper_doi               10.1039/d4sc07336c
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety
'C97.57 H82.564 N16 O17.952, C H2 Cl2, 3(C2 H3 N)'
_chemical_formula_sum            'C104.52 H93.44 Cl2 N19 O17.94'
_chemical_formula_weight         1973.60
_chemical_name_systematic        AOF-isoQuinolineLinker
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-10-29
_audit_creation_method
;
Olex2 1.5-ac6-020
(compiled 2024.02.14 svn.r2f8d729c for Rigaku Oxford Diffraction, GUI svn.r6966)
;
_audit_update_record
;
2024-10-29 deposited with the CCDC.	2024-11-13 downloaded from the CCDC.
;
_cell_angle_alpha                95.6610(10)
_cell_angle_beta                 93.9890(10)
_cell_angle_gamma                105.3540(10)
_cell_formula_units_Z            2
_cell_length_a                   13.16060(10)
_cell_length_b                   17.3713(2)
_cell_length_c                   24.3400(2)
_cell_measurement_reflns_used    56376
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      74.8780
_cell_measurement_theta_min      3.3840
_cell_volume                     5313.14(9)
_computing_cell_refinement       'CrysAlisPro 1.171.42.100a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.100a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.100a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-ac6-020 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac6-020 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.968
_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     95.00 123.00   0.50    0.10    --   82.00  15.00-150.00   56
  2  \w    100.00 132.00   0.50    0.10    --   85.25  50.00-115.09   64
  3  \w     99.00 135.00   0.50    0.10    --   85.25  42.00  13.15   72
  4  \w     88.00 132.00   0.50    0.10    --   82.00  15.00  90.00   88
  5  \w     93.00 131.00   0.50    0.10    --   82.00  15.00 150.00   76
  6  \w     73.00 115.00   0.50    0.10    --   82.00  15.00  60.00   84
  7  \w     66.00  92.00   0.50    0.10    --   82.00  15.00 -30.00   52
  8  \w     79.00 118.00   0.50    0.10    --   82.00  15.00 -90.00   78
  9  \w    100.00 132.00   0.50    0.10    --   82.00  15.00-120.00   64
 10  \w     64.00 132.00   0.50    0.10    --   82.00  15.00-180.00  136
 11  \w    107.00 132.00   0.50    0.10    --   82.00  15.00 -30.00   50
 12  \w     80.00 106.00   0.50    0.10    --   82.00  15.00   0.00   52
 13  \w     60.00 104.00   0.50    0.10    --   57.59  15.00  30.00   88
 14  \w    101.00 127.00   0.50    0.10    --   82.00  15.00 120.00   52
 15  \w     47.00  73.00   0.50    0.10    --   82.00  15.00 150.00   52
 16  \w     46.00  71.00   0.50    0.10    --   85.25 -85.00 158.10   50
 17  \w     39.00  64.00   0.50    0.10    --   85.25-120.00 109.24   50
 18  \w     40.00  65.00   0.50    0.10    --   85.25-136.00  26.86   50
 19  \w     40.00  65.00   0.50    0.10    --   85.25-123.00   0.02   50
 20  \w     73.00 100.00   0.50    0.10    --   85.25-123.00   0.02   54
 21  \w     39.00  98.00   0.50    0.10    --   85.25-117.00  65.44  118
 22  \w     42.00  81.00   0.50    0.10    --   85.25-113.00 -92.29   78
 23  \w     39.00 101.00   0.50    0.10    --   85.25-128.00-119.37  124
 24  \w     44.00  97.00   0.50    0.10    --   85.25-114.00-150.30  106
 25  \w     47.00  73.00   0.50    0.10    --   85.25-117.00-134.38   52
 26  \w     37.00  62.00   0.50    0.10    --   82.00-111.00 -30.00   50
 27  \w     37.00  62.00   0.50    0.10    --   82.00-111.00-180.00   50
 28  \w     68.00  93.00   0.50    0.10    --   82.00-111.00   0.00   50
