Literature DB >> 21202432

Dineodymium(III) ditungstate(VI), Nd(2)W(2)O(9).

Peter Held1, Petra Becker.   

Abstract

Single crystals of monoclinic Nd(2)W(2)O(9) were obtained by growth from tungsten borate flux in an atmosphere of air. The crystal structure consists of chains of distorted [WO(6)] octa-hedra that run along the c axis of the structure, and of [NdO(9)] polyhedra that are connected via common faces and common edges to form a three-dimensional framework.

Entities:  

Year:  2008        PMID： 21202432      PMCID： PMC2961361          DOI： 10.1107/S1600536808009914

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


Related literature

For literature on related structures, see: Lacorre et al. (2000 ▶), Goutenoire et al. (2000 ▶) and Evans et al. (2005 ▶) for La2Mo2O9; Laligant et al. (2001 ▶) for La2W2O9; Yoshimura et al. (1976 ▶) for Ce2W2O9; Borisov & Klevtsova (1970 ▶) for Pr2W2O9; Aruga et al. (2005 ▶) for Eu2W2O9.

Experimental

Crystal data

Nd2W2O9 M = 800.17 Monoclinic, a = 7.6501 (11) Å b = 9.8547 (10) Å c = 9.2326 (13) Å β = 107.538 (11)° V = 663.69 (15) Å3 Z = 4 Mo Kα radiation μ = 49.96 mm−1 T = 290 (1) K 0.25 × 0.15 × 0.13 mm

Data collection

Stoe IPDSII diffractometer Absorption correction: numerical [X-SHAPE (Stoe & Cie, 1999 ▶) and X-RED (Stoe & Cie, 2001 ▶)] T min = 0.080, T max = 0.469 15723 measured reflections 2330 independent reflections 2072 reflections with I > 2σ(I) R int = 0.088

