Synthesis, characterisation and antibacterial activity of novel Ga(III) polypyridyl catecholate complexes
More O'Ferrall, Lewis; Piatek, Magdalena; Twamley, Brendan; Kavanagh, Kevin; O'Connor, Christine; Griffith, Darren Martin; Dalton Transactions  (2023) –; doi:10.1039/D3DT01761C

data_7713685
_publ_section_title
;
 Synthesis, characterisation and antibacterial activity of novel Ga(III)
 polypyridyl catecholate complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT01761C
_journal_year                    2023
_chemical_formula_moiety         'C27 H20 Ga N4 O4, F6 P'
_chemical_formula_sum            'C27 H20 F6 Ga N4 O4 P'
_chemical_formula_weight         679.16
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-12-21
_audit_creation_method
;
Olex2 1.5
(compiled 2021.11.18 svn.ra9532c28 for OlexSys, GUI svn.r6429)
;
_audit_update_record
;
2023-04-04 deposited with the CCDC.	2023-08-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.5153(14)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.4395(7)
_cell_length_b                   8.6262(3)
_cell_length_c                   26.9096(7)
_cell_measurement_reflns_used    9867
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      69.417
_cell_measurement_theta_min      3.862
_cell_volume                     5313.3(3)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       'APEX 3 (Bruker, 2017) '
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 8.33
_diffrn_detector_type            APEX2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'Kappa diffractometer'
_diffrn_measurement_device_type  'Bruker APEX2 Kappa Duo'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_detector       APEX2
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0716
_diffrn_reflns_av_unetI/netI     0.0358
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            103969
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.114
_diffrn_reflns_theta_min         1.930
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           0.6
_diffrn_source_power             0.029778
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           49.63
_exptl_absorpt_coefficient_mu    2.771
_exptl_absorpt_correction_T_max  0.7533
_exptl_absorpt_correction_T_min  0.5861
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1033 before and 0.0796 after correction.
The Ratio of minimum to maximum transmission is 0.7780.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.698
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2736
_exptl_crystal_size_max          0.226
_exptl_crystal_size_mid          0.136
_exptl_crystal_size_min          0.032
_refine_diff_density_max         1.149
_refine_diff_density_min         -0.800
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1057
_refine_ls_number_reflns         10065
_refine_ls_number_restraints     1185
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0845
_refine_ls_R_factor_gt           0.0688
_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^)+(0.0855P)^2^+13.1540P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1797
_refine_ls_wR_factor_ref         0.1916
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7921
_reflns_number_total             10065
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01761c2.cif
_cod_data_source_block           2
_cod_database_code               7713685
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.917
_shelx_estimated_absorpt_t_min   0.573
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H) groups, H35 of C23A
 At 1.2 times of:
  H2 of C2, H37 of C37, H30 of C30, H40 of C40, H49 of C49, H50 of C50, H38
  of C38, H51 of C51, H23 of C23, H46 of C46, H22 of C22, H29 of C29, H21 of
  C21, H39 of C39, H43 of C43, H27 of C27, H44 of C44, H45 of C45, H8 of C8,
