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_7713686
_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 O5, 2.083(H2 O), 0.2(C H4 O), 0.5(Cl), 0.5(F6 P)'
_chemical_formula_sum            'C27.2 H24.97 Cl0.5 F3 Ga N4 O7.28 P0.5'
_chemical_formula_weight         684.34
_space_group_crystal_system      tetragonal
_space_group_IT_number           142
_space_group_name_Hall           '-I 4bd 2c'
_space_group_name_H-M_alt        'I 41/a c d :2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-02-21
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2023-04-04 deposited with the CCDC.	2023-08-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            32
_cell_length_a                   32.0378(10)
_cell_length_b                   32.0378(10)
_cell_length_c                   23.4142(11)
_cell_measurement_reflns_used    9927
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.295
_cell_measurement_theta_min      2.451
_cell_volume                     24032.8(15)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       'APEX 3 (Bruker, 2017) '
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_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                 'CMOS area detector'
_diffrn_detector_area_resol_mean 5.12
_diffrn_detector_type            'Bruker PHOTON 50'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Quest ECO'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_collimation    '0.5 mm double-pinhole'
_diffrn_radiation_detector       'Bruker PHOTON 50'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.1062
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            109222
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.477
_diffrn_reflns_theta_min         2.659
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           20.0
_diffrn_source_power             1.0
_diffrn_source_type              'Siemens, KFF Mo 2K -90 C'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.057
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6740
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Krause, 2015) was used for absorption correction.
wR2(int) was 0.0749 before and 0.0680 after correction.
The Ratio of minimum to maximum transmission is 0.9045.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             11150
_exptl_crystal_recrystallization_method 'Crystallized from bench MeOH.'
_exptl_crystal_size_max          0.197
_exptl_crystal_size_mid          0.168
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.837
_refine_diff_density_min         -0.699
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     464
_refine_ls_number_reflns         5574
_refine_ls_number_restraints     82
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0881
_refine_ls_R_factor_gt           0.0652
_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^)+(0.0915P)^2^+221.6168P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1767
_refine_ls_wR_factor_ref         0.1949
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4291
_reflns_number_total             5574
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01761c2.cif
_cod_data_source_block           3
_cod_original_cell_volume        24032.8(19)
_cod_original_sg_symbol_H-M      'I 41/a c d'
_cod_original_formula_sum        'C27.20 H24.97 Cl0.50 F3 Ga N4 O7.28 P0.50'
_cod_database_code               7713686
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.875
_shelx_estimated_absorpt_t_min   0.819
_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, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O6S-C5S
 1.4 with sigma of 0.01
 O33-H33
 0.84 with sigma of 0.01
 O36-H36
 0.84 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
P1 \\sim F1 \\sim F2 \\sim F3 \\sim F4 \\sim F5 \\sim F6: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(O4S) \\sim Ueq, Uanis(O6S) \\sim Ueq, Uanis(C5S) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
Uanis(O1S) \\sim Ueq, Uanis(O3S) \\sim Ueq, Uanis(O2S) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(F5) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(Cl2) = Uanis(Cl1) = Uanis(Cl3)
4. Rigid body (RIGU) restrains
 F1, F2, F3, F4, F5, F6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 1*[Sof(Cl1)]+1*[Sof(Cl2)]+1*[Sof(Cl3)]=0.5 with esd of 0.000001
 Fixed Sof: C5S(0.2) H5SA(0.2) H5SB(0.2) H5SC(0.2) O6S(0.2) H6S(0.2) O4S(0.25)
 H4SA(0.25) H4SB(0.25) O2S(0.33333) H2SA(0.33333) H2SB(0.33333) P1(0.5) F1(0.5)
 F2(0.5) F3(0.5) F4(0.5) F5(0.5) F6(0.5) O3S(0.5) H3SA(0.5) H3SB(0.5)
6.a Riding coordinates:
 C5S(H5SA,H5SB,H5SC), O4S(H4SA,H4SB), O2S(H2SA,H2SB), O3S(H3SA,H3SB)
6.b Free rotating group:
 O1S(H1SA,H1SB), P1(F1,F2,F3,F4,F5,F6)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C11(H11), C14(H14),
 C15(H15), C16(H16), C17(H17), C20(H20), C21(H21), C22(H22), C23(H23), C28(H28),
  C30(H30)
6.d Idealised tetrahedral OH refined as rotating group:
 O6S(H6S)
;
_shelx_res_checksum              11061
_olex2_exptl_crystal_mounting_method 'mounted in oil on a MiTeGen microloop'
_olex2_submission_original_sample_id LMOF74PF6
_olex2_submission_special_instructions 'No special instructions were received'