Implementing the design cues of dissociation dynamics and transmetalation in gallium(iii) complexes to promote the anti-proliferative activity of ligands targeting intracellular iron(ii) trafficking.
Dharmasivam, Mahendiran; Faiz, Sadia; Kaya, Busra; Wijesinghe, Tharushi P.; Suleymanoglu, Mediha; Azad, Mahan Gholam; Richardson, Vera; Zahoor, Ameer Fawad; Kalinowski, Danuta; Lewis, William; Bernhardt, Paul V.; Anjum, Rukhsana; Richardson, Des R.; Chemical science 17 (2026) 6546–6563; doi:10.1039/d5sc06084b

data_1576513
_publ_section_title
;
 Implementing the design cues of dissociation dynamics and transmetalation
 in gallium(iii) complexes to promote the anti-proliferative activity of
 ligands targeting intracellular iron(ii) trafficking.
;
_journal_issue                   13
_journal_name_full               'Chemical science'
_journal_page_first              6546
_journal_page_last               6563
_journal_paper_doi               10.1039/d5sc06084b
_journal_volume                  17
_journal_year                    2026
_chemical_absolute_configuration ad
_chemical_formula_moiety         '2(C19 H14 N4 O2)'
_chemical_formula_sum            'C19 H14 N4 O2'
_chemical_formula_weight         330.34
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-09-30
_audit_creation_method
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_audit_update_record
;
2020-02-09 deposited with the CCDC.	2025-11-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.122(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.5860(4)
_cell_length_b                   9.8008(7)
_cell_length_c                   27.2637(18)
_cell_measurement_reflns_used    3120
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.3320
_cell_measurement_theta_min      4.5640
_cell_volume                     1490.40(18)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53a (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 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 5.2930
_diffrn_detector_type            'Agilent Diffraction Atlas detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.987
_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     -5.00  44.00   1.00    2.00    --  -39.07  19.00-120.00   49
  2  \w     -4.00  41.00   1.00    2.00    --  -39.07  19.00 150.00   45
  3  \w      4.00  36.00   1.00    2.00    --  -39.07  19.00 -60.00   32
  4  \w     -6.00  33.00   1.00    2.00    --  -39.07  38.00-180.00   39
  5  \w      8.00  38.00   1.00    2.00    --  -39.07  19.00 -90.00   30
  6  \w     78.00 122.00   1.00    2.00    --   39.07 178.00   0.00   44
  7  \w    105.00 173.00   1.00    8.00    --  106.69 112.00  30.00   68
  8  \w     27.00  53.00   1.00    8.00    --  106.69 -30.00 -30.00   26
  9  \w     31.00  83.00   1.00    8.00    --  106.69 -61.00 150.00   52
 10  \w     31.00  57.00   1.00    8.00    --  106.69 -30.00-180.00   26
 11  \w     33.00  72.00   1.00    8.00    --  106.69 -45.00 -60.00   39
 12  \w     29.00  56.00   1.00    8.00    --  106.69 -30.00-120.00   27
 13  \w     78.00 158.00   1.00    8.00    --  106.69  45.00 -30.00   80
 14  \w     44.00  71.00   1.00    8.00    --  106.69 -45.00  90.00   27
 15  \w    144.00 178.00   1.00    8.00    --  106.69 112.00   0.00   34
 16  \w     33.00 115.00   1.00    8.00    --  106.69 -77.00  30.00   82
 17  \w     -4.00  29.00   1.00    2.00    --  -39.07  19.00-150.00   33
 18  \w     -5.00  32.00   1.00    2.00    --  -39.07  19.00 120.00   37
 19  \w     -1.00  25.00   1.00    2.00    --  -39.07  19.00  90.00   26
 20  \w     80.00 124.00   1.00    2.00    --   39.07 178.00-120.00   44
 21  \w     66.00 107.00   1.00    8.00    --  106.69-111.00-180.00   41
 22  \w     48.00  96.00   1.00    8.00    --  106.69-111.00 -30.00   48
 23  \w     29.00 140.00   1.00    8.00    --  106.69  15.00 120.00  111
 24  \w     77.00 169.00   1.00    8.00    --  106.69  45.00 -90.00   92
;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'SuperNova-Duo, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.2273535000
_diffrn_orient_matrix_UB_12      -0.0835554000
_diffrn_orient_matrix_UB_13      0.0087120000
_diffrn_orient_matrix_UB_21      0.0827356000
_diffrn_orient_matrix_UB_22      -0.1106922000
_diffrn_orient_matrix_UB_23      -0.0354959000
