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_7715790
_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         'C21 H24 Cl3 N3 Pd3 S3, 2(C2 H6 O S)'
_chemical_formula_sum            'C25 H36 Cl3 N3 O2 Pd3 S5'
_chemical_formula_weight         996.518
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                 91.4728(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.6057(5)
_cell_length_b                   19.0596(10)
_cell_length_c                   19.8471(11)
_cell_measurement_reflns_used    9765
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      28.363
_cell_measurement_theta_min      2.380
_cell_volume                     3632.4(3)
_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 0.9971
_diffrn_measured_fraction_theta_max 0.9973
_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  0.0378
_diffrn_reflns_av_unetI/netI     0.0198
_diffrn_reflns_Laue_measured_fraction_full 0.9971
_diffrn_reflns_Laue_measured_fraction_max 0.9973
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            86053
_diffrn_reflns_point_group_measured_fraction_full 0.9971
_diffrn_reflns_point_group_measured_fraction_max 0.9973
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         28.38
_diffrn_reflns_theta_min         2.37
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.006
_exptl_absorpt_correction_T_max  0.9281
_exptl_absorpt_correction_T_min  0.8493
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0725 before and 0.0512 after correction.
The Ratio of minimum to maximum transmission is 0.9151.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.822
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1961.078
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.1640
_refine_diff_density_min         -2.8309
_refine_diff_density_rms         0.1494
_refine_ls_d_res_high            0.7477
_refine_ls_d_res_low             8.5903
_refine_ls_goodness_of_fit_ref   1.0503
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    74
_refine_ls_number_parameters     459
_refine_ls_number_reflns         9079
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.0488
_refine_ls_R_factor_all          0.0370
_refine_ls_R_factor_gt           0.0328
_refine_ls_shift/su_max          0.0007
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+20.1843P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0737
_refine_ls_wR_factor_ref         0.0764
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              11
_reflns_limit_h_min              -12
_reflns_limit_k_max              25
_reflns_limit_k_min              0
_reflns_limit_l_max              26
_reflns_limit_l_min              -10
_reflns_number_gt                8298
_reflns_number_total             9079
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4dt00756e1.cif
_cod_data_source_block           mo_21VAA018_0m
_cod_depositor_comments
'Adding full bibliography for 7715787--7715791.cif.'
_cod_database_code               7715790
_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
 C24-C25 \\sim C7a-C8a
 with sigma of 0.04
 O4-C24 \\sim O4a-C7a
 with sigma of 0.04
 S5-C24 \\sim S3a-C7a
 with sigma of 0.02
 S4-O5 \\sim S1a-O5a
 with sigma of 0.02
 S4-C22 \\sim S1a-C9a
 with sigma of 0.02
 S4-C23 \\sim S1a-C10a
 with sigma of 0.02
 S5-O4 \\sim S3a-O4a
 with sigma of 0.02
 S5-C25 \\sim S3a-C8a
 with sigma of 0.02
 O4-C25 \\sim O4a-C8a
 with sigma of 0.04
 O5-C22 \\sim O5a-C9a
 with sigma of 0.04
 O5-C23 \\sim O5a-C10a
 with sigma of 0.04
 C22-C23 \\sim C9a-C10a
 with sigma of 0.04
3. Others
 Sof(S1a)=Sof(O5a)=Sof(C9a)=Sof(Hl)=Sof(Hm)=Sof(Hn)=Sof(C10a)=Sof(Ho)=Sof(Hp)=
 Sof(Hq)=1-FVAR(1)
 Sof(S4)=Sof(O5)=Sof(C22)=Sof(Hf)=Sof(Hg)=Sof(Hh)=Sof(C23)=Sof(Hi)=Sof(Hj)=
 Sof(Hk)=FVAR(1)
 Sof(S3a)=Sof(O4a)=Sof(C7a)=Sof(Hr)=Sof(Hs)=Sof(Ht)=Sof(C8a)=Sof(Hu)=Sof(Hv)=
 Sof(Hw)=1-FVAR(2)
 Sof(S5)=Sof(O4)=Sof(C24)=Sof(H)=Sof(Ha)=Sof(Hb)=Sof(C25)=Sof(Hc)=Sof(Hd)=
 Sof(He)=FVAR(2)
4.a Ternary CH refined with riding coordinates:
 N9(H9), N10(H10)
4.b Aromatic/amide H refined with riding coordinates:
 C10(H10a), C11(H11), C20(H20), C12(H12), C13(H13), C4(H4), C17(H17), C19(H19),
  C5(H5), C3(H3), C6(H6), C18(H18)
4.c Idealised Me refined as rotating group:
 C8(H8a,H8b,H8c), C15(H15a,H15b,H15c), C1(H1a,H1b,H1c), C24(H,Ha,Hb), C25(Hc,
 Hd,He), C22(Hf,Hg,Hh), C23(Hi,Hj,Hk), C9a(Hl,Hm,Hn), C10a(Ho,Hp,Hq), C7a(Hr,Hs,
 Ht), C8a(Hu,Hv,Hw)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 194 electrons were 
found in a volume of 242\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1[CH3SOCH3] per Asymmetric Unit 
which account for 168 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'