Novel Pd(ii) pincer complexes bearing salicylaldimine-based benzothiazole derivatives: synthesis, structural characterization, DNA/BSA binding, and biological evaluation
Wongsuwan, Sutthida; Chatwichien, Jaruwan; Sirisaksoontorn, Weekit; Chainok, Kittipong; Songsasen, Apisit; Chotima, Ratanon; New Journal of Chemistry 47 (2023) 10624–10637; doi:10.1039/D3NJ00458A

data_7062488
_publ_section_title
;
 Novel Pd(ii) pincer complexes bearing salicylaldimine-based benzothiazole
 derivatives: synthesis, structural characterization, DNA/BSA binding, and
 biological evaluation
;
_journal_issue                   22
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              10624
_journal_page_last               10637
_journal_paper_doi               10.1039/D3NJ00458A
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety         'C21 H16 N2 O S'
_chemical_formula_sum            'C21 H16 N2 O S'
_chemical_formula_weight         444.42
_chemical_name_common            ABPT-CH3
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-11-16
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2021-03-06 deposited with the CCDC.	2023-05-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.121(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.5754(8)
_cell_length_b                   12.9309(7)
_cell_length_c                   19.9574(11)
_cell_measurement_reflns_used    4135
_cell_measurement_temperature    0.0
_cell_measurement_theta_max      25.769
_cell_measurement_theta_min      3.151
_cell_volume                     3437.6(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      0.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.3199
_diffrn_reflns_av_unetI/netI     0.2256
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            81789
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.072
_diffrn_reflns_theta_min         2.809
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.199
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.4288
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1260 before and 0.1057 after correction.
The Ratio of minimum to maximum transmission is 0.5753.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_description       rod
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.261
_refine_diff_density_min         -0.175
_refine_diff_density_rms         0.047
_refine_ls_abs_structure_details
;
 Flack x determined using 1153 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.4(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.919
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     911
_refine_ls_number_reflns         13557
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.919
_refine_ls_R_factor_all          0.3047
_refine_ls_R_factor_gt           0.0722
_refine_ls_shift/su_max          0.989
_refine_ls_shift/su_mean         0.200
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0325P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1004
_refine_ls_wR_factor_ref         0.1623
_reflns_Friedel_coverage         0.909
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                3388
_reflns_number_total             13557
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj00458a2.cif
_cod_data_source_block           622p21c_a
_cod_depositor_comments
;
Adding full bibliography for 7062488--7062493.cif.

2024-11-08
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C84 H64 N8 O4 S4'
_cod_original_formula_weight         1377.67
_cod_original_formula_moiety
'2(C21 H16 N2 O S), C21 H17 N2 O S, C21 H15 N2 O S'
_cod_original_formula_units_Z            2
_cod_database_code               7062488
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.994
_shelx_estimated_absorpt_t_min   0.969
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H00C of O00C, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, H00T of O00T, HA of O, H00H of O00H
2.a Riding coordinates:
 C00M(H00M)
2.b Aromatic/amide H refined with riding coordinates:
 C00K(H00K), C00L(H00L), C00P(H00P), C11(H11), C00V(H00V), C00W(H00W), N(H),
 C9(H9), C011(H011), C7(H7), C2(H2), C019(H019), C01B(H01F), C01C(H01C),
 C01D(H01D), C5(H5), C01I(H01I), C01K(H01K), C01M(H01M), C01Q(H01Q), C01R(H01R),
  C01S(H01S), C12(H12), C01W(H01W), C01Z(H01Z), C020(H020), C021(H021),
 C022(H022), C023(H023), C024(H024), C025(H025), C026(H026), C027(H027), C1(H1),
  C029(H029), C6(H6), C02C(H02J), C02E(H02E), C02F(H02F), C3(H3), C02H(H02H),
 C02I(H02L), C02K(H02K), C02O(H02O), C10(H10), C02Q(H02Q), C02R(H02R)
2.c Idealised Me refined as rotating group:
 C01O(H01G,H01H,H01J), C01Y(H01A,H01B,H01E), C02N(H02D,H02G,H02I), C02S(H02A,
 H02B,H02C)
2.d Idealised tetrahedral OH refined as rotating group:
 O(HA), O00H(H00H), O00T(H00T)
;
_shelx_res_checksum              26688
_olex2_submission_special_instructions 'No special instructions were received'