Impact of ligand steric hindrance on the phenoxazinone synthase-like reactivity and antibacterial activity of cobalt(iii) complexes of N2O donor ligands
Vidya, Kannan Sree; Yamuna, Ganesh; Bhuvanesh, Nattamai; Ghosh, Ayyan; Dasgupta, Sreeja; Mandal, Sukanta; Vasanthkumar, Rajkumar; Gurusaravanan, Packiaraj; Sundaravel, Karuppasamy; New Journal of Chemistry 49 (2025) 8576–8593; doi:10.1039/D5NJ00515A

data_7063880
_publ_section_title
;
 Impact of ligand steric hindrance on the phenoxazinone synthase-like
 reactivity and antibacterial activity of cobalt(iii) complexes of N2O
 donor ligands
;
_journal_issue                   20
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              8576
_journal_page_last               8593
_journal_paper_doi               10.1039/D5NJ00515A
_journal_volume                  49
_journal_year                    2025
_chemical_formula_moiety         'C16 H23 Co N4 O2, 2(N O3)'
_chemical_formula_sum            'C16 H23 Co N6 O8'
_chemical_formula_weight         486.33
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-11-01
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2025-02-03 deposited with the CCDC.	2025-04-15 downloaded from the CCDC.
;
_cell_angle_alpha                101.111(2)
_cell_angle_beta                 103.881(2)
_cell_angle_gamma                96.082(2)
_cell_formula_units_Z            2
_cell_length_a                   9.4192(2)
_cell_length_b                   10.3525(2)
_cell_length_c                   10.7729(3)
_cell_measurement_reflns_used    16506
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      79.4900
_cell_measurement_theta_min      4.8730
_cell_volume                     987.84(4)
_computing_cell_refinement       'CrysAlisPro 1.171.43.68a (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 42.101a 64-bit (release 31-08-2023))'
_computing_data_reduction        'CrysAlisPro 1.171.43.68a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     16.00  42.00   0.50    0.10    --   30.00  55.00 -34.82   52
  2  \w     -1.00  25.00   0.50    0.10    --   18.00  67.00  59.82   52
  3  \w      0.00  26.00   0.50    0.10    --   18.00  66.00 162.17   52
  4  \w     35.00 119.00   0.50    0.10    --   47.47  44.00 169.89  168
  5  \w     46.00  74.00   0.50    0.50    --  113.25 -61.00  60.00   56
  6  \w     43.00  74.00   0.50    0.50    --  113.25 -61.00 120.00   62
  7  \w     43.00  75.00   0.50    0.50    --  113.25 -61.00  30.00   64
  8  \w     43.00  74.00   0.50    0.50    --  113.25 -61.00  90.00   62
  9  \w     43.00  75.00   0.50    0.50    --  113.25 -61.00 -60.00   64
 10  \w     45.00  73.00   0.50    0.50    --  113.25 -61.00-150.00   56
 11  \w     43.00  75.00   0.50    0.50    --  113.25 -61.00-180.00   64
 12  \w     51.00 116.00   0.50    0.10    --   47.47-157.00-105.00  130
 13  \w     46.00  71.00   0.50    0.50    --  113.25-125.00-120.00   50
 14  \w     75.00 111.00   0.50    0.50    --  113.25-125.00-120.00   72
 15  \w     51.00 134.00   0.50    0.50    --  113.25-157.00-105.00  166
 16  \w     44.00  73.00   0.50    0.50    --  113.25-125.00 -30.00   58
 17  \w     77.00 102.00   0.50    0.50    --  113.25-125.00 -30.00   50
 18  \w     44.00 109.00   0.50    0.50    --  113.25-120.00  49.00  130
