Structure cristalline du tri-μ-hydroxo-tri(pyridine-2 carboxylato)tribéryllium monohydraté, [Be₃(OH)₃(C₅H₄NCOO)₃].H₂O. Mise en evidence d'un cycle béryllium–oxygène d'ordre 6

Abstract

(Refu le 16 juillet 1973(Refu le 16 juillet , accept6 le 12 oetobre 1973 The crystal structure of a picolinic acid polynuclear chelate with beryllium has been determined. Tri-/zhydroxo-tri(pyridine-2-carboxylato)triberyllium monohydrate, [Bea(OH)a(C~H4NCOO)a].H20, crystallizes in the monoclinic system, space group P2Jc with a= 15.914, b=9.262, c= 15.480 ~, fl= 105"43 ° and Z= 4. The Cu Kg intensities were collected on a four-circle Siemens AED diffractometer and the structure was determined by means of the symbolic addition procedure. Before refinement, the atomic parameters were divided into different groups and the anisotropic full-matrix least-squares method was successively applied to each (R = 0.045).

Isolation of [Be3(μ-OH)3(H2O)6]3+. Synthesis, 9Be NMR Spectroscopy, and Crystal Structure of [Be3(μ-OH)3(H2O)6](picrate)3·6H2O

“…Beryllium hydrolysis has been studied by several authors, and the complex [Be 3 (μ-OH) 3 (H 2 O) 6 ] 3+ has been inferred to be the main species through both potentiometric and NMR measurements 2d,, We report here the isolation of this trimeric species as the picrate salt [Be 3 (μ-OH) 3 (H 2 O) 6 ](C 6 H 2 N 3 O 7 ) 3 ·6H 2 O. The compound has been characterized by 9 Be NMR and X-ray analysis.…”

Reactions of Beryllium Halides in Liquid Ammonia: The Tetraammineberyllium Cation [Be(NH3)4]2+, its Hydrolysis Products, and the Action of Be2+ as a Fluoride‐Ion Acceptor

“…The chair conformation of the [Be 3 A C H T U N G T R E N N U N G (m-OH) 3 ] ring has also been found in the crystal structures of compounds containing chelating ligands at the beryllium atoms. [23,[75][76][77] 3 ] ring to be almost planar and distortions from planarity in crystals were traced back to hydrogen bonding. [30] Our own quantum chemical calculations revealed the cation to be perfectly planar in the gas phase with point group D 3h (see below).…”

N‐Methylimidazolkomplexe des Berylliums: [Be(Me‐Im)4]I2 und [Be3(μ‐OH)3(Me‐Im)6]Cl3

“…Diese Abstände entsprechen auch den Be–N‐Bindungslängen in Pyrazolylboraten wie beispielsweise in [Be 3 (μ‐OH) 3 {HB(3,5‐Me 2 pz) 3 } 3 ] 15 mit Be–N = 176.4(4) pm. Deutlich länger sind die Be–N‐Bindungen dagegen in dem Pyridin‐2‐carboxylatkomplex [Be 3 (μ‐OH) 3 (C 5 H 4 N‐CO 2 ) 3 ]·H 2 O 13 mit im Mittel 179.1 pm.…”

“…[BeCl 3 (L)] – 12 führen, wohl aber bei Zutritt von Luftfeuchtigkeit zwei Kristallvarianten von Tris(μ‐hydroxo)hexamethylimidazoltriberyllium‐Trichlorid, [Be 3 (μ‐OH) 3 (Me‐Im) 6 ]Cl 3 , bilden. Kristallstrukturanalysen von Komplexen mit dem [Be 3 (μ‐OH) 3 ] 3+ ‐Fragment liegen vor von dem Pyridin‐2‐carboxylat [Be 3 (μ‐OH) 3 (C 5 H 4 N‐CO 2 ) 3 ]·H 2 O 13, von den Pyrazolylboraten [Be 3 (μ‐OH) 3 {HB(pz) 3 } 3 ] 14 und [Be 3 (μ‐OH) 3 {HB(3,5‐Me 2 pz) 3 } 3 ] 15 sowie von dem Kaliummalonat K 3 [Be 3 (μ‐OH) 3 (O 2 CCH 2 CO 2 ) 3 ]·6H 2 O 16 und dem Chloridoderivat (Ph 4 P) 2 [Be 3 (μ‐OH) 3 (H 2 O) 6 ]Cl 5 , das auch durch DFT‐Rechnungen charakterisiert wurde 17. Das in wässrigen Lösungen stabile [Be 3 (μ‐OH) 3 (H 2 O) 6 ] 3+ ‐Ion wurde auch kernresonanzspektroskopisch untersucht 18.…”