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ISSN: 2056-9890
Volume 71| Part 3| March 2015| Pages 278-280

Crystal structure of the mixed-metal thio­phosphate Nb1.18V0.82PS10

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aDepartment of Energy Systems Research and Department of Chemistry, Ajou University, Suwon 443-749, Republic of Korea
*Correspondence e-mail: hsyun@ajou.ac.kr

Edited by T. J. Prior, University of Hull, England (Received 22 January 2015; accepted 13 February 2015; online 18 February 2015)

The mixed-metal thio­phosphate, Nb1.18V0.82PS10 (niobium vanadium phospho­rus deca­sulfide), has been prepared though solid state reactions using an alkali-metal halide flux. The title compound is isostructural with two-dimensional Nb2PS10. [M2S12] (M = Nb or V) dimers built up from two bicapped trigonal prisms and tetra­hedral [PS4] units share sulfur atoms to construct 1[M2PS10] chains along the a axis. These chains are linked through the di­sulfide bonds between [PS4] units in adjacent chains to form layers parallel to the ab plane. These layers then stack on top of each other to complete the three-dimensional structure with van der Waals gaps. The M sites are occupied by 59% of Nb and 41% of V and the average M—S and MM distances in the title compound are in between those of V2PS10 and Nb2PS10. The classical charge balance of the title compound can be represented by [(Nb/V)4+]2[P5+][S2−]3[S]7.

1. Chemical context

Ternary group 5 metal thio­phosphates, M2PS10 (M = V, Nb) have been reported to have low-dimensional structures with partially filled d orbitals which can accommodate electrons. Therefore, they are of potential importance as cathode materials for high-energy density lithium batteries (Rouxel, 1986[Rouxel, J. (1986). J. Solid State Chem. 64, 305-321.]). While both are composed of the same linear chains, i.e. 1[M2PS10], V2PS10 has a chain structure (Brec et al., 1983a[Brec, R., Ouvrard, G., Evain, M., Grenouilleau, P. & Rouxel, J. (1983a). J. Solid State Chem. 47, 174-184.]) and Nb2PS10 adopts a layered structure (Brec et al., 1983b[Brec, R., Grenouilleau, P., Evain, M. & Rouxel, J. (1983b). Rev. Chim. Miner. 20, 295-304.]). To understand the cause of different dimensionality between these phases, we have conducted research on the synthesis of the mixed phases, (Nb/V)2PS10. We report here the synthesis and structural characterization of a mixed-metallic thio­phosphate, namely Nb1.18V0.82PS10.

2. Structural commentary

The title compound, Nb-rich Nb1.18V0.82PS10, is isostructural with Nb2PS10 and detailed descriptions of this structural type have been given previously (Brec et al., 1983b[Brec, R., Grenouilleau, P., Evain, M. & Rouxel, J. (1983b). Rev. Chim. Miner. 20, 295-304.]). The usual [M2S12] (M = Nb, V) dimeric units (Yun et al., 2003[Yun, H., Ryu, G., Lee, S. & Hoffmann, R. (2003). Inorg. Chem. 42, 2253-2260.]) built up from two bicapped trigonal prisms and tetra­hedral [PS4] units (Yu & Yun, 2011[Yu, J. & Yun, H. (2011). Acta Cryst. E67, i24.]) share S atoms (Fig. 1[link]) to construct an 1[M2PS10] chain along the a axis. These chains are linked through the di­sulfide bonds between [PS4] units in adjacent chains to form layers parallel to the ab plane (Fig. 2[link]). These layers then stack on top of each other to complete the three-dimensional structure with van der Waals gaps shown in Fig. 3[link]. There is no bonding inter­action, only van der Waals forces, between the layers.

[Figure 1]
Figure 1
A view of the [M2S12] dimer unit (M = Nb or V) and its neighbouring tetra­hedral [PS4] group. Open circles are S atoms, filled circle are M atoms and gray circles are P atoms. Displacement ellipsoids are drawn at the 60% probability level.
[Figure 2]
Figure 2
View of the M2PS10 layers showing the two-dimensional nature of the compound. Atoms are as marked in Fig. 1[link].
[Figure 3]
Figure 3
The structure of Nb1.18V0.82PS10, viewed down the c axis.

