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Ulrich Englich

Publications and source records attributed to Ulrich Englich.

7 recordsLinked to original sources
PubMed2006

From monomers to solids: controlled hydrolysis to form novel, heteroleptic hydroxide-containing complexes.

Four novel alkaline earth metal tetranuclear aryloxide/pyrazolate hydroxides of the general formula M4(ligand)6(OH)2(donor)n have been prepared by either adding stoichiometric quantities of water to preformed alkaline earth metal aryloxides or in a direct metalation regime combining metal, ligand (alcohol, pyrazole), and donor with stoichiometric amounts of water. The compounds are considered as potential intermediates in the sol-gel process. A nonhydrolyzable magnesium aryloxide has also been obtained using the same reaction scheme. Unexpectedly, a dimeric strontium complex with further association of a second dimer via hydrogen bonding from the solvent of crystallization, ethylenediamine, has been isolated by the treatment of strontium metal with a mixture of alcohol and water. All compounds were characterized using X-ray crystallography, 1H and 13C NMR, and IR spectroscopy.

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PubMed2005

Crystallographic data collection using a 0.22% bandwidth multilayer.

To bridge the gap between traditional multilayer and crystal optics a high-resolution multilayer monochromator with a bandwidth of 0.22% has been designed and installed on a bending-magnet beamline (F3) at the Cornell High Energy Synchrotron Source (CHESS) to provide an unfocused monochromatic X-ray beam for protein crystallography experiments. Crystallographic data of excellent quality from a medium-sized protein, Concanavalin A, were collected and processed using standard crystallographic programs. The data were successfully used for a structure solution and refinement. The flux from the multilayer monochromator is enhanced, relative to that from a flat Si(111) monochromator, by a factor of 5; consequently, data collection is faster and/or smaller samples may be used. At the same time, the bandwidth is narrow enough to avoid streaked spots. This experiment suggests that multilayer optics may play a valuable role in satisfying the demands of the structural biology community for rapid X-ray data collection, particularly at under-utilized bending-magnet beamlines.

Concanavalin A↗
PubMed2002

A novel group of alkaline earth metal amides: syntheses and characterization of M[N(2,6-(i)Pr(2)C(6)H(3))(SiMe(3))](2)(THF)(2) (M = Mg, Ca, Sr, Ba) and the linear, two-coordinate Mg[N(2,6-(i)Pr(2)C(6)H(3))(SiMe(3))](2).

Novel alkaline earth metal aryl-substituted silylamides were prepared using alkane (Mg) and salt elimination reactions (Mg, Ca, Sr, and Ba). The salt elimination regime involved the treatment of the alkaline earth metal iodides with 2 equiv of the respective potassium amide KNDiip(SiMe(3)), (Diip = 2,6-i-Pr(2)C(6)H(3)). The organomagnesium source for the alkane elimination was ((n)()Bu/(s)()Bu)(2)Mg. All compounds were characterized using (1)H, (13)C NMR, and IR spectroscopy, in addition to X-ray crystallography (except Mg[NDiip(SiMe(3))](2)THF(2)). Crystal data with Mo Kalpha (lambda = 0.710 73 A) are as follows: Mg[NDiip(SiMe(3))](2), 1, a = 9.4687(6) A, b = 9.6818(6) A, c = 17.9296(1) A, alpha = 96.487(1) degrees, beta = 94.537(1) degrees, gamma = 89.222(1) degrees, V = 1608.8(2) A(3), Z = 2 (two independent molecules), triclinic, space group P(-)1, R1 (all data) = 0.0508; (n)()BuMg[NDiip(SiMe(3))]THF(2), 2, a = 9.5413(1) A, b = 16.493(2) A, c = 9.8218(1) A, beta = 108.149(2) degrees, V = 1468.7(4) A(3), Z = 2, monoclinic, space group P2(1), R1(all data) = 0.1232; Ca[NDiip(SiMe(3))](2)THF(2), 4, a = 9.7074(1) A, b = 20.9466(4) A, c = 21.6242(3) A, alpha = 73.573(1) degrees, beta = 78.632(1) degrees, gamma = 89.621(1) degrees, V = 4129.1(1) A(3), Z = 4 (two independent molecules), triclinic, space group P(-)1, R1 (all data) = 0.0902; Sr[NDiip(SiMe(3))](2)THF(2), 5, a = 20.5874(5) A, b = 9.8785(2) A, c = 20.8522(5) A, beta = 102.035(2) degrees, V = 4147.6(2) A(3), Z = 4 (two independent molecules), monoclinic, space group P2/n, R1 (all data) = 0.0756; Ba[NDiip(SiMe(3))](2)THF(2), 6, a = 20.5476(2) A, b = 10.0353(2) A, c = 20.9020(4) A, beta = 101.657(1) degrees, V = 4221.0(1) A(3), Z = 4 (two independent molecules), monoclinic, space group P2/n, R1 (all data) = 0.0573.

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PubMed1999

Formation of Separated versus Contact Ion Triplets in Magnesium Thiolates. Synthesis and Characterization of [Mg(15-crown-5)(SCPh(3))(2)] and [Mg(15-crown-5)(THF)(2)][S-2,4,6-tBu(3)C(6)H(2))](2).