 29  \w     50.00  78.00   0.50    0.10    --   82.00-111.00  30.00   56
 30  \w     37.00  62.00   0.50    0.10    --   82.00-111.00 120.00   50
 31  \w     57.00  93.00   0.50    0.10    --   82.00-111.00 150.00   72
 32  \w     37.00  62.00   0.50    0.10    --   82.00-108.00 140.00   50
 33  \w     32.00  57.00   0.50    0.10    --   70.97-108.00 140.00   50
 34  \w     19.00  44.00   0.50    0.10    --   57.59-108.00 140.00   50
 35  \w     42.00  93.00   0.50    0.10    --   85.25 -97.00  68.46  102
 36  \w     43.00  92.00   0.50    0.10    --   85.25 -96.00  -2.45   98
 37  \w     16.00  44.00   0.50    0.10    --   57.59 -95.00 -30.00   56
 38  \w     68.00  93.00   0.50    0.10    --   82.00-111.00 -90.00   50
 39  \w     40.00  92.00   0.50    0.10    --   85.25-109.00-112.33  104
 40  \w     42.00  93.00   0.50    0.10    --   85.25-102.00 -71.96  102
 41  \w     40.00  90.00   0.50    0.10    --   82.00 -95.00 -60.00  100
 42  \w     39.00  64.00   0.50    0.10    --   82.00 -95.00  30.00   50
 43  \w     47.00  92.00   0.50    0.10    --   85.25 -96.00  91.08   90
 44  \w     40.00  86.00   0.50    0.10    --   82.00 -95.00 150.00   92
 45  \w     39.00  65.00   0.50    0.10    --   82.00 -95.00 120.00   52
 46  \w     49.00  82.00   0.50    0.10    --   85.25 -88.00  91.33   66
 47  \w     15.00  55.00   0.50    0.10    --   57.59 -95.00  60.00   80
 48  \w     24.00  65.00   0.50    0.10    --   57.59 -95.00-150.00   82
 49  \w     39.00  65.00   0.50    0.10    --   82.00 -95.00 -90.00   52
 50  \w     41.00  69.00   0.50    0.10    --   82.00 -72.00 -51.30   56
 51  \w     45.00  70.00   0.50    0.10    --   85.25 -76.00 -71.33   50
 52  \w    106.00 131.00   0.50    0.10    --   85.25 125.00  47.31   50
 53  \w     46.00  71.00   0.50    0.10    --   85.25 -78.00  42.86   50
 54  \w   -107.00 -65.00   0.50    0.10    --  -58.57 -15.00 -30.00   84
 55  \w    -56.00 -31.00   0.50    0.10    --  -58.57 -15.00 -30.00   50
 56  \w   -123.00 -37.00   0.50    0.10    --  -72.73 -15.00  60.00  172
 57  \w   -125.00 -39.00   0.50    0.10    --  -74.54 -15.00 150.00  172
 58  \w    -92.00 -66.00   0.50    0.10    --  -79.50 102.00 -18.39   52
 59  \w    -58.00 -33.00   0.50    0.10    --  -79.50 115.00  41.04   50
 60  \w    -64.00 -38.00   0.50    0.10    --  -72.73 125.00   0.00   52
 61  \w    -97.00 -72.00   0.50    0.10    --  -79.50 115.00  80.93   50
 62  \w    -97.00 -64.00   0.50    0.10    --  -79.50 115.00  41.04   66
 63  \w    -97.00 -72.00   0.50    0.10    --  -78.00 114.00 176.71   50
 64  \w    -64.00 -37.00   0.50    0.10    --  -79.50 115.00 -53.50   54
 65  \w    -63.00 -37.00   0.50    0.10    --  -72.73 108.00-121.00   52
 66  \w    -97.00 -66.00   0.50    0.10    --  -79.50 117.00-175.77   62
 67  \w    -97.00 -45.00   0.50    0.10    --  -78.00 114.00-154.62  104
 68  \w    -84.00 -59.00   0.50    0.10    --  -74.54 108.00-121.00   50
 69  \w    -67.00 -14.00   0.50    0.10    --  -58.57 108.00-121.00  106
 70  \w    -97.00 -71.00   0.50    0.10    --  -79.50 115.00 -53.50   52
 71  \w    -97.00 -32.00   0.50    0.10    --  -78.00 114.00 104.06  130
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0357034000
_diffrn_orient_matrix_UB_12      -0.0025274000
_diffrn_orient_matrix_UB_13      0.0612734000
_diffrn_orient_matrix_UB_21      0.0296200000
_diffrn_orient_matrix_UB_22      0.0925381000
_diffrn_orient_matrix_UB_23      0.0101044000
_diffrn_orient_matrix_UB_31      -0.1128352000
