Structure-activity effects in the anti-leishmanial activity of di-alkyl gallium quinolin-8-olates
Duffin, Rebekah N.; Andrews, Philip Craig; Dalton Transactions  (2023) –; doi:10.1039/D3DT02542J

data_7714203
_publ_section_title
;
 Structure-activity effects in the anti-leishmanial activity of di-alkyl
 gallium quinolin-8-olates
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02542J
_journal_year                    2023
_chemical_formula_moiety         '2(C13 H16 Ga N O)'
_chemical_formula_sum            'C26 H32 Ga2 N2 O2'
_chemical_formula_weight         543.97
_chemical_name_systematic        'Diethylgallium 8-hydroxyquinolinolate'
_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             2023-09-04
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-09-04 deposited with the CCDC.	2023-10-03 downloaded from the CCDC.
;
_cell_angle_alpha                91.428(2)
_cell_angle_beta                 103.785(3)
_cell_angle_gamma                101.757(3)
_cell_formula_units_Z            2
_cell_length_a                   9.9300(4)
_cell_length_b                   10.5992(4)
_cell_length_c                   12.2053(3)
_cell_measurement_reflns_used    8119
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      79.3660
_cell_measurement_theta_min      4.6600
_cell_volume                     1217.78(8)
_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    'ShelXT (Sheldrick, 2015)'
_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 0.997
_diffrn_measured_fraction_theta_max 0.957
_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    -87.00 -61.00   0.50    1.00    --  -47.74 -75.00 -62.00   52
  2  \w     36.00 106.00   0.50    1.00    --   47.74  75.00  64.00  140
  3  \w    -24.00  59.00   0.50    1.00    --   47.74 -75.00 -62.00  166
  4  \w   -111.00 -73.00   0.50    4.00    --  -91.75 -75.00 -62.00   76
  5  \w    -67.00 -41.00   0.50    4.00    --  -91.75  75.00  64.00   52
  6  \w   -146.00-117.00   0.50    4.00    --  -91.75 -75.00 -62.00   58
  7  \w     93.00 178.00   0.50    4.00    --  113.25  75.00  64.00  170
  8  \w     55.00  82.00   0.50    4.00    --  113.25 -75.00 -62.00   54
  9  \w    -68.00  22.00   0.50    1.00    --  -47.74  75.00  64.00  180
 10  \w   -117.00 -74.00   0.50    1.00    --  -47.74-125.00   0.00   86
 11  \w   -117.00 -76.00   0.50    1.00    --  -47.74-125.00  90.00   82
 12  \w     37.00  91.00   0.50    1.00    --   47.74-125.00  60.00  108
 13  \w      0.00  36.00   0.50    1.00    --   47.74 -99.00-120.00   72
 14  \w     55.00  81.00   0.50    1.00    --   47.74 -99.00-120.00   52
 15  \w     45.00  91.00   0.50    1.00    --   47.74-125.00 -30.00   92
 16  \w    -67.00 -25.00   0.50    4.00    --  -91.75  45.00 -90.00   84
 17  \w    -68.00 -17.00   0.50    4.00    --  -91.75  30.00-120.00  102
 18  \w     43.00  81.00   0.50    4.00    --  113.25-125.00 -60.00   76
 19  \w     78.00 106.00   0.50    4.00    --  113.25 -94.00   0.00   56
 20  \w     44.00  69.00   0.50    4.00    --  113.25 -45.00 150.00   50
 21  \w     63.00 106.00   0.50    4.00    --  113.25 -94.00 120.00   86
 22  \w     43.00  74.00   0.50    4.00    --  113.25 -45.00-180.00   62
 23  \w     42.00  74.00   0.50    4.00    --  113.25 -94.00   0.00   64
 24  \w    125.00 162.00   0.50    4.00    --  113.25  15.00   0.00   74
 25  \w     49.00 105.00   0.50    4.00    --  113.25 -94.00-150.00  112
 26  \w     46.00  72.00   0.50    4.00    --  113.25 -94.00 -90.00   52
 27  \w     45.00  73.00   0.50    4.00    --  113.25 -45.00 -30.00   56
 28  \w    107.00 177.00   0.50    4.00    --  113.25  30.00 150.00  140
 29  \w     77.00 103.00   0.50    4.00    --  113.25 -94.00 -90.00   52
