Gallium reactivates 1st and 2nd generation quinolone antibiotics towards drug-resistantKlebsiella pneumoniae
Sultana, Tania; Duffin, Rebekah. N.; Blair, Victoria L.; Andrews, Philip Craig; Chemical Communications  (2023) –; doi:10.1039/D3CC02916F

data_7132052
_publ_section_title
;
 Gallium reactivates 1st and 2nd generation quinolone antibiotics towards
 drug-resistantKlebsiella pneumoniae
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D3CC02916F
_journal_year                    2023
_chemical_formula_moiety         'C36 H33 Ga N6 O9, C2 H6 O S'
_chemical_formula_sum            'C38 H39 Ga N6 O10 S'
_chemical_formula_weight         841.53
_chemical_name_systematic        'gallium tris-naladixate'
_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             2022-12-01
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2023-05-24 deposited with the CCDC.	2023-08-21 downloaded from the CCDC.
;
_cell_angle_alpha                79.9703(12)
_cell_angle_beta                 77.8647(13)
_cell_angle_gamma                86.5916(12)
_cell_formula_units_Z            2
_cell_length_a                   9.57906(15)
_cell_length_b                   12.08921(18)
_cell_length_c                   16.5051(2)
_cell_measurement_reflns_used    21853
_cell_measurement_temperature    122.98(10)
_cell_measurement_theta_max      78.7330
_cell_measurement_theta_min      4.2560
_cell_volume                     1839.56(5)
_computing_cell_refinement       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.15
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.977
_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     36.00 122.00   0.50    0.12    --   50.49  66.00  49.00  172
  2  \w     97.00 178.00   0.50    0.40    --  111.50  66.00  49.00  162
  3  \w    104.00 178.00   0.50    0.40    --  111.50  45.00 -60.00  148
  4  \w    104.00 178.00   0.50    0.40    --  111.50  45.00 -90.00  148
  5  \w    108.00 178.00   0.50    0.40    --  111.50  30.00 -30.00  140
  6  \w     98.00 178.00   0.50    0.40    --  111.50  61.00-180.00  160
  7  \w     63.00 118.00   0.50    0.40    --  111.50   0.00-180.00  110
  8  \w      2.00  57.00   0.50    0.12    --   50.49   0.00-120.00  110
  9  \w     63.00 118.00   0.50    0.40    --  111.50   0.00  90.00  110
 10  \w      2.00  57.00   0.50    0.12    --   50.49   0.00 120.00  110
 11  \w    -99.00 -44.00   0.50    0.12    --  -50.49   0.00  60.00  110
 12  \w    -65.00  21.00   0.50    0.12    --  -50.49  66.00  49.00  172
 13  \w   -105.00 -18.00   0.50    0.40    --  -90.00  66.00  49.00  174
 14  \w    -55.00  21.00   0.50    0.12    --  -50.49  19.00  30.00  152
 15  \w    -62.00  21.00   0.50    0.12    --  -50.49  57.00-180.00  166
 16  \w    -78.00 -18.00   0.50    0.40    --  -90.00  45.00-120.00  120
 17  \w   -161.00 -75.00   0.50    0.40    --  -90.00 -66.00 -85.00  172
 18  \w   -122.00 -35.00   0.50    0.12    --  -50.49 -66.00 -85.00  174
 19  \w    -20.00  65.00   0.50    0.12    --   50.49 -66.00 -85.00  170
 20  \w     41.00  76.00   0.50    0.40    --  111.50 -45.00-180.00   70
 21  \w     41.00 131.00   0.50    0.40    --  111.50 -77.00-120.00  180
 22  \w     41.00 127.00   0.50    0.40    --  111.50 -66.00 -85.00  172
 23  \w     41.00  76.00   0.50    0.40    --  111.50 -45.00 -60.00   70
 24  \w     41.00  76.00   0.50    0.40    --  111.50 -45.00 -30.00   70
 25  \w     41.00 131.00   0.50    0.40    --  111.50 -77.00  60.00  180
 26  \w     41.00  76.00   0.50    0.40    --  111.50 -45.00  90.00   70
 27  \w     41.00  66.00   0.50    0.40    --  111.50 -45.00 120.00   50
 28  \w     40.00  66.00   0.50    0.40    --  111.50 -30.00 150.00   52
 29  \w     40.00  66.00   0.50    0.40    --  111.50 -30.00 120.00   52
 30  \w     98.00 160.00   0.50    0.40    --  111.50 125.00  90.00  124
 31  \w     45.00  72.00   0.50    0.40    --  111.50 -45.00  60.00   54