The M sites occupied by statistically disordered Nb (59%) and V (41%) are surrounded by eight S atoms in a bicapped trigonal prismatic fashion and the average M—S bond length [2.51 (6) Å] in the title compound is between those of Nb2PS10 [2.54 (6) Å; Brec et al., 1983b[Brec, R., Grenouilleau, P., Evain, M. & Rouxel, J. (1983b). Rev. Chim. Miner. 20, 295-304.]] and V2PS10 [2.46 (7) Å; Brec et al., 1983a[Brec, R., Ouvrard, G., Evain, M., Grenouilleau, P. & Rouxel, J. (1983a). J. Solid State Chem. 47, 174-184.]]. The M atoms associate in pairs, with MM inter­actions alternating in the sequence of one short [2.855 (1) Å] and one long distance [3.728 (1) Å]. This MM distance, which is longer than that of V2PS10 [2.852 (2) Å] and shorter than that of Nb2PS10 [2.869 (1) Å], is indicative of a d1d1 interaction. The long distance implies that there is no significant bonding (Angenault et al., 2000[Angenault, J., Cieren, X. & Quarton, M. (2000). J. Solid State Chem. 153, 55-65.]), which is consistent with the highly resistive nature of the crystal since no inter­metallic bond can be set. The P—S distances in the tetra­hedral [PS4] unit are in good agreement with those found in other thio­phosphates (Brec et al., 1983b[Brec, R., Grenouilleau, P., Evain, M. & Rouxel, J. (1983b). Rev. Chim. Miner. 20, 295-304.]). There is no terminal S atom in this unit and this is responsible for the absence of the rather short P—S distances (< 2.0 Å) found in V2PS10 (Brec et al., 1983a[Brec, R., Ouvrard, G., Evain, M., Grenouilleau, P. & Rouxel, J. (1983a). J. Solid State Chem. 47, 174-184.]) and other related compounds, such as KNb2PS10 (Do & Yun, 1996[Do, J. & Yun, H. (1996). Inorg. Chem. 35, 3729-3730.]).

The classical charge balance of the title compound can be represented by [(Nb/V)4+]2[P5+][S2−]3[S]7. This study does not provide conclusive results on the different dimensionality between Nb2PS10 and V2PS10 and thus we believe that further studies to search for V-rich phases are necessary.

3. Synthesis and crystallization

The compound Nb1.18V0.82PS10 was prepared by the reaction of the elements Nb, V, P and S by the use of the reactive alkali metal halides. A combination of the pure elements, Nb powder (CERAC 99.8%), V powder (CERAC 99.5%), P powder (CERAC 99.95%) and S powder (Aldrich 99.999%) were mixed in a fused-silica tube in an Nb:V:P:S molar ratio of 1:1:1:10 with KCl. The mass ratio of the reactants and the halides flux was 2:1. The tube was evacuated to 0.133 Pa, sealed and heated gradually (100 K h−1) to 650 K, where it was kept for 12 h. The tube was cooled to 473 K at a rate of 4 K h−1 and then quenched to room temperature. The excess halides were removed with distilled water and black needle shaped crystals were obtained. The crystals are stable in air and water. A qualitative X-ray fluorescence analysis of selected crystals indicated the presence of Nb, V, S and P. The final composition of the title compound was determined by single-crystal X-ray diffraction.

4. Refinement

Crystal data, data collection and structure refinement details are summarized in Table 1[link]. The refinement of the model with occupational disorder on the M sites caused significant decrease of the R factor (wR2 = 0.103) in comparison with the case where full occupation by either metal had been considered (wR2 > 0.176). No evidence was found for ordering of this site and thus a statistically disordered structure is assumed. Also the displacement parameters in the disordered model became plausible. The disordered atoms were supposed to have the same displacement parameters. The Nb:V ratios on both M sites are almost the same, i.e. 59:41. The program STRUCTURE TIDY (Gelato & Parthé, 1987[Gelato, L. M. & Parthé, E. (1987). J. Appl. Cryst. 20, 139-143.]) was used to standardize the positional parameters. A difference Fourier synthesis calculated with phase based on the final parameters shows that the highest residual electron density (1.04 e Å−3) is 1.40 Å from the M1 site and the deepest hole (−1.06 e Å−3) is 0.79 Å from the M2 site.

