Homoleptic gallium(III) and indium(III) <i>tris</i>(flavonolate) complexes: influence of the metal ion on antibacterial activity and mammalian cell viability.
Burke, Kirralee J.; Duffin, Rebekah N.; Andrews, Philip C.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 16201–16218; doi:10.1039/d5dt02012c

data_7719657
_publ_section_title
;
 Homoleptic gallium(III) and indium(III) <i>tris</i>(flavonolate)
 complexes: influence of the metal ion on antibacterial activity and
 mammalian cell viability.
;
_journal_issue                   43
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16201
_journal_page_last               16218
_journal_paper_doi               10.1039/d5dt02012c
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C57 H54 In N3 O9, 2(C H2 Cl2), H2 O'
_chemical_formula_sum            'C59 H60 Cl4 In N3 O10'
_chemical_formula_weight         1227.72
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-07-12
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-04-03 deposited with the CCDC.	2025-10-07 downloaded from the CCDC.
;
_cell_angle_alpha                90.9830(10)
_cell_angle_beta                 114.0430(10)
_cell_angle_gamma                119.0670(10)
_cell_formula_units_Z            2
_cell_length_a                   14.9079(2)
_cell_length_b                   15.0015(2)
_cell_length_c                   16.0866(2)
_cell_measurement_reflns_used    40208
_cell_measurement_temperature    128.00(10)
_cell_measurement_theta_max      78.0760
_cell_measurement_theta_min      3.5190
_cell_volume                     2765.47(8)
_computing_cell_refinement       'CrysAlisPro 1.171.43.95a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.43.95a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.43.95a (Rigaku OD, 2023)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      128.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_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    -79.00  19.00   0.50    1.00    --  -50.44  99.00 -95.00  196
  2  \w    -79.00  19.00   0.50    1.00    --  -50.44  99.00 -95.00  196
  3  \w    -80.00 -20.00   0.50    4.00    --  -90.00  99.00 -95.00  120
  4  \w     42.00 106.00   0.50    4.00    --  111.50 -99.00 157.00  128
  5  \w     42.00 106.00   0.50    4.00    --  111.50 -99.00 157.00  128
  6  \w    107.00 178.00   0.50    4.00    --  111.50  99.00 -95.00  142
  7  \w    -99.00 -44.00   0.50    1.00    --  -50.44   0.00 -30.00  110
  8  \w   -122.00 -45.00   0.50    1.00    --  -50.44 -37.00-150.00  154
  9  \w    -56.00  21.00   0.50    1.00    --  -50.44  37.00-180.00  154
 10  \w   -119.00 -73.00   0.50    1.00    --  -50.44-125.00 -30.00   92
 11  \w    -99.00 -44.00   0.50    1.00    --  -50.44   0.00 120.00  110
 12  \w   -122.00 -45.00   0.50    1.00    --  -50.44 -37.00-150.00  154
 13  \w    -20.00  62.00   0.50    1.00    --   50.44 -57.00 -60.00  164
 14  \w     34.00  93.00   0.50    1.00    --   50.44-125.00  90.00  118
 15  \w     -1.00  80.00   0.50    1.00    --   50.44 -99.00 157.00  162
 16  \w    -68.00 -17.00   0.50    4.00    --  -90.00  30.00 120.00  102
 17  \w   -160.00 -86.00   0.50    4.00    --  -90.00 -99.00 157.00  148
 18  \w     63.00 118.00   0.50    4.00    --  111.50   0.00 120.00  110
 19  \w     40.00  66.00   0.50    4.00    --  111.50 -30.00-180.00   52
 20  \w     40.00  66.00   0.50    4.00    --  111.50 -30.00 -60.00   52
 21  \w     41.00 131.00   0.50    4.00    --  111.50 -77.00-150.00  180
 22  \w     40.00  66.00   0.50    4.00    --  111.50 -30.00 -30.00   52
 23  \w     41.00 131.00   0.50    4.00    --  111.50 -77.00-150.00  180
 24  \w     40.00  66.00   0.50    4.00    --  111.50 -30.00 150.00   52
 25  \w     41.00  76.00   0.50    4.00    --  111.50 -45.00   0.00   70
 26  \w     40.00  66.00   0.50    4.00    --  111.50 -30.00 120.00   52
 27  \w     40.00 116.00   0.50    4.00    --  111.50 -15.00-150.00  152
 28  \w     42.00 106.00   0.50    4.00    --  111.50 -99.00 -36.66  128
 29  \w     41.00 106.00   0.50    4.00    --  111.50 -94.00-150.00  130
 30  \w     42.00 105.00   0.50    4.00    --  111.50 -94.00  90.00  126
 31  \w     41.00  66.00   0.50    4.00    --  111.50 -45.00 120.00   50
 32  \w     47.00  76.00   0.50    4.00    --  111.50 -45.00-150.00   58
 33  \w    104.00 130.00   0.50    4.00    --  111.50  45.00-120.00   52
 34  \w    138.00 164.00   0.50    4.00    --  111.50  45.00-120.00   52
 35  \w     43.00  68.00   0.50    4.00    --  111.50 -45.00-120.00   50
 36  \w     70.00 105.00   0.50    4.00    --  111.50 -94.00-120.00   70
 37  \w     59.00  85.00   0.50    4.00    --  111.50-125.00 120.00   52
 38  \w     43.00  81.00   0.50    4.00    --  111.50-125.00  60.00   76
 39  \w     71.00 109.00   0.50    4.00    --  111.50-125.00-120.00   76
 40  \w     59.00 102.00   0.50    4.00    --  111.50 -94.00  60.00   86
 41  \w     41.00  74.00   0.50    4.00    --  111.50 -45.00 150.00   66
 42  \w     46.00  73.00   0.50    4.00    --  111.50 -45.00 -60.00   54
