Polydentate chalcogen reagents for the facile preparation of Pd<sub>2</sub> and Pd<sub>4</sub> complexes
Bibliographic record
Abstract
The silylated organochalcogen reagents 1,2-(Me3SiSCH2)2C6H4, and 1,2-(Me3SiSeCH2)2C6H4, were prepared from the corresponding organobromides and lithium trimethylsilanechalcogenolate Li[ESiMe3] (E = S, Se). They have been characterized by multinuclear NMR spectroscopy ((1)H, (13)C, (77)Se) and electrospray ionization mass spectrometry. and react under mild conditions with (1,3-bis(diphenylphosphino)propane)palladium(ii) chloride, [PdCl2(dppp)], to provide the dinuclear organochalcogenolate-bridged complexes [(dppp)2Pd2-μ-κ(2)S-{1,2-(SCH2)2C6H4}]X2, []X2 and [(dppp)2Pd2-μ-κ(2)Se-{1,2-(SeCH2)2C6H4}]X2, []X2 (X = Cl, Br) in good yield, respectively. Furthermore, the tetranuclear palladium complex [(dppp)4Pd4-μ-κ(4)S-{1,2,4,5-(SCH2)4C6H2}]X4, []X4 (X = Cl, Br) can be synthesized from the reaction of the tetrathiotetrasilane 1,2,4,5-(Me3SiSCH2)4C6H2, and [PdCl2(dppp)]. The structures of []X2, []X2 and []X4 were determined by single crystal X-ray diffraction methods. A variety of NMR experiments including two-dimensional homonuclear and heteronuclear correlated spectra were used to probe the solution behaviour of the dinuclear complexes in more detail. These complexes were further characterized by electrospray ionization (ESI) mass spectrometry, and for []X2 and []X2, UV-Vis absorption spectroscopy.
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How this classification was reachedexpand
Full frame machine prediction
Teacher imitationNot calibrated prevalence, not ground truth. Human validation pending. The Gemma side is a direct model label for every work in the frame, read from the title-only record. The Codex side is a classifier learned from the 10,348 direct Codex labels and calibrated to design-weighted sample rates; fields without enough sample support carry no Codex call. Candidate is the union of the two sides; consensus is their intersection. These outputs are machine_predicted_unvalidated and are not human labels.
Distilled classifier scores by category (both heads)
| Category | Codex | Gemma |
|---|---|---|
| Metaresearch | 0.000 | 0.000 |
| Meta-epidemiology (narrow) | 0.001 | 0.000 |
| Meta-epidemiology (broad) | 0.000 | 0.000 |
| Bibliometrics | 0.000 | 0.000 |
| Science and technology studies | 0.000 | 0.000 |
| Scholarly communication | 0.000 | 0.000 |
| Open science | 0.000 | 0.000 |
| Research integrity | 0.000 | 0.000 |
| Insufficient payload (model declined to judge) | 0.003 | 0.001 |
Machine scores (provisional)
The two teacher heads of the student model, read on this work. A score orders the frame for review; it never asserts a category, and the validation status ships verbatim with every row.
Baseline scores from an immature model (maturity gate not passed, 7 training rounds). Scores rank; they never assert a category.
score_only:v0-immature-baseline · verbatim from the scoring run: score_only means the number may rank works, and no category label ships from itClassification
machine, unvalidatedMachine predicted; a candidate call from one source (direct Gemma or distilled Codex), not a consensus.
How this classification was reached, model by model and score by score, is at the end of the page under "How this classification was reached".