Highly selective organo-gallium hydroxamate mediated inhibition of antibiotic resistant <i>Klebsiella pneumoniae</i>.
Duffin, Rebekah N.; Kelderman, Jenisi T. A.; Herdman, Megan E.; Andrews, Philip C.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 649–661; doi:10.1039/d4dt02440k

data_7717475
_publ_section_title
;
 Highly selective organo-gallium hydroxamate mediated inhibition of
 antibiotic resistant <i>Klebsiella pneumoniae</i>.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              649
_journal_page_last               661
_journal_paper_doi               10.1039/d4dt02440k
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         '2(C20 H31 Ga4 N O4)'
_chemical_formula_sum            'C40 H62 Ga8 N2 O8'
_chemical_formula_weight         1256.67
_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             2022-09-26
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2024-02-01 deposited with the CCDC.	2024-11-06 downloaded from the CCDC.
;
_cell_angle_alpha                85.4710(10)
_cell_angle_beta                 86.0980(10)
_cell_angle_gamma                77.3800(10)
_cell_formula_units_Z            2
_cell_length_a                   9.76440(10)
_cell_length_b                   12.35930(10)
_cell_length_c                   22.2325(3)
_cell_measurement_reflns_used    32999
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      80.0560
_cell_measurement_theta_min      3.6530
_cell_volume                     2606.49(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  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.00(10)
_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 0.978
_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    109.00 177.00   0.50    0.33    --  111.50  30.00 150.00  136
  2  \w    104.00 178.00   0.50    0.33    --  111.50  45.00  30.00  148
  3  \w    108.00 178.00   0.50    0.33    --  111.50  30.00 -30.00  140
  4  \w    101.00 178.00   0.50    0.33    --  111.50  80.00 -86.00  154
  5  \w    107.00 178.00   0.50    0.33    --  111.50  15.00-120.00  142
  6  \w     63.00 118.00   0.50    0.33    --  111.50   0.00 -90.00  110
  7  \w     67.00 116.00   0.50    0.33    --  111.50   0.00   0.00   98
  8  \w     76.00 109.00   0.50    0.33    --  111.50   0.00 150.00   66
  9  \w     40.00  66.00   0.50    0.33    --  111.50 -30.00 120.00   52
 10  \w    -20.00  71.00   0.50    0.08    --   50.49 -80.00 150.00  182
 11  \w     41.00 133.00   0.50    0.33    --  111.50 -80.00 150.00  184
 12  \w     41.00  76.00   0.50    0.33    --  111.50 -45.00 150.00   70
 13  \w     41.00  76.00   0.50    0.33    --  111.50 -45.00  60.00   70
 14  \w     41.00  76.00   0.50    0.33    --  111.50 -45.00 120.00   70
 15  \w     41.00 125.00   0.50    0.33    --  111.50 -61.00  30.00  168
 16  \w     41.00  76.00   0.50    0.33    --  111.50 -45.00  30.00   70
 17  \w     41.00  76.00   0.50    0.33    --  111.50 -45.00   0.00   70
 18  \w     40.00  65.00   0.50    0.33    --  111.50 -30.00  60.00   50
 19  \w     41.00  76.00   0.50    0.33    --  111.50 -45.00 -30.00   70
 20  \w     41.00  66.00   0.50    0.33    --  111.50 -30.00 -30.00   50
 21  \w     45.00  76.00   0.50    0.33    --  111.50 -45.00 -60.00   62
 22  \w     40.00  66.00   0.50    0.33    --  111.50 -30.00-180.00   52
 23  \w     42.00  71.00   0.50    0.33    --  111.50 -45.00-180.00   58
 24  \w     69.00 119.00   0.50    0.33    --  111.50 -61.00-150.00  100
 25  \w     41.00 106.00   0.50    0.33    --  111.50 -94.00 -30.00  130
 26  \w     46.00  72.00   0.50    0.33    --  111.50-108.00 -41.14   52
 27  \w     78.00 108.00   0.50    0.33    --  111.50-108.00 -41.14   60
 28  \w     41.00 108.00   0.50    0.33    --  111.50-110.00 -61.85  134
 29  \w     41.00 111.00   0.50    0.33    --  111.50-125.00 -60.00  140
 30  \w     41.00 106.00   0.50    0.33    --  111.50 -94.00   0.00  130
 31  \w     41.00 106.00   0.50    0.33    --  111.50 -94.00  90.00  130
 32  \w     68.00 105.00   0.50    0.33    --  111.50 -94.00  30.00   74
 33  \w     41.00 106.00   0.50    0.33    --  111.50 -94.00 120.00  130