 43  \w     74.00 114.00   0.50    4.00    --  111.50   0.00  60.00   80
 44  \w     40.00  65.00   0.50    4.00    --  111.50 -30.00-150.00   50
 45  \w     68.00 104.00   0.50    4.00    --  111.50 -94.00 120.00   72
 46  \w     50.00 100.00   0.50    4.00    --  111.50 -94.00 -30.00  100
 47  \w     41.00  75.00   0.50    4.00    --  111.50 -45.00  60.00   68
 48  \w    115.00 161.00   0.50    4.00    --  111.50  15.00  90.00   92
 49  \w     52.00 106.00   0.50    4.00    --  111.50 -94.00-180.00  108
 50  \w     71.00 106.00   0.50    4.00    --  111.50 -94.00  30.00   70
 51  \w     63.00  89.00   0.50    4.00    --  111.50 -61.00-120.00   52
 52  \w     98.00 124.00   0.50    4.00    --  111.50 -61.00-120.00   52
 53  \w     42.00  69.00   0.50    4.00    --  111.50 -45.00  90.00   54
 54  \w    105.00 157.00   0.50    4.00    --  111.50 125.00 150.00  104
 55  \w     61.00 106.00   0.50    4.00    --  111.50 -94.00   0.00   90
 56  \w     92.00 152.00   0.50    4.00    --  111.50  77.00 -90.00  120
 57  \w    104.00 177.00   0.50    4.00    --  111.50  61.00  90.00  146
 58  \w     64.00 109.00   0.50    4.00    --  111.50   0.00-120.00   90
;
_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      -0.1128024000
_diffrn_orient_matrix_UB_12      -0.0844513000
_diffrn_orient_matrix_UB_13      -0.0883411000
_diffrn_orient_matrix_UB_21      0.0085596000
_diffrn_orient_matrix_UB_22      0.0858827000
_diffrn_orient_matrix_UB_23      -0.0531229000
_diffrn_orient_matrix_UB_31      0.0725914000
_diffrn_orient_matrix_UB_32      -0.0194285000
_diffrn_orient_matrix_UB_33      -0.0350910000
_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  0.0532
_diffrn_reflns_av_unetI/netI     0.0284
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            57579
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.248
_diffrn_reflns_theta_min         3.500
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.703
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53951
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.95a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orangish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_description       block
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.299
_refine_diff_density_min         -2.004
_refine_diff_density_rms         0.114
_refine_ls_extinction_coef       0.00050(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     720
_refine_ls_number_reflns         11836
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0618
_refine_ls_R_factor_gt           0.0602
_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^)+(0.1066P)^2^+4.7753P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1639
_refine_ls_wR_factor_ref         0.1656
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11255
_reflns_number_total             11836
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02012c2.cif
_cod_data_source_block           kb_in4deaf_1_auto
_cod_depositor_comments
'Adding full bibliography for 7719654--7719657.cif.'
_cod_original_cell_volume        2765.46(7)
_cod_database_code               7719657
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'In Cl O N C H'
_shelx_estimated_absorpt_t_max   0.599
_shelx_estimated_absorpt_t_min   0.367
_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, All O(H,H) groups
2. Restrained distances
 Cl15-C60
 1.74 with sigma of 0.02
 C60-Cl16
 1.74 with sigma of 0.02
 Cl14-C59
 1.74 with sigma of 0.02
 C59-Cl13
 1.74 with sigma of 0.02
 Cl13-C59 \\sim Cl14-C59 \\sim Cl16-C60 \\sim Cl15-C60
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Cl15) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(Cl15) = Uanis(C60) = Uanis(Cl16) = Uanis(Cl13) = Uanis(C59) = Uanis(Cl14)
4. Rigid body (RIGU) restrains
 Cl14, C59, Cl16, Cl13, C60, Cl15
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C37A(0.5) H37A(0.5) H37B(0.5) C37(0.5) H37C(0.5) H37D(0.5)
 C38A(0.5) H38A(0.5) H38B(0.5) H38C(0.5) C38(0.5) H38D(0.5) H38E(0.5) H38F(0.5)
 Cl15(0.5) C60(0.5) H60A(0.5) H60B(0.5) Cl16(0.5) Cl14(0.5) C59(0.5) H59A(0.5)
 H59B(0.5) Cl13(0.5)
6.a Free rotating group:
 O7(H7A,H7B)
6.b Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C18(H18A,H18B), C56(H56A,H56B), C54(H54A,H54B), C36(H36A,
 H36B), C58(H58A,H58B), C37A(H37A,H37B), C37(H37C,H37D), C60(H60A,H60B),
 C59(H59A,H59B)
6.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C26(H26), C7(H7), C5(H5), C34(H34), C23(H23), C53(H53), C15(H15),
 C6(H6), C4(H4), C14(H14), C12(H12), C52(H52), C45(H45), C42(H42), C33(H33),
 C25(H25), C50(H50), C24(H24), C43(H43), C49(H49), C44(H44), C31(H31), C30(H30)
6.d Idealised Me refined as rotating group:
 C55(H55A,H55B,H55C), C19(H19A,H19B,H19C), C17(H17A,H17B,H17C), C57(H57A,H57B,
 H57C), C35(H35A,H35B,H35C), C38A(H38A,H38B,H38C), C38(H38D,H38E,H38F)
;
_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 1.666
_oxdiff_exptl_absorpt_empirical_full_min 0.513