Reactivity of Schiff base-[C,N,S] pincer palladacycles: hydrolysis renders singular trinuclear, tetranuclear, and heteropentanuclear Pd<sub>3</sub>W<sub>2</sub> coordinated complexes.
Reigosa, Francisco; Polo, Paula M.; Pereira, M. Teresa; Vila, José M; Dalton transactions (Cambridge, England : 2003) 53 (2024) 9680–9691; doi:10.1039/d4dt00756e

data_7715787
_publ_section_title
;
 Reactivity of Schiff base-[C,N,S] pincer palladacycles: hydrolysis
 renders singular trinuclear, tetranuclear, and heteropentanuclear
 Pd<sub>3</sub>W<sub>2</sub> coordinated complexes.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9680
_journal_page_last               9691
_journal_paper_doi               10.1039/d4dt00756e
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C16 H16 Cl N O Pd S'
_chemical_formula_sum            'C16 H16 Cl N O Pd S'
_chemical_formula_weight         412.245
_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'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-07-06
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-02-18 deposited with the CCDC.	2024-04-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.9138(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.1340(2)
_cell_length_b                   11.6466(3)
_cell_length_c                   17.0711(4)
_cell_measurement_reflns_used    9734
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      38.568
_cell_measurement_theta_min      2.559
_cell_volume                     1582.37(7)
_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  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.9993
_diffrn_measured_fraction_theta_max 0.9955
_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON III-14'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_av_unetI/netI     0.0233
_diffrn_reflns_Laue_measured_fraction_full 0.9993
_diffrn_reflns_Laue_measured_fraction_max 0.9955
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            63757
_diffrn_reflns_point_group_measured_fraction_full 0.9993
_diffrn_reflns_point_group_measured_fraction_max 0.9955
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         38.57
_diffrn_reflns_theta_min         2.44
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.471
_exptl_absorpt_correction_T_max  0.8753
_exptl_absorpt_correction_T_min  0.7871
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0621 before and 0.0491 after correction.
The Ratio of minimum to maximum transmission is 0.8992.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.730
_exptl_crystal_description       block
_exptl_crystal_F_000             821.481
_exptl_crystal_size_max          0.156
_exptl_crystal_size_mid          0.127
_exptl_crystal_size_min          0.092
_refine_diff_density_max         0.7329
_refine_diff_density_min         -1.1601
_refine_diff_density_rms         0.1269
_refine_ls_d_res_high            0.5700
_refine_ls_d_res_low             8.3517
_refine_ls_goodness_of_fit_ref   1.0366
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    26
_refine_ls_number_parameters     193
_refine_ls_number_reflns         8909
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0366
_refine_ls_R_factor_all          0.0312
_refine_ls_R_factor_gt           0.0232
_refine_ls_shift/su_max          -0.0005
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0204P)^2^+0.8244P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0510
_refine_ls_wR_factor_ref         0.0547
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              13
_reflns_limit_h_min              -14
_reflns_limit_k_max              20
_reflns_limit_k_min              0
_reflns_limit_l_max              29
_reflns_limit_l_min              0
_reflns_number_gt                7719
_reflns_number_total             8909
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4dt00756e1.cif
_cod_data_source_block           20VAA042B
_cod_depositor_comments
'Adding full bibliography for 7715787--7715791.cif.'
_cod_database_code               7715787
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12)
2.b Idealised Me refined as rotating group:
 C14(H14a,H14b,H14c), C15(H15a,H15b,H15c), C16(H16a,H16b,H16c)
;
_olex2_submission_special_instructions 'No special instructions were received'