Refinement

R[F 2 > 2σ(F 2)] = 0.037 wR(F 2) = 0.093 S = 1.09 2330 reflections 119 parameters Δρmax = 2.34 e Å−3 Δρmin = −1.62 e Å−3 Data collection: X-AREA (Stoe & Cie, 2001 ▶); cell refinement: X-AREA; data reduction: X-AREA; program(s) used to solve structure: SIR92 (Altomare et al., 1993 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: ATOMS (Dowty, 2002 ▶); software used to prepare material for publication: SHELXL97. Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536808009914/si2082sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536808009914/si2082Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
Nd2W2O9F000 = 1360
Mr = 800.17Dx = 8.008 Mg m−3
Monoclinic, P21/cMo Kα radiation λ = 0.71073 Å
a = 7.6501 (11) ÅCell parameters from 25 reflections
b = 9.8547 (10) Åθ = 20.1–27.6º
c = 9.2326 (13) ŵ = 49.96 mm−1
β = 107.538 (11)ºT = 290 (1) K
V = 663.69 (15) Å3Prism, light purple
Z = 40.25 × 0.15 × 0.13 mm
Stoe IPDSII diffractometer2330 independent reflections
Radiation source: fine-focus sealed tube2072 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.088
T = 290(1) Kθmax = 32.2º
ω and φ scansθmin = 2.8º
Absorption correction: numerical[X-SHAPE (Stoe & Cie, 1999) and X-RED (Stoe & Cie, 2001)]h = −11→11
Tmin = 0.080, Tmax = 0.469k = −14→14
15723 measured reflectionsl = −13→13
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: full  w = 1/[σ2(Fo2) + (0.0439P)2 + 16.1611P] where P = (Fo2 + 2Fc2)/3
R[F2 > 2σ(F2)] = 0.037(Δ/σ)max < 0.001
wR(F2) = 0.093Δρmax = 2.34 e Å−3
S = 1.09Δρmin = −1.62 e Å−3
2330 reflectionsExtinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
119 parametersExtinction coefficient: 0.00391 (19)
Primary atom site location: structure-invariant direct methods
Experimental. A suitable single-crystal was carefully selected under a polarizing microscope and mounted in a glass capillary. The scattering intensities were collected on an imaging plate diffractometer (IPDS II, Stoe & Cie) equipped with a fine focus sealed tube X-ray source (Mo Kα, λ = 0.71073 Å) operating at 50 kV and 30 mA. Intensity data for the title compound were collected at room temperature by ω-scans in 180 frames (0 < ω < 180°; φ = 0° and 90°, Δω = 2°, exposure time of 10 min) in the 2Θ range 2.29 to 59.53°. Structure solution and refinement were carried out using the programs SIR92 (Altomare et al., 1993) and SHELXL97 (Sheldrick, 2008). A numerical absorption correction (X-RED (Stoe & Cie, 2001) was applied after optimization of the crystal shape (X-SHAPE (Stoe & Cie, 1999)). The last cycles of refinement included atomic positions and anisotropic parameters for all atoms. The final difference maps were free of any chemically significant features. The refinement was based on F2 for ALL reflections.
