PMCCPMCCPMCC

Search tips
Search criteria 

Advanced

 
Logo of actaeInternational Union of Crystallographysearchopen accessarticle submissionjournal home pagethis article
 
Acta Crystallogr Sect E Struct Rep Online. 2010 July 1; 66(Pt 7): i51–i52.
Published online 2010 June 16. doi:  10.1107/S1600536810021768
PMCID: PMC3006697

The quinter­nary thio­phosphate Cs0.5Ag0.5Nb2PS10

Abstract

The quinter­nary thio­phosphate Cs0.5Ag0.5Nb2PS10, cesium silver tris­(disulfido)[tetra­thio­phosphato(V)]diniobate(IV), has been prepared from the elements using a CsCl flux. The crystal structure is made up of 1[Nb2PS10] chains expanding along [010]. These chains are built up from bicapped trigonal-prismatic [Nb2S12] units and tetra­hedral [PS4] groups and are linked through a linear S—Ag—S bridge, forming a two-dimensional layer. These layers then stack on top of each other, completing the three-dimensional structure with an undulating van der Waals gap. The disordered Cs+ ions reside on sites with half-occupation in the voids of this arrangement. Short [2.8843 (5) Å] and long [3.7316 (4) Å] Nb—Nb distances alternate along the chains, and anionic S2 2− and S2− species are observed. The charge balance of the com­pound can be represented by the formula [Cs+]0.5[Ag+]0.5[Nb4+]2[PS4 3−][S2 2−]3.

Related literature

For Nb2PS10-related quaternary thio­phosphates, see: Do & Yun (1996 [triangle]) for KNb2PS10, Kim & Yun (2002 [triangle]) for RbNb2PS10, Kwak et al. (2007 [triangle]) for CsNb2PS10, Bang et al. (2008 [triangle]) for TlNb2PS10, and Do & Yun (2009 [triangle]) for Ag0.88Nb2PS10. For quintenary thio­phosphates, see: Kwak & Yun (2008 [triangle]) for K0.34Cu0.5Nb2PS10, Dong et al. (2005a [triangle]) for K0.5Ag0.5Nb2PS10, and Dong et al. (2005b [triangle]) for Rb0.38Ag0.5Nb2PS10. PLATON (Spek, 2009 [triangle]) was used for structure validation. For typical Nb—P and P—S bond length, see: Brec et al. (1983 [triangle]), and for typical Nb4+–Nb4+ bond lengths, see: Angenault et al. (2000 [triangle]). For general background, see: Lee et al. (1988 [triangle]).

Experimental

Crystal data

  • Cs0.5Ag0.5Nb2PS10
  • M r = 657.78
  • Monoclinic, An external file that holds a picture, illustration, etc.
Object name is e-66-00i51-efi1.jpg
  • a = 7.3594 (3) Å
  • b = 12.8534 (4) Å
  • c = 13.7788 (6) Å
  • β = 91.0886 (12)°
  • V = 1303.15 (8) Å3
  • Z = 4
  • Mo Kα radiation
  • μ = 5.54 mm−1
  • T = 290 K
  • 0.30 × 0.06 × 0.04 mm

Data collection

  • Rigaku R-AXIS RAPID diffractometer
  • Absorption correction: multi-scan (ABSCOR; Higashi, 1995 [triangle]) T min = 0.602, T max = 1.000
  • 12389 measured reflections
  • 2991 independent reflections
  • 2430 reflections with I > 2σ(I)
  • R int = 0.049

Refinement

  • R[F 2 > 2σ(F 2)] = 0.034
  • wR(F 2) = 0.075
  • S = 1.08
  • 2991 reflections
  • 133 parameters
  • Δρmax = 1.18 e Å−3
  • Δρmin = −1.27 e Å−3

Data collection: RAPID-AUTO (Rigaku, 2006 [triangle]); cell refinement: RAPID-AUTO; data reduction: RAPID-AUTO; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 [triangle]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 [triangle]); molecular graphics: locally modified version of ORTEP (Johnson, 1965 [triangle]); software used to prepare material for publication: WinGX (Farrugia, 1999 [triangle]).

