Di-anionic self-associating supramolecular amphiphiles (SSAs) as antimicrobial agents against MRSA and <i>Escherichia coli</i>.
White, Lisa J.; Boles, Jessica E.; Clifford, Melanie; Patenall, Bethany L.; Hilton, Kira H. L. F.; Ng, Kendrick K. L.; Ellaby, Rebecca J.; Hind, Charlotte K.; Mulvihill, Daniel P.; Hiscock, Jennifer R.; Chemical communications (Cambridge, England)  (2021) –; doi:10.1039/d1cc05455d

data_7129148
_publ_section_title
;
 Di-anionic self-associating supramolecular amphiphiles (SSAs) as
 antimicrobial agents against MRSA and <i>Escherichia coli</i>.
;
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_paper_doi               10.1039/d1cc05455d
_journal_year                    2021
_chemical_formula_moiety         'C16 H24 N4 O8 S2, 1.252(H2 O), 2(C16 H36 N)'
_chemical_formula_sum            'C48 H98.72 N6 O9.24 S2'
_chemical_formula_weight         972.00
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2020-08-04
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2020-08-04 deposited with the CCDC.	2021-10-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.294(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.7250(3)
_cell_length_b                   35.2054(13)
_cell_length_c                   16.1782(6)
_cell_measurement_reflns_used    4634
_cell_measurement_temperature    99.98(11)
_cell_measurement_theta_max      70.2680
_cell_measurement_theta_min      4.6200
_cell_volume                     5537.6(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (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 2013/4 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.98(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2887
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.970
_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    -63.00  31.00   1.00   10.00    --  -42.16  57.00 -30.00   94
  2  \w   -116.00 -70.00   1.00   10.00    --  -42.16 -38.00-180.00   46
  3  \w    -50.00 -23.00   1.00   10.00    --  -42.16 -38.00-180.00   27
  4  \w     25.00  90.00   1.00   10.00    --   42.16  38.00  60.00   65
  5  \w     31.00 107.00   1.00   22.50    --  102.14-125.00 -60.00   76
  6  \w     38.00 101.00   1.00   22.50    --  102.14-125.00  30.00   63
  7  \w     33.00 112.00   1.00   22.50    --  102.14 -45.00 120.00   79
  8  \w     23.00  55.00   1.00   22.50    --  102.14 -94.00 -30.00   32
  9  \w     99.00 168.00   1.00   22.50    --  102.14  30.00-150.00   69
 10  \w    118.00 168.00   1.00   22.50    --  102.14 125.00-180.00   50
 11  \w     66.00 131.00   1.00   22.50    --  102.14 -61.00  30.00   65
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0744327000
_diffrn_orient_matrix_UB_12      -0.0364529000
_diffrn_orient_matrix_UB_13      -0.0288546000
_diffrn_orient_matrix_UB_21      -0.1398968000
_diffrn_orient_matrix_UB_22      0.0194806000
_diffrn_orient_matrix_UB_23      0.0124435000
_diffrn_orient_matrix_UB_31      0.0005318000
_diffrn_orient_matrix_UB_32      0.0143999000
_diffrn_orient_matrix_UB_33      -0.0898894000
_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  0.0484
_diffrn_reflns_av_unetI/netI     0.0677
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22649
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.325
_diffrn_reflns_theta_min         3.711
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.312
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.487
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
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    1.166
_exptl_crystal_description       plate
_exptl_crystal_F_000             2139
_exptl_crystal_size_max          0.265
_exptl_crystal_size_mid          0.125
_exptl_crystal_size_min          0.013
_refine_diff_density_max         1.002
_refine_diff_density_min         -0.512
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     645
_refine_ls_number_reflns         10422
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0875
_refine_ls_R_factor_gt           0.0583
_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^)+(0.0722P)^2^+2.6877P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1424
_refine_ls_wR_factor_ref         0.1615
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7447
_reflns_number_total             10422
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc05455d2.cif
_cod_data_source_block           jrh20200013b_res
_cod_database_code               7129148
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         S2C20H20N2O4
_chemical_oxdiff_usercomment     'lisa 2-69 100 k second collection'
_reflns_odcompleteness_completeness 99.54
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Others
 Sof(H29C)=Sof(H29D)=Sof(C30B)=Sof(H30C)=Sof(H30D)=1-FVAR(1)
 Sof(H29A)=Sof(H29B)=Sof(C30A)=Sof(H30A)=Sof(H30B)=FVAR(1)
 Sof(C31B)=Sof(H31C)=Sof(H31D)=1-FVAR(2)
 Sof(C31A)=Sof(H31A)=Sof(H31B)=FVAR(2)
 Sof(C32B)=Sof(H32D)=Sof(H32E)=Sof(H32F)=1-FVAR(3)
 Sof(C32A)=Sof(H32A)=Sof(H32B)=Sof(H32C)=FVAR(3)
 Sof(O10)=Sof(H10A)=Sof(H10B)=FVAR(4)
3.a Free rotating group:
 O9(H9A,H9B), O10(H10A,H10B)
3.b Secondary CH2 refined with riding coordinates:
 C42(H42A,H42B), C37(H37A,H37B), C20(H20A,H20B), C41(H41A,H41B), C38(H38A,
 H38B), C33(H33A,H33B), C39(H39A,H39B), C45(H45A,H45B), C1(H1A,H1B), C43(H43A,
 H43B), C16(H16A,H16B), C46(H46A,H46B), C21(H21A,H21B), C34(H34A,H34B),
 C47(H47A,H47B), C25(H25A,H25B), C22(H22A,H22B), C35(H35A,H35B), C19(H19A,H19B),
  C29(H29A,H29B), C29(H29C,H29D), C26(H26A,H26B), C23(H23A,H23B), C18(H18A,
 H18B), C27(H27A,H27B), C30A(H30A,H30B), C31A(H31A,H31B), C30B(H30C,H30D),
 C31B(H31C,H31D)
3.c Aromatic/amide H refined with riding coordinates:
 N2(H2), N3(H3), N4(H4), N1(H1), C11(H11), C7(H7), C9(H9), C8(H8)
3.d Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C), C5(H5A,H5B,H5C), C14(H14A,H14B,H14C), C13(H13A,H13B,
 H13C), C4(H4A,H4B,H4C), C36(H36A,H36B,H36C), C48(H48A,H48B,H48C), C24(H24A,
 H24B,H24C), C44(H44A,H44B,H44C), C28(H28A,H28B,H28C), C17(H17A,H17B,H17C),
 C32A(H32A,H32B,H32C), C32B(H32D,H32E,H32F)
;
_shelx_res_checksum              99419
_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 1.197
_oxdiff_exptl_absorpt_empirical_full_min 0.796