Switchable foldamer ion channels with antibacterial activity
Peters, Anna D.; Borsley, Stefan; della Sala, Flavio; Cairns-Gibson, Dominic F.; Leonidou, Marios; Clayden, Jonathan; Whitehead, George F. S.; Vitorica-Yrzebal, Inigo; Takano, Eriko; Burthem, John; Cockroft, Scott Lee; Webb, Simon; Chemical Science  (2020) –; doi:10.1039/D0SC02393K

data_1558183
_publ_section_title
;
 Switchable foldamer ion channels with antibacterial activity
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D0SC02393K
_journal_year                    2020
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C52 H83 Cl Cu N13 O9 Si, C H O3'
_chemical_formula_sum            'C53 H84 Cl Cu N13 O12 Si'
_chemical_formula_weight         1222.41
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-11-20
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-04-27 deposited with the CCDC.	2020-06-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.1099(2)
_cell_length_b                   24.1351(9)
_cell_length_c                   34.1137(11)
_cell_measurement_reflns_used    5809
_cell_measurement_temperature    150.00(2)
_cell_measurement_theta_max      58.1550
_cell_measurement_theta_min      2.2200
_cell_volume                     7500.5(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_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_temperature      150.00(2)
_diffrn_detector                 'CCD plate'
_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    -56.00  38.00   1.00    4.00    --  -45.10  57.00-120.00   94
  2  \w   -121.00 -16.00   1.00    4.00    --  -45.10 -50.00  30.51  105
  3  \w    -27.00   0.00   1.00    4.00    --  -45.10  51.00  16.00   27
  4  \w    -77.00 -50.00   1.00    4.00    --  -45.10  51.00  16.00   27
  5  \w   -112.00 -18.00   1.00    4.00    --  -45.10 -66.00 140.51   94
  6  \w   -113.00 -80.00   1.00   25.00    -- -107.20  76.00  30.00   33
  7  \w   -169.00 -19.00   1.00   25.00    -- -107.20 -19.00 -90.00  150
  8  \w   -155.00 -90.00   1.00   25.00    -- -107.20 -57.00 -60.00   65
  9  \w    -83.00 -57.00   1.00   25.00    -- -107.20  76.00 -90.00   26
 10  \w   -118.00 -93.00   1.00   25.00    -- -107.20  57.00 -60.00   25
 11  \w    -57.00 -19.00   1.00   25.00    -- -107.20  57.00 -90.00   38
 12  \w   -146.00 -33.00   1.00   25.00    -- -107.20  76.00 120.00  113
 13  \w   -120.00 -87.00   1.00   25.00    -- -107.20  76.00  90.00   33
 14  \w    -83.00 -56.00   1.00   25.00    -- -107.20  76.00  90.00   27
 15  \w   -105.00 -70.00   1.00   25.00    -- -107.20  76.00-150.00   35
 16  \w    -58.00 -31.00   1.00   25.00    -- -107.20  76.00-150.00   27
 17  \w   -131.00 -93.00   1.00   25.00    -- -107.20  57.00 -90.00   38
 18  \w    -45.00 -18.00   1.00   25.00    -- -107.20  76.00  30.00   27
 19  \w    -52.00 -18.00   1.00   25.00    -- -107.20  76.00  60.00   34
 20  \w   -122.00 -97.00   1.00   25.00    -- -107.20  76.00  60.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0000301000
_diffrn_orient_matrix_UB_12      -0.0636895000
_diffrn_orient_matrix_UB_13      -0.0030405000
_diffrn_orient_matrix_UB_21      -0.1686316000
_diffrn_orient_matrix_UB_22      -0.0003264000
_diffrn_orient_matrix_UB_23      0.0036508000
_diffrn_orient_matrix_UB_31      -0.0136332000
_diffrn_orient_matrix_UB_32      0.0043148000
_diffrn_orient_matrix_UB_33      -0.0448849000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1119
_diffrn_reflns_av_unetI/netI     0.0849
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            40375
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        58.922
_diffrn_reflns_theta_max         58.922
_diffrn_reflns_theta_min         2.242
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.354
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51259