Table 1
Selected geometric parameters (Å, °)

Supplementary Material

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536810021768/wm2357sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536810021768/wm2357Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Acknowledgments

This work was supported by the Priority Research Centers Program through the National Research Foundation of Korea (NRF) funded by the Ministry of Education, Science and Technology (NRF-2009–0094047). Use was made of the X-ray facilities supported by Ajou University.

supplementary crystallographic information

Comment

During an effort to expand representatives of group 5 transition metal thiophosphates by substituting various monovalent cations, we were able to prepare a new derivative in this system. Here we report the synthesis and characterization of the new layered quinternary thiophosphate, Cs0.5Ag0.5Nb2PS10.

The title compound is isostructural with the previously reported K0.34Cu0.5Nb2PS10 (Kwak & Yun, 2008). The 1[Nb2PS10] chains found in this structure are composed of the typical biprismatic [Nb2S12] and tetrahedral [PS4] units. The Nb atoms are surrounded by 8 S atoms in a bicapped trigonal-prismatic fashion. Two prisms are sharing a rectangular face to form the [Nb2S12] unit. These units are bound through the S—S prism edges and through one of the capping sulfur atoms to make 1[Nb2S9] chains. One of the S atoms at the prism edge and two other capping S atoms are bound to the P atom to which an additional S atom (S1) is attached to complete the 1[Nb2PS10] chains. These anionic chains propagate parallel to [010] and are linked through the linear S—Ag—S bridge to form a two-dimensional layer along (201). These layers then stack on top of each other to complete the three-dimensional structure with an undulating van der Waals gap. The disordered Cs+ cations reside in the voids of this arrangement.

The Nb—S and P—S distances are in agreement with those found in other related phases (Brec et al., 1983). Along the chain, The Nb(1)···Nb(2) interactions alternate in the sequence of one short (2.8843 (5) Å) and one long (3.7316 (4) Å) distance. The short distance is close to that of the typical Nb4+—Nb4+ bond (Angenault et al., 2000), and the long Nb···Nb distance shows that there is no significant intermetallic bonding interaction. Such an arrangement is consistent with the high electric resistivity of the crystal along the needle axis (b axis).

The coordination around the Ag atom (1 symmetry) can be described as a [2 + 4] interaction. Four S atoms are bound to the Ag atoms in the plane (Ag—S6, 3.139 (3) Å, Ag—S9, 3.232 (3) Å), whereas two trans S atoms are coordinated to the Ag atom at short distances of Ag—S1 = 2.4625 (13) Å. The large ADPs of Ag could be explained by the second-order Jahn-Teller coupling between the filled Ag eg and the empty s orbitals (Lee et al., 1988), which is a common trend of d10 elements. The charge balance of the compound can be represented by the formula [Cs+]0.5[Ag+]0.5[Nb4+]2[PS43-][S22-]3.

For Nb2PS10-related quaternary thiophosphates, see: Do & Yun (1996) for KNb2PS10, Kim & Yun (2002) for RbNb2PS10, Kwak et al. (2007) for CsNb2PS10, Bang et al. (2008) for TlNb2PS10, and Do & Yun (2009) for Ag0.88Nb2PS10; for quinternary thiophosphates, see: Kwak & Yun (2008) for K0.34Cu0.5Nb2PS10, Dong et al. (2005a) for K0.5Ag0.5Nb2PS10, and Dong et al. (2005b) for Rb0.38Ag0.5Nb2PS10.