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.
xyzUiso*/Ueq
W10.57359 (5)0.72579 (4)−0.03462 (4)0.01073 (11)
W2−0.07053 (5)0.75136 (4)0.26320 (4)0.01058 (11)
Nd10.28098 (7)0.95544 (5)0.07401 (5)0.01298 (13)
Nd20.22931 (7)0.55245 (5)0.15396 (5)0.01243 (13)
O1−0.0113 (10)0.3795 (7)0.0941 (7)0.0131 (12)
O20.4920 (10)0.5969 (7)−0.1761 (7)0.0144 (12)
O30.7367 (9)0.8644 (7)0.1417 (7)0.0128 (12)
O40.7687 (10)0.6210 (8)0.0779 (8)0.0152 (13)
O50.0438 (10)0.5887 (7)0.3447 (8)0.0139 (12)
O60.0995 (10)0.7810 (7)0.1630 (8)0.0149 (13)
O70.4449 (9)0.8935 (6)−0.1077 (7)0.0109 (11)
O80.4091 (10)0.7091 (8)0.0739 (8)0.0147 (12)
O9−0.2605 (10)0.6904 (8)0.3610 (7)0.0143 (13)
U11U22U33U12U13U23
W10.01099 (18)0.01014 (18)0.01053 (17)0.00011 (11)0.00245 (12)0.00011 (11)
W20.01064 (18)0.01036 (17)0.01018 (17)0.00025 (11)0.00230 (12)0.00037 (11)
Nd10.0138 (2)0.0122 (2)0.0118 (2)−0.00143 (15)0.00216 (16)0.00027 (15)
Nd20.0124 (2)0.0116 (2)0.0123 (2)−0.00062 (15)0.00227 (16)0.00016 (15)
O10.016 (3)0.009 (3)0.011 (3)0.002 (2)−0.001 (2)0.003 (2)
O20.022 (3)0.010 (3)0.009 (3)−0.002 (2)0.001 (2)−0.003 (2)
O30.015 (3)0.011 (3)0.011 (3)0.006 (2)0.001 (2)0.001 (2)
O40.013 (3)0.017 (3)0.012 (3)0.006 (2)−0.001 (2)0.005 (2)
O50.018 (3)0.009 (3)0.012 (3)0.002 (2)0.001 (2)0.004 (2)
O60.013 (3)0.015 (3)0.019 (3)−0.004 (2)0.008 (2)0.004 (2)
O70.014 (3)0.006 (3)0.011 (3)0.002 (2)0.001 (2)0.002 (2)
O80.011 (3)0.019 (3)0.016 (3)−0.004 (2)0.007 (2)−0.001 (3)
O90.017 (3)0.015 (3)0.012 (3)0.001 (2)0.007 (2)0.002 (2)
W1—O21.794 (7)Nd1—Nd2vi3.7787 (9)
W1—O81.837 (7)Nd1—Nd2viii3.9479 (9)
W1—O41.855 (7)Nd2—O82.331 (7)
W1—O71.938 (6)Nd2—O7vii2.379 (6)
W1—O9i1.990 (7)Nd2—O12.447 (7)
W1—O32.202 (7)Nd2—O62.473 (8)
W1—Nd1ii3.3885 (7)Nd2—O1ix2.485 (6)
W1—Nd2iii3.4651 (7)Nd2—O2iii2.548 (8)
W1—Nd13.5344 (7)Nd2—O52.598 (7)
W2—O1iv1.796 (6)Nd2—O3x2.601 (7)
W2—O61.833 (7)Nd2—O4iii2.743 (8)
W2—O51.872 (6)Nd2—W2xi3.3800 (7)
W2—O3v1.917 (6)Nd2—W1iii3.4651 (7)
W2—O92.020 (7)O1—W2xi1.796 (6)
W2—O4v2.196 (7)O1—Nd2ix2.485 (6)
W2—Nd2iv3.3800 (7)O2—Nd1vi2.439 (7)
W2—Nd23.3934 (7)O2—Nd2iii2.548 (8)
Nd1—O5vi2.377 (6)O3—W2xii1.917 (6)
Nd1—O9iv2.409 (8)O3—Nd2viii2.601 (7)
Nd1—O2vii2.439 (7)O3—Nd1ii2.641 (7)
Nd1—O72.455 (7)O4—W2xii2.196 (7)
Nd1—O62.499 (7)O4—Nd2iii2.743 (8)
Nd1—O7ii2.513 (7)O5—Nd1vii2.377 (6)
Nd1—O82.618 (8)O7—Nd2vi2.379 (6)
Nd1—O3ii2.641 (7)O7—Nd1ii2.513 (7)
Nd1—O5iv3.096 (7)O9—W1xiii1.990 (7)
Nd1—W1ii3.3885 (7)O9—Nd1xi2.409 (8)