 32  \w     40.00  66.00   0.50    0.40    --  111.50 -30.00  30.00   52
 33  \w     40.00  66.00   0.50    0.40    --  111.50 -30.00 -60.00   52
 34  \w     40.00  66.00   0.50    0.40    --  111.50 -30.00-180.00   52
 35  \w     97.00 123.00   0.50    0.40    --  111.50-140.00 -85.65   52
 36  \w     41.00 106.00   0.50    0.40    --  111.50 -94.00-180.00  130
 37  \w     41.00 111.00   0.50    0.40    --  111.50-125.00-180.00  140
 38  \w     41.00 106.00   0.50    0.40    --  111.50 -94.00-120.00  130
 39  \w     80.00 106.00   0.50    0.40    --  111.50-100.00 -71.27   52
 40  \w     41.00 106.00   0.50    0.40    --  111.50 -94.00 -60.00  130
 41  \w     41.00 106.00   0.50    0.40    --  111.50 -94.00   0.00  130
 42  \w     75.00 101.00   0.50    0.40    --  111.50 -94.00  60.00   52
 43  \w     41.00  67.00   0.50    0.40    --  111.50 -94.00  60.00   52
 44  \w     41.00 106.00   0.50    0.40    --  111.50 -94.00 120.00  130
 45  \w     79.00 105.00   0.50    0.40    --  111.50 -94.00 150.00   52
 46  \w     41.00  68.00   0.50    0.40    --  111.50 -94.00 150.00   54
 47  \w     41.00 106.00   0.50    0.40    --  111.50 -94.00  90.00  130
 48  \w     46.00 105.00   0.50    0.40    --  111.50 -94.00  30.00  118
 49  \w     68.00 104.00   0.50    0.40    --  111.50 -94.00 -30.00   72
 50  \w     41.00 106.00   0.50    0.40    --  111.50 -94.00-150.00  130
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0534531000
_diffrn_orient_matrix_UB_12      0.0819033000
_diffrn_orient_matrix_UB_13      -0.0701648000
_diffrn_orient_matrix_UB_21      -0.1441092000
_diffrn_orient_matrix_UB_22      -0.0597002000
_diffrn_orient_matrix_UB_23      0.0229734000
_diffrn_orient_matrix_UB_31      -0.0587488000
_diffrn_orient_matrix_UB_32      0.0805247000
_diffrn_orient_matrix_UB_33      0.0626193000
_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  0.0534
_diffrn_reflns_av_unetI/netI     0.0402
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            38980
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.440
_diffrn_reflns_theta_min         3.714
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.140
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95391
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.113a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_description       irregular
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.781
_refine_diff_density_min         -0.889
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     513
_refine_ls_number_reflns         7899
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_gt           0.0429
_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^)+(0.0562P)^2^+1.7708P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1142
_refine_ls_wR_factor_ref         0.1178
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7003
_reflns_number_total             7899
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc02916f2.cif
_cod_data_source_block           ts_ganal3_auto
_cod_database_code               7132052
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Ga H N C O'
_chemical_oxdiff_usercomment     'colourless plates'
_shelx_estimated_absorpt_t_max   0.919
_shelx_estimated_absorpt_t_min   0.783
_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.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C27(H27A,H27B), C15(H15A,H15B)
2.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C2(H2), C26(H26), C9(H9), C21(H21), C8(H8), C20(H20), C33(H33),
 C32(H32)
2.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C28(H28A,H28B,H28C), C16(H16A,H16B,H16C), C36(H36A,H36B,
 H36C), C37(H37A,H37B,H37C), C7(H7A,H7B,H7C), C31(H31A,H31B,H31C), C19(H19A,
 H19B,H19C)
;
_shelx_res_checksum              58253
_shelx_hkl_checksum              80656
_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 1.424
_oxdiff_exptl_absorpt_empirical_full_min 0.818