Experimental

Cs0.5Ag0.5Nb2PS10 was prepared by the reaction of elemental powders, using the reactive halide-flux technique. Ag powder (CERAC 99.999%), Nb powder (CERAC 99.8%), P powder (CERAC 99.5%) and S powder (Aldrich 99.999%) were mixed in a fused silica tube in a molar ratio of Ag:Nb:P:S=1:2:1:10 and then CsCl was added in a weight ratio of AgNb2PS10:CsCl=1:3. The tube was evacuated to 0.133 Pa, sealed and heated gradually (50 K/h) to 973 K, where it was kept for 72 h. The tube was cooled to room temperature at the rate of 4 K/h. The excess halide was removed with distilled water and dark red needle-shaped crystals were obtained. The crystals are stable in air and water. A qualitative X-ray fluorescence analysis of the needles indicated the presence of Cs, Ag, Nb, P, and S. The composition of the compound was determined by single-crystal X-ray diffraction.

Refinement

Refinement went smoothly but the anisotropic displacement parameters (ADPs) of the Cs (Wyckoff position 4e) and Ag (2a) atoms were large compared with those of the other atoms. Because non-stoichiometry in these phases is sometimes observed and the distance between Cs atoms is too short if full occupancy is assumed, the occupancies of each metal atom were checked by refining the site occupation factors (SOFs) while those of the other atoms were fixed. With the non-stoichiometric model, the SOF of the Cs site was reduced significantly from 1 to 0.49 and the residuals improved also. As no evidence was found for ordering of the Cs site at Wyckoff position 2c, a statistically disordered structure was finally modelled. The final difference Fourier map showed that the highest residual electron density (1.18 e/Å3) is 0.94 Å from the Nb2 site and the deepest hole (-1.27 e/Å3) is 0.84 Å from the Nb2 site. No additional symmetry, as tested by PLATON (Spek, 2009), has been detected in this structure.

Figures

Fig. 1.
A view of the Cs0.5Ag0.5Nb2PS10 structure. Anisotropic displacement ellipsoids are drawn at the 90% probability level. Symmetry codes are given in Table 1.

Crystal data

Cs0.5Ag0.5Nb2PS10F(000) = 1232
Mr = 657.78Dx = 3.353 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 8832 reflections
a = 7.3594 (3) Åθ = 3.2–27.5°
b = 12.8534 (4) ŵ = 5.54 mm1
c = 13.7788 (6) ÅT = 290 K
β = 91.0886 (12)°Needle, dark brown
V = 1303.15 (8) Å30.30 × 0.06 × 0.04 mm
Z = 4

Data collection

Rigaku R-AXIS RAPID diffractometer2430 reflections with I > 2σ(I)
graphiteRint = 0.049
ω scansθmax = 27.5°, θmin = 3.2°
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)h = −9→9
Tmin = 0.602, Tmax = 1.000k = −16→14
12389 measured reflectionsl = −17→17
2991 independent reflections

Refinement

Refinement on F2133 parameters
Least-squares matrix: full0 restraints
R[F2 > 2σ(F2)] = 0.034w = 1/[σ2(Fo2) + (0.0248P)2 + 3.4157P] where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.075(Δ/σ)max < 0.001
S = 1.08Δρmax = 1.18 e Å3
2991 reflectionsΔρmin = −1.27 e Å3

Special details

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2)

xyzUiso*/UeqOcc. (<1)
Cs−0.0009 (4)0.02093 (15)0.48715 (19)0.0512 (5)0.5
Ag0000.0539 (2)
Nb10.42651 (5)0.03565 (3)0.24995 (3)0.01333 (11)
Nb20.43445 (5)0.32590 (3)0.25353 (3)0.01280 (11)
P0.11427 (16)0.18631 (9)0.14370 (10)0.0170 (3)
S1−0.03805 (19)0.18878 (10)0.02229 (11)0.0292 (3)
S20.07865 (16)0.05281 (9)0.22287 (10)0.0210 (3)
S30.08568 (16)0.31790 (9)0.22464 (10)0.0207 (3)
S40.33249 (16)0.47121 (9)0.35994 (9)0.0187 (3)
S50.38477 (17)0.18131 (9)0.37848 (9)0.0190 (3)
S60.39304 (16)0.18214 (8)0.11963 (9)0.0161 (2)
S70.42828 (17)0.44324 (9)0.10942 (9)0.0194 (3)
S80.58572 (16)0.41695 (9)0.39426 (9)0.0184 (3)
S90.63765 (16)0.17797 (9)0.31795 (9)0.0189 (3)
S100.67972 (16)0.38737 (9)0.14538 (9)0.0204 (3)

