scholarly journals N-Heterocyclic Carbene-Supported Aryl- and Alk- oxides of Beryllium and Magnesium

Catalysts ◽  
2019 ◽  
Vol 9 (11) ◽  
pp. 934 ◽  
Author(s):  
Jacob E. Walley ◽  
Yuen-Onn Wong ◽  
Lucas A. Freeman ◽  
Diane A. Dickie ◽  
Robert J. Gilliard

Recently, we have witnessed significant progress with regard to the synthesis of molecular alkaline earth metal reagents and catalysts. To provide new precursors for light alkaline earth metal chemistry, molecular aryloxide and alkoxide complexes of beryllium and magnesium are reported. The reaction of beryllium chloride dietherate with two equivalents of 1,3-diisopropyl-4,5-dimethylimidizol-2-ylidine (sIPr) results in the formation of a bis(N-heterocyclic carbene) (NHC) beryllium dichloride complex, (sIPr)2BeCl2 (1). Compound 1 reacts with lithium diisopropylphenoxide (LiODipp) or sodium ethoxide (NaOEt) to form the terminal aryloxide (sIPr)Be(ODipp)2 (2) and alkoxide dimer [(sIPr)Be(OEt)Cl]2 (3), respectively. Compounds 2 and 3 represent the first beryllium alkoxide and aryloxide species supported by NHCs. Structurally related dimers of magnesium, [(sIPr)Mg(OEt)Brl]2 (4) and [(sIPr)Mg(OEt)Me]2 (5), were also prepared. Compounds 1-5 were characterized by single crystal X-ray diffraction studies, 1H, 13C, and 9Be NMR spectroscopy where applicable.

Author(s):  
Igor Oshchapovsky ◽  
Volodymyr Pavlyuk ◽  
Grygoriy Dmytriv ◽  
Alexandra Griffin

The structure of lanthanum tetrazinc, LaZn4, has been determined from single-crystal X-ray diffraction data for the first time, approximately 70 years after its discovery. The compound exhibits a new structure type in the space groupCmcm, with one La atom and two Zn atoms occupying sites withm2msymmetry, and one Zn atom occupying a site with 2.. symmetry. The structure is closely related to the BaAl4, La3Al11, BaNi2Si2and CaCu5structure types, which can be presented as close-packed arrangements of 18-vertex clusters, in this case LaZn18. The kindred structure types contain related 18-vertex clusters around atoms of the rare earth or alkaline earth metal.


Author(s):  
Jeffrey A. Rood ◽  
Ashley L. Huttenstine ◽  
Zachery A. Schmidt ◽  
Michael R. White ◽  
Allen G. Oliver

Reaction of alkaline earth metal salts with diphenylphosphinic acid in dimethylformamide solvent afforded four coordination polymers: [Mg3(O2PPh2)6(DMF)2]·2DMF (I), [Ca(O2PPh2)2(DMF)2] (II), [Sr(O2PPh2)2(DMF)2] (III) and [Ba(O2PPh2)2(DMF)2] (IV) (where DMF isN,N-dimethylformamide). Single-crystal X-ray diffraction revealed that all four compounds produce linear chain structures in the solid state, with the Ca, Sr and Ba forming isostructural crystals. The bulk materials were characterized by FT–IR and1H NMR spectroscopy and elemental analyses.


2020 ◽  
Vol 235 (4-5) ◽  
pp. 137-141
Author(s):  
Maximilian K. Reimann ◽  
Rainer Pöttgen

AbstractThe copper-rich intermetallic compounds CaCu9Mg2 and SrCu9Mg2 were synthesized by induction melting of the elements and subsequent annealing in a muffle furnace. CaCu9Mg2 and SrCu9Mg2 crystallize with the TbCu9Mg2 type structure, space group P 63/mmc, which is a ternary ordered variant of CeNi3. The polycrystalline samples were characterized through their X-ray powder patterns. The CaCu9Mg2 structure was refined from single-crystal X-ray diffraction data. a = 504.13(9), c = 1622.5(3) pm, wR2 = 0.0635, 302 F2 values and 19 variables. The two striking coordination polyhedra in the CaCu9Mg2 structure are Ca@Cu18Mg2 and Mg@Cu12Mg3Ca. These polyhedra condense to layers which are stacked in ABA′B′ sequence. The X-ray data give no hint for Ca/Mg mixing.


1998 ◽  
Vol 547 ◽  
Author(s):  
Duncan H. Gregory ◽  
Marten G. Barker ◽  
Daniel J. Siddons ◽  
Peter P. Edwards ◽  
Marcin Slaski

AbstractThe ternary transition metal nitrides of general formulation AMN2 (A = alkaline earth metal, M = transition metal) have been systematically studied. These compounds have been synthesised by high temperature solid state reaction from their component binary nitrides in sealed systems. The structures of these materials have been determined by powder X-ray diffraction (PXD) and two layered structure-types (α-NaFeO2-type and KCoO2-type) have been observed, thus far. Intriguingly, magnetic measurements performed on nitride samples indicate they may not be diamagnetic (d = 0, S = 0) as their nominal stoichiometry suggests.


