Literature DB >> 23794965

Synchrotron powder study of Na3V(PO3)3N.

Minwoong Kim1, Seung-Joo Kim.   

Abstract

Polycrystalline tris-odium vanadium(III) nitridotriphosphate, Na3V(PO3)3N, was prepared by thermal nitridation of a mixture of NaPO3 and V2O5. The title compound is isotypic with Na3Al(PO3)3N. In the crystal, the P-atom and the three O-atom sites are on general positions, whereas the Na-, V- and N-atom sites are located on threefold rotation axes. The P atom is coordinated by three O atoms and one N atom in form of a slightly distorted tetra-hedron. Three PO3N tetra-hedra build up a nitridotriphosphate group, (PO3)3N, by sharing a common N atom. The V atom is coordinated by six O atoms in form of a slightly distorted octa-hedron. The Na(+) ions occupy three crystallographically distinct sites. One Na(+) ion is situated in an irregular polyhedral coordination environment composed of six O atoms and one N atom, while the other two Na(+) cations are surrounded by six and nine O atoms, respectively.

Entities:  

Year:  2013        PMID: 23794965      PMCID: PMC3684863          DOI: 10.1107/S1600536813012427

Source DB:  PubMed          Journal:  Acta Crystallogr Sect E Struct Rep Online        ISSN: 1600-5368


Related literature

For structure determination of the isotypic Na3Al(PO3)3N, see: Conanec et al. (1994 ▶). For the preparation of various related materials, A 3 B(PO3)3N (A = Na, K; B = Al, Ga, Cr, Mn, Fe) and A 2 B 2(PO3)3N (A = Na; B = Mg, Mn, Fe, Co), see: Conanec et al. (1996 ▶); Feldmann (1987 ▶). For studies focused on the ionic conductivity of Na2Mg2(PO3)3N, see: Lee et al. (2012 ▶). For a review of structural features of metal nitridophosphate compounds, see: Marchand & Laurent (1991 ▶); Marchand et al. (2000 ▶). For bond-valence-sum calculations, see: Brese & O’Keeffe (1991 ▶). For comparison of bond lengths in related structures, see: Conanec et al. (1994 ▶); Jacobs & Nymwegen (1997 ▶); Lee et al. (2012 ▶); Shannon (1976 ▶); Zatovsky (2010 ▶).

Experimental

Crystal data

n class="Chemical">Na3V(PO3)3N M = 370.83 Cubic, a = 9.44783 (5) Å n class="Chemical">V = 843.33 (1) Å3 Z = 4 Synchrotron radiation, λ = 1.547400 Å T = 298 K Flat sheet, 20 × 20 mm

Data collection

Pohang Light Source 9B HRPD Beamline diffractometer Specimen mounting: packed powder pellet Data n class="Chemical">collectionpan> mode: reflectionpan> Scan method: step 2θmin = 10.060°, 2θmax = 130.500°, 2θstep = 0.010°

