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_7715789
_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         '0.5(C32 H38 N4 O4 Pd4 S4), Cl O4, C H Cl3'
_chemical_formula_sum            'C17 H20 Cl4 N2 O6 Pd2 S2'
_chemical_formula_weight         767.131
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_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                105.262(3)
_cell_angle_beta                 104.871(3)
_cell_angle_gamma                107.653(4)
_cell_formula_units_Z            4
_cell_length_a                   11.6987(6)
_cell_length_b                   15.0875(8)
_cell_length_c                   18.3377(9)
_cell_measurement_reflns_used    5856
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      73.99
_cell_measurement_theta_min      3.40
_cell_volume                     2769.0(3)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_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 0.9987
_diffrn_measured_fraction_theta_max 0.9982
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1983
_diffrn_reflns_av_unetI/netI     0.1049
_diffrn_reflns_Laue_measured_fraction_full 0.9987
_diffrn_reflns_Laue_measured_fraction_max 0.9982
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            68334
_diffrn_reflns_point_group_measured_fraction_full 0.9987
_diffrn_reflns_point_group_measured_fraction_max 0.9982
_diffrn_reflns_theta_full        67.6786
_diffrn_reflns_theta_max         70.07
_diffrn_reflns_theta_min         3.31
_diffrn_source_current           1.1
_diffrn_source_power             0.05500000000000001
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    15.748
_exptl_absorpt_correction_T_max  0.7848
_exptl_absorpt_correction_T_min  0.4670
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1359 before and 0.0904 after correction.
The Ratio of minimum to maximum transmission is 0.5951.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.840
_exptl_crystal_description       needle
_exptl_crystal_F_000             1518.474
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.5888
_refine_diff_density_min         -1.8224
_refine_diff_density_rms         0.3095
_refine_ls_d_res_high            0.8200
_refine_ls_d_res_low             13.3549
_refine_ls_extinction_coef       0.00019(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.0204
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    68
_refine_ls_number_parameters     602
_refine_ls_number_reflns         10523
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0204
_refine_ls_R_factor_all          0.1213
_refine_ls_R_factor_gt           0.0676
_refine_ls_shift/su_max          0.0008
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1010P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1638
_refine_ls_wR_factor_ref         0.2051
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              13
_reflns_limit_h_min              -14
_reflns_limit_k_max              17
_reflns_limit_k_min              -18
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                6205
_reflns_number_total             10523
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4dt00756e1.cif
_cod_data_source_block           20VAA038
_cod_depositor_comments
'Adding full bibliography for 7715787--7715791.cif.'
_cod_database_code               7715789
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 N00M(H00M), N00N(H00N), N00P(H00P), N00T(H00T), C01Q(H2), C01W(H3)
2.b Aromatic/amide H refined with riding coordinates:
 C00W(H00W), C00Y(H00Y), C00Z(H00Z), C014(H014), C017(H017), C019(H019),
 C01A(H01j), C01C(H01l), C01J(H01u), C01K(H01K), C01N(H01N), C01O(H01O),
 C01S(H01y), C01T(H01z), C01U(H01), C01V(H1)
2.c Idealised Me refined as rotating group:
 C018(H01a,H01b,H01c), C01B(H01d,H01e,H01f), C01G(H01m,H01p,H01q), C01H(H01r,
 H01s,H01t), C01L(H01g,H01h,H01i), C01P(H01v,H01w,H01x)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'