Polypyridyl-based Co(III) Complexes of Vitamin B6 Schiff base for Photoactivated Antibacterial Therapy
Mandal, Apurba; Rai, Rohit; Saha, Sukanta; Kushwaha, Rajesh; Li , Wei; Gogoi, Hemonta; Mandal, Arif Ali; Yadav, Ashish Kumar; Huang, Huaiyi; Dutta, Arnab; Dhar, Prodyut; Banerjee, Samya; Dalton Transactions  (2023) –; doi:10.1039/D3DT02967K

data_7714375
_publ_section_title
;
 Polypyridyl-based Co(III) Complexes of Vitamin B6 Schiff base for
 Photoactivated Antibacterial Therapy
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02967K
_journal_year                    2023
_chemical_formula_moiety
'0.5(C25 H21 Co N4 O2), 0.5(C24.906 H19 Co N4.06 O2), Cl O4, C2 H3 N'
_chemical_formula_sum            'C26.95 H23 Cl Co N5.03 O6'
_chemical_formula_weight         607.73
_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   geom
_audit_creation_date             2023-10-14
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-10-26 deposited with the CCDC.	2023-11-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.006(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.4253(3)
_cell_length_b                   14.5947(3)
_cell_length_c                   25.4953(5)
_cell_measurement_reflns_used    14825
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      23.2090
_cell_measurement_theta_min      1.6290
_cell_volume                     5285.96(19)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.15
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \f    -50.56 125.84   0.30    6.00  75.04 -15.82  31.50    --   588
  2  \w   -115.73  16.27   0.30    6.00    --  -15.82 -59.25  20.08  440
  3  \w    -68.38   0.32   0.30    6.00    --  -15.82  94.56  73.16  229
  4  \w   -115.72  16.28   0.30    6.00    --  -15.82 -59.24 173.08  440
  5  \f     46.27 229.87   0.30    6.00  13.01 -15.82 -31.50    --   612
  6  \w    -68.38   0.32   0.30    6.00    --  -15.82  94.56   1.16  229
  7  \w   -115.72  16.28   0.30    6.00    --  -15.82 -59.25-135.92  440
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0671
_diffrn_reflns_av_unetI/netI     0.0437
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            71259
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.001
_exptl_absorpt_coefficient_mu    0.803
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56993
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic bluish violet'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   bluish
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.527
_exptl_crystal_description       needle
_exptl_crystal_F_000             2495
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.763
_refine_diff_density_min         -1.574
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     702
_refine_ls_number_reflns         9312
_refine_ls_number_restraints     871
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.1221
_refine_ls_R_factor_gt           0.1027
_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^)+(0.0949P)^2^+56.0957P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2444
_refine_ls_wR_factor_ref         0.2592
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7464
_reflns_number_total             9312
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02967k2.cif
_cod_data_source_block           ard_ss_sb_01_fs_autored
_cod_database_code               7714375
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.992
_shelx_estimated_absorpt_t_min   0.976
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H6A,H6B,H6C} of C6, All C(H,H) groups
 At 1.5 times of:
  {H21A,H21B,H21C} of C21
2. Restrained distances
 C24-N6 \\sim N6-C010
 with sigma of 0.02
 C016-C24 \\sim C016-N24A
 with sigma of 0.02
 C24-N6 \\sim N24A-N6
 with sigma of 0.02
3. Rigid bond restraints
 C24, C016
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N6, C010
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N6, C24
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
N6 \\sim C010 \\sim C24: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
Uanis(C01N) \\sim Ueq, Uanis(C01W) \\sim Ueq, Uanis(C023) \\sim Ueq,
Uanis(C01X) \\sim Ueq, Uanis(C016) \\sim Ueq, Uanis(C010) \\sim Ueq,
Uanis(C00Z) \\sim Ueq, Uanis(C01V) \\sim Ueq, Uanis(C020) \\sim Ueq,
Uanis(C01U) \\sim Ueq, Uanis(C01F) \\sim Ueq, Uanis(C00R) \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.001
Uanis(O10) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(O9) \\sim
Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(N6) \\sim Ueq, Uanis(C24) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.001
Uanis(C21) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(C01V) \\sim Ueq, Uanis(C020) \\sim Ueq, Uanis(C01U) \\sim Ueq,
Uanis(C01X) \\sim Ueq, Uanis(C023) \\sim Ueq, Uanis(C01W) \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.001
Uanis(O10) \\sim Ueq, Uanis(O9) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(O5) \\sim
Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(Co1) \\sim Ueq, Uanis(Co02) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.001
Uanis(C24) \\sim Ueq, Uanis(N6) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.001
Uanis(N6) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(C24) \\sim Ueq, Uanis(N24A) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.001
Uanis(N6) = Uanis(C24)
Uanis(C24) = Uanis(N6)
Uanis(N24A) = Uanis(C24) = Uanis(N6)
Uanis(C01X) = Uanis(C010)
Uanis(C023) = Uanis(C01W) = Uanis(C01X)
Uanis(C00Z) = Uanis(C010)
Uanis(C00Z) = Uanis(O007)
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(N24A)=1-FVAR(1)
 Sof(C24)=FVAR(1)
7.a Secondary CH2 refined with riding coordinates:
 C00O(H00A,H00B), C14(H14A,H14B), C01A(H01A,H01B), C13(H13A,H13B)
7.b Aromatic/amide H refined with riding coordinates:
 C23(H23), C19(H19), C00T(H00T), C00U(H00U), C16(H16), C00X(H00X), C9(H9),
 C012(H012), C8(H8), C17(H17), C18(H18), C017(H017), C018(H018), C019(H019),
 C10(H10), C01E(H01E), C01F(H01F), C01G(H01G), C11(H11), C01I(H01I), C5(H5),
 C01L(H01L), C01M(H01M), C01N(H01N), C3(H3), C4(H4), C1(H1), C01U(H01U),
 C01W(H01W), C01X(H01X), C020(H020), C023(H023)
7.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C6(H6A,H6B,H6C)
;
_shelx_res_checksum              500
_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
;