ChemInform Abstract: Synthesis and X-Ray Diffraction Crystal Structure of Zn[N(tBu)(SiMe3)]2. The First Solid-State Characterization of a Homoleptic Zinc Amide

AbstractLi3Y(BO3)2 was prepared by high-temperature solid state synthesis at 900°C in a platinum crucible from lithium carbonate, boric acid, and yttrium(III) oxide. The compound crystallizes monoclinically in the space group P21/c (no. 14) (Z=4) isotypically to Li3Gd(BO3)2. The structure was refined from single-crystal X-ray diffraction data: a=8.616(3), b=6.416(3), c=10.014(2) Å, β=116.6(2)°, V=494.9(3) Å3, R1=0.0211, and wR2=0.0378 for all data. The crystal structure of Li3Y(BO3)2 consists of [Y2O14] dinuclear units, which are interconnected to each other by planar B(1)O3 groups and LiO4 tetrahedra via common edges and corners along the a axis.

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Synthesis and structural characterization of Ca12Ge17B8O58

Zeitschrift für Naturforschung B ◽

10.1515/znb-2016-0126 ◽

2016 ◽

Vol 71 (11) ◽

pp. 1141-1146

Author(s):

Sebastian Bräuchle ◽

Klaus Wurst ◽

Hubert Huppertz

Keyword(s):

Crystal Structure ◽

High Temperature ◽

Solid State ◽

Three Dimensional ◽

X Ray Diffraction ◽

Open Structure ◽

X Ray ◽

Tetragonal Crystal ◽

Tetragonal Crystal System

AbstractCa12Ge17B8O58 was prepared by high-temperature solid state synthesis at 1100°C in a platinum crucible from calcium carbonate, boric acid, and germanium(IV) oxide. The compound crystallizes in the tetragonal crystal system in the space group P4̅ (No. 81) isotypically to Cd12Ge17B8O58. The structure was refined from single-crystal X-ray diffraction data: a = 15.053(8), c = 4.723(2) Å, V = 1070.2(2) Å3, R1 = 0.0151, and wR2 = 0.0339 for all data. The crystal structure of Ca12Ge17B8O58 consists of [Ge4O12]n chains composed of GeO4 tetrahedra and GeO6 octahedra. The chains are interconnected into a [Ge4O10.5]n network via corner sharing. By additional [Ge(B2O7)4]28– clusters, these units are connected to a three-dimensional [Ge17B8O58]24– framework. The open structure forms three types of tunnels with five-, six-, and seven-membered rings (MRs) along the c axis, where the Ca2+ are located.

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Synthesis and structural characterization of Li3K3Eu7(BO3)9

Zeitschrift für Naturforschung B ◽

10.1515/znb-2017-0146 ◽

2017 ◽

Vol 72 (12) ◽

pp. 959-965 ◽

Cited By ~ 2

Author(s):

Sebastian Bräuchle ◽

Markus Seibald ◽

Hubert Huppertz

Keyword(s):

Crystal Structure ◽

High Temperature ◽

Solid State ◽

Potassium Carbonate ◽

Diffraction Data ◽

Lithium Carbonate ◽

X Ray Diffraction ◽

Orthorhombic Space Group ◽

X Ray

AbstractLi3K3Eu7(BO3)9 was prepared by high-temperature solid state synthesis at 900°C in a platinum crucible from lithium carbonate, potassium carbonate, boric acid, and europium(III) oxide. The title compound crystallizes in the orthorhombic space group Pca21 (no. 29) (Z=4). The structure was refined from single-crystal X-ray diffraction data: a=21.126(2), b=6.502(2), c=17.619(2) Å, V=2420.1(2) Å3, R1=0.0183 and wR2=0.0412 for all data. The crystal structure of Li3K3Eu7(BO3)9 is isotypic to Li3K3Y7(BO3)9 featuring isolated BO3 units and LiO6 octahedra forming [Li3B4O21] units in the ac plane, which are linked by additional BO3 units. The K+ and Eu3+ cations are arranged in the cavities of the structure.

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A MOF based on a lead(II) 2-oxido-6-methylpyridine-4-carboxylate network

Zeitschrift für Naturforschung B ◽

10.1515/znb-2019-0208 ◽

2020 ◽

Vol 75 (4) ◽

pp. 365-369

Author(s):

Long Tang ◽

Yu Pei Fu ◽

Na Cui ◽

Ji Jiang Wang ◽

Xiang Yang Hou ◽

...

