Liposomal formulation of a gold(III) metalloantibiotic: a promising strategy against antimicrobial resistance.
Llamedo, Alejandro; Rodríguez, Pablo; Gabasa, Yaiza; Soengas, Raquel G.; Rodríguez-Solla, Humberto; Elorriaga, David; García-Alonso, Francisco J; Soto, Sara M.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 15205–15214; doi:10.1039/d4dt01867b

data_7716896
_publ_section_title
;
 Liposomal formulation of a gold(III) metalloantibiotic: a promising
 strategy against antimicrobial resistance.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15205
_journal_page_last               15214
_journal_paper_doi               10.1039/d4dt01867b
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         '2(C28 H35 Au N4 P S3), 2(F6 P), C H Cl3'
_chemical_formula_sum            'C57 H71 Au2 Cl3 F12 N8 P4 S6'
_chemical_formula_weight         1912.74
_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             2024-06-10
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-06-11 deposited with the CCDC.	2024-08-26 downloaded from the CCDC.
;
_cell_angle_alpha                95.849(2)
_cell_angle_beta                 98.779(2)
_cell_angle_gamma                102.500(2)
_cell_formula_units_Z            2
_cell_length_a                   11.5343(3)
_cell_length_b                   15.5640(3)
_cell_length_c                   21.2129(5)
_cell_measurement_reflns_used    20747
_cell_measurement_temperature    273
_cell_measurement_theta_max      69.3500
_cell_measurement_theta_min      3.9890
_cell_volume                     3638.20(15)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      273
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.2640
_diffrn_detector_type            Onyx
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.984
_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   -121.00 -11.00   1.00    7.50    --  -43.48 -19.00-150.00  110
  2  \w    -27.00  -2.00   1.00    7.50    --  -43.48 125.00 -90.00   25
  3  \w    -68.00  27.00   1.00    7.50    --  -43.48  37.00  30.00   95
  4  \w     11.00  92.00   1.00    7.50    --   43.48-125.00-180.00   81
  5  \w     12.00  77.00   1.00   45.00    --   94.50 -94.00  30.00   65
  6  \w     31.00  57.00   1.00   45.00    --   94.50 -61.00 120.00   26
  7  \w     12.00 100.00   1.00   45.00    --   94.50 -94.00 -90.00   88
  8  \w     73.00 121.00   1.00   45.00    --   94.50 -30.00  30.00   48
  9  \w    119.00 168.00   1.00   45.00    --   94.50  30.00-150.00   49
 10  \w     17.00  70.00   1.00   45.00    --   94.50 -94.00  90.00   53
 11  \w     12.00 108.00   1.00   45.00    --   94.50 -94.00 120.00   96
 12  \w     21.00  46.00   1.00   45.00    --   94.50-125.00  30.00   25
 13  \w     63.00 119.00   1.00   45.00    --   94.50-125.00  30.00   56
 14  \w     44.00  70.00   1.00   45.00    --   94.50-125.00 -90.00   26
 15  \w     18.00 107.00   1.00   45.00    --   94.50 -94.00  60.00   89
 16  \w     88.00 114.00   1.00   45.00    --   94.50  30.00-150.00   26
 17  \w     16.00 112.00   1.00   45.00    --   94.50 -15.00-150.00   96
 18  \w     66.00 163.00   1.00   45.00    --   94.50  77.00 -30.00   97
 19  \w     81.00 120.00   1.00   45.00    --   94.50-125.00 -90.00   39
 20  \w     68.00 107.00   1.00   45.00    --   94.50  61.00-180.00   39
 21  \w     71.00 114.00   1.00   45.00    --   94.50 -61.00 120.00   43
 22  \w    132.00 158.00   1.00   45.00    --   94.50  30.00 120.00   26
 23  \w     40.00  83.00   1.00   45.00    --   94.50 -45.00-120.00   43
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Onyx, Nova'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1278807000
_diffrn_orient_matrix_UB_12      -0.0062551000
_diffrn_orient_matrix_UB_13      -0.0094257000
_diffrn_orient_matrix_UB_21      0.0541825000
_diffrn_orient_matrix_UB_22      0.0663879000
_diffrn_orient_matrix_UB_23      0.0618472000
_diffrn_orient_matrix_UB_31      -0.0072467000
_diffrn_orient_matrix_UB_32      -0.0777023000
_diffrn_orient_matrix_UB_33      0.0399229000
_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  0.0338
_diffrn_reflns_av_unetI/netI     0.0353
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            34851
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.552
_diffrn_reflns_theta_min         2.937
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Nova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.566
_exptl_absorpt_correction_T_max  0.458
_exptl_absorpt_correction_T_min  0.253
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.746
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1884
_exptl_crystal_size_max          0.219
_exptl_crystal_size_mid          0.154
_exptl_crystal_size_min          0.099
_refine_diff_density_max         0.679
_refine_diff_density_min         -1.193
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1024
_refine_ls_number_reflns         13442
_refine_ls_number_restraints     921
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0385
_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^)+(0.0581P)^2^+2.7507P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1007
_refine_ls_wR_factor_ref         0.1067
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11592
_reflns_number_total             13442
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01867b2.cif
_cod_data_source_block           23025_rs804
_cod_depositor_comments          'Adding full bibliography for 7716896.cif.'