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
Cs0.0270 (3)0.0779 (16)0.0489 (13)−0.0003 (11)0.0060 (7)−0.0283 (10)
Ag0.0518 (4)0.0298 (3)0.0800 (6)−0.0028 (3)0.0017 (4)−0.0287 (4)
Nb10.0150 (2)0.00814 (18)0.0168 (2)0.00081 (16)−0.00185 (16)0.00082 (16)
Nb20.0145 (2)0.00802 (19)0.0158 (2)−0.00071 (16)−0.00210 (16)−0.00048 (16)
P0.0157 (5)0.0115 (5)0.0235 (7)0.0014 (5)−0.0057 (5)−0.0025 (5)
S10.0325 (7)0.0228 (6)0.0316 (8)0.0023 (6)−0.0168 (6)−0.0038 (6)
S20.0181 (5)0.0140 (5)0.0310 (7)−0.0014 (5)−0.0023 (5)0.0030 (5)
S30.0168 (5)0.0146 (5)0.0305 (7)0.0023 (5)−0.0034 (5)−0.0073 (5)
S40.0190 (5)0.0146 (5)0.0225 (7)−0.0007 (5)0.0017 (5)−0.0031 (5)
S50.0256 (6)0.0126 (5)0.0189 (6)0.0001 (5)0.0008 (5)0.0007 (5)
S60.0186 (5)0.0104 (5)0.0193 (6)0.0019 (5)−0.0015 (5)−0.0007 (5)
S70.0269 (6)0.0131 (5)0.0180 (6)−0.0009 (5)−0.0044 (5)0.0004 (5)
S80.0233 (6)0.0124 (5)0.0195 (6)−0.0013 (5)−0.0043 (5)0.0000 (5)
S90.0185 (5)0.0128 (5)0.0251 (7)−0.0001 (5)−0.0054 (5)0.0009 (5)
S100.0217 (6)0.0152 (5)0.0244 (7)−0.0003 (5)0.0048 (5)−0.0021 (5)

Geometric parameters (Å, °)

