A Gliclazide Complex based on Palladium towards Alzheimer’s Disease: Promising Protective Activity against Aβ-induced Toxicity in C. Elegans
García-García, Amalia; Rojas, Sara; Rivas Garcia, Lorenzo; Navarro-Hortal, María; Romero-Márquez, José; Fernandez-Bolanos, Jose G; Choquesillo-Lazarte, Duane; Salinas-Castillo, Alfonso; Lopez, Oscar; Quiles, José L.; Rodríguez Diéguez, Antonio; Chemical Communications  (2022) –; doi:10.1039/D1CC04404D

data_7129401
_publ_section_title
;
 A Gliclazide Complex based on Palladium towards Alzheimer&#x2019;s
 Disease: Promising Protective Activity against A\b-induced Toxicity in C.
 Elegans
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_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC04404D
_journal_year                    2022
_chemical_formula_moiety         'C30 H40 N6 O6 Pd S2'
_chemical_formula_sum            'C30 H40 N6 O6 Pd S2'
_chemical_formula_weight         751.20
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-08-10
_audit_creation_method
;
Olex2 1.5
(compiled 2021.07.19 svn.r715e62df for OlexSys, GUI svn.r6383)
;
_audit_update_record
;
2021-08-10 deposited with the CCDC.	2021-12-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.313(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.161(2)
_cell_length_b                   11.7499(16)
_cell_length_c                   17.900(3)
_cell_measurement_reflns_used    2718
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      17.37
_cell_measurement_theta_min      2.34
_cell_volume                     3207.8(8)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'Bruker Apex3, 2019'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  multilayer
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1795
_diffrn_reflns_av_unetI/netI     0.0812
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            16749
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        17.222
_diffrn_reflns_theta_max         17.222
_diffrn_reflns_theta_min         2.188
_diffrn_source                   'high brilliance microfocus sealed tube'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.761
_exptl_absorpt_correction_T_max  0.0087
_exptl_absorpt_correction_T_min  0.0026
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1212 before and 0.0890 after correction.
The Ratio of minimum to maximum transmission is 0.2989.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_description       block
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.600
_refine_diff_density_min         -0.536
_refine_diff_density_rms         0.181
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.199
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     408
_refine_ls_number_reflns         1947
_refine_ls_number_restraints     132
_refine_ls_restrained_S_all      1.156
_refine_ls_R_factor_all          0.1012
_refine_ls_R_factor_gt           0.0598
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1011P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1414
_refine_ls_wR_factor_ref         0.1821
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1404
_reflns_number_total             1947
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc04404d2.cif
_cod_data_source_block           AML124B
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7129401
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.935
_shelx_estimated_absorpt_t_min   0.928
_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
2. Rigid body (RIGU) restrains
 N1A, C1A, C2A, C6A, C7A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1A, N3A, C8A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C9B, C10B, C11B, C12B, C13B, C14B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C2B, C3B, C4B, C5B, C6B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C2A, C3A, C4A, C5A, C6A, H14B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Ternary CH refined with riding coordinates:
 C2A(H2AA), C2B(H2BA), C6A(H6A), C6B(H6B)
3.b Secondary CH2 refined with riding coordinates:
 C1A(H1AA,H1AB), C1B(H1BA,H1BB), C3A(H3AA,H3AB), C3B(H3BA,H3BB), C4A(H4AA,
 H4AB), C4B(H4BA,H4BB), C5A(H5AA,H5AB), C5B(H5BA,H5BB), C7A(H7AA,H7AB),
 C7B(H7BA,H7BB)
3.c Aromatic/amide H refined with riding coordinates:
 N2A(H2A), N2B(H2B), C10A(H10A), C10B(H10B), C11A(H11A), C11B(H11B),
 C13A(H13A), C13B(H13B), C14A(H14A), C14B(H14B)
3.d Idealised Me refined as rotating group:
 C15A(H15A,H15B,H15C), C15B(H15D,H15E,H15F)
;
_olex2_submission_special_instructions 'No special instructions were received'