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_7704149
_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_formula_moiety
'2(C13 H24 Co N5 O2), Cl, 3(F6 P), 0.33(H2 O)'
_chemical_formula_sum            'C26 H48.67 Cl Co2 F18 N10 O4.33 P3'
_chemical_formula_weight         1158.95
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-12-19
_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                 90.2890(19)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.0010(7)
_cell_length_b                   16.7068(8)
_cell_length_c                   16.6727(8)
_cell_measurement_reflns_used    9194
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.66
_cell_measurement_theta_min      3.04
_cell_volume                     4178.4(3)
_computing_cell_refinement       'SAINT v8.38A (Bruker, 2016)'
_computing_data_collection       'APEX 3 (Bruker, 2017) '
_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 0.999
_diffrn_measured_fraction_theta_max 0.991
_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  0.1324
_diffrn_reflns_av_unetI/netI     0.0385
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            9027
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.005
_diffrn_reflns_theta_min         2.438
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Siemens, KFF Mo 2K -90 C'
_exptl_absorpt_coefficient_mu    1.103
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6778
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0916 before and 0.0830 after correction. The Ratio of minimum to maximum transmission is 0.9093. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.842
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2349
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.779
_refine_diff_density_min         -0.987
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     598
_refine_ls_number_reflns         9027
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0502
_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^)+(0.0403P)^2^+20.3916P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1142
_refine_ls_wR_factor_ref         0.1214
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7972
_reflns_number_total             9027
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01123a2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7704149--7704151.cif.'
_cod_database_code               7704149
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.917
_shelx_estimated_absorpt_t_min   0.755
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.588(2)
 0.0796(13) 0.1666(14) 0.1656(15)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
3. Restrained distances
 H21A-H6D
 2.2 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(N13) \\sim Ueq, Uanis(C12) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
5. Others
 Fixed Sof: Cl1A(0.2) Cl1(0.8) O6(0.33333) H6C(0.33333) H6D(0.33333)
6.a Riding coordinates:
 O6(H6C,H6D)
6.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C5(H5A,H5B), C6(H6A,H6B), C8(H8A,H8B), C9(H9A,H9B),
 N1(H1A,H1B), N4(H4A,H4B), N7(H7A,H7B), C22(H22A,H22B), C23(H23A,H23B),
 C25(H25A,H25B), C26(H26A,H26B), C28(H28A,H28B), C29(H29A,H29B), N21(H21A,H21B),
  N24(H24A,H24B), N27(H27A,H27B)
6.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C32(H32),
 C36(H36), C37(H37), C38(H38), C39(H39), C40(H40)
;
_shelx_res_checksum              18540
_olex2_exptl_crystal_mounting_method 'mounted in oil on a MiTeGen microloop'
_olex2_submission_original_sample_id KMD10a
_olex2_submission_special_instructions 'No special instructions were received'