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_7715791
_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         'C28 H32 Cl4 N4 Pd4 S4, 3(C H Cl3)'
_chemical_formula_sum            'C31 H35 Cl13 N4 Pd4 S4'
_chemical_formula_weight         1478.459
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_Int_Tables_number      61
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-02-19
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-02-20 deposited with the CCDC.	2024-04-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.6947(8)
_cell_length_b                   22.0850(16)
_cell_length_c                   40.285(3)
_cell_measurement_reflns_used    9014
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      28.224
_cell_measurement_theta_min      2.175
_cell_volume                     9515.0(12)
_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      100.00
_diffrn_measured_fraction_theta_full 0.9992
_diffrn_measured_fraction_theta_max 0.9956
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0686
_diffrn_reflns_av_unetI/netI     0.0392
_diffrn_reflns_Laue_measured_fraction_full 0.9992
_diffrn_reflns_Laue_measured_fraction_max 0.9956
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            98993
_diffrn_reflns_point_group_measured_fraction_full 0.9992
_diffrn_reflns_point_group_measured_fraction_max 0.9956
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         28.34
_diffrn_reflns_theta_min         2.16
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.425
_exptl_absorpt_correction_T_max  0.7786
_exptl_absorpt_correction_T_min  0.5881
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0779 before and 0.0670 after correction.
The Ratio of minimum to maximum transmission is 0.7553.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.064
_exptl_crystal_description       plate
_exptl_crystal_F_000             5733.334
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.5765
_refine_diff_density_min         -1.8640
_refine_diff_density_rms         0.3349
_refine_ls_d_res_high            0.7486
_refine_ls_d_res_low             9.4458
_refine_ls_goodness_of_fit_ref   1.0448
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    68
_refine_ls_number_parameters     573
_refine_ls_number_reflns         11826
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.0437
_refine_ls_R_factor_all          0.0832
_refine_ls_R_factor_gt           0.0727
_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^)+(0.0079P)^2^+258.5733P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1326
_refine_ls_wR_factor_ref         0.1378
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              14
_reflns_limit_h_min              0
_reflns_limit_k_max              29
_reflns_limit_k_min              0
_reflns_limit_l_max              53
_reflns_limit_l_min              0
_reflns_number_gt                10502
_reflns_number_total             11826
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4dt00756e1.cif
_cod_data_source_block           mo_22VAA005_0m
_cod_depositor_comments
'Adding full bibliography for 7715787--7715791.cif.'
_cod_database_code               7715791
_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. Restrained distances
 Cl12-C31 \\sim Cl14-C31a
 with sigma of 0.02
 Cl11-C31 \\sim Cl15-C31a
 with sigma of 0.02
 Cl8-Cl10 \\sim Cl9a-Cl17
 with sigma of 0.04
 Cl13-C31 \\sim Cl16-C31a
 with sigma of 0.02
 Cl12-Cl11 \\sim Cl14-Cl15
 with sigma of 0.04
 Cl12-Cl13 \\sim Cl14-Cl16
 with sigma of 0.04
 Cl10-C30 \\sim Cl17-C30a
 with sigma of 0.02
 Cl11-Cl13 \\sim Cl15-Cl16
 with sigma of 0.04
 Cl8-Cl9 \\sim Cl9a-Cl8a
 with sigma of 0.04
 Cl9-Cl10 \\sim Cl8a-Cl17
 with sigma of 0.04
 Cl8-C30 \\sim Cl9a-C30a
 with sigma of 0.02
 Cl9-C30 \\sim Cl8a-C30a
 with sigma of 0.02
3. Others
 Sof(C31a)=Sof(H31a)=Sof(Cl14)=Sof(Cl15)=Sof(Cl16)=1-FVAR(1)
 Sof(Cl12)=Sof(Cl11)=Sof(Cl13)=Sof(C31)=Sof(H31)=FVAR(1)
 Sof(C30a)=Sof(H30a)=Sof(Cl9a)=Sof(Cl8a)=Sof(Cl17)=1-FVAR(2)
 Sof(Cl8)=Sof(Cl9)=Sof(Cl10)=Sof(C30)=Sof(H30)=FVAR(2)
4.a Ternary CH refined with riding coordinates:
 N2(H2), N4(H4), N1(H1), N3(H3), C29(H29), C30(H30), C31(H31), C31a(H31a),
 C30a(H30a)
4.b Aromatic/amide H refined with riding coordinates:
 C20(H20), C10(H10), C11(H11), C19(H19), C27(H27), C18(H18), C4(H4a), C5(H5),
 C17(H17), C12(H12), C13(H13), C3(H3a), C6(H6), C26(H26), C25(H25), C24(H24)
4.c Idealised Me refined as rotating group:
 C22(H22a,H22b,H22c), C1(H1a,H1b,H1c), C8(H8a,H8b,H8c), C15(H15a,H15b,H15c)
;
_olex2_submission_special_instructions 'No special instructions were received'