Synthesis and characterisation of Co(iii) complexes of N-formyl hydroxylamines and antibacterial activity of a Co(iii) peptide deformylase inhibitor complex.
Kozsup, Máté; Keogan, Donal M.; Fitzgerald-Hughes, Deirdre; Enyedy, Éva A; Twamley, Brendan; Buglyó, Péter; Griffith, Darren M.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 6980–6988; doi:10.1039/d0dt01123a

data_7704150
_publ_section_title
;
 Synthesis and characterisation of Co(iii) complexes of N-formyl
 hydroxylamines and antibacterial activity of a Co(iii) peptide
 deformylase inhibitor complex.
;
_journal_issue                   21
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6980
_journal_page_last               6988
_journal_paper_doi               10.1039/d0dt01123a
_journal_volume                  49
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C22 H34 F N7 O4, C4 H8 O'
_chemical_formula_sum            'C26 H42 F N7 O5'
_chemical_formula_weight         551.66
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-04-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-03-24 deposited with the CCDC.	2020-04-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 126.2917(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.6357(10)
_cell_length_b                   9.0441(4)
_cell_length_c                   17.7227(8)
_cell_measurement_reflns_used    9921
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.25
_cell_measurement_theta_min      3.23
_cell_volume                     2795.2(2)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2016)'
_computing_data_collection       'APEX 3 (Bruker, 2016) '
_computing_data_reduction        'SAINT V8.38A (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_av_unetI/netI     0.0242
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            31597
_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         27.280
_diffrn_reflns_theta_min         2.537
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Siemens, KFF Mo 2K -90 C'
_exptl_absorpt_coefficient_mu    0.097
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.7140
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0596 before and 0.0556 after correction. The Ratio of minimum to maximum transmission is 0.9577. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.439
_exptl_crystal_size_mid          0.188
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.265
_refine_diff_density_min         -0.350
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details
;
 Flack x determined using 2520 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.1(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     410
_refine_ls_number_reflns         6264
_refine_ls_number_restraints     106
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0370
_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^)+(0.0482P)^2^+1.6353P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0880
_refine_ls_wR_factor_ref         0.0926
_reflns_Friedel_coverage         0.878
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                5719
_reflns_number_total             6264
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01123a2.cif
_cod_data_source_block           GSK322
_cod_depositor_comments
'Adding full bibliography for 7704149--7704151.cif.'
_cod_database_code               7704150
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.986
_shelx_estimated_absorpt_t_min   0.959
_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
2. Restrained distances
 N15-H15 = N16-H16
 0.9 with sigma of 0.01
 O12-H12
 0.9 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C35A \\sim C36A \\sim C37A \\sim C38A \\sim C35 \\sim C36 \\sim C37 \\sim C38:
within 2A with sigma of 0.004 and sigma for terminal atoms of 0.008
4. Others
 Fixed Sof: O34(0.85) O34A(0.15) C35A(0.15) H35C(0.15) H35D(0.15) C36A(0.15)
 H36C(0.15) H36D(0.15) C37A(0.15) H37C(0.15) H37D(0.15) C38A(0.15) H38C(0.15)
 H38D(0.15) C35(0.85) H35A(0.85) H35B(0.85) C36(0.85) H36A(0.85) H36B(0.85)
 C37(0.85) H37A(0.85) H37B(0.85) C38(0.85) H38A(0.85) H38B(0.85)
5.a Ternary CH refined with riding coordinates:
 C5(H5), C7(H7), C32(H32)
5.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C6(H6A,H6B), C8(H8A,H8B),
 C25(H25A,H25B), C26(H26A,H26B), C28(H28A,H28B), C29(H29A,H29B), C31(H31A,H31B),
  C33(H33A,H33B), C35A(H35C,H35D), C36A(H36C,H36D), C37A(H37C,H37D), C38A(H38C,
 H38D), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B)
5.c Aromatic/amide H refined with riding coordinates:
 C10(H10)
5.d Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C)
;
_shelx_res_checksum              99195
_olex2_exptl_crystal_mounting_method 'mounted in oil on a MiTeGen microloop'
_olex2_submission_original_sample_id DG-GSKBi
_olex2_submission_special_instructions 'No special instructions were received'