O2—W1—O8100.9 (3)O8—Nd1—Nd2vi84.50 (16)
O2—W1—O493.3 (3)O3ii—Nd1—Nd2vi43.46 (15)
O8—W1—O4102.3 (3)W1ii—Nd1—Nd2vi81.091 (15)
O2—W1—O7108.8 (3)W1—Nd1—Nd2vi64.843 (14)
O8—W1—O784.6 (3)O5vi—Nd1—Nd2viii159.13 (18)
O4—W1—O7155.3 (3)O9iv—Nd1—Nd2viii74.28 (17)
O2—W1—O9i94.2 (3)O2vii—Nd1—Nd2viii38.63 (18)
O8—W1—O9i160.6 (3)O7—Nd1—Nd2viii84.99 (15)
O4—W1—O9i88.8 (3)O6—Nd1—Nd2viii118.17 (17)
O7—W1—O9i79.0 (3)O7ii—Nd1—Nd2viii35.06 (14)
O2—W1—O3166.6 (3)O8—Nd1—Nd2viii86.62 (16)
O8—W1—O388.9 (3)O3ii—Nd1—Nd2viii98.06 (15)
O4—W1—O375.5 (3)W1ii—Nd1—Nd2viii64.182 (13)
O7—W1—O381.0 (3)W1—Nd1—Nd2viii76.989 (16)
O9i—W1—O378.4 (3)Nd2vi—Nd1—Nd2viii116.337 (18)
O2—W1—Nd1ii129.2 (2)O8—Nd2—O7vii80.4 (2)
O8—W1—Nd1ii116.3 (2)O8—Nd2—O1149.9 (2)
O4—W1—Nd1ii110.0 (2)O7vii—Nd2—O1129.0 (2)
O7—W1—Nd1ii47.2 (2)O8—Nd2—O671.9 (3)
O9i—W1—Nd1ii44.4 (2)O7vii—Nd2—O686.5 (2)
O3—W1—Nd1ii51.18 (18)O1—Nd2—O6111.1 (2)
O2—W1—Nd2iii45.4 (2)O8—Nd2—O1ix79.9 (2)
O8—W1—Nd2iii122.5 (2)O7vii—Nd2—O1ix151.4 (2)
O4—W1—Nd2iii51.9 (2)O1—Nd2—O1ix74.3 (3)
O7—W1—Nd2iii142.0 (2)O6—Nd2—O1ix67.7 (2)
O9i—W1—Nd2iii76.8 (2)O8—Nd2—O2iii81.3 (3)
O3—W1—Nd2iii121.46 (17)O7vii—Nd2—O2iii74.0 (2)
Nd1ii—W1—Nd2iii120.734 (19)O1—Nd2—O2iii99.8 (2)
O2—W1—Nd1123.3 (2)O6—Nd2—O2iii149.1 (2)
O8—W1—Nd146.0 (2)O1ix—Nd2—O2iii122.9 (2)
O4—W1—Nd1132.0 (2)O8—Nd2—O5128.2 (2)
O7—W1—Nd141.7 (2)O7vii—Nd2—O573.2 (2)
O9i—W1—Nd1115.0 (2)O1—Nd2—O573.8 (2)
O3—W1—Nd170.08 (18)O6—Nd2—O562.9 (2)
Nd1ii—W1—Nd172.141 (17)O1ix—Nd2—O5103.6 (2)
Nd2iii—W1—Nd1166.031 (17)O2iii—Nd2—O5129.8 (2)
O1iv—W2—O696.6 (3)O8—Nd2—O3x139.7 (2)
O1iv—W2—O5106.8 (3)O7vii—Nd2—O3x66.3 (2)
O6—W2—O591.3 (3)O1—Nd2—O3x64.6 (2)
O1iv—W2—O3v93.3 (3)O6—Nd2—O3x125.3 (2)
O6—W2—O3v98.6 (3)O1ix—Nd2—O3x138.9 (2)
O5—W2—O3v156.4 (3)O2iii—Nd2—O3x68.4 (2)
O1iv—W2—O991.1 (3)O5—Nd2—O3x64.0 (2)
O6—W2—O9171.5 (3)O8—Nd2—O4iii91.3 (2)
O5—W2—O983.0 (3)O7vii—Nd2—O4iii134.1 (2)
O3v—W2—O984.5 (3)O1—Nd2—O4iii64.5 (2)
O1iv—W2—O4v166.5 (3)O6—Nd2—O4iii133.7 (2)
O6—W2—O4v90.9 (3)O1ix—Nd2—O4iii67.0 (2)
O5—W2—O4v84.0 (3)O2iii—Nd2—O4iii60.1 (2)
O3v—W2—O4v74.5 (3)O5—Nd2—O4iii138.4 (2)
O9—W2—O4v82.2 (3)O3x—Nd2—O4iii95.7 (2)
O1iv—W2—Nd2iv44.5 (2)O8—Nd2—W2xi160.01 (19)
O6—W2—Nd2iv109.4 (2)O7vii—Nd2—W2xi100.57 (16)
O5—W2—Nd2iv144.8 (2)O1—Nd2—W2xi30.95 (15)
O3v—W2—Nd2iv50.0 (2)O6—Nd2—W2xi128.07 (16)
O9—W2—Nd2iv78.7 (2)O1ix—Nd2—W2xi104.97 (16)
O4v—W2—Nd2iv122.34 (18)O2iii—Nd2—W2xi79.85 (16)
O1iv—W2—Nd2120.5 (2)O5—Nd2—W2xi70.14 (16)
O6—W2—Nd245.2 (2)O3x—Nd2—W2xi34.37 (14)
O5—W2—Nd249.4 (2)O4iii—Nd2—W2xi73.54 (16)
O3v—W2—Nd2129.1 (2)O8—Nd2—W2103.17 (19)
O9—W2—Nd2127.1 (2)O7vii—Nd2—W286.45 (16)
O4v—W2—Nd272.57 (19)O1—Nd2—W286.55 (17)
