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_7714201
_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         '1(C17 H24 Ga N O)'
_chemical_formula_sum            'C17 H24 Ga N O'
_chemical_formula_weight         328.09
_chemical_name_systematic        'Di-t-butylgallium 8-hydroxyquinolinolate'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-09-22
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-09-27 deposited with the CCDC.	2023-10-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   15.9380(3)
_cell_length_b                   16.7591(2)
_cell_length_c                   25.8720(3)
_cell_measurement_reflns_used    14053
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      78.3690
_cell_measurement_theta_min      4.1290
_cell_volume                     6910.58(17)
_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    'XT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      123.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0551
_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            35676
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.270
_diffrn_reflns_theta_min         3.417
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    2.133
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51747
_exptl_crystal_density_diffrn    1.261
_exptl_crystal_description       plate
_exptl_crystal_F_000             2752
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.571
_refine_diff_density_min         -0.405
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     534
_refine_ls_number_reflns         7410
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0657
_refine_ls_R_factor_gt           0.0523
_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^)+(0.0630P)^2^+5.4714P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1347
_refine_ls_wR_factor_ref         0.1448
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5766
_reflns_number_total             7410
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02542j2.cif
_cod_data_source_block           GatBu28Qc_7
_cod_database_code               7714201
_shelx_shelxl_version_number     2018/3
_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. Restrained distances
 C10'-C11'
 1.54 with sigma of 0.02
 C10'-C12'
 1.54 with sigma of 0.02
 C10'-C13'
 1.55 with sigma of 0.02
 C10-C11
 1.54 with sigma of 0.02
 C10-C12
 1.54 with sigma of 0.02
 C10-C13
 1.55 with sigma of 0.02
 C14-C15
 1.54 with sigma of 0.02
 C14-C16
 1.54 with sigma of 0.02
 C14-C17
 1.55 with sigma of 0.02
 C14'-C15'
 1.54 with sigma of 0.02
 C14'-C16'
 1.54 with sigma of 0.02
 C14'-C17'
 1.55 with sigma of 0.02
 C27'-C28'
 1.54 with sigma of 0.02
 C27'-C29'
 1.54 with sigma of 0.02
 C27'-C30'
 1.54 with sigma of 0.02
 C31'-C32'
 1.54 with sigma of 0.02
 C31'-C33'
 1.54 with sigma of 0.02
 C31'-C34'
 1.55 with sigma of 0.02
 C15-C17
 2.5 with sigma of 0.02
 Ga1-C10 \\sim Ga1'-C10'
 with sigma of 0.02
 Ga1-C14 \\sim Ga1'-C14'
 with sigma of 0.02
 Ga2-C31 \\sim Ga2'-C31'
 with sigma of 0.02
 Ga2-C27 \\sim Ga2'-C27'
 with sigma of 0.02
 Ga2-O2 \\sim Ga2'-O2'
 with sigma of 0.02
 C25-O2 \\sim C25-O2'
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O2') \\sim Ueq, Uanis(C10') \\sim Ueq, Uanis(C11') \\sim Ueq, Uanis(C12')
\\sim Ueq, Uanis(C14') \\sim Ueq, Uanis(C16') \\sim Ueq, Uanis(C17') \\sim Ueq,
Uanis(C15) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C17) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(Ga1')=Sof(C10')=Sof(C11')=Sof(H11d)=Sof(H11e)=Sof(H11f)=Sof(C12')=
 Sof(H12d)=Sof(H12e)=Sof(H12f)=Sof(C13')=Sof(H13d)=Sof(H13e)=Sof(H13f)=
 Sof(C14')=Sof(C15')=Sof(H15d)=Sof(H15e)=Sof(H15f)=Sof(C16')=Sof(H16d)=
 Sof(H16e)=Sof(H16f)=Sof(C17')=Sof(H17d)=Sof(H17e)=Sof(H17f)=1-FVAR(1)
 Sof(Ga1)=Sof(C10)=Sof(C11)=Sof(H11a)=Sof(H11b)=Sof(H11c)=Sof(C12)=Sof(H12a)=
 Sof(H12b)=Sof(H12c)=Sof(C13)=Sof(H13a)=Sof(H13b)=Sof(H13c)=Sof(C14)=Sof(C15)=
 Sof(H15a)=Sof(H15b)=Sof(H15c)=Sof(C16)=Sof(H16a)=Sof(H16b)=Sof(H16c)=Sof(C17)=
 Sof(H17a)=Sof(H17b)=Sof(H17c)=FVAR(1)
 Sof(Ga2')=Sof(O2)=Sof(C27')=Sof(C28')=Sof(H28d)=Sof(H28e)=Sof(H28f)=Sof(C29')=
 Sof(H29d)=Sof(H29e)=Sof(H29f)=Sof(C30')=Sof(H30d)=Sof(H30e)=Sof(H30f)=
 Sof(C31')=Sof(C32')=Sof(H32d)=Sof(H32e)=Sof(H32f)=Sof(C33')=Sof(H33d)=
 Sof(H33e)=Sof(H33f)=Sof(C34')=Sof(H34d)=Sof(H34e)=Sof(H34f)=1-FVAR(2)
 Sof(Ga2)=Sof(O2')=Sof(C27)=Sof(C28)=Sof(H28a)=Sof(H28b)=Sof(H28c)=Sof(C29)=
 Sof(H29a)=Sof(H29b)=Sof(H29c)=Sof(C30)=Sof(H30a)=Sof(H30b)=Sof(H30c)=Sof(C31)=
 Sof(C32)=Sof(H32a)=Sof(H32b)=Sof(H32c)=Sof(C33)=Sof(H33a)=Sof(H33b)=Sof(H33c)=
 Sof(C34)=Sof(H34a)=Sof(H34b)=Sof(H34c)=FVAR(2)
5.a Me refined with riding coordinates:
 C11(H11a,H11b,H11c), C11'(H11e,H11d,H11f), C12(H12a,H12b,H12c), C12'(H12e,
 H12f,H12d), C13(H13a,H13b,H13c), C13'(H13e,H13d,H13f), C15(H15c,H15a,H15b),
 C15'(H15d,H15e,H15f), C16(H16b,H16a,H16c), C16'(H16e,H16f,H16d), C17(H17a,H17b,
 H17c), C17'(H17d,H17f,H17e), C28(H28b,H28a,H28c), C28'(H28d,H28e,H28f),
 C29(H29a,H29b,H29c), C29'(H29d,H29e,H29f), C30(H30a,H30b,H30c), C30'(H30d,H30e,
 H30f), C32(H32a,H32b,H32c), C32'(H32d,H32f,H32e), C33(H33a,H33b,H33c),
 C33'(H33d,H33e,H33f), C34(H34a,H34b,H34c), C34'(H34d,H34e,H34f)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C6(H6), C7(H7), C18(H18), C19(H19), C20(H20),
 C22(H22), C23(H23), C24(H24)
;
_shelx_res_checksum              77094
_olex2_submission_special_instructions 'No special instructions were received'