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_7704151
_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         '5(H2 O), 2(Cl), C25 H24 Co N5 O2'
_chemical_formula_sum            'C25 H34 Cl2 Co N5 O7'
_chemical_formula_weight         646.40
_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             2018-12-05
_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                 105.564(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.2195(12)
_cell_length_b                   13.7845(11)
_cell_length_c                   14.5792(13)
_cell_measurement_reflns_used    9966
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.54
_cell_measurement_theta_min      2.70
_cell_volume                     2946.5(4)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0380
_diffrn_reflns_av_unetI/netI     0.0471
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13118
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.564
_diffrn_reflns_theta_min         2.860
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Siemens, KFF Mo 2K -90 C'
_exptl_absorpt_coefficient_mu    0.815
_exptl_absorpt_correction_T_max  0.745553
_exptl_absorpt_correction_T_min  0.658290
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.

Final HKLF 4 output contains 47479 reflections, Rint = 0.0701
 (21198 with I > 3sig(I), Rint = 0.0547)
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.295
_refine_diff_density_min         -2.060
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     390
_refine_ls_number_reflns         13118
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0870
_refine_ls_R_factor_gt           0.0697
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0586P)^2^+17.6837P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1685
_refine_ls_wR_factor_ref         0.1798
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10966
_reflns_number_total             13118
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01123a2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7704149--7704151.cif.'
_cod_database_code               7704151
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.938
_shelx_estimated_absorpt_t_min   0.764
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.8304(15)
 0.1696(15)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
3. Uiso/Uaniso restraints and constraints
Cl2D \\sim Cl2B \\sim Cl2C \\sim Cl2A: within 2A with sigma of 0.005 and sigma
for terminal atoms of 0.01
Cl2B \\sim Cl2C \\sim Cl2A \\sim Cl2D: within 2A with sigma of 0.005 and sigma
for terminal atoms of 0.01
Uanis(O4) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Others
 1*[Sof(Cl2D)]+1*[Sof(Cl2B)]+1*[Sof(Cl2C)]+1*[Sof(Cl2A)]=1 with esd of 0.001
5.a Riding coordinates:
 O5(H5A,H5B), O1(H1A,H1B), O4(H4A,H4B), O3(H3A,H3B), O2(H2A,H2B)
5.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C14(H14A,H14B), C21(H21A,H21B)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C9(H9), C10(H10), C11(H11), C12(H12),
 C16(H16), C17(H17), C18(H18), C19(H19), C24(H24), C28(H28), C29(H29), C30(H30),
  C31(H31), C32(H32)
;
_shelx_res_checksum              13936
_olex2_exptl_crystal_mounting_method 'mounted in oil on a MiTeGen microloop'
_olex2_submission_original_sample_id KMD9
_olex2_submission_special_instructions 'No special instructions were received'