Cs—Csi0.644 (3)Nb2—S82.5075 (12)
Cs—S10ii3.444 (3)Nb2—S52.5643 (13)
Cs—S10iii3.469 (3)Nb2—S92.5670 (12)
Cs—S7iv3.536 (3)Nb2—S32.5920 (12)
Cs—S7v3.581 (3)Nb2—S62.6250 (12)
Cs—S23.722 (3)Nb2—Nb1viii2.8843 (5)
Cs—S1v3.773 (2)P—S11.9962 (18)
Cs—S53.835 (3)P—S32.0391 (17)
Cs—S3v3.915 (3)P—S22.0527 (17)
Cs—S3iv3.956 (3)P—S62.0851 (17)
Cs—S9vi4.044 (3)S1—Csix3.773 (2)
Cs—S2i4.157 (3)S2—Csi4.157 (3)
Ag—S12.4625 (13)S3—Csix3.915 (3)
Ag—S1vii2.4625 (13)S3—Csx3.956 (3)
Nb1—S4iii2.4953 (13)S4—S82.0371 (17)
Nb1—S7iii2.4958 (12)S4—Nb1viii2.4953 (13)
Nb1—S8iii2.5055 (13)S5—S92.0542 (18)
Nb1—S10iii2.5231 (13)S7—S102.0372 (17)
Nb1—S92.5658 (12)S7—Nb1viii2.4958 (12)
Nb1—S22.5895 (12)S7—Csx3.536 (3)
Nb1—S52.5993 (13)S7—Csix3.581 (3)
Nb1—S62.6103 (12)S8—Nb1viii2.5055 (13)
Nb1—Nb2iii2.8843 (5)S9—Csxi4.044 (3)
Nb2—S102.4910 (13)S10—Nb1viii2.5231 (13)
Nb2—S72.4932 (13)S10—Csxii3.444 (3)
Nb2—S42.4985 (12)S10—Csviii3.469 (3)
Csi—Cs—S10ii86.8 (5)S9—Nb1—Nb2iii117.38 (3)
Csi—Cs—S10iii82.5 (5)S2—Nb1—Nb2iii115.30 (3)
S10ii—Cs—S10iii169.32 (5)S5—Nb1—Nb2iii136.98 (3)
Csi—Cs—S7iv88.8 (5)S6—Nb1—Nb2iii133.76 (3)
S10ii—Cs—S7iv73.85 (7)S10—Nb2—S748.25 (4)
S10iii—Cs—S7iv105.80 (8)S10—Nb2—S4110.06 (4)
Csi—Cs—S7v80.9 (5)S7—Nb2—S490.81 (4)
S10ii—Cs—S7v105.35 (8)S10—Nb2—S889.91 (4)
S10iii—Cs—S7v73.00 (7)S7—Nb2—S8109.55 (4)
S7iv—Cs—S7v169.64 (5)S4—Nb2—S848.02 (4)
Csi—Cs—S2128.9 (5)S10—Nb2—S5138.22 (4)
S10ii—Cs—S2134.71 (8)S7—Nb2—S5166.52 (4)
S10iii—Cs—S254.41 (5)S4—Nb2—S595.72 (4)
S7iv—Cs—S279.52 (6)S8—Nb2—S583.45 (4)
S7v—Cs—S2107.01 (8)S10—Nb2—S991.02 (4)
Csi—Cs—S1v139.1 (6)S7—Nb2—S9136.48 (4)
S10ii—Cs—S1v61.86 (5)S4—Nb2—S9122.02 (4)
S10iii—Cs—S1v127.50 (7)S8—Nb2—S980.28 (4)
S7iv—Cs—S1v105.15 (7)S5—Nb2—S947.20 (4)
S7v—Cs—S1v82.99 (6)S10—Nb2—S3130.35 (5)
S2—Cs—S1v91.71 (4)S7—Nb2—S384.19 (4)
Csi—Cs—S5131.1 (6)S4—Nb2—S379.18 (4)
S10ii—Cs—S5125.61 (7)S8—Nb2—S3124.13 (4)
S10iii—Cs—S562.86 (5)S5—Nb2—S385.47 (4)
S7iv—Cs—S5131.64 (7)S9—Nb2—S3126.33 (4)
S7v—Cs—S557.45 (5)S10—Nb2—S683.03 (4)
S2—Cs—S555.08 (4)S7—Nb2—S682.29 (4)
S1v—Cs—S564.82 (4)S4—Nb2—S6155.03 (4)
Csi—Cs—S3v88.9 (5)S8—Nb2—S6156.36 (4)
S10ii—Cs—S3v52.55 (5)S5—Nb2—S686.88 (4)
S10iii—Cs—S3v126.89 (9)S9—Nb2—S677.33 (4)
S7iv—Cs—S3v126.40 (9)S3—Nb2—S676.27 (4)
S7v—Cs—S3v53.89 (5)S10—Nb2—Nb1viii55.41 (3)
S2—Cs—S3v137.18 (6)S7—Nb2—Nb1viii54.72 (3)
S1v—Cs—S3v51.72 (4)S4—Nb2—Nb1viii54.67 (3)
S5—Cs—S3v86.11 (6)S8—Nb2—Nb1viii54.84 (3)
Csi—Cs—S3iv81.7 (5)S5—Nb2—Nb1viii138.05 (3)
S10ii—Cs—S3iv126.35 (9)S9—Nb2—Nb1viii119.58 (3)
S10iii—Cs—S3iv52.02 (5)S3—Nb2—Nb1viii112.65 (3)