_diffrn_orient_matrix_UB_32      -0.0039220000
_diffrn_orient_matrix_UB_33      0.0151496000
_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  0.0243
_diffrn_reflns_av_unetI/netI     0.0189
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            113760
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.622
_diffrn_reflns_theta_min         3.408
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.155
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69799
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.100a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_description       block
_exptl_crystal_F_000             2062
_exptl_crystal_preparation
'SolidPhaseSynthesis (SPS) and solution phase coupling'
_exptl_crystal_recrystallization_method
'Liquid-liquid diffusion CHCl3 - MeCN in NMR tube'
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.21
_refine_diff_density_max         2.918
_refine_diff_density_min         -1.534
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1335
_refine_ls_number_reflns         21386
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0864
_refine_ls_R_factor_gt           0.0806
_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^)+(0.1312P)^2^+7.1535P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2309
_refine_ls_wR_factor_ref         0.2368
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18896
_reflns_number_total             21386
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc07336c2.cif
_cod_data_source_block           sw_emnd_auto
_cod_depositor_comments
'Adding full bibliography for 1573400--1573401.cif.'
_cod_database_code               1573401
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C102 H92 N16 O18'
_chemical_oxdiff_usercomment     '400um big yellow block DCM MeCN'
_shelx_estimated_absorpt_t_max   0.794
_shelx_estimated_absorpt_t_min   0.643
_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 C(H,H,H) groups
2. Restrained distances
 Cl-C03Y = Cl1-C03Y
 1.77 with sigma of 0.02
3. Others
 Sof(O00M)=Sof(C03P)=Sof(H03Y)=Sof(H)=Sof(C03S)=Sof(H03)=Sof(H2)=Sof(HI)=
 Sof(HJ)=Sof(C040)=Sof(H04A)=Sof(H04B)=Sof(H04C)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C02Z(H02Z), C038(H038), C03R(H03Z)
4.b Secondary CH2 refined with riding coordinates:
 C02V(H02A,H02E), C039(H03A,H03B), C03O(H03W,H03X), C03P(H03Y,H), C03Y(H7,HK)
4.c Aromatic/amide H refined with riding coordinates:
 N00K(H00K), N00L(H00L), N00P(H00P), N00Q(H00Q), N00T(H00T), N00V(H00V),
 N00Z(H00Z), C019(H019), C01F(H01F), C021(H021), C022(H022), C026(H026),
 C028(H028), C02B(H02B), C02C(H02C), C02D(H02D), C02J(H02J), C02L(H02L),
 C02M(H02M), C02N(H02N), C02O(H02O), C02P(H02P), C02Q(H02Q), C02R(H02R),
 C02S(H02S), C02W(H02W), C02X(H02X), C02Y(H02Y), C030(H030), C031(H031),
 C032(H032), C033(H033), C035(H035), C036(H036), C037(H037), C03A(H03C),
 C03C(H03D), C03D(H03E), C03F(H03F), C03J(H03J)
4.d Idealised Me refined as rotating group:
 C03I(H03G,H03H,H03I), C03K(H03K,H03L,H03M), C03L(H03N,H03O,H03P), C03M(H03Q,
 H03R,H03S), C03N(H03T,H03U,H03V), C03Q(H4,HA,HB), C03T(H1,HC,HD), C03U(H5,HE,
 HF), C03V(H6,HG,HH), C03Z(H3,HL,HM), C048(H04D,H04E,H04F)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              32775
_shelx_hkl_checksum              73571
_shelx_fab_checksum              35248
_olex2_exptl_crystal_mounting_method 'nylon loop immersion oil'
_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 1.587
_oxdiff_exptl_absorpt_empirical_full_min 0.556