  H10 of C10, H14 of C14, H17 of C17, H20A of C20A, H20 of C20, H9 of C9, H23A
  of C23A, H21A of C21A, H5 of C5, H16A of C16A, H3 of C3, H4 of C4, H11 of C11,
   H14A of C14A, H15A of C15A, H15 of C15, H17A of C17A, H22A of C22A, H16 of
  C16, H57 of C57, H64 of C64, H65A of C65A, H58 of C58, H56 of C56, H62 of C62,
   H65 of C65, H55 of C55, H64A of C64A, H62A of C62A, H52 of C52
2. Restrained distances
 O35-H35
 0.98 with sigma of 0.01
 O69A-C68A \\sim O70-C68
 with sigma of 0.01
 O69-C68 \\sim O70A-C68A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
O60 \\sim O60A \\sim C61 \\sim C61A \\sim C62 \\sim C62A \\sim C63 \\sim C63A
\\sim C64 \\sim C64A \\sim C65 \\sim C65A \\sim C66 \\sim C66A \\sim O67 \\sim
O67A \\sim C68 \\sim C68A \\sim O69 \\sim O69A \\sim O70 \\sim O70A: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
N13 \\sim C14 \\sim C15 \\sim C16 \\sim C17 \\sim C18 \\sim C19 \\sim C19A
\\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim N24 \\sim N24A: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
N13 \\sim N13A \\sim C14 \\sim C14A \\sim C15 \\sim C15A \\sim C16 \\sim C16A
\\sim C17 \\sim C17A \\sim C18 \\sim C18A \\sim C19 \\sim C19A \\sim C20 \\sim
C20A \\sim C21 \\sim C21A \\sim C22 \\sim C22A \\sim C23 \\sim C23A \\sim N24
\\sim N24A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
Ga1 \\sim Ga1A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
P1 \\sim F1 \\sim F2 \\sim F3 \\sim F4 \\sim F5 \\sim F6 \\sim P1A \\sim F1A
\\sim F2A \\sim F3A \\sim F4A \\sim F5A \\sim F6A: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 2A
P2 \\sim F7 \\sim F8 \\sim F9 \\sim F10 \\sim F11 \\sim F12 \\sim P2A \\sim F7A
\\sim F8A \\sim F9A \\sim F10A \\sim F11A \\sim F12A: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
4. Others
 Sof(O60)=Sof(C61)=Sof(C62)=Sof(H62)=Sof(C63)=Sof(C64)=Sof(H64)=Sof(C65)=
 Sof(H65)=Sof(C66)=Sof(O67)=Sof(C68)=Sof(O69)=Sof(O70)=Sof(H70)=1-FVAR(1)
 Sof(O60A)=Sof(C61A)=Sof(C62A)=Sof(H62A)=Sof(C63A)=Sof(C64A)=Sof(H64A)=
 Sof(C65A)=Sof(H65A)=Sof(C66A)=Sof(O67A)=Sof(C68A)=Sof(O69A)=Sof(O70A)=
 Sof(H70A)=FVAR(1)
 Sof(P2A)=Sof(F7A)=Sof(F8A)=Sof(F9A)=Sof(F10A)=Sof(F11A)=Sof(F12A)=1-FVAR(2)
 Sof(P2)=Sof(F7)=Sof(F8)=Sof(F9)=Sof(F10)=Sof(F11)=Sof(F12)=FVAR(2)
 Sof(Ga1)=Sof(N13)=Sof(C14)=Sof(H14)=Sof(C15)=Sof(H15)=Sof(C16)=Sof(H16)=
 Sof(C17)=Sof(H17)=Sof(C18)=Sof(C19)=Sof(C20)=Sof(H20)=Sof(C21)=Sof(H21)=
 Sof(C22)=Sof(H22)=Sof(C23)=Sof(H23)=Sof(N24)=1-FVAR(3)
 Sof(Ga1A)=Sof(N13A)=Sof(C14A)=Sof(H14A)=Sof(C15A)=Sof(H15A)=Sof(C16A)=
 Sof(H16A)=Sof(C17A)=Sof(H17A)=Sof(C18A)=Sof(C20A)=Sof(H20A)=Sof(C21A)=
 Sof(H21A)=Sof(C22A)=Sof(H22A)=Sof(C23A)=Sof(H23A)=Sof(C19A)=Sof(N24A)=FVAR(3)
 Sof(P1)=Sof(F1)=Sof(F2)=Sof(F3)=Sof(F4)=Sof(F5)=Sof(F6)=1-FVAR(4)
 Sof(P1A)=Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(F4A)=Sof(F5A)=Sof(F6A)=FVAR(4)
5.a Free rotating group:
 N13A(C14A,C15A,C16A,C17A,C18A,C20A,C21A,C22A,C23A), P1A(F1A,F2A,F3A,F4A,F5A,
 F6A), P2(F7,F8,F9,F10,F11,F12), P2A(F7A,F8A,F9A,F10A,F11A,F12A)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C11(H11),
 C14A(H14A), C15A(H15A), C16A(H16A), C17A(H17A), C20A(H20A), C21A(H21A),
 C22A(H22A), C23A(H23A), C14(H14), C15(H15), C16(H16), C17(H17), C20(H20),
 C21(H21), C22(H22), C23(H23), C27(H27), C29(H29), C30(H30), C37(H37), C38(H38),
  C39(H39), C40(H40), C43(H43), C44(H44), C45(H45), C46(H46), C49(H49),
 C50(H50), C51(H51), C52(H52), C55(H55), C56(H56), C57(H57), C58(H58), C62(H62),
  C62A(H62A), C64(H64), C64A(H64A), C65(H65), C65A(H65A)
5.c Idealised tetrahedral OH refined as rotating group:
 O70(H70), O70A(H70A)
;
_shelx_res_checksum              98312
_olex2_exptl_crystal_mounting_method 'mounted in oil on a MiTeGen microloop'
_olex2_submission_original_sample_id LMOF46PF6
_olex2_submission_special_instructions 'No special instructions were received'