 19  \w     44.00  70.00   0.50    0.50    --  113.25-125.00 120.00   52
 20  \w     85.00 111.00   0.50    0.50    --  113.25-125.00 120.00   52
 21  \w     55.00 104.00   0.50    0.50    --  113.25 -95.00 150.00   98
 22  \w     78.00 105.00   0.50    0.50    --  113.25 -95.00  90.00   54
 23  \w     42.00 106.00   0.50    0.50    --  113.25 -95.00 -30.00  128
 24  \w     47.00  97.00   0.50    0.50    --  113.25 -95.00 -90.00  100
 25  \w     31.00  90.00   0.50    0.10    --   47.47-120.00  49.00  118
 26  \w    -33.00  -5.00   0.50    0.10    --  -22.00 -61.00  92.29   56
 27  \w    -54.00 -28.00   0.50    0.10    --  -42.00 -50.00 165.36   52
 28  \w    -42.00 -11.00   0.50    0.10    --  -26.00 -55.00  54.78   62
 29  \w    -42.00 -15.00   0.50    0.10    --  -30.00 -55.00  39.11   54
 30  \w    -38.00 -11.00   0.50    0.10    --  -26.00 -57.00 -16.47   54
 31  \w    -57.00 -29.00   0.50    0.10    --  -42.00 -49.00-174.21   56
 32  \w    -42.00 -15.00   0.50    0.10    --  -30.00 -55.00-160.99   54
 33  \w   -117.00 -33.00   0.50    0.10    --  -46.00 -47.00-154.37  168
 34  \w   -117.00 -33.00   0.50    0.10    --  -46.00 -47.00 -99.14  168
 35  \w   -122.00 -37.00   0.50    0.10    --  -50.00 -45.00 -80.90  170
 36  \w   -117.00 -33.00   0.50    0.10    --  -46.00 -47.00 -41.42  168
 37  \w   -117.00 -33.00   0.50    0.10    --  -46.00 -47.00   0.42  168
 38  \w   -117.00 -33.00   0.50    0.10    --  -46.00 -46.00  31.51  168
 39  \w   -117.00 -33.00   0.50    0.10    --  -46.00 -47.00 117.01  168
 40  \w   -161.00 -77.00   0.50    0.50    --  -91.75-120.00  49.00  168
 41  \w   -142.00 -57.00   0.50    0.10    --  -70.00 -47.00 164.58  170
 42  \w   -138.00 -53.00   0.50    0.10    --  -66.00 -47.00  93.31  170
 43  \w   -142.00 -57.00   0.50    0.10    --  -70.00 -47.00  47.24  170
 44  \w   -142.00 -57.00   0.50    0.10    --  -70.00 -47.00 -19.46  170
 45  \w   -142.00 -57.00   0.50    0.10    --  -70.00 -47.00 -56.71  170
 46  \w   -142.00 -57.00   0.50    0.10    --  -70.00 -47.00 -85.36  170
 47  \w   -142.00 -57.00   0.50    0.10    --  -70.00 -47.00-102.69  170
 48  \w   -142.00 -57.00   0.50    0.10    --  -70.00 -47.00-142.39  170
 49  \w   -125.00 -85.00   0.50    0.50    --  -91.75 -47.00 -65.23   80
 50  \w   -119.00 -51.00   0.50    0.10    --  -47.47-157.00-105.00  136
 51  \w   -143.00 -51.00   0.50    0.50    --  -91.75-157.00-105.00  184
 52  \w   -106.00 -81.00   0.50    0.50    --  -91.75 -47.00 -39.81   50
 53  \w   -106.00 -81.00   0.50    0.50    --  -91.75 -47.00 -53.10   50
 54  \w   -105.00 -79.00   0.50    0.50    --  -91.75 -46.00  20.53   52
 55  \w    -84.00 -58.00   0.50    0.10    --  -70.00 -47.00 130.13   52
 56  \w   -120.00 -83.00   0.50    0.50    --  -91.75 -47.00  91.72   74
 57  \w   -160.00-127.00   0.50    0.50    --  -91.75 -47.00  91.72   66
 58  \w   -134.00 -49.00   0.50    0.10    --  -62.00 -46.00 177.45  170
 59  \w   -104.00 -79.00   0.50    0.50    --  -91.75 -46.00 169.68   50
 60  \w   -134.00 -49.00   0.50    0.10    --  -62.00 -46.00  80.91  170
 61  \w   -138.00 -53.00   0.50    0.10    --  -66.00 -46.00  -5.09  170
 62  \w   -118.00 -80.00   0.50    0.50    --  -91.75 -46.00 -93.52   76
 63  \w   -113.00 -80.00   0.50    0.50    --  -91.75 -46.00-108.72   66