S7iv—Cs—S3iv53.79 (5)S6—Nb2—Nb1viii133.06 (3)
S7v—Cs—S3iv123.87 (8)S1—P—S3112.52 (8)
S2—Cs—S3iv51.42 (5)S1—P—S2112.54 (8)
S1v—Cs—S3iv137.41 (7)S3—P—S2112.78 (8)
S5—Cs—S3iv100.03 (7)S1—P—S6113.93 (9)
S3v—Cs—S3iv170.63 (4)S3—P—S6102.73 (7)
Csi—Cs—S9vi137.7 (6)S2—P—S6101.48 (7)
S10ii—Cs—S9vi75.21 (6)P—S1—Ag91.46 (6)
S10iii—Cs—S9vi113.01 (7)P—S1—Csix94.72 (7)
S7iv—Cs—S9vi49.70 (4)Ag—S1—Csix161.76 (7)
S7v—Cs—S9vi140.51 (6)P—S2—Nb190.68 (5)
S2—Cs—S9vi59.66 (4)P—S2—Cs129.50 (7)
S1v—Cs—S9vi62.08 (4)Nb1—S2—Cs91.32 (6)
S5—Cs—S9vi89.44 (4)P—S2—Csi136.28 (7)
S3v—Cs—S9vi108.21 (6)Nb1—S2—Csi89.76 (5)
S3iv—Cs—S9vi79.11 (6)P—S3—Nb290.27 (5)
Csi—Cs—S2i44.2 (5)P—S3—Csix89.92 (6)
S10ii—Cs—S2i50.32 (4)Nb2—S3—Csix104.61 (6)
S10iii—Cs—S2i120.06 (6)P—S3—Csx99.22 (6)
S7iv—Cs—S2i99.18 (6)Nb2—S3—Csx103.24 (6)
S7v—Cs—S2i73.35 (5)S8—S4—Nb1viii66.22 (5)
S2—Cs—S2i173.07 (6)S8—S4—Nb266.22 (5)
S1v—Cs—S2i95.19 (7)Nb1viii—S4—Nb270.56 (3)
S5—Cs—S2i127.91 (8)S9—S5—Nb266.47 (5)
S3v—Cs—S2i48.73 (4)S9—S5—Nb165.71 (5)
S3iv—Cs—S2i122.41 (5)Nb2—S5—Nb192.55 (4)
S9vi—Cs—S2i124.54 (8)S9—S5—Cs146.11 (7)
S1—Ag—S1vii180.00 (10)Nb2—S5—Cs140.15 (6)
S4iii—Nb1—S7iii90.82 (4)Nb1—S5—Cs88.67 (5)
S4iii—Nb1—S8iii48.08 (4)P—S6—Nb189.39 (5)
S7iii—Nb1—S8iii109.54 (4)P—S6—Nb288.37 (5)
S4iii—Nb1—S10iii109.13 (4)Nb1—S6—Nb290.92 (4)
S7iii—Nb1—S10iii47.89 (4)S10—S7—Nb265.82 (5)
S8iii—Nb1—S10iii89.23 (4)S10—S7—Nb1viii66.76 (5)
S4iii—Nb1—S991.47 (4)Nb2—S7—Nb1viii70.64 (3)
S7iii—Nb1—S978.95 (4)S10—S7—Csx171.29 (7)
S8iii—Nb1—S9137.40 (4)Nb2—S7—Csx118.24 (6)
S10iii—Nb1—S9121.46 (4)Nb1viii—S7—Csx121.50 (5)
S4iii—Nb1—S2130.77 (4)S10—S7—Csix161.56 (7)
S7iii—Nb1—S2124.06 (4)Nb2—S7—Csix117.07 (6)
S8iii—Nb1—S285.24 (4)Nb1viii—S7—Csix131.67 (5)
S10iii—Nb1—S280.24 (4)S4—S8—Nb1viii65.70 (5)
S9—Nb1—S2125.60 (4)S4—S8—Nb265.76 (5)
S4iii—Nb1—S5138.34 (4)Nb1viii—S8—Nb270.25 (3)
S7iii—Nb1—S582.43 (4)S5—S9—Nb167.42 (5)
S8iii—Nb1—S5167.42 (4)S5—S9—Nb266.33 (5)
S10iii—Nb1—S596.47 (4)Nb1—S9—Nb293.27 (4)
S9—Nb1—S546.87 (4)S5—S9—Csxi111.56 (7)
S2—Nb1—S584.69 (4)Nb1—S9—Csxi104.00 (5)
S4iii—Nb1—S683.16 (4)Nb2—S9—Csxi160.34 (6)
S7iii—Nb1—S6155.62 (4)S7—S10—Nb265.93 (5)
S8iii—Nb1—S683.80 (4)S7—S10—Nb1viii65.35 (5)
S10iii—Nb1—S6155.76 (4)Nb2—S10—Nb1viii70.23 (3)
S9—Nb1—S677.61 (4)S7—S10—Csxii110.68 (8)
S2—Nb1—S676.07 (4)Nb2—S10—Csxii176.58 (7)
S5—Nb1—S686.46 (4)Nb1viii—S10—Csxii109.02 (5)
S4iii—Nb1—Nb2iii54.77 (3)S7—S10—Csviii108.80 (8)
S7iii—Nb1—Nb2iii54.64 (3)Nb2—S10—Csviii168.71 (5)
S8iii—Nb1—Nb2iii54.91 (3)Nb1viii—S10—Csviii98.55 (4)
S10iii—Nb1—Nb2iii54.37 (3)