Keyword(s):

Crystal Structure ◽

Solid State ◽

Carboxylic Acid ◽

Thermogravimetric Analysis ◽

Metal Organic Framework ◽

X Ray Diffraction ◽

X Ray ◽

Connected Node ◽

Metal Organic ◽

Solid State Fluorescence

AbstractA new metal-organic framework, [Pb(hmpcaH)2]n (1), has been hydrothermally synthesized from Pb(OAc)2 · 3H2O and 2-hydroxy-6-methylpyridine-4-carboxylic acid (hmpcaH2; 2), and characterized by IR spectroscopy, elemental and thermogravimetric analysis, and single-crystal X-ray diffraction. In complex 1, each hmpcaH− ligand represents a three-connected node to combine with the hexacoordinated Pb(II) ions, generating a 3D binodal (3,6)-connected ant network. The crystal structure of 2 was determined. The solid-state fluorescence properties of 1 and 2 were investigated.

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Characterization of some mesogenic alkyl 1-thioglycosides

Canadian Journal of Chemistry ◽

10.1139/v02-157 ◽

2002 ◽

Vol 80 (8) ◽

pp. 1162-1165 ◽

Cited By ~ 2

Author(s):

B Henrissat ◽

G K Hamer ◽

M G Taylor ◽

R H Marchessault

Keyword(s):

Phase Transition ◽

Liquid Crystal ◽

Solid State ◽

Solid State Nmr ◽

Liquid Crystalline ◽

Liquid Crystal Phase ◽

X Ray Diffraction ◽

X Ray ◽

Liquid Crystalline Phases

A series of dodecyl 1-thio-β-D-glycosides has been synthesized and characterized (DSC, NMR, CP MAS, X-ray diffraction) as possible new marking materials with liquid-crystalline properties. These compounds undergo solid to liquid crystal phase transitions at various temperatures, which depend on the nature of the carbohydrate part of the structure. Their liquid-crystalline phases show extreme shear thinning behaviour.Key words: liquid crystal, powder X-ray diffraction, phase transition, thioglycoside, solid-state NMR, marking material

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Investigation of Solvatomorphism and Its Photophysical Implications for Archetypal Trinuclear Au3(1-Methylimidazolate)3

Molecules ◽

10.3390/molecules26154404 ◽

2021 ◽

Vol 26 (15) ◽

pp. 4404

Author(s):

Shengyang Guan ◽

David C. Mayer ◽

Christian Jandl ◽

Sebastian J. Weishäupl ◽

Angela Casini ◽

...

Keyword(s):

Crystal Structure ◽

Solid State ◽

Density Functional ◽

Bulk Material ◽

Variable Temperature ◽

Active Phase ◽

Solvent Free ◽

X Ray Diffraction ◽

X Ray ◽

Aurophilic Interactions

A new solvatomorph of [Au3(1-Methylimidazolate)3] (Au3(MeIm)3)—the simplest congener of imidazolate-based Au(I) cyclic trinuclear complexes (CTCs)—has been identified and structurally characterized. Single-crystal X-ray diffraction revealed a dichloromethane solvate exhibiting remarkably short intermolecular Au⋯Au distances (3.2190(7) Å). This goes along with a dimer formation in the solid state, which is not observed in a previously reported solvent-free crystal structure. Hirshfeld analysis, in combination with density functional theory (DFT) calculations, indicates that the dimerization is generally driven by attractive aurophilic interactions, which are commonly associated with the luminescence properties of CTCs. Since Au3(MeIm)3 has previously been reported to be emissive in the solid-state, we conducted a thorough photophysical study combined with phase analysis by means of powder X-ray diffraction (PXRD), to correctly attribute the photophysically active phase of the bulk material. Interestingly, all investigated powder samples accessed via different preparation methods can be assigned to the pristine solvent-free crystal structure, showing no aurophilic interactions. Finally, the observed strong thermochromism of the solid-state material was investigated by means of variable-temperature PXRD, ruling out a significant phase transition being responsible for the drastic change of the emission properties (hypsochromic shift from 710 nm to 510 nm) when lowering the temperature down to 77 K.

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