Synthesis and structural characterization of zinc complexes of the imidoamido phosphate anions OP[(NHR)<sub>3</sub><i><sub>x</sub></i>(NR)]<i><sup>x</sup></i><sup></sup> (R = Me, <i>t</i>-Bu; <i>x</i> = 13) and EP[(NH-<i>t</i>-Bu)<sub>2</sub>(N-<i>t</i>-Bu)]<sup></sup> (E = S, NSiMe<sub>3</sub>)
Bibliographic record
Abstract
The reaction of OP(NH-t-Bu)3 with 1 equiv. of ZnMe2 generates the dimeric eight-membered ring {MeZn[(µ-NH-t-Bu)(µ-N-t-Bu)P(NH-t-Bu)(µ-O)]}2 (5) and the cubane {[MeZn]3[OP(N-t-Bu)3][OP(NH-t-Bu)3]} (6), which contains the first known trisimidophosphate trianion. A related complex {Zn[ZnMe]2[OP(N-t-Bu)(NH-t-Bu)2][OP(N-t-Bu)3]} (7) is obtained by the reaction of OP(NH-t-Bu)3 with ZnMe2 in a 2:3 molar ratio. The treatment of OP(NHMe)3 with 1 equiv. of ZnMe2 produces the oxide-templated cluster {Zn4(µ4-O)[OP(NMe)(NHMe)2]4[OP(NMe)2(NHMe)]}2 (8). Each half of this centrosymmetric dimer contains a tetrahedral arrangement of four 4-coordinate Zn2+ ions surrounding the central µ4-O2- anion. The reaction of SP(NH-t-Bu)3 with ZnMe2 in a 1:1 molar ratio generates the dimer {MeZn(µ-S)(µ-N-t-Bu)P(NH-t-Bu)2}2 (10), which has a ladder-type structure. When a 2:1 molar ratio of the same reagents is employed, the bis(N,S)-chelated complex {Zn[(µ-S)(µ-N-t-Bu)P(NH-t-Bu)2]2} (11) is obtained. The monomeric N,N′-chelated complex {MeZn[(µ-N-t-Bu)(µ-NSiMe3)P(NH-t-Bu)2]} (12) results from the reaction of Me3SiNP(NH-t-Bu)3 with 1 equiv. of dimethylzinc. All new compounds have been characterized by multinuclear (1H, 13C, and 31P) NMR spectroscopy and, in the case of 5, 6, 7, 8, and 10, by X-ray structural determinations.Key words: zinc, phosphate, imido ligands, sulfur.
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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) | 0.000 | 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) | 0.001 | 0.000 |
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".