Symmetry codes: (i) −x, −y, −z+1; (ii) x−1, −y+1/2, z+1/2; (iii) −x+1, y−1/2, −z+1/2; (iv) −x, y−1/2, −z+1/2; (v) x, −y+1/2, z+1/2; (vi) x−1, y, z; (vii) −x, −y, −z; (viii) −x+1, y+1/2, −z+1/2; (ix) x, −y+1/2, z−1/2; (x) −x, y+1/2, −z+1/2; (xi) x+1, y, z; (xii) x+1, −y+1/2, z−1/2.

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: WM2357).

References

  • Angenault, J., Cieren, X. & Quarton, M. (2000). J. Solid State Chem.153, 55–65.
  • Bang, H., Kim, Y., Kim, S. & Kim, S. (2008). J. Solid State Chem.181, 1978–1802.
  • Brec, R., Grenouilleau, P., Evain, M. & Rouxel, J. (1983). Rev. Chim. Mineral.20, 295–304.
  • Do, J. & Yun, H. (1996). Inorg. Chem.35, 3729–3730. [PubMed]
  • Do, J. & Yun, H. (2009). Acta Cryst. E65, i56–i57. [PMC free article] [PubMed]
  • Dong, Y., Kim, S. & Yun, H. (2005b). Acta Cryst. C61, i25–i26. [PubMed]
  • Dong, Y., Kim, S., Yun, H. & Lim, H. (2005a). Bull. Kor. Chem. Soc.26, 309–311.
  • Farrugia, L. J. (1999). J. Appl. Cryst.32, 837–838.
  • Higashi, T. (1995). ABSCOR Rigaku Corporation, Tokyo, Japan.
  • Johnson, C. K. (1965). ORTEP Report ORNL-3794. Oak Ridge National Laboratory, Tennessee, USA.
  • Kim, C.-K. & Yun, H.-S. (2002). Acta Cryst. C58, i53–i54. [PubMed]
  • Kwak, J., Kim, C., Yun, H. & Do, J. (2007). Bull. Kor. Chem. Soc.28, 701–704.
  • Kwak, J. & Yun, H. (2008). Bull. Kor. Chem. Soc.29, 273–275.
  • Lee, S., Colombet, P., Ouvrard, G. & Brec, R. (1988). Inorg. Chem.27, 1291–1294.
  • Rigaku (2006). RAPID-AUTO Rigaku Corporation, Tokyo, Japan.
  • Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. [PubMed]
  • Spek, A. L. (2009). Acta Cryst. D65, 148–155. [PMC free article] [PubMed]

Articles from Acta Crystallographica Section E: Structure Reports Online are provided here courtesy of International Union of Crystallography