Synthesis and structural characterization of BaSr2Ge3O9

2016 ◽  
Vol 71 (12) ◽  
pp. 1225-1232
Author(s):  
Sebastian Bräuchle ◽  
Clivia Hejny ◽  
Hubert Huppertz
Keyword(s):  
High Temperature ◽  
Solid State ◽  
Structural Characterization ◽  
Diffraction Data ◽  
Barium Carbonate ◽  
Strontium Carbonate ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
X Ray

AbstractBaSr2Ge3O9 was prepared by high-temperature solid-state synthesis at 1100°C in a platinum crucible from barium carbonate, strontium carbonate, and germanium(IV) oxide. The compound crystallizes in the triclinic space group P1̅ (no. 2) isotypically to walstromite BaCa2Si3O9. The structure was refined from single-crystal X-ray diffraction data: a=7.104(5), b=10.060(7), c=7.099(5) Å, α=83.0(2), β=77.0(2), γ=70.2(2)°, V=464.3(6) Å3, R1=0.0230, and wR2=0.0602 for all data. BaSr2Ge3O9 is characterized by three-membered rings of germanate tetrahedra. There are three crystallographically different Ge sites (Ge1, Ge2, and Ge3) in each [Ge3O9]6− ring. The rings occur in layers with the apices of alternating rings pointing in opposite directions. The Sr2+ and Ba2+ ions are located in between. The Sr1 cation is eight-fold coordinated, while Sr2 is octahedrally surrounded by oxide anions, and the Ba cation again eight-fold coordinated.

Synthesis and structural characterization of Li3Y(BO3)2

2017 ◽  
Vol 72 (2) ◽  
pp. 153-158 ◽  
Author(s):  
Sebastian Bräuchle ◽  
Hubert Huppertz
Keyword(s):  
Crystal Structure ◽  
High Temperature ◽  
Solid State ◽  
Boric Acid ◽  
Structural Characterization ◽  
Diffraction Data ◽  
Lithium Carbonate ◽  
X Ray Diffraction ◽  
X Ray

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.

Synthesis and structural characterization of Li3K3Eu7(BO3)9

2017 ◽  
Vol 72 (12) ◽  
pp. 959-965 ◽  
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.

Niobium-bearing arsenides and germanides from elemental mixtures not involving niobium: a new twist to an old problem in solid-state synthesis

2018 ◽  
Vol 74 (5) ◽  
pp. 623-627 ◽  
Author(s):  
Sviatoslav Baranets ◽  
Hua He ◽  
Svilen Bobev
Keyword(s):  
High Temperature ◽  
Solid State ◽  
Diffraction Data ◽  
Alkaline Earth ◽  
Alkaline Earth Metals ◽  
X Ray Diffraction ◽  
X Ray ◽  
High Temperature Reactions ◽  
First Time ◽  
Synthetic Work

Three isostructural transition-metal arsenides and germanides, namely niobium nickel arsenide, Nb0.92(1)NiAs, niobium cobalt arsenide, NbCoAs, and niobium nickel germanide, NbNiGe, were obtained as inadvertent side products of high-temperature reactions in sealed niobium containers. In addition to reporting for the very first time the structures of the title compounds, refined from single-crystal X-ray diffraction data, this article also serves as a reminder that niobium containers may not be suitable for the synthesis of ternary arsenides and germanides by traditional high-temperature reactions. Synthetic work involving alkali or alkaline-earth metals, transition or early post-transition metals, and elements from groups 14 or 15 under such conditions may yield Nb-containing products, which at times could be the major products of such reactions.

Energetic Materials: The Preparation and Structural Characterization of Three Biguanidinium Dinitramides

1997 ◽  
Vol 53 (3) ◽  
pp. 504-512 ◽  
Author(s):  
A. Martin ◽  
A. A. Pinkerton ◽  
R. D. Gilardi ◽  
J. C. Bottaro
Keyword(s):  
Hydrogen Bonding ◽  
Structural Characterization ◽  
Diffraction Data ◽  
Energetic Materials ◽  
Room Temperature ◽  
Asymmetric Structure ◽  
X Ray Diffraction ◽  
X Ray ◽  
Bond Lengths

Three biguanidinium salts of the energetic dinitramide anion have been prepared and structurally characterized from room-temperature X-ray diffraction data. Biguanidinium mono-dinitramide, (BIGH)(DN), triclinic, P\overline 1, a = 4.3686 (4), b = 9.404 (2), c = 10.742 (1) Å, \alpha = 83.54 (1), \beta = 80.386 (9), \gamma = 79.93 (1)°, V = 426.8 (1) Å3, Z = 2, D x = 1.62 g cm−3. Biguanidinium bis-dinitramide, (BIGH2)(DN)2, monoclinic, C2/c, a = 11.892 (2), b = 8.131 (1), c = 13.038 (2) Å, \beta = 115.79 (1)°, V = 1135.1 (3) Å3, Z = 4, D x = 1.84 g cm−3. Biguanidinium bis-dinitramide monohydrate, (BIGH2)(DN)2.H2O, orthorhombic, P212121, a = 6.4201 (6), b = 13.408 (1), c = 14.584 (2) Å, V = 1255.4 (4) Å3, Z = 4, D x = 1.76 g cm−3. All three structures are characterized by extensive hydrogen bonding. Both the mono- and diprotontated cations consist of two planar halves twisted with respect to each other. The dinitramide anion has a surprisingly variable and asymmetric structure. The two halves of the anion are twisted with respect to each other; however, the twist varies from 5.1 to 28.9°. In addition, the two ends of the anion have significantly different geometries, e.g. the `equivalent' N—N bond lengths differ by up to 0.045 Å.