_cod_database_code               7716896
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         C41H50N3OAuPS3
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.79
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 P4A-F11A = P4A-F12A = P4A-F13A = P4A-F14A = P4A-F15 = P4A-F16A
 1.57 with sigma of 0.02
 P4-F11 = P4-F12 = P4-F13 = P4-F14 = P4-F15 = P4-F16
 1.57 with sigma of 0.02
 P3-F1 = P3-F2 = P3-F3 = P3-F4 = P3-F5 = P3-F6
 1.57 with sigma of 0.02
 P3A-F1A = P3A-F2A = P3A-F3A = P3A-F4A = P3A-F5A = P3A-F6A
 1.57 with sigma of 0.02
 F11A-F12A = F11A-F13A = F11A-F14A = F11A-F15A
 2.22 with sigma of 0.04
 F16A-F12A = F16A-F13A = F16A-F14A = F16A-F15A
 2.22 with sigma of 0.04
 F11-F12 = F11-F13 = F11-F14 = F11-F15
 2.22 with sigma of 0.04
 F16-F12 = F16-F13 = F16-F14 = F16-F15
 2.22 with sigma of 0.04
 F1A-F2A = F1A-F3A = F1A-F4A = F1A-F5A
 2.22 with sigma of 0.04
 F1-F2 = F1-F3 = F1-F4 = F1-F5
 2.22 with sigma of 0.04
 F6A-F2A = F6A-F3A = F6A-F4A = F6A-F5A
 2.22 with sigma of 0.04
 F2A-F3A = F3A-F4A = F4A-F5A = F5A-F2A
 2.22 with sigma of 0.04
 F6-F2 = F6-F3 = F6-F4 = F6-F5
 2.22 with sigma of 0.04
 F2-F3 = F3-F4 = F4-F5 = F5-F2
 2.22 with sigma of 0.04
 N7-C52 \\sim N7-C52A \\sim N3-C24 \\sim N3-C24A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C24 \\sim C24A \\sim C25 \\sim N4A \\sim C26 \\sim C26A \\sim C27 \\sim C27A
\\sim C28 \\sim C28A \\sim N4 \\sim C25A: within 2A with sigma of 0.001 and
sigma for terminal atoms of 0.002 within 2A
C52 \\sim C52A \\sim C53 \\sim N8A \\sim C54 \\sim C56A \\sim C55 \\sim C55A
\\sim C56 \\sim C54A \\sim N8 \\sim C53A: within 2A with sigma of 0.001 and
sigma for terminal atoms of 0.002 within 2A
P4 \\sim P4A \\sim F11 \\sim F11A \\sim F12 \\sim F12A \\sim F13 \\sim F13A
\\sim F14 \\sim F14A \\sim F15A \\sim F15 \\sim F16 \\sim F16A: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
P3 \\sim P3A \\sim F1 \\sim F1A \\sim F2 \\sim F2A \\sim F3 \\sim F3A \\sim F4
\\sim F4A \\sim F5 \\sim F5A \\sim F6 \\sim F6A: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 2A
4. Others
 Sof(F15A)=Sof(P3A)=Sof(F6A)=Sof(F4A)=Sof(F3A)=Sof(F5A)=Sof(F1A)=Sof(F2A)=
 Sof(F11A)=Sof(F12A)=Sof(F13A)=Sof(F14A)=Sof(F16A)=Sof(P4A)=Sof(C52A)=Sof(N8A)=
 Sof(C56A)=Sof(H56A)=Sof(C55A)=Sof(H55A)=Sof(C54A)=Sof(H54A)=Sof(C53A)=
 Sof(H53A)=Sof(C24A)=Sof(C25A)=Sof(H25A)=Sof(C26A)=Sof(H26A)=Sof(C27A)=
 Sof(H27A)=Sof(C28A)=Sof(H28A)=Sof(N4A)=1-FVAR(1)
 Sof(P4)=Sof(P3)=Sof(F13)=Sof(C52)=Sof(C53)=Sof(H53)=Sof(C54)=Sof(H54)=
 Sof(C55)=Sof(H55)=Sof(C56)=Sof(H56)=Sof(N8)=Sof(F2)=Sof(F3)=Sof(F5)=Sof(F12)=
 Sof(F16)=Sof(F4)=Sof(F1)=Sof(F6)=Sof(F11)=Sof(F14)=Sof(F15)=Sof(C24)=Sof(N4)=
 Sof(C28)=Sof(H28)=Sof(C27)=Sof(H27)=Sof(C26)=Sof(H26)=Sof(C25)=Sof(H25)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C35(H35), C38(H38), C57(H57)
5.b Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C23(H23A,H23B), C22(H22A,H22B), C21(H21A,H21B), C51(H51A,
 H51B), C48(H48A,H48B), C49(H49A,H49B), C50(H50A,H50B)
5.c Aromatic/amide H refined with riding coordinates:
 C14(H14), C17(H17), C42(H42), C45(H45), C15(H15), C16(H16), C44(H44),
 C43(H43), C34(H34), C6(H6), C2(H2), C30(H30), C33(H33), C5(H5), C53(H53),
 C54(H54), C55(H55), C56(H56), C4(H4), C3(H3), C32(H32), C31(H31), C28(H28),
 C27(H27), C26(H26), C25(H25), C56A(H56A), C55A(H55A), C54A(H54A), C53A(H53A),
 C25A(H25A), C26A(H26A), C27A(H27A), C28A(H28A)
5.d Fitted hexagon refined as free rotating group:
 C52(C53,C54,C55,C56,N8), C24(N4,C28,C27,C26,C25), C52A(N8A,C56A,C55A,C54A,
 C53A), C24A(C25A,C26A,C27A,C28A,N4A)
5.e Idealised Me refined as rotating group:
 C36(H36A,H36B,H36C), C9(H9A,H9B,H9C), C12(H12A,H12B,H12C), C8(H8A,H8B,H8C),
 C11(H11A,H11B,H11C), C37(H37A,H37B,H37C), C39(H39A,H39B,H39C), C40(H40A,H40B,
 H40C)
;
_shelx_res_checksum              13398
_shelx_hkl_checksum              25946
_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 1.591
_oxdiff_exptl_absorpt_empirical_full_min 0.612