Skip to main content
OSTI.GOVU.S. Department of Energy Office of Scientific and Technical Information
U.S. Department of Energy
Office of Scientific and Technical Information
 

Crystal Growth of Four Oxovanadium(IV) Tartrates Prepared via a Mild Two-Step Hydrothermal Method: Observation of Spin-Dimer Behavior and Second Harmonic Generation

Journal Article · · Inorganic Chemistry
 [1];  [1];  [1];  [1];  [1];  [2];  [2];  [1]
  1. Univ. of South Carolina, Columbia, SC (United States)
  2. Univ. of Houston, TX (United States)
+ Show Author Affiliations
Here, four new oxovanadium(IV) tartrates, namely, A2[(VO)2(C4H4O6)(C4H2O6)(H2O)2]·(H2O)2, where A = Cs, 1, Rb, 2; K2[(VO)2(C4H2O6)2(H2O)2]·(H2O)2, 3; and Na2[(VO)2(C4H4O6)(C4H2O6)(H2O)7]·(H2O)2, 4, were prepared utilizing a two-step, mild hydrothermal route involving l-(+)-tartaric acid as the reducing agent. All four compounds were structurally characterized by single-crystal and powder X-ray diffraction methods and were found to crystallize in the non-centrosymmetric orthorhombic space groups P212121 for 1, 2, and 4 and C2221 for 3. The temperature dependence of the magnetic susceptibility of these compounds was measured, and 1, 2, and 4 were found to be paramagnetic down to 2 K, while 3 was found to exhibit spin-dimer behavior. Compounds 1, 2, and 3 were found to be second harmonic generation active. Furthermore, all compounds were characterized by IR and UV–vis spectroscopies.
Research Organization:
Energy Frontier Research Centers (EFRC) (United States). Heterogeneous Functional Materials Center (HeteroFoaM)
Sponsoring Organization:
National Science Foundation (NSF); USDOE Office of Science (SC), Basic Energy Sciences (BES) (SC-22). Materials Sciences & Engineering Division
Grant/Contract Number:
SC0001061
OSTI ID:
1370134
Journal Information:
Inorganic Chemistry, Journal Name: Inorganic Chemistry Journal Issue: 8 Vol. 54; ISSN 0020-1669
Publisher:
American Chemical Society (ACS)Copyright Statement
Country of Publication:
United States
Language:
English

References (42)

