Group 10 complexes of benzothiazolehydrazone- and imidazo[1,5-<i>a</i>]pyridine-based ligands: structural artistry, biophysical study, and catalytic activity.
Rayasingh, Amlan Ranjan; Manivannan, Vadivelu; Dalton transactions (Cambridge, England : 2003) 54 (2025) 16939–16954; doi:10.1039/d5dt02077h

data_7719705
_publ_section_title
;
 Group 10 complexes of benzothiazolehydrazone- and
 imidazo[1,5-<i>a</i>]pyridine-based ligands: structural artistry,
 biophysical study, and catalytic activity.
;
_journal_issue                   45
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16939
_journal_page_last               16954
_journal_paper_doi               10.1039/d5dt02077h
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety
'C22 H16.619 N3 Ni0.5 O2, 1.344(Cl0.744), 1[H2O]'
_chemical_formula_sum            'C22 H18.62 Cl N3 Ni0.5 O3'
_chemical_formula_weight         437.82
_chemical_name_systematic        1071Ni
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2025-08-26
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2025-08-26 deposited with the CCDC.	2025-10-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.237(7)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.587(5)
_cell_length_b                   13.925(4)
_cell_length_c                   18.008(5)
_cell_measurement_reflns_used    9166
_cell_measurement_temperature    298.00
_cell_measurement_theta_max      24.92
_cell_measurement_theta_min      2.38
_cell_volume                     4452(2)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      298.00
_diffrn_detector_area_resol_mean 7.9
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  CMOS-PHOTONII-7
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0398
_diffrn_reflns_av_unetI/netI     0.0183
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            50189
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.323
_diffrn_reflns_theta_min         2.013
_diffrn_source                   'X-ray Tube'
_diffrn_source_current           0.0
_diffrn_source_power             0.0
_diffrn_source_voltage           0.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.608
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6562
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1533 before and 0.0647 after correction.
The Ratio of minimum to maximum transmission is 0.8806.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'light green'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_description       block
_exptl_crystal_F_000             1813
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.691
_refine_diff_density_min         -0.666
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         3960
_refine_ls_number_restraints     848
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.0840
_refine_ls_R_factor_gt           0.0736
_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^)+(0.0958P)^2^+13.3283P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1929
_refine_ls_wR_factor_ref         0.2052
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3458
_reflns_number_total             3960
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02077h2.cif
_cod_data_source_block           1f
_cod_depositor_comments
'Adding full bibliography for 7719702--7719718.cif.'
_cod_original_formula_sum        'C22 H18.62 Cl N3 Ni0.50 O3'
_cod_database_code               7719705
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.942
_shelx_estimated_absorpt_t_min   0.898
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 C22-C17 \\sim C22A-C17A
 with sigma of 0.02
 C22-C21 \\sim C22A-C21A
 with sigma of 0.02
 C22-C13 \\sim C22A-C13A
 with sigma of 0.02
 C17-C16 \\sim C17A-C16A
 with sigma of 0.02
 C17-C18 \\sim C17A-C18A
 with sigma of 0.02
 C15-C14 \\sim C15A-C14A
 with sigma of 0.02
 C15-C16 \\sim C15A-C16A
 with sigma of 0.02
 C14-C13 \\sim C14A-C13A
 with sigma of 0.02
 C14-O4 \\sim C14A-O2A
 with sigma of 0.02
 C21-C20 \\sim C21A-C20A
 with sigma of 0.02
 C12-C13 \\sim C12-C13A
 with sigma of 0.02
 C20-C19 \\sim C20A-C19A
 with sigma of 0.02
 C19-C18 \\sim C19A-C18A
 with sigma of 0.02
 C22-C14 \\sim C22A-C14A
 with sigma of 0.04
 C22-C12 \\sim C22A-C12
 with sigma of 0.04
 C22-C20 \\sim C22A-C20A
 with sigma of 0.04
 C22-C16 \\sim C22A-C16A
 with sigma of 0.04
 C22-C18 \\sim C22A-C18A
 with sigma of 0.04
 C17-C15 \\sim C17A-C15A
 with sigma of 0.04
 C17-C21 \\sim C17A-C21A
 with sigma of 0.04
 C17-C13 \\sim C17A-C13A
 with sigma of 0.04
 C17-C19 \\sim C17A-C19A
 with sigma of 0.04
 C15-C13 \\sim C15A-C13A
 with sigma of 0.04
 C15-O4 \\sim C15A-O2A
 with sigma of 0.04
 C14-C12 \\sim C14A-C12
 with sigma of 0.04
 C14-C16 \\sim C14A-C16A
 with sigma of 0.04
 C21-C13 \\sim C21A-C13A
 with sigma of 0.04
 C21-C19 \\sim C21A-C19A
 with sigma of 0.04
 C20-C18 \\sim C20A-C18A
 with sigma of 0.04
 C13-O4 \\sim C13A-O2A
 with sigma of 0.04
 C16-C18 \\sim C16A-C18A
 with sigma of 0.04
 Ni1-H2A \\sim Ni1-H2B
 with sigma of 0.02
3. Restrained planarity
 C22, C17, C15, C14, C21, C20, C13, C16, C19, C18
 with sigma of 0.001
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
Uanis(Cl1) = Uanis(Cl2)
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(C22A)=Sof(C17A)=Sof(C15A)=Sof(H15A)=Sof(C14A)=Sof(C21A)=Sof(H21A)=
 Sof(C20A)=Sof(H20A)=Sof(C13A)=Sof(O2A)=Sof(C16A)=Sof(H16A)=Sof(C19A)=Sof(H19A)=
 Sof(C18A)=Sof(H18A)=1-FVAR(1)
 Sof(C22)=Sof(C17)=Sof(C15)=Sof(H15)=Sof(C14)=Sof(C21)=Sof(H21)=Sof(C20)=
 Sof(H20)=Sof(C13)=Sof(O4)=Sof(H4A)=Sof(C16)=Sof(H16)=Sof(C19)=Sof(H19)=
 Sof(C18)=Sof(H18)=FVAR(1)
 Fixed Sof: Cl2A(0.5) Cl2(0.256) Cl1(0.244)
7.a Free rotating group:
 O2(H2A,H2B)
7.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C1(H1), C8(H8), C3(H3), C15(H15), C2(H2), C21(H21), C9(H9), C20(H20),
 C16(H16), C11(H11), C10(H10), C19(H19), C18(H18), C15A(H15A), C21A(H21A),
 C20A(H20A), C16A(H16A), C19A(H19A), C18A(H18A)
7.c Idealised tetrahedral OH refined as rotating group:
 O4(H4A)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              71891
_shelx_fab_checksum              70127
_olex2_submission_special_instructions 'No special instructions were received'