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_7714202
_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         '0.1(C30 H40 Ga2 N2 O2)'
_chemical_formula_sum            'C3 H4 Ga0.2 N0.2 O0.2'
_chemical_formula_weight         60.01
_chemical_name_systematic        'Diisopropylgallium 8-hydroxyquinolinolate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-09-01
_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                90
_cell_angle_beta                 101.958(4)
_cell_angle_gamma                90
_cell_formula_units_Z            20
_cell_length_a                   10.9604(5)
_cell_length_b                   11.6541(5)
_cell_length_c                   11.3776(5)
_cell_measurement_reflns_used    10045
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      32.1610
_cell_measurement_theta_min      3.4960
_cell_volume                     1421.76(11)
_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 n/a (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -42.00  32.00   0.50    1.50    --    9.22 -78.00 -60.00  148
  2  \w     -1.00  28.00   0.50    1.50    --    9.22 -99.00   0.00   58
  3  \w     -9.00  43.00   0.50    1.50    --    9.22 -99.00  90.00  104
  4  \w    -23.00  25.00   0.50    1.50    --   -8.90 -99.00 150.00   96
  5  \w    -23.00  25.00   0.50    1.50    --   -8.90 -99.00  90.00   96
  6  \w    -23.00  25.00   0.50    1.50    --   -8.90 -99.00-120.00   96
  7  \w    -42.00  14.00   0.50    1.50    --   -8.90 -78.00 -60.00  112
  8  \w    -32.00  21.00   0.50    1.50    --   -8.90  78.00  63.00  106
;
_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      0.0204563000
_diffrn_orient_matrix_UB_12      -0.0512506000
_diffrn_orient_matrix_UB_13      -0.0234081000
_diffrn_orient_matrix_UB_21      -0.0551401000
_diffrn_orient_matrix_UB_22      -0.0010258000
_diffrn_orient_matrix_UB_23      -0.0454582000
_diffrn_orient_matrix_UB_31      0.0302278000
_diffrn_orient_matrix_UB_32      0.0327606000
_diffrn_orient_matrix_UB_33      -0.0381269000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0884
_diffrn_reflns_av_unetI/netI     0.1297
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            14882
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.499
_diffrn_reflns_theta_min         3.385
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.924
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61476
_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    1.402
_exptl_crystal_description       block
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.776
_refine_diff_density_min         -0.591
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     167
_refine_ls_number_reflns         2638
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0309
_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^)+(0.0399P)^2^+0.8886P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0783
_refine_ls_wR_factor_ref         0.0818
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2287
_reflns_number_total             2638
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02542j2.cif
_cod_data_source_block           gaiso8q_auto
_cod_original_formula_sum        'C3 H4 Ga0.20 N0.20 O0.20'
_cod_database_code               7714202
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Ga C H N O'
_shelx_estimated_absorpt_t_max   0.861
_shelx_estimated_absorpt_t_min   0.775
_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 Ternary CH refined with riding coordinates:
 C13(H13), C10(H10)
2.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C5(H5), C3(H3), C1(H1), C2(H2), C6(H6)
2.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C11(H11A,H11B,H11C), C12(H12A,H12B,
 H12C)
;
_shelx_res_checksum              82880
_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 1.294
_oxdiff_exptl_absorpt_empirical_full_min 0.752