 30  \w     39.00  65.00   0.50    4.00    --  113.25 -30.00 -90.00   52
 31  \w     43.00 105.00   0.50    4.00    --  113.25 -94.00 150.00  124
 32  \w     96.00 178.00   0.50    4.00    --  113.25 125.00-180.00  164
 33  \w     39.00  93.00   0.50    4.00    --  113.25 -15.00-120.00  108
 34  \w     50.00 104.00   0.50    4.00    --  113.25 -94.00 -60.00  108
 35  \w     44.00  70.00   0.50    4.00    --  113.25 -45.00 120.00   52
 36  \w     66.00 101.00   0.50    4.00    --  113.25 -94.00  60.00   70
 37  \w     93.00 156.00   0.50    4.00    --  113.25  77.00   0.00  126
 38  \w     78.00 103.00   0.50    4.00    --  113.25 -94.00 -30.00   50
 39  \w     73.00 100.00   0.50    4.00    --  113.25-125.00 150.00   54
 40  \w    130.00 170.00   0.50    4.00    --  113.25  45.00 -90.00   80
 41  \w     74.00 105.00   0.50    4.00    --  113.25 -94.00-120.00   62
 42  \w     46.00  72.00   0.50    4.00    --  113.25-125.00 150.00   52
 43  \w    115.00 178.00   0.50    4.00    --  113.25  45.00  30.00  126
 44  \w     49.00  75.00   0.50    4.00    --  113.25 -45.00  60.00   52
;
_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      -0.0140547000
_diffrn_orient_matrix_UB_12      0.0699274000
_diffrn_orient_matrix_UB_13      0.1075634000
_diffrn_orient_matrix_UB_21      0.1362723000
_diffrn_orient_matrix_UB_22      0.1010312000
_diffrn_orient_matrix_UB_23      0.0016923000
_diffrn_orient_matrix_UB_31      -0.0894353000
_diffrn_orient_matrix_UB_32      0.0841199000
_diffrn_orient_matrix_UB_33      -0.0736171000
_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  0.0516
_diffrn_reflns_av_unetI/netI     0.0506
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15501
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.354
_diffrn_reflns_theta_min         3.740
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.906
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59063
_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 yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_description       plate
_exptl_crystal_F_000             560
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.554
_refine_diff_density_min         -1.163
_refine_diff_density_rms         0.162
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         5122
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0586
_refine_ls_R_factor_gt           0.0520
_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^)+(0.1120P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1412
_refine_ls_wR_factor_ref         0.1467
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4464
_reflns_number_total             5122
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02542j2.cif
_cod_data_source_block           gaet28q_auto
_cod_database_code               7714203
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Ga C H N O'
_shelx_estimated_absorpt_t_max   0.944
_shelx_estimated_absorpt_t_min   0.801
_diffrn_oxdiff_digest_frames
;
01fe4e55a23c72d5eaf462953d13b7845a03786fd10
;
_diffrn_oxdiff_digest_hkl
;
01447e19e12079cf3392936e317ed48781b731
;
_reflns_odcompleteness_completeness 99.52
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_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:
 C12(H12A,H12B), C23(H23A,H23B), C25(H25A,H25B), C10(H10A,H10B)
2.b Aromatic/amide H refined with riding coordinates:
 C20(H20), C7(H7), C14(H14), C5(H5), C15(H15), C3(H3), C16(H16), C1(H1),
 C6(H6), C19(H19), C2(H2), C18(H18)
2.c Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C13(H13A,H13B,H13C), C11(H11A,H11B,H11C), C26(H26A,H26B,
 H26C)
;
_shelx_res_checksum              65375
_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 1.719
_oxdiff_exptl_absorpt_empirical_full_min 0.653