Table 1
Experimental details

Crystal data
Chemical formula Nb1.18V0.82PS10
Mr 502.97
Crystal system, space group Orthorhombic, P21212
Temperature (K) 290
a, b, c (Å) 12.8472 (4), 13.6212 (4), 7.1972 (3)
V3) 1259.47 (8)
Z 4
Radiation type Mo Kα
μ (mm−1) 3.42
Crystal size (mm) 0.20 × 0.02 × 0.02
 
Data collection
Diffractometer Rigaku R-AXIS RAPID S
Absorption correction Multi-scan (ABSCOR; Higashi, 1995[Higashi, T. (1995). ABSCOR. Rigaku Corporation, Tokyo, Japan.])
Tmin, Tmax 0.503, 1.000
No. of measured, independent and observed [I > 2σ(I)] reflections 11897, 2757, 2053
Rint 0.081
(sin θ/λ)max−1) 0.639
 
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.045, 0.103, 1.13
No. of reflections 2757
No. of parameters 121
Δρmax, Δρmin (e Å−3) 1.04, −1.06
Absolute structure Flack (1983[Flack, H. D. (1983). Acta Cryst. A39, 876-881.])
Absolute structure parameter 0.64 (13)
Computer programs: RAPID-AUTO (Rigaku, 2006[Rigaku (2006). RAPID-AUTO. Rigaku Corporation, Tokyo, Japan.]), SHELXS2013 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]), SHELXL2013 (Sheldrick, 2015[Sheldrick, G. M. (2015). Acta Cryst. C71, 3-8.]), DIAMOND (Brandenburg, 1999[Brandenburg, K. (1999). DIAMOND. Crystal Impact GbR, Bonn, Germany.]) and WinGX (Farrugia, 2012[Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.]).

Supporting information


Chemical context top

Ternary group 5 metal thio­phosphates, M2PS10 (M = V, Nb) have been reported to have low-dimensional structures with partially filled d orbitals which can accommodate electrons. Therefore, they are of potential importance as cathode materials for high-energy density lithium batteries (Rouxel, 1986). While both are composed of the same linear chains, i.e. 1[M2PS10], V2PS10 has a one-dimensional chain structure (Brec et al., 1983a) and Nb2PS10 adopts a two-dimensional layered structure (Brec et al., 1983b). To understand the cause of different dimensionality between these phases, we have conducted research on the synthesis of the mixed phases, (Nb/V)2PS10. We report here the synthesis and structural characterization of a mixed-metallic thio­phosphate, namely Nb1.18V0.82PS10.

Structural commentary top

The title compound, Nb-rich Nb1.18V0.82PS10, is isostructural with Nb2PS10 and detailed descriptions of this structural type have been given previously (Brec et al., 1983b). The usual bicapped trigonal prismatic dimers [M2S12] (Yun et al., 2003) and tetra­hedral [PS4] units (Yu & Yun, 2011) share S atoms (Fig. 1) to build an 1[M2PS10] chain along the a axis. These chains are linked through the di­sulfide bonds between [PS4] units in adjacent chains to form layers parallel to the ab plane (Fig. 2). These layers then stack on top of each other to complete the three-dimensional structure with van der Waals gaps shown in Fig. 3. There is no bonding inter­action, only van der Waals forces, between the layers.

The M sites occupied by statistically disordered Nb (59%) and V (41%) are surrounded by eight S atoms in a bicapped trigonal prismatic fashion and the average M—S bond distance [2.513 (2) Å] in the title compound is between those of Nb2PS10 [2.54 (6) Å; Brec et al., 1983b] and V2PS10 [2.46 (7) Å; Brec et al., 1983a]. The M atoms associate in pairs, with M···M inter­actions alternating in the sequence of one short [2.855 (1) Å] and one long distance [3.728 (1) Å]. This MM bond distance, which is longer than that of V2PS10 [2.852 (2) Å] and shorter than that of Nb2PS10 [2.869 (1) Å], is indicative of the d1d1 inter­metallic bond. The long distance implies that there is no significant bonding inter­action (Angenault et al., 2000), which is consistent with the highly resistive nature of the crystal since no inter­metallic bond can be set. The P—S distances in the tetra­hedral [PS4] unit are in good agreement with those found in other thio­phosphates (Brec et al., 1983b). There is no terminal S atom in this unit and this is responsible for the absence of the rather short P—S distances (< 2.0 Å) found in V2PS10 (Brec et al., 1983a) and other related compounds, such as KNb2PS10 (Do & Yun, 1996).

The classical charge balance of the title compound can be represented by [(Nb/V)4+]2[P5+][S2-]3[S-]7. This study does not provide conclusive results on the different dimensionality between Nb2PS10 and V2PS10 and thus we believe that further studies to search for V-rich phases are necessary.