 64  \w   -158.00-127.00   0.50    0.50    --  -91.75 -46.00 -93.52   62
 65  \w   -106.00 -79.00   0.50    0.50    --  -91.75 -45.00   0.00   54
 66  \w   -109.00 -77.00   0.50    0.50    --  -90.00 -46.00  36.71   64
 67  \w    -87.00 -61.00   0.50    0.10    --  -74.00 -46.00 116.42   52
 68  \w   -138.00 -53.00   0.50    0.10    --  -66.00 -45.00 135.66  170
 69  \w   -152.00-126.00   0.50    0.50    --  -91.75 -46.00 169.68   52
 70  \w   -117.00 -81.00   0.50    0.50    --  -91.75 -45.00  60.00   72
 71  \w   -163.00-126.00   0.50    0.50    --  -91.75 -45.00  60.00   74
 72  \w   -157.00-118.00   0.50    0.50    --  -91.75 -45.00 120.00   78
 73  \w   -112.00 -79.00   0.50    0.50    --  -91.75 -45.00 120.00   66
 74  \w   -109.00 -83.00   0.50    0.50    --  -91.75 -45.00 150.00   52
 75  \w   -161.00-135.00   0.50    0.50    --  -91.75 -45.00   0.00   52
 76  \w   -160.00-134.00   0.50    0.50    --  -91.75 -45.00 -30.00   52
 77  \w   -164.00-131.00   0.50    0.50    --  -91.75 -43.00-132.76   66
 78  \w   -105.00 -79.00   0.50    0.50    --  -91.75 -45.00-150.00   52
 79  \w   -103.00 -78.00   0.50    0.50    --  -91.75 -43.00-132.76   50
 80  \w   -105.00 -79.00   0.50    0.50    --  -91.75 -45.00 -30.00   52
 81  \w   -106.00 -77.00   0.50    0.50    --  -90.00 -37.00-176.35   58
 82  \w    -92.00 -65.00   0.50    0.10    --  -78.00 -40.00 -37.82   54
 83  \w   -109.00 -74.00   0.50    0.50    --  -86.00 -41.00  59.50   70
 84  \w   -106.00 -80.00   0.50    0.50    --  -91.75 -39.00  87.12   52
 85  \w   -107.00 -79.00   0.50    0.50    --  -91.75 -42.00 127.92   56
 86  \w    -84.00  -9.00   0.50    0.10    --  -47.47 120.00 134.00  150
 87  \w    -84.00 -22.00   0.50    0.50    --  -91.75 120.00 134.00  124
 88  \w   -108.00 -29.00   0.50    0.10    --  -47.47 157.00 -70.00  158
 89  \w    108.00 142.00   0.50    0.50    --  113.25  61.00-150.00   68
 90  \w    150.00 177.00   0.50    0.50    --  113.25  61.00-150.00   54
 91  \w    145.00 178.00   0.50    0.50    --  113.25  61.00-180.00   66
 92  \w    107.00 137.00   0.50    0.50    --  113.25  61.00-180.00   60
 93  \w    106.00 133.00   0.50    0.50    --  113.25  61.00-120.00   54
 94  \w    139.00 177.00   0.50    0.50    --  113.25  61.00-120.00   76
 95  \w    106.00 178.00   0.50    0.50    --  113.25  61.00 -60.00  144
 96  \w    102.00 142.00   0.50    0.50    --  113.25  45.00  30.00   80
 97  \w    148.00 176.00   0.50    0.50    --  113.25  45.00  30.00   56
 98  \w    143.00 177.00   0.50    0.50    --  113.25  45.00 120.00   68
 99  \w    105.00 137.00   0.50    0.50    --  113.25  45.00 120.00   64
100  \w    117.00 142.00   0.50    0.50    --  113.25  45.00  60.00   50
101  \w    110.00 136.00   0.50    0.50    --  113.25  45.00 150.00   52
102  \w    150.00 177.00   0.50    0.50    --  113.25  45.00  60.00   54
103  \w    105.00 178.00   0.50    0.50    --  113.25  45.00  90.00  146
104  \w    102.00 154.00   0.50    0.50    --  113.25  45.00   0.00  104
105  \w     90.00 145.00   0.50    0.50    --  102.00  35.00 -28.82  110
106  \w    102.00 155.00   0.50    0.50    --  113.25  45.00 -90.00  106
107  \w    101.00 173.00   0.50    0.50    --  113.25  45.00-180.00  144
108  \w     73.00 120.00   0.50    0.10    --   47.47 157.00 -70.00   94