_diffrn_orient_matrix_UB_31      0.1331606000
_diffrn_orient_matrix_UB_32      -0.0735943000
_diffrn_orient_matrix_UB_33      0.0432971000
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_wavelength_determination fundamental
_diffrn_radiation_xray_symbol    K-L~2,3~
_diffrn_reflns_av_R_equivalents  0.0528
_diffrn_reflns_av_unetI/netI     0.0573
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            8533
_diffrn_reflns_point_group_measured_fraction_full 0.713
_diffrn_reflns_point_group_measured_fraction_max 0.698
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.369
_diffrn_reflns_theta_min         4.511
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           0.8
_diffrn_source_power             0.04
_diffrn_source_target            Cu
_diffrn_source_type              'Agilent Diffraction microfocus tube'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.810
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.769
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53a (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 colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_description       plate
_exptl_crystal_F_000             688
_exptl_crystal_recrystallization_method 'crystallised from DMSO'
_exptl_crystal_size_max          0.184
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.027
_refine_diff_density_max         0.537
_refine_diff_density_min         -0.414
_refine_diff_density_rms         0.091
_refine_ls_abs_structure_details
;
 Flack x determined using 714 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.0(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     459
_refine_ls_number_reflns         4095
_refine_ls_number_restraints     741
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.0978
_refine_ls_R_factor_gt           0.0888
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1192P)^2^+3.4256P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2455
_refine_ls_wR_factor_ref         0.2520
_reflns_Friedel_coverage         0.413
_reflns_Friedel_fraction_full    0.425
_reflns_Friedel_fraction_max     0.409
_reflns_number_gt                3577
_reflns_number_total             4095
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc06084b2.cif
_cod_data_source_block           drr19_s1874
_cod_depositor_comments
'Adding full bibliography for 1576509--1576516.cif.'
_cod_original_cell_volume        1490.39(17)
_cod_database_code               1576513
_sydney_internal_submission_code drr19_s1874
_sydney_internal_submission_date 2019-08-26
_sydney_internal_submission_number s1874
_sydney_internal_client_code     rukh
_sydney_internal_client_email    rukhsanaanjum@yahoo.com
_sydney_internal_client_name     'Rukhsana Anjum'
_sydney_internal_supervisor_code drr
_sydney_internal_supervisor_name 'Des Richards'
_sydney_internal_collection_date 2019-09-27
_sydney_internal_collection_user wlew0588
_sydney_internal_process_date    2019-09-27
_sydney_internal_process_user    wlew0588
_sydney_internal_solution_date   2019-09-30
_sydney_internal_solution_user   wlew0588
_sydney_internal_refine_date     3019-09-30
_sydney_internal_refine_user     wlew0588
_sydney_internal_check_and_archive_date 2019-09-30
_sydney_internal_check_user      wlew0588
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C19 H14 N4 O2'
_chemical_oxdiff_usercomment     SF-53
_shelx_estimated_absorpt_t_max   0.978
_shelx_estimated_absorpt_t_min   0.865
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N1-H1 \\sim N5-H5a
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.008 and sigma
for terminal atoms of 0.016 within 2A
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C10(H10), C11(H11), C13(H13), C14(H14), C15(H15),
 C16(H16), C19(H19), C23(H23), C24(H24), C25(H25), C30(H30), C31(H31), C33(H33),
  C34(H34), C35(H35), C36(H36), C39(H39)
5.b Idealised Me refined as rotating group:
 C6(H6a,H6b,H6c), C26(H26a,H26b,H26c)
;
_shelx_res_checksum              7109
_olex2_date_sample_data_collection 2019-09-27
_olex2_date_sample_submission    2019-08-26
_olex2_exptl_crystal_mounting_method 'in paratone on a micromount'
_olex2_submission_original_sample_id SF-53
_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 2.038
_oxdiff_exptl_absorpt_empirical_full_min 0.600