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_7713684
_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         'C31 H20 Ga N4 O4, 0.75(C2 H6 O1), F6 P'
_chemical_formula_sum            'C32.5 H24.5 F6 Ga N4 O4.75 P'
_chemical_formula_weight         761.75
_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             2021-07-15
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2023-04-04 deposited with the CCDC.	2023-08-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.0030(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.8706(9)
_cell_length_b                   8.8591(5)
_cell_length_c                   23.0866(12)
_cell_measurement_reflns_used    9159
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.500
_cell_measurement_theta_min      2.481
_cell_volume                     3069.1(3)
_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 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Quest ECO'
_diffrn_measurement_method       '\w and \f 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  0.0873
_diffrn_reflns_av_unetI/netI     0.0472
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            47191
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.633
_diffrn_reflns_theta_min         2.481
_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    1.035
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6752
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0734 before and 0.0645 after correction.
The Ratio of minimum to maximum transmission is 0.9056.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.649
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1542
_exptl_crystal_size_max          0.284
_exptl_crystal_size_mid          0.117
_exptl_crystal_size_min          0.072
_refine_diff_density_max         1.134
_refine_diff_density_min         -1.104
_refine_diff_density_rms         0.091
_refine_ls_extinction_coef       0.0014(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     535
_refine_ls_number_reflns         7116
_refine_ls_number_restraints     228
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0876
_refine_ls_R_factor_gt           0.0581
_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^)+(0.0561P)^2^+7.4699P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1330
_refine_ls_wR_factor_ref         0.1465
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5278
_reflns_number_total             7116
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01761c2.cif
_cod_data_source_block           5
_cod_original_formula_sum        'C32.50 H24.50 F6 Ga N4 O4.75 P'
_cod_database_code               7713684
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.929
_shelx_estimated_absorpt_t_min   0.758
_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, All O(H) groups
2. Uiso/Uaniso restraints and constraints
C30 \\sim C30A \\sim C31 \\sim C32 \\sim C33 \\sim C34 \\sim C35 \\sim C37
\\sim O29 \\sim O29A \\sim O36 \\sim O38 \\sim O39: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
C30A \\sim C31A \\sim C32A \\sim C33A \\sim C34A \\sim C35A \\sim C37A \\sim
O29A \\sim O36A \\sim O38A \\sim O39A: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
C41A \\sim C42A \\sim O40A \\sim C41B \\sim C42B \\sim O40B: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(O38A) = Uanis(O38)
Uanis(O39A) = Uanis(O39)
Uanis(C37A) = Uanis(C37)
Uanis(C34A) = Uanis(C34)
3. Others
 Sof(C41B)=Sof(H41A)=Sof(H41B)=Sof(C42B)=Sof(H42C)=Sof(H42B)=Sof(H42A)=
 Sof(O40B)=Sof(H40B)=0.75*(1-FVAR(2))
 Sof(C41A)=Sof(H41D)=Sof(H41C)=Sof(C42A)=Sof(H42D)=Sof(H42F)=Sof(H42E)=
 Sof(O40A)=Sof(H40A)=0.75*FVAR(2)
 Sof(O29A)=Sof(C30A)=Sof(C31A)=Sof(H31A)=Sof(C32A)=Sof(H32A)=Sof(C33A)=
 Sof(H33A)=Sof(C34A)=Sof(C35A)=Sof(C37A)=Sof(O36A)=Sof(O38A)=Sof(H38A)=
 Sof(O39A)=1-FVAR(2)
 Sof(C30)=Sof(C31)=Sof(H31)=Sof(C32)=Sof(H32)=Sof(C33)=Sof(H33)=Sof(C34)=
 Sof(C35)=Sof(C37)=Sof(O29)=Sof(O36)=Sof(O38)=Sof(H38)=Sof(O39)=FVAR(2)
4.a Riding coordinates:
 O38A(H38A), O40A(H40A), O40B(H40B)
4.b Free rotating group:
 O29A(C30A,C31A,C32A,C33A,C34A,C35A,C37A,O36A,O38A)
4.c Secondary CH2 refined with riding coordinates:
 C41A(H41D,H41C), C41B(H41A,H41B)
4.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11), C16(H16),
 C17(H17), C18(H18), C20(H20), C21(H21), C23(H23), C24(H24), C25(H25), C31(H31),
  C32(H32), C33(H33), C31A(H31A), C32A(H32A), C33A(H33A)
4.e Idealised Me refined as rotating group:
 C42A(H42D,H42F,H42E), C42B(H42C,H42B,H42A)
4.f Idealised tetrahedral OH refined as rotating group:
 O38(H38)
;
_shelx_res_checksum              85782
_olex2_exptl_crystal_mounting_method 'mounted in oil on a MiTeGen microloop'
_olex2_submission_original_sample_id LMOF40r3
_olex2_submission_special_instructions 'No special instructions were received'