1979 ◽  
Vol 34 (6) ◽  
pp. 886-887 ◽  
Author(s):  
Hans G. Kraft ◽  
Bernd M. Rode

The preparation of two new alkaline earth metal complexes with acetylacetone, where the latter acts as a ligand in its diketoform, is described. The solid compounds are characterized by elemental analysis, IR spectra and X-ray diffraction patterns.


2017 ◽  
Vol 46 (27) ◽  
pp. 8727-8735 ◽  
Author(s):  
Fabian Dankert ◽  
Kirsten Reuter ◽  
Carsten Donsbach ◽  
Carsten von Hänisch

A series of disila-crown ether complexes have been characterized by single crystal X-ray diffraction. The complex stability of different systems were studied by DFT calculations and proton NMR experiments.


2007 ◽  
Vol 62 (1) ◽  
pp. 23-27 ◽  
Author(s):  
Olaf Reckeweg ◽  
Jay C. Molstad ◽  
Scott Levy ◽  
Francis J. DiSalvo

Single crystals of the isotypic hydrides Ba2H3X (X = Cl or Br) were obtained by solid-state reactions of Ba, NaCl, NaNH2 and metallic Na, or Ba, NH4Br and Na, respectively, in sealed, silicajacketed stainless-steel ampoules. The crystal structures of the new compounds were determined by means of single crystal X-ray diffraction. Ba2H3Cl and Ba2H3Br crystallize in a stuffed anti CdI2 structure and adopt the space group P3̄m1 (No. 164) with the lattice parameters a = 443.00(6), c = 723.00(14) pm and a = 444.92(4), c = 754.48(14) pm, respectively. The hydride positions are derived by crystallographic reasoning and with the help of EUTAX calculations. The results are compared with known data for binary and ternary alkaline earth metal hydrides.


1998 ◽  
Vol 13 (6) ◽  
pp. 1607-1613 ◽  
Author(s):  
N. J. Welham

This paper outlines the formation of alkaline earth metal titanates, of the general formula MTiO3, directly from the metal oxides and rutile by mechanical activation in a laboratory ball mill at room temperature. X-ray diffraction analysis showed that the reaction was essentially complete within 100 h for all metals except magnesium. The titanates formed all had a Scherrer crystallite size of 11–12 nm and a lattice strain of 0.5–0.6%, neither of which were affected by extended milling. Annealing studies confirmed that the titanate was formed during milling and showed that grain growth could be achieved at temperatures below that generally used for their formation. Mixed cation titanates could also be formed by milling, but tended to be barium rich until annealed.


2010 ◽  
Vol 65 (9) ◽  
pp. 1077-1083 ◽  
Author(s):  
Christine Walbaum ◽  
Ingo Pantenburg ◽  
Gerd Meyer

Salts of alkaline earth metal cations sequestered in dibenzo-18-crown-6 (Db18c6) and benzo-15- crown-5 (B15c5), respectively, with I5−, I7− and I82− as the anions, have been synthesized and their crystal structures determined by single-crystal X-ray diffraction. [Ca(Db18c6)(H2O)3](I5)2- (Db18c6)(H2O) (1): monoclinic, P21 (no. 4), a = 1322.1(2), b = 1849.1(2), c = 1344.0(2) pm, β = 114.70(1)◦, V = 2985.2(6) × 106 pm3, Z = 2; [Sr(B15c5)2](I7)2 (2): triclinic, P1 (no. 2), a = 973.9(5), b = 1244.0(5), c = 1293.3(5) pm, α = 115.28(1), β = 90.18(1), γ = 104.57(1)◦, V = 1360.2(10) × 106 pm3, Z = 2; [Ba(Db18c6)2]I8 (3): orthorhombic, Pbcn (no. 60), a = 1452.0(2), b = 1924.6(2), c = 1912.1(2) pm, V = 5343.3(10) × 106 pm3, Z = 4. Compound 1 contains two crystallographically independent V-shaped pentaiodide anions, I5 −, which are linked to dimers by weak interionic contacts. The unusual heptaiodide anion, I7−, in 2 can be described as a V-shaped pentaiodide unit, which is connected to a slightly widened iodine molecule to give the rare Z form. Secondary bonding distances lead to almost planar ten-membered iodine rings, which are connected through common edges to form ribbons with staircase-like folding. 3 is built of sandwich-like cations and centrosymmetric octaiodide anions, I82−. An inspection for secondary contacts reveals that the iodine substructure of 3 consists of essentially isolated octaiodide units.


Sign in / Sign up

Export Citation Format

Share Document