The synthesis and structural characterization of two magnesium thiolate complexes are described. Both compounds were prepared by analogous reactions routes, namely, alkane elimination and transamination, but using differently sized ligands. Utilization of the smaller HSCPh(3), resulted in the formation of [Mg(15-crown-5)(SCPh(3))(2)], 1, displaying a seven-coordinate magnesium center with two magnesium-sulfur bonds. Employment of the sterically more encumbered HS-2,4,6-tBu(3)C(6)H(2) yielded a separated cation and anions as displayed in [Mg(15-crown-5)(THF)(2)][S-2,4,6-tBu(3)C(6)H(2)](2), 2. Compound 2 exhibits a seven-coordinate cation, completing its coordination environment with five metal-crown-ether interactions in addition to two tetrahydrofuran (THF) contacts. The compounds were characterized by IR and NMR spectroscopy in addition to X-ray crystallography. Crystal data with Mo Kalpha (lambda = 0.710 73 Å) are as follows: 1, C(48)H(50)MgO(5)S(2), a = 8.4785(4) Å, b = 9.3595(5) Å, c = 13.8306(6) Å, alpha = 87.332(1) degrees, beta = 85.929(1) degrees, gamma = 68.733(1) degrees, Z = 1, triclinic; 2, C(54)H(94)MgO(7)S(2), a = 13.6755(2) Å, b = 12.8045(6) Å, c = 32.7127(12) Å, beta = 97.87(1) degrees, Z = 4, monoclinic.

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PubMed1998

Syntheses and Structure Determinations of Calcium Thiolates.

The exploration of synthetic methodologies toward heavy alkaline-earth chalcogenolates resulted in the preparation and structural characterization of a family of calcium thiolates, including [Ca(SC(6)F(5))(2)(py)(4)], 1 (py = pyridine), the separated ion-triple [Ca(18-crown-6)(NH(3))(3))][SMes](2).2THF, 2 (Mes = 2,4,6-tBu(3)C(6)H(2)), and the contact triple [Ca(18-crown-6)(SMes)(2)].THF, 3. Compound 1 was prepared by treating [Ca(N(SiMe(3))(2))(2)](2) with 4 equiv of HSC(6)F(5) under addition of pyridine. The thiolates 2 and 3 were synthesized by treatment of calcium metal dissolved in dry, liquid NH(3) under addition of 2 equiv of HSMes and crown ether or, alternatively, by the reduction of MesSSMes with calcium metal in dry, liquid ammonia. We also report two reaction products isolated during attempted calcium thiolate syntheses: [CaBr(4)(THF)(2)(&mgr;(2)-Li)(2)(THF)(4)], 4, isolated as the product of a salt elimination reaction between CaBr(2) and 2 equiv of [Li(THF)(n)()S-2,4,6-(i)()Pr(3)C(6)H(2)](m)(). [(NH(4))(py)(SC(6)F(5))], 5, was obtained as the sole product in the reaction of metallic calcium with HSC(6)F(5) in liquid ammonia under addition of pyridine. All compounds were characterized by single-crystal X-ray crystallography in addition to IR and NMR spectroscopy.

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PubMed1998

A Convenient Synthetic Strategy toward Heavy Alkali Metal Bis(trimethylsilyl)phosphides: Crystal Structures of the Ladder-Type Polymers [A(thf)P(SiMe(3))(2)](infinity) (A = K, Rb, Cs).

A series of highly reactive heavy alkali metal phosphides was prepared by treating trimethylsilyl-substituted phosphines with alkali metal tert-butyl alcoholates. The compounds are formed in excellent yield and purity, and the side product can be easily removed in a vacuum. The high synthetic potential of this reaction route was further shown by utilizing excess alkali metal tert-butyl alcoholates in reaction with silyl substituted phosphines. In all cases, only monometalated products were isolated. In the course of this work the crystal structures of the bis(trimethylsilyl)phosphides [K(thf)P(SiMe(3))(2)](infinity), 1a, [Rb(thf)P(SiMe(3))(2)](infinity), 1b, and [Cs(thf)P(SiMe(3))(2)](infinity), 1c, were obtained. The compounds display polymeric ladder-type structures. Compounds 1a,b are isomorphous, while compound 1c displays a slightly altered local geometry. Despite small differences in local geometry, the coordination spheres for the phosphorus atoms and the alkali metal are fairly similar. The five coordinate phosphorus atoms are connected to three alkali metal centers in addition to two trimethylsilyl groups. The alkali metals are four coordinate with ligations to three phosphorus centers in addition to one thf oxygen donor. Compounds 1a-c were characterized using elemental analysis, NMR spectroscopy, and X-ray crystallography. Crystal data with Mo Kalpha (lambda = 0.710 73 Å) at 150 K are as follows: 1a, a = 6.4261(2) Å, b = 12.4119(2) Å, c = 21.5447(4) Å, V = 1718.41(7) Å(3), Z = 4, orthorhombic, space group P2(1)2(1)2(1), 3427 independent reflections, R1 (all data) = 0.0351; 1b, a = 6.5338(2) Å, b = 12.5664(3) Å, c = 21.5537(5) Å, V = 1769.70(8) Å(3), Z = 4, orthorhombic, space group P2(1)2(1)2(1), 4195 independent reflections, R1 (all data) = 0.0776; 1c, a = 11.3515(1) Å, b = 22.3445(3) Å, c = 7.2501(1) Å, beta = 96.017(1) degrees, V = 1828.81(4) Å(3), Z = 4, monoclinic, space group P2(1)/c, 4343 independent reflections, R1 (all data) = 0.0811.

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