Crystal structure and X-ray diffraction data of a new hexagonal perovskite compound, Ba4CuNb3O12

2011 ◽  
Vol 26 (3) ◽  
pp. 244-247
Author(s):  
N. Kumada ◽  
W. Zhang ◽  
Q. Dong ◽  
T. Mochizuki ◽  
Y. Yonesaki ◽  
...  
Keyword(s):  
Crystal Structure ◽  
High Temperature ◽  
Chemical Composition ◽  
Solid State ◽  
Diffraction Data ◽  
Solid State Reaction ◽  
Inert Atmosphere ◽  
X Ray Diffraction ◽  
X Ray ◽  
Barium Copper

A new barium copper niobate, Ba4CuNb3O12, was successfully prepared by high-temperature solid-state reaction in an inert atmosphere. Rietveld-refinement analysis of the XRD data of the compound showed that it has the 8H-type hexagonal perovskite structure with space group P63/mmc (#194), a = 5.830(1) Å, c = 19.123(1) Å, and chemical composition of Ba4Cu1.84Nb2.16O12-δ.

Synthesis and structural characterization of Ca12Ge17B8O58

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.

scholarly journals Structural Characterization of Caddisfly Silk with Solid-State NMR and X-Ray Diffraction

2014 ◽  
Vol 106 (2) ◽  
pp. 227a ◽  
Author(s):  
J. Bennett Addison ◽  
Warner S. Weber ◽  
Qiushi Mou ◽  
Gregory P. Holland ◽  
Jeffery L. Yarger
Keyword(s):  
Solid State ◽  
Structural Characterization ◽  
Solid State Nmr ◽  
X Ray Diffraction ◽  
X Ray

Multifaceted Sn–Sn bonding in the solid state. Synthesis and structural characterization of four new Ca–Li–Sn compounds

2019 ◽  
Vol 48 (38) ◽  
pp. 14398-14407 ◽  
Author(s):  
Alexander Ovchinnikov ◽  
Svilen Bobev
Keyword(s):  
Solid State ◽  
Single Crystal ◽  
Ab Initio ◽  
Structural Characterization ◽  
Chemical Bonding ◽  
X Ray Diffraction ◽  
X Ray ◽  
Rich Diversity ◽  
New Compounds

Four new ternary Ca–Li–Sn phases have been characterized using single-crystal X-ray diffraction and ab initio calculations. The new compounds demonstrate rich diversity of Sn-based polyanionic structures with various chemical bonding patterns.

The synthesis and structural characterization of linear and macrocyclic bis(dinitrosyliron) complexes supported by bis(phosphine) bridging ligands

2003 ◽  
Vol 81 (6) ◽  
pp. 468-475 ◽  
Author(s):  
Lijuan Li ◽  
Nada Reginato ◽  
Michael Urschey ◽  
Mark Stradiotto ◽  
John D Liarakos
Keyword(s):  
Solid State ◽  
Structural Characterization ◽  
Mononuclear Complex ◽  
Phosphine Ligands ◽  
Molecular Structures ◽  
X Ray Diffraction ◽  
Bridging Ligands ◽  
X Ray ◽  
Phosphine Complexes

Reactions involving Fe(NO)2(CO)2 and the bis(phosphine) ligands bis(diphenylphosphino)methane (DPPM), bis(diphenylphosphino)acetylene (DPPA), 1,6-bis(diphenylphosphino)hexane (DPPH), and 1,4-bis(diphenyl phosphino)benzene (DPPB) have been examined. From these reactions, the mononuclear complex, Fe(κ1-DPPM)(NO)2(CO) 3, linear dinuclear species of the type Fe2(µ-L)(NO)4(CO)2 (L = Ph2PCH2PPh2 4, Ph2PC[Formula: see text]CPPh2 5, Ph2PCH2(CH3)4CH2PPh2 6, and Ph2P(p-C6H4)PPh2 7), and macrocyclic dinuclear species of the type Fe2(µ-L)2(NO)4 (L = Ph2PCH2PPh2 8 and Ph2PC[Formula: see text]CPPh2 9) were isolated and spectroscopically characterized. For 4, 5, 8, and 9, the solid-state molecular structures of the products were determined by use of single-crystal X-ray diffraction techniques. Key words: dinitrosyliron, iron nitrosyls, dinuclear macrocycles, bis(phosphine) complexes.

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