Nd2iv—W2—Nd2153.578 (17)O6—Nd2—W231.75 (16)
O5vi—Nd1—O9iv108.0 (2)O1ix—Nd2—W277.98 (17)
O5vi—Nd1—O2vii156.0 (2)O2iii—Nd2—W2159.08 (15)
O9iv—Nd1—O2vii92.4 (2)O5—Nd2—W233.16 (14)
O5vi—Nd1—O775.9 (2)O3x—Nd2—W297.17 (16)
O9iv—Nd1—O7119.6 (2)O4iii—Nd2—W2139.03 (14)
O2vii—Nd1—O7105.4 (2)W2xi—Nd2—W296.814 (16)
O5vi—Nd1—O679.4 (2)O8—Nd2—W1iii93.93 (19)
O9iv—Nd1—O6119.7 (2)O7vii—Nd2—W1iii102.97 (16)
O2vii—Nd1—O679.5 (2)O1—Nd2—W1iii75.32 (17)
O7—Nd1—O6120.2 (2)O6—Nd2—W1iii161.63 (17)
O5vi—Nd1—O7ii127.1 (2)O1ix—Nd2—W1iii98.99 (16)
O9iv—Nd1—O7ii60.9 (2)O2iii—Nd2—W1iii30.07 (15)
O2vii—Nd1—O7ii73.7 (2)O5—Nd2—W1iii134.69 (15)
O7—Nd1—O7ii69.7 (2)O3x—Nd2—W1iii73.07 (16)
O6—Nd1—O7ii153.1 (2)O4iii—Nd2—W1iii32.17 (14)
O5vi—Nd1—O890.9 (2)W2xi—Nd2—W1iii66.284 (15)
O9iv—Nd1—O8160.7 (2)W2—Nd2—W1iii161.709 (19)
O2vii—Nd1—O870.3 (2)W2xi—O1—Nd2104.6 (3)
O7—Nd1—O860.1 (2)W2xi—O1—Nd2ix148.7 (4)
O6—Nd1—O866.9 (2)Nd2—O1—Nd2ix105.7 (2)
O7ii—Nd1—O8104.5 (2)W1—O2—Nd1vi145.5 (4)
O5vi—Nd1—O3ii66.4 (2)W1—O2—Nd2iii104.6 (3)
O9iv—Nd1—O3ii63.2 (2)Nd1vi—O2—Nd2iii104.7 (3)
O2vii—Nd1—O3ii136.4 (2)W2xii—O3—W1103.7 (3)
O7—Nd1—O3ii64.7 (2)W2xii—O3—Nd2viii95.7 (2)
O6—Nd1—O3ii143.4 (2)W1—O3—Nd2viii152.7 (3)
O7ii—Nd1—O3ii63.0 (2)W2xii—O3—Nd1ii133.4 (3)
O8—Nd1—O3ii123.9 (2)W1—O3—Nd1ii88.3 (2)
O5vi—Nd1—W1ii105.15 (17)Nd2viii—O3—Nd1ii92.2 (2)
O9iv—Nd1—W1ii35.29 (17)W1—O4—W2xii106.1 (3)
O2vii—Nd1—W1ii98.77 (17)W1—O4—Nd2iii95.9 (3)
O7—Nd1—W1ii84.57 (15)W2xii—O4—Nd2iii147.0 (3)
O6—Nd1—W1ii154.94 (18)W2—O5—Nd1vii130.8 (4)
O7ii—Nd1—W1ii34.47 (14)W2—O5—Nd297.5 (3)
O8—Nd1—W1ii136.43 (15)Nd1vii—O5—Nd298.8 (3)
O3ii—Nd1—W1ii40.51 (15)W2—O6—Nd2103.0 (3)
O5vi—Nd1—W190.51 (18)W2—O6—Nd1145.6 (4)
O9iv—Nd1—W1141.30 (17)Nd2—O6—Nd1110.3 (3)
O2vii—Nd1—W180.66 (17)W1—O7—Nd2vi130.6 (3)
O7—Nd1—W131.71 (14)W1—O7—Nd1106.5 (3)
O6—Nd1—W196.60 (18)Nd2vi—O7—Nd1102.8 (2)
O7ii—Nd1—W180.69 (15)W1—O7—Nd1ii98.3 (3)
O8—Nd1—W130.35 (15)Nd2vi—O7—Nd1ii107.6 (2)
O3ii—Nd1—W196.28 (15)Nd1—O7—Nd1ii110.3 (2)
W1ii—Nd1—W1107.859 (18)W1—O8—Nd2143.0 (4)
O5vi—Nd1—Nd2vi42.80 (18)W1—O8—Nd1103.6 (3)
O9iv—Nd1—Nd2vi106.32 (16)Nd2—O8—Nd1110.9 (3)
O2vii—Nd1—Nd2vi143.23 (18)W1xiii—O9—W2138.0 (4)
O7—Nd1—Nd2vi37.87 (14)W1xiii—O9—Nd1xi100.3 (3)
O6—Nd1—Nd2vi115.25 (18)W2—O9—Nd1xi120.4 (3)
O7ii—Nd1—Nd2vi87.96 (15)
  2 in total

1.  A short history of SHELX.

Authors:  George M Sheldrick
Journal:  Acta Crystallogr A       Date:  2007-12-21       Impact factor: 2.290

2.  Designing fast oxide-ion conductors based on La2Mo2O9

Authors: 
Journal:  Nature       Date:  2000-04-20       Impact factor: 49.962
  2 in total

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