 34  \w     41.00 106.00   0.50    0.33    --  111.50 -94.00 150.00  130
 35  \w     46.00 107.00   0.50    0.33    --  111.50-103.00 160.85  122
 36  \w     41.00 106.00   0.50    0.33    --  111.50 -94.00  60.00  130
 37  \w     34.00  95.00   0.50    0.08    --   50.49-125.00  30.00  122
 38  \w     41.00  77.00   0.50    0.33    --  111.50 -94.00 -60.00   72
 39  \w     78.00 104.00   0.50    0.33    --  111.50 -94.00-120.00   52
 40  \w     73.00 106.00   0.50    0.33    --  111.50 -97.00-171.03   66
 41  \w     43.00 105.00   0.50    0.33    --  111.50 -94.00-150.00  124
 42  \w    -71.00  21.00   0.50    0.08    --  -50.49  80.00 -86.00  184
 43  \w   -111.00 -18.00   0.50    0.33    --  -90.00  80.00 -86.00  186
 44  \w    -56.00  20.00   0.50    0.08    --  -50.49  38.00-180.00  152
 45  \w    -55.00  21.00   0.50    0.08    --  -50.49  19.00 -90.00  152
 46  \w    -99.00 -44.00   0.50    0.08    --  -50.49   0.00 -90.00  110
 47  \w   -161.00 -85.00   0.50    0.33    --  -90.00 -30.00-180.00  152
 48  \w   -122.00 -73.00   0.50    0.08    --  -50.49-125.00 -90.00   98
 49  \w   -122.00 -73.00   0.50    0.08    --  -50.49-125.00   0.00   98
 50  \w   -161.00 -79.00   0.50    0.33    --  -90.00 -80.00 150.00  164
 51  \w    -86.00 -13.00   0.50    0.08    --  -50.49 125.00  30.00  146
;
_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      -0.0212456000
_diffrn_orient_matrix_UB_12      -0.0880402000
_diffrn_orient_matrix_UB_13      0.0507579000
_diffrn_orient_matrix_UB_21      0.1272116000
_diffrn_orient_matrix_UB_22      0.0201736000
_diffrn_orient_matrix_UB_23      0.0314017000
_diffrn_orient_matrix_UB_31      -0.0978664000
_diffrn_orient_matrix_UB_32      0.0907136000
_diffrn_orient_matrix_UB_33      0.0358115000
_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  0.0673
_diffrn_reflns_av_unetI/netI     0.0462
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            54923
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.420
_diffrn_reflns_theta_min         3.673
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.906
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72458
_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_colour            'clear whiteish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.601
_exptl_crystal_description       plate
_exptl_crystal_F_000             1256
_exptl_crystal_preparation       hexane
_exptl_crystal_recrystallization_method hexane
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.363
_refine_diff_density_min         -1.128
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     537
_refine_ls_number_reflns         11188
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0497
_refine_ls_R_factor_gt           0.0451
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0622P)^2^+3.2609P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1248
_refine_ls_wR_factor_ref         0.1285
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9858
_reflns_number_total             11188
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02440k2.cif
_cod_data_source_block           game2bpha_auto
_cod_depositor_comments
'Adding full bibliography for 7717469--7717476.cif.'
_cod_database_code               7717475
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Ga C H N O'
_shelx_estimated_absorpt_t_max   0.867
_shelx_estimated_absorpt_t_min   0.591
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C6(H6), C8(H8), C11(H11), C10(H10), C26(H26), C31(H31), C2(H2),
 C5(H5), C9(H9), C32(H32), C28(H28), C22(H22), C29(H29), C3(H3), C4(H4),
 C30(H30), C25(H25), C23(H23), C24(H24)
2.b Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C16(H16A,H16B,H16C), C15(H15A,H15B,H15C), C14(H14A,H14B,
 H14C), C19(H19A,H19B,H19C), C17(H17A,H17B,H17C), C20(H20A,H20B,H20C), C40(H40A,
 H40B,H40C), C38(H38A,H38B,H38C), C34(H34A,H34B,H34C), C39(H39A,H39B,H39C),
 C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C35(H35A,H35B,H35C)
;
_shelx_res_checksum              98497
_shelx_hkl_checksum              47526
_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 2.324
_oxdiff_exptl_absorpt_empirical_full_min 0.474