Synthesis and characterization of the alkali borate-nitrates Na3–x Kx[B6O10]NO3 (x=0.5, 0.6, 0.7)

2017 ◽  
Vol 72 (3) ◽  
pp. 215-223
Author(s):  
Teresa S. Ortner ◽  
Daniel Schildhammer ◽  
Martina Tribus ◽  
Bastian Joachim ◽  
Hubert Huppertz
Keyword(s):  
Crystal Structure ◽  
Synthesis And Characterization ◽  
The Novel ◽  
Orthorhombic Space Group ◽  
Cell Parameters ◽  
Potassium Borate ◽  
Mixed Alkali ◽  
New Type ◽  
Oxygen Framework

AbstractThree novel mixed alkali borate-nitrates Na3−xKx[B6O10]NO3(x=0.5, 0.6, 0.7) were synthesized hydrothermally; their crystal structures were determined through Rietveld analyses, and supported through EDX as well as vibrational spectroscopy. The phases represent solid solutions of the alkali borate-nitrate Na3(NO3)[B6O10], which was reported in 2002 as a “New type of boron-oxygen framework in the Na3(NO3)[B6O10] crystal structure” (O. V. Yakubovich, I. V. Perevoznikova, O. V. Dimitrova, V. S. Urusov,Dokl. Phys.2002,47, 791). Only two of the three crystallographically independent Na+positions in the new structures are partially substituted by K+; a pure potassium borate-nitrate was not formed until now. The cell parameters of the novel phases vary froma=1261.72(5)–1267.12(5),b=1004.19(5)–1007.96(4),c=770.55(3)–774.38(3) pm, andV=0.97630(6)–0.98905(6) nm3in the orthorhombic space groupPnma(no. 62), in alignment with increasing K+content.

Hydrothermal synthesis and characterization of the praseodymium borate-nitrate Pr[B5O8(OH)(H2O)0.87]NO3·2H2O

2017 ◽  
Vol 72 (9) ◽  
pp. 677-685
Author(s):  
Teresa S. Ortner ◽  
Hubert Huppertz
Keyword(s):  
Hydrothermal Synthesis ◽  
Synthesis And Characterization ◽  
The Novel ◽  
X Ray Diffraction ◽  
Unit Cell Parameters ◽  
X Ray ◽  
Cell Parameters ◽  
Rare Earth Borate ◽  
Ir And Raman

AbstractThe praseodymium borate-nitrate Pr[B5O8(OH)(H2O)0.87]NO3·2H2O was obtained in a hydrothermal synthesis. It crystallizes monoclinically in the space groupP21/n(no. 14) with four formula units (Z=4) and unit cell parameters ofa=641.9(3),b=1551.8(7),c=1068.4(5) pm, withβ=90.54(2)° yieldingV=1.0643(8) nm3. The defect variant constitutes the missing member in the series of isostructural, early rare earth borate-nitrates of the compositionRE[B5O8(OH)(H2O)x]NO3·2H2O [RE=La (x=0; 1), Ce (x=1), Nd (x=0.85), Sm (x=0)]. In addition to powder and single-crystal X-ray diffraction data, the novel borate-nitrate was characterized through IR and Raman spectroscopy.

Synthesis and Crystal Structure of Ulm-16, A New Open Framework Fluorinated Gallium Phosphate with 16-Ring Channels

1996 ◽  
Vol 431 ◽  
Author(s):  
Thierry Loiseau ◽  
Gérard Férey
Keyword(s):  
Crystal Structure ◽  
Synthesis And Characterization ◽  
Hydration Water ◽  
Orthorhombic Space Group ◽  
Synthesis And Crystal Structure ◽  
Open Framework ◽  
Structural Relationships ◽  
Vertex Sharing ◽  
Fully Connected

AbstractThe synthesis and characterization of ULM-16, a new fluorinated gallophosphate Ga4(PO4)F2 • 1.5 NC6H14 • 0.5 H2O • 0.5 H3O, is described. This material is hydrothermally prepared at 180°C using cyclohexylamine as the structuring agent. It cristallizes in the orthorhombic space group Pbcn (n° 60) with a = 27.329(4) Å, b = 17.377(2) Å, c = 10.2124(5) Å, V = 4849.6 (9) Å3 and Z = 8. The structure is built up from vertex-linked GaO4 and PO4 tetrahedra, GaO4F trigonal bipyramids and GaO4F2 octahedra forming hexameric units and infinite double crankshaft chains (called cc or UUDD). The hexameric unit is similar to that found in ULM-3, ULM-4, ULM-5 and ULM-8. The two types of building units are fully connected by vertex-sharing with respect to a strict Ga-P alternation. The 3-D framework consists of cylindrical tunnels delimited by sixteen and six polyhedra running along [001]. The cyclohexylamine molecules are trapped in the wider pores and interact with the bridging fluorine atoms and hydration water through hydrogen bonds. The ULM-16 topology is closely related to that of ULM-5 where, in ULM-16, the infinite crankshaft chains replace the isolated D4R cages of ULM-5. TGA curve (under argon) indicates that the ULM-16 structure is intact up to 800°C. Structural relationships will be stated explicitly for the different structures of the ULM-n series containing the hexameric units.

Two lithium tricyanomethanide compounds: syntheses and single-crystal structure determination of LiK[C(CN)3]2 and Li[C(CN)3]·½ (H3C)2CO

2015 ◽  
Vol 70 (3) ◽  
pp. 191-196 ◽  
Author(s):  
Olaf Reckeweg ◽  
Francis J. DiSalvo
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Single Crystals ◽  
Structure Determination ◽  
Monoclinic Space Group ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
Cell Parameters ◽  
New Compounds

AbstractThe new compounds LiK[C(CN)3]2 and Li[C(CN)3]·½ (H3C)2CO were synthesized and their crystal structures were determined. Li[C(CN)3]·½ (H3C)2CO crystallizes in the orthorhombic space group Ima2 (no. 46) with the cell parameters a=794.97(14), b=1165.1(2) and c=1485.4(3) pm, while LiK[C(CN)3]2 adopts the monoclinic space group P21/c (no. 14) with the cell parameters a=1265.7(2), b=1068.0(2) and c=778.36(12) pm and the angle β=95.775(7)°. Single crystals of K[C(CN)3] were also acquired, and the crystal structure was refined more precisely than before corroborating earlier results.

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