109  \w     73.00 161.00   0.50    0.50    --  113.25 157.00 -70.00  176
110  \w     98.00 178.00   0.50    0.50    --  113.25 120.00 134.00  160
111  \w    -17.00   9.00   0.50    0.10    --   10.00  86.00 -65.07   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1676476000
_diffrn_orient_matrix_UB_12      -0.0061651000
_diffrn_orient_matrix_UB_13      -0.0155507000
_diffrn_orient_matrix_UB_21      0.0170028000
_diffrn_orient_matrix_UB_22      0.1520521000
_diffrn_orient_matrix_UB_23      0.0131518000
_diffrn_orient_matrix_UB_31      -0.0270597000
_diffrn_orient_matrix_UB_32      -0.0210470000
_diffrn_orient_matrix_UB_33      -0.1498389000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.043
_diffrn_reflns_av_unetI/netI     0.0493
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4493
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.749
_diffrn_reflns_theta_min         4.340
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           '1 mA'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_diffrn_source_voltage           '50 kV'
_exptl_absorpt_coefficient_mu    7.354
_exptl_absorpt_correction_T_max  0.762
_exptl_absorpt_correction_T_min  0.613
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.68a (Rigaku Oxford Diffraction, 2023) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.635
_exptl_crystal_description       block
_exptl_crystal_F_000             504
_exptl_crystal_size_max          0.173
_exptl_crystal_size_mid          0.102
_exptl_crystal_size_min          0.101
_refine_diff_density_max         0.329
_refine_diff_density_min         -0.627
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         4493
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0331
_refine_ls_R_factor_gt           0.0312
_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^)+(0.0447P)^2^+0.0446P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0829
_refine_ls_wR_factor_ref         0.0834
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4262
_reflns_number_total             4493
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by -179.4855\% 
around [0.00 0.71 0.71] (reciprocal) or [0.27 0.69 0.67] (direct)
;
_cod_data_source_file            d5nj00515a2.cif
_cod_data_source_block           kssv28_twin1_hklf4
_cod_database_code               7063880
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C16H24CoN4O2
_shelx_estimated_absorpt_t_max   0.524
_shelx_estimated_absorpt_t_min   0.363
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5372(13)
 0.4628(13)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
3.a Riding coordinates:
 O1(H1)
3.b Ternary CH refined with riding coordinates:
 N2(H2), N4(H4)
3.c Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C14(H14A,H14B), C15(H15A,H15B),
 C16(H16A,H16B)
3.d Aromatic/amide H refined with riding coordinates:
 C1(H1A), C2(H2A), C3(H3), C4(H4A), C9(H9), C10(H10), C11(H11), C12(H12)
;
_shelx_res_checksum              18912
_shelx_hkl_checksum              14607
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder'
_olex2_submission_original_sample_id KSB_231101_SDc_KSSV28
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.725
_oxdiff_exptl_absorpt_empirical_full_min 0.572
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2