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_7714376
_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(C35 H28 Co N5 O3), 0.5(C35 H27 Co N5 O3), F6 P, 0.875(H2 O), 0.5(C2 H4 O), 1[C2H6O], 0.5[H2O]'
_chemical_formula_sum            'C36 H31.5 Co F6 N5 O4.5 P'
_chemical_formula_weight         810.06
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-10-10
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2023-10-26 deposited with the CCDC.	2023-11-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.004(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.4901(4)
_cell_length_b                   15.8579(3)
_cell_length_c                   21.6752(4)
_cell_measurement_reflns_used    10038
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      25.5500
_cell_measurement_theta_min      1.6550
_cell_volume                     7331.5(2)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150.15
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -22.01 115.09   0.30    5.00  13.01 -15.82 -31.50    --   457
  2  \w   -115.72  16.28   0.30    5.00    --  -15.82 -59.25  20.08  440
  3  \w   -115.72  16.28   0.30    5.00    --  -15.82 -59.25  71.08  440
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0536
_diffrn_reflns_av_unetI/netI     0.0412
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            66736
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.600
_exptl_absorpt_coefficient_mu    0.590
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65874
_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 brownish brown'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.468
_exptl_crystal_description       block
_exptl_crystal_F_000             3316
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.992
_refine_diff_density_min         -0.622
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1015
_refine_ls_number_reflns         12896
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0643
_refine_ls_R_factor_gt           0.0522
_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^)+(0.0706P)^2^+12.5539P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1383
_refine_ls_wR_factor_ref         0.1487
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10540
_reflns_number_total             12896
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02967k2.cif
_cod_data_source_block           ard_ss_sb_03_fs_autored
_cod_original_formula_sum        'C36 H31.50 Co F6 N5 O4.50 P'
_cod_database_code               7714376
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.994
_shelx_estimated_absorpt_t_min   0.988
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 P004-F005 \\sim P0-F0
 with sigma of 0.02
 P004-F017 \\sim P0-F1
 with sigma of 0.02
 P004-F01T \\sim P0-F01U
 with sigma of 0.02
 P004-F02L \\sim P0-F02M
 with sigma of 0.02
 P004-F02T \\sim P0-F02U
 with sigma of 0.02
 P004-F02V \\sim P0-F02W
 with sigma of 0.02
 F005-F017 \\sim F0-F1
 with sigma of 0.04
 F005-F01T \\sim F0-F01U
 with sigma of 0.04
 F005-F02L \\sim F0-F02M
 with sigma of 0.04
 F005-F02T \\sim F0-F02U
 with sigma of 0.04
 F005-F02V \\sim F0-F02W
 with sigma of 0.04
 F017-F01T \\sim F1-F01U
 with sigma of 0.04
 F017-F02L \\sim F1-F02M
 with sigma of 0.04
 F017-F02T \\sim F1-F02U
 with sigma of 0.04
 F017-F02V \\sim F1-F02W
 with sigma of 0.04
 F01T-F02L \\sim F01U-F02M
 with sigma of 0.04
 F01T-F02T \\sim F01U-F02U
 with sigma of 0.04
 F01T-F02V \\sim F01U-F02W
 with sigma of 0.04
 F02L-F02T \\sim F02M-F02U
 with sigma of 0.04
 F02L-F02V \\sim F02M-F02W
 with sigma of 0.04
 F02T-F02V \\sim F02U-F02W
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C35) \\sim Ueq, Uanis(O6) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.001
Uanis(F0) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
4. Others
 Sof(F02M)=Sof(F02W)=Sof(P0)=Sof(F0)=Sof(F1)=Sof(F01U)=Sof(F02U)=1-FVAR(1)
 Sof(P004)=Sof(F005)=Sof(F017)=Sof(F01T)=Sof(F02L)=Sof(F02T)=Sof(F02V)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C019(H01A,H01B), C34(H34A,H34B)
5.b Aromatic/amide H refined with riding coordinates:
 N5(H5), C00T(H00T), C15(H15), C7(H7), C016(H016), C22(H22), C23(H23),
 C01H(H01H), C01J(H01J), C2(H2), C1(H1), C25(H25), C38(H38), C01R(H01R),
 C01U(H01U), C19(H19), C14(H14), C01X(H01X), C01Y(H01Y), C13(H13), C022(H022),
 C023(H023), C024(H024), C3(H3A), C4(H4), C027(H027), C24(H24), C11(H11),
 C02B(H02B), C02D(H02D), C02G(H02G), C02H(H02H), C02I(H02I), C02M(H02M),
 C12(H12), C02O(H02O), C02P(H02P), C02Q(H02Q), C30(H30), C32(H32), C31(H31),
 C28(H28), C29(H29), C35(H35)
5.c Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C02K(H02A,H02C,H02E), C36(H36A,H36B,H36C)
5.d Idealised tetrahedral OH refined as rotating group:
 O00A(H00A), O3(H3)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              68862
_shelx_fab_checksum              17029
_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
;