Synthesis and crystallization top

The compound Nb1.18V0.82PS10 was prepared by the reaction of the elemental Nb, V, P and S by the use of the reactive alkali metal halides. A combination of the pure elements, Nb powder (CERAC 99.8%), V powder (CERAC 99.5%), P powder (CERAC 99.95%) and S powder (Aldrich 99.999%) were mixed in a fused-silica tube in an Nb:V:P:S molar ratio of 1:1:1:10 with KCl. The mass ratio of the rea­cta­nts and the halides flux was 2:1. The tube was evacuated to 0.133 Pa, sealed and heated gradually (100 K h-1) to 650 K, where it was kept for 12 h. The tube was cooled to 473 K at a rate of 4 K h-1 and then quenched to room temperature. The excess halides were removed with distilled water and black needle shaped crystals were obtained. The crystals are stable in air and water. A qualitative X-ray fluorescence analysis of selected crystals indicated the presence of Nb, V, S and P. The final composition of the title compound was determined by single-crystal X-ray diffraction.

Refinement top

Crystal data, data collection and structure refinement details are summarized in Table 1. The refinement of the model with occupational disorder on the M sites caused significant decrease of the R factor (wR2 = 0.103) in comparison with the case where full occupation by either metal had been considered (wR2 > 0.176). No evidence was found for ordering of this site and thus a statistically disordered structure is assumed. Also the displacement parameters in the disordered model became plausible. The disordered atoms were supposed to have the same displacement parameters. The Nb:V ratios on both M sites are almost the same, i.e. 59:41. The program STRUCTURE TIDY (Gelato & Parthé, 1987) was used to standardize the positional parameters. A difference Fourier synthesis calculated with phase based on the final parameters shows that the highest residual electron density (1.04 e Å-3) is 1.40 Å from the M1 site and the deepest hole (-1.06 e Å-3) is 0.79 Å from the M2 site.

Related literature top

For the structure of V2PS10, see: Brec et al.(1983a). For the structure of Nb2PS10, see: Brec et al.(1983b). For the structure of [M2S12], see: Yun et al. (2003). For the structure of [PS4], see: Yu & Yun, (2011).

Computing details top

Data collection: RAPID-AUTO (Rigaku, 2006); cell refinement: RAPID-AUTO (Rigaku, 2006); data reduction: RAPID-AUTO (Rigaku, 2006); program(s) used to solve structure: SHELXS2013 (Sheldrick, 2008); program(s) used to refine structure: SHELXL2013 (Sheldrick, 2015); molecular graphics: DIAMOND (Brandenburg, 1999); software used to prepare material for publication: WinGX (Farrugia, 2012).

Figures top
[Figure 1] Fig. 1. A view of the bicapped trigonal biprismatic dimer [M2S12] unit (M = Nb or V) and its neighbouring tetrahedral [PS4] groups. Open circles are S atoms, filled circle are M atoms and gray circles are P atoms. Displacement ellipsoids are drawn at the 60% probability level.
[Figure 2] Fig. 2. View of the M2PS10 layers showing the two-dimensional nature of the compound. Atoms are as marked in Fig. 1.
[Figure 3] Fig. 3. The structure of Nb1.18V0.82PS10, viewed down the c axis.
Niobium vanadium phosphorus decasulfide top
Crystal data top
Nb1.18V0.82PS10F(000) = 969
Mr = 502.97Dx = 2.653 Mg m3
Orthorhombic, P21212Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2 2abCell parameters from 8753 reflections
a = 12.8472 (4) Åθ = 3.2–27.5°
b = 13.6212 (4) ŵ = 3.42 mm1
c = 7.1972 (3) ÅT = 290 K
V = 1259.47 (8) Å3Needle, black
Z = 40.2 × 0.02 × 0.02 mm
Data collection top
Rigaku R-AXIS RAPID S
diffractometer
2757 independent reflections
Radiation source: Sealed X-ray tube2053 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.081
ω scansθmax = 27.0°, θmin = 3.2°
Absorption correction: multi-scan
(ABSCOR; Higashi, 1995)
h = 1614
Tmin = 0.503, Tmax = 1.000k = 1717
11897 measured reflectionsl = 99
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.045 w = 1/[σ2(Fo2) + (0.0386P)2 + 1.1529P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.103(Δ/σ)max < 0.001
S = 1.13Δρmax = 1.04 e Å3
2757 reflectionsΔρmin = 1.06 e Å3
121 parametersAbsolute structure: Flack (1983)
0 restraintsAbsolute structure parameter: 0.64 (13)
Crystal data top
Nb1.18V0.82PS10V = 1259.47 (8) Å3
Mr = 502.97Z = 4
Orthorhombic, P21212Mo Kα radiation
a = 12.8472 (4) ŵ = 3.42 mm1
b = 13.6212 (4) ÅT = 290 K
c = 7.1972 (3) Å0.2 × 0.02 × 0.02 mm
Data collection top
Rigaku R-AXIS RAPID S
diffractometer