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.30c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.083
_exptl_crystal_description       needle
_exptl_crystal_F_000             2596
_exptl_crystal_size_max          0.329
_exptl_crystal_size_mid          0.014
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.345
_refine_diff_density_min         -0.497
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details
;
 Flack x determined using 2213 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.04(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     785
_refine_ls_number_reflns         10629
_refine_ls_number_restraints     253
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.1081
_refine_ls_R_factor_gt           0.0715
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1002P)^2^+2.1138P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1715
_refine_ls_wR_factor_ref         0.1949
_reflns_Friedel_coverage         0.769
_reflns_Friedel_fraction_full    0.972
_reflns_Friedel_fraction_max     0.972
_reflns_number_gt                7251
_reflns_number_total             10629
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc02393k2.cif
_cod_data_source_block           s5009r
_cod_original_cell_volume        7500.6(4)
_cod_database_code               1558183
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N O'
_shelx_estimated_absorpt_t_max   0.987
_shelx_estimated_absorpt_t_min   0.664
_reflns_odcompleteness_completeness 79.05
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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, All O(H) groups
2. Restrained distances
 O0A-C2A = O2-C2A = O1A-C2A
 1.28 with sigma of 0.01
 Si2-C52A \\sim Si2-C51 \\sim Si1-C50A \\sim Si1-C49 \\sim Si1-C50 \\sim
Si1-C52 \\sim Si2-C51A
 with sigma of 0.02
 C52-C50 \\sim C51A-C51 \\sim C50A-C50 \\sim C51-C52A \\sim C51A-C52A \\sim
C52-C50A
 with sigma of 0.02
 O48-C48 \\sim O48-C48A
 with sigma of 0.02
 C49-C48 \\sim C49A-C48A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Si1 \\sim Si2 \\sim C50A \\sim C51 \\sim C52A \\sim C50 \\sim C49 \\sim C52
\\sim C49A \\sim C51A \\sim C48 \\sim C48A \\sim O48: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 Si1, Si2, C50A, C51, C52A, C50, C49, C52, C49A, C51A, C48, C48A, O48
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C48A)=Sof(H48A)=Sof(H48B)=Sof(Si2)=Sof(C51)=Sof(H51A)=Sof(H51B)=Sof(H51C)=
 Sof(C52A)=Sof(H52A)=Sof(H52B)=Sof(H52C)=Sof(C49A)=Sof(H49C)=Sof(H49D)=
 Sof(C51A)=Sof(H51D)=Sof(H51E)=Sof(H51F)=1-FVAR(1)
 Sof(Si1)=Sof(C50A)=Sof(H50A)=Sof(H50B)=Sof(H50C)=Sof(C50)=Sof(H50D)=Sof(H50E)=
 Sof(H50F)=Sof(C49)=Sof(H49A)=Sof(H49B)=Sof(C52)=Sof(H52D)=Sof(H52E)=Sof(H52F)=
 Sof(C48)=Sof(H48C)=Sof(H48D)=FVAR(1)
6.a Riding coordinates:
 N10(H10), O1A(H1A)
6.b Secondary CH2 refined with riding coordinates:
 C48A(H48A,H48B), C12(H12A,H12B), C13(H13A,H13B), C6(H6A,H6B), C49(H49A,H49B),
 C49A(H49C,H49D), C48(H48C,H48D)
6.c Me refined with riding coordinates:
 C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C42(H42A,H42B,H42C), C41(H41A,H41B,
 H41C), C38(H38A,H38B,H38C), C37(H37A,H37B,H37C), C34(H34A,H34B,H34C), C33(H33A,
 H33B,H33C), C30(H30A,H30B,H30C), C29(H29A,H29B,H29C), C26(H26A,H26B,H26C),
 C25(H25A,H25B,H25C), C22(H22A,H22B,H22C), C21(H21A,H21B,H21C), C17(H17A,H17B,
 H17C), C18(H18A,H18B,H18C), C50A(H50A,H50B,H50C), C51(H51A,H51B,H51C),
 C52A(H52A,H52B,H52C), C50(H50D,H50E,H50F), C52(H52D,H52E,H52F), C51A(H51D,H51E,
 H51F)
6.d Aromatic/amide H refined with riding coordinates:
 N7(H7), N8(H8), N9(H9), N11(H11), N12(H12), N13(H13), C7(H7A), C8(H8A),
 C9(H9A), C10(H10A), C1(H1), C2(H2), C3(H3), C4(H4), C15(H15)
;
_shelx_res_checksum              29556
_shelx_fab_checksum              56262
_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 2.516
_oxdiff_exptl_absorpt_empirical_full_min 0.462