The First Noncluster Vanadium(IV) Coordination Polymers: Solvothermal Syntheses, Crystal Structure, and Ion Exchange journal August 2001
Preparation of Vanadium Phosphate Catalysts from VOPO4 · 2H2O: Effect of Microwave Irradiation on Morphology and Catalytic Property journal July 2007
Oxovanadium(IV) complexes of citric and tartaric acids in aqueous solution journal November 1995
Relationships between the carbon-oxygen stretching frequencies of carboxylato complexes and the type of carboxylate coordination journal October 1980
Structures and magnetism of rubidium and cesium salts of dimeric oxovanadium(IV) tartrate(4−) complexes journal November 1988
Simple correction for the sample shape and radial offset effects on SQUID magnetometers: Magnetic measurements on Ln2O3 (Ln=Gd, Dy, Er) standards journal January 2015
Infrared Spectra-Structure Correlation Study of Vanadium-Oxygen Compounds. journal June 1963
Formation Principles for Templated Vanadium Selenite Oxalates journal August 2013
Synthesis and Crystal Structures of Various Phases of the Microporous Three-Dimensional Coordination Polymer [Zr(OH) 2 (C 2 O 4 )] n journal October 2013
Observation of Multiple Crystal-to-Crystal Transitions in a New Reduced Vanadium Oxalate Hybrid Material, Ba 3 [(VO) 2 (C 2 O 4 ) 5 (H 2 O) 6 ]·(H 2 O) 3 , Prepared via a Mild, Two-Step Hydrothermal Method journal August 2014
Structural Characterization of a Nanocrystalline Inorganic−Organic Hybrid with Fiberlike Morphology and One-Dimensional Antiferromagnetic Properties journal July 2009
Noncentrosymmetric Polar Oxide Material, Pb 3 SeO 5 : Synthesis, Characterization, Electronic Structure Calculations, and Structure−Property Relationships journal October 2009
Lithium Batteries and Cathode Materials journal October 2004
Oxidation states of vanadium journal July 1968
Spin-Gap Formation and Thermal Structural Studies in Reduced Hybrid Layered Vanadates journal June 2006
Vanadium(V) Tartrato Complexes:  Speciation in the H 3 O + (OH - )/H 2 VO 4 - /(2 R ,3 R )-Tartrate System and X-ray Crystal Structures of Na 4 [V 4 O 8 ( rac -tart) 2 ]·12H 2 O and (NEt 4 ) 4 [V 4 O 8 (( R , R )-tart) 2 ]·6H 2 O (tart = C 4 H 2 O 6 4 - ) journal May 2007
Low-Temperature Solvothermal Approach to the Synthesis of La 4 Ni 3 O 8 by Topotactic Oxygen Deintercalation journal July 2011
Two New Noncentrosymmetric (NCS) Polar Oxides: Syntheses, Characterization, and Structure–Property Relationships in BaMTe 2 O 7 (M = Mg 2+ or Zn 2+ ) journal January 2012
Crystal Growth, Structural Characterization, and Magnetic Properties of New Uranium(IV) Containing Mixed Metal Oxalates: Na 2 U 2 M(C 2 O 4 ) 6 (H 2 O) 4 (M = Mn 2+ , Fe 2+ , Co 2+ , and Zn 2+ ) journal January 2013
Crystal Growth, Structure, Polarization, and Magnetic Properties of Cesium Vanadate, Cs 2 V 3 O 8 : A Structure–Property Study journal April 2013
Synthesis of Divalent Europium Borate via in Situ Reductive Techniques journal June 2013
The Electronic Structure of the Vanadyl Ion journal February 1962
M(bipyridine)V 4 O 10 (M = Cu, Ag):  Hybrid Analogues of Low-Dimensional Reduced Vanadates journal August 2007
BiO(IO 3 ): A New Polar Iodate that Exhibits an Aurivillius-Type (Bi 2 O 2 ) 2+ Layer and a Large SHG Response journal August 2011
Synthesis, crystal structure, spectroscopic and magnetic properties of strontium oxovanadium( IV ) tartrate: molecular precursor for SrVO 3 journal January 1995
Synthesis and characterization of vanadosilicate mesoporous molecularsieves MCM-41 journal January 1997
Synthesis of lower-valent molybdenum oxides in aqueous solutions by reducing Na2MoO4 with NaBH4 journal January 1997
Synthesis of reduced vanadium oxides in aqueous solutions journal January 1998
Bulk and surface properties of highly dispersed VOx/ZrO2, VOx/SiO2 and VOx/TiO2/SiO2 systems and their relevance for propane oxidation journal January 2004
Bulk characterization methods for non-centrosymmetric materials: second-harmonic generation, piezoelectricity, pyroelectricity, and ferroelectricity journal January 2006
Layered vanadium and molybdenum oxides: batteries and electrochromics journal January 2009
Synthetically persistent, self assembled [VIV2VV4] polyoxovanadates: Facile synthesis, structure and magnetic analysis journal January 2011
Transition metal hydrogenophosphates: a potential source of new protonic and lithium conductors journal January 2011
A Powder Technique for the Evaluation of Nonlinear Optical Materials journal July 1968
Paramagnetic resonance in diluted copper salts I. Hyperfine structure in diluted copper Tutton salts
  • Bleaney, Brebis; Bowers, K. D.; Ingram, D. J. E.
  • Proceedings of the Royal Society of London. Series A. Mathematical and Physical Sciences, Vol. 228, Issue 1173, p. 147-157 https://doi.org/10.1098/rspa.1955.0039
journal February 1955
Electron spin resonance in three spin- 1 2 dimer systems: VO ( HPO 4 ) ⋅ 0.5 H 2 O , KZn ( H 2 O ) ( VO ) 2 ( PO 4 ) 2 ( H 2 PO 4 ) , and CsV 2 O 5 journal May 2010
OLEX2 : a complete structure solution, refinement and analysis program journal January 2009
A short history of SHELX journal December 2007
Bond-valence parameters obtained from a systematic analysis of the Inorganic Crystal Structure Database journal August 1985
Bond-valence parameters for solids journal April 1991
Magnetic Susceptibilities of A V 2 O 5 ( A = L i and Cs) with Square Pyramidal V(IV)O 5 journal October 1996
Determination of Vanadium(IV) and Vanadium(V) in Benfield Samples by IEC with Conductivity Detection journal May 2010

Cited By (2)

Application of a mild hydrothermal method to the synthesis of mixed transition-metal( ii )/uranium( iv ) fluorides journal January 2017
A pair of new chiral polyoxovanadates with decent NLO properties journal January 2018

Figures / Tables (13)

Figure 1(p. 2)figure Figure 1
Table 1(p. 3)table Table 1
Table 2(p. 4)table Table 2
Table 3(p. 4)table Table 3
Figure 2(p. 5)figure Figure 2
Figure 3(p. 5)figure Figure 3
Figure 4(p. 6)figure Figure 4
Figure 5(p. 6)figure Figure 5
Figure 6(p. 7)figure Figure 6
Figure 7(p. 7)figure Figure 7
Figure 8(p. 8)figure Figure 8
Figure 9(p. 8)figure Figure 9
Figure 10(p. 9)figure Figure 10

Similar Records

A new perspective on vanadyl tartrate dimers. Part II. Structure and spectroscopic properties of calcium vanadyl tartrate tetrahydrate
Journal Article · Thu Dec 30 23:00:00 EST 1993 · Journal of Coordination Chemistry · OSTI ID:75724
Electron-transfer reactions of oxovanadium(IV) and dioxovanadium(V) ions with metal tris(polypyridine) complexes in aqueous media
Journal Article · Wed Jun 18 00:00:00 EDT 1986 · Inorg. Chem.; (United States) · OSTI ID:5454958
Crystal structure of potassium sodium tartrate trihydrate
Journal Article · Mon Nov 14 23:00:00 EST 2011 · Crystallography Reports · OSTI ID:22054244

Related Subjects

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY