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_1558181
_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_formula_moiety         'C52 H83 Cl2 Cu N13 O9 Si, Cl'
_chemical_formula_sum            'C52 H83 Cl2 Cu N13 O9 Si'
_chemical_formula_weight         1196.84
_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   geom
_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                98.168(5)
_cell_angle_beta                 91.134(5)
_cell_angle_gamma                103.075(5)
_cell_formula_units_Z            2
_cell_length_a                   8.9253(5)
_cell_length_b                   15.5724(9)
_cell_length_c                   25.2322(14)
_cell_measurement_reflns_used    6229
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      44.3470
_cell_measurement_theta_min      1.7720
_cell_volume                     3376.5(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.99(10)
_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    -52.00  -4.00   1.00   10.00    --  -43.90 -38.00 120.00   48
  2  \w    -84.00 -45.00   1.00   10.00    --  -43.90  76.00  30.00   39
  3  \w    -17.00  14.00   1.00   10.00    --  -43.90  76.00  30.00   31
  4  \w   -122.00 -71.00   1.00   10.00    --  -43.90 -76.00  30.00   51
  5  \w    -66.00 -10.00   1.00   10.00    --  -43.90 -76.00  30.00   56
  6  \w   -121.00 -20.00   1.00   10.00    --  -43.90 -76.00 -90.00  101
  7  \w    -84.00  -1.00   1.00   10.00    --  -43.90  76.00-120.00   83
  8  \w   -130.00  -4.00   1.00   10.00    --  -43.90 -76.00 120.00  126
  9  \w    -81.00   2.00   1.00   10.00    --  -43.90  76.00 120.00   83
 10  \w   -128.00 -88.00   1.00   10.00    --  -43.90 -76.00-180.00   40
 11  \w    -77.00 -10.00   1.00   10.00    --  -43.90 -76.00-180.00   67
 12  \w    -77.00  20.00   1.00   10.00    --  -43.90  57.00-120.00   97
 13  \w   -133.00  -5.00   1.00   10.00    --  -43.90 -38.00 -30.00  128
 14  \w    -72.00  24.00   1.00   10.00    --  -43.90  57.00  90.00   96
 15  \w    -84.00  37.00   1.00   10.00    --  -43.90  76.00 -30.00  121
 16  \w   -107.00  -5.00   1.00   10.00    --  -43.90 -76.00 -60.00  102
 17  \w   -133.00 -71.00   1.00   10.00    --  -43.90 -38.00 120.00   62
;
_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      0.1123232000
_diffrn_orient_matrix_UB_12      0.0284858000
_diffrn_orient_matrix_UB_13      0.0498338000
_diffrn_orient_matrix_UB_21      0.0702037000
_diffrn_orient_matrix_UB_22      0.0883954000
_diffrn_orient_matrix_UB_23      -0.0203199000
_diffrn_orient_matrix_UB_31      -0.1180929000
_diffrn_orient_matrix_UB_32      0.0439167000
_diffrn_orient_matrix_UB_33      0.0303202000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0689
_diffrn_reflns_av_unetI/netI     0.0684
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            23647
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        44.703
_diffrn_reflns_theta_max         44.703
_diffrn_reflns_theta_min         1.771
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    1.815
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66996
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.177
_exptl_crystal_description       block
_exptl_crystal_F_000             1270
_exptl_crystal_size_max          0.093
_exptl_crystal_size_mid          0.046
_exptl_crystal_size_min          0.013
_refine_diff_density_max         0.717
_refine_diff_density_min         -0.369
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     663
_refine_ls_number_reflns         5344
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0924
_refine_ls_R_factor_gt           0.0716
_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^)+(0.1303P)^2^+3.5044P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2020
_refine_ls_wR_factor_ref         0.2197
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3936
_reflns_number_total             5344
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc02393k2.cif
_cod_data_source_block           s5222r
_cod_database_code               1558181
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.981
_shelx_estimated_absorpt_t_min   0.877
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     44.45
_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.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C7(H7A,H7B), C6(H6A,H6B), C48(H48A,H48B), C49(H49A,H49B)
2.b Aromatic/amide H refined with riding coordinates:
 N12(H12), N7(H7), N13(H13), N11(H11), N8(H8), N10(H10), N9(H9), C15(H15),
 C12(H12A), C2(H2), C11(H11A), C9(H9A), C1(H1), C10(H10A), C4(H4), C3(H3)
2.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C46(H46A,H46B,H46C), C42(H42A,H42B,
 H42C), C41(H41A,H41B,H41C), C22(H22A,H22B,H22C), C45(H45A,H45B,H45C), C21(H21A,
 H21B,H21C), C34(H34A,H34B,H34C), C25(H25A,H25B,H25C), C38(H38A,H38B,H38C),
 C37(H37A,H37B,H37C), C30(H30A,H30B,H30C), C26(H26A,H26B,H26C), C33(H33A,H33B,
 H33C), C29(H29A,H29B,H29C), C51(H51A,H51B,H51C), C50(H50A,H50B,H50C), C52(H52A,
 H52B,H52C)
;
_shelx_res_checksum              79791
_shelx_fab_checksum              10538
_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 1.557
_oxdiff_exptl_absorpt_empirical_full_min 0.717