Refinement

R p = 0.091 R wp = 0.119 R exp = 0.075 R Bragg = 0.056 χ2 = 2.519 12045 data points 288 parameters Data collectionpan>: local software at 9B HRPD beamline; cell refinement: DICVOL (Boultif & Louër, 2004 ▶); data reduction: local software at 9B HRPD beamline; method used to solve structure: coordinates taken from an isotypic compound; program(s) used to refine structure: FULLPROF (Rodriguez-Carvajal, 2001 ▶); molecular graphics: DIAMOND (Brandenburg, 1999 ▶); software used to prepare material for publication: FULLPROF. Click here for additionn class="Chemical">al data file. Crystal structure: contains datablock(s) global, I. DOI: 10.1107/S1600536813012427/wm2731sup1.cif Click here for additionn class="Chemical">al data file. Rietveld powder data: contains datablock(s) I. DOI: 10.1107/S1600536813012427/wm2731Isup2.rtv Additional supplementary materials: crystallographic information; 3D view; checkCIF report
Na3V(PO3)3NDx = 2.92 Mg m3
Mr = 370.83Synchrotron radiation, λ = 1.547400 Å
Cubic, P213T = 298 K
Hall symbol: P 2ac 2ab 3Particle morphology: powder
a = 9.44783 (5) Ågreen
V = 843.33 (1) Å3flat sheet, 20 × 20 mm
Z = 4
Pohang Light Source 9B HRPD Beamline diffractometerData collection mode: reflection
Radiation source: synchrotronScan method: step
Si 111 monochromatormin = 10.060°, 2θmax = 130.500°, 2θstep = 0.010°
Specimen mounting: packed powder pellet
Rp = 0.09112045 data points
Rwp = 0.11935 parameters
Rexp = 0.0750 restraints
RBragg = 0.056(Δ/σ)max = 0.02
χ2 = 2.519
xyzUiso*/Ueq
P10.3326 (3)0.0844 (3)0.2446 (3)0.0143 (4)*
V10.08073 (17)−0.08073 (17)0.41927 (17)0.0144 (6)*
Na10.0136 (3)0.0136 (3)0.0136 (3)0.0278 (18)*
Na20.3913 (4)0.3913 (4)0.3913 (4)0.0171 (18)*
Na30.6989 (5)0.1989 (5)0.3011 (5)0.0310 (19)*
O10.2722 (6)−0.0265 (6)0.3479 (5)0.0130 (14)*
O20.3727 (5)0.0002 (6)0.1109 (5)0.0073 (15)*
O30.4543 (6)0.1700 (6)0.3106 (6)0.0160 (18)*
N10.1937 (7)0.1937 (7)0.1937 (7)0.012 (3)*
P1—O31.538 (6)Na1—N12.947 (7)
P1—O21.540 (6)Na2—O3viii2.304 (7)
P1—O11.541 (6)Na2—O3v2.304 (7)
P1—N11.738 (7)Na2—O32.304 (7)
V1—O1i1.997 (6)Na2—O2ix2.456 (6)
V1—O1ii1.997 (6)Na2—O2x2.456 (6)
V1—O11.997 (6)Na2—O2xi2.456 (6)
V1—O2iii2.013 (5)Na3—O32.329 (7)
V1—O2iv2.013 (5)Na3—O3x2.329 (7)
V1—O2v2.013 (5)Na3—O3xii2.329 (7)
Na1—O1vi2.561 (6)Na3—O1xiii2.964 (7)
Na1—O1vii2.561 (6)Na3—O1xiv2.964 (7)
Na1—O1i2.561 (6)Na3—O1xi2.964 (7)
Na1—O3vii2.604 (6)N1—P1viii1.738 (7)
Na1—O3i2.604 (6)N1—P1v1.738 (7)
Na1—O3vi2.604 (6)
O3—P1—O2114.9 (6)O1—V1—O2iii90.5 (4)
O3—P1—O1112.2 (6)O1i—V1—O2iv92.2 (4)
O2—P1—O1105.0 (5)O1ii—V1—O2iv90.5 (4)
O3—P1—N1111.4 (6)O1—V1—O2iv176.8 (5)
O2—P1—N1105.4 (6)O2iii—V1—O2iv86.5 (3)
O1—P1—N1107.4 (6)O1i—V1—O2v90.5 (4)
O1i—V1—O1ii90.8 (4)O1ii—V1—O2v176.8 (5)
O1i—V1—O190.8 (4)O1—V1—O2v92.2 (4)
O1ii—V1—O190.8 (4)O2iii—V1—O2v86.5 (3)
O1i—V1—O2iii176.8 (5)O2iv—V1—O2v86.5 (3)
O1ii—V1—O2iii92.2 (4)
  1 in total

1.  NASICON-type Na(3)V(2)(PO(4))(3).

Authors:  Igor V Zatovsky
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2010-01-27
  1 in total
  1 in total

1.  Structural features of the oxidonitridophosphates K3 M III(PO3)3N (M III = Al, Ga).

Authors:  Igor V Zatovsky; Ivan V Ogorodnyk; Vyacheslav N Baumer; Ivan D Zhilyak; Ruslana V Horda; Nataliya Yu Strutynska
Journal:  Acta Crystallogr E Crystallogr Commun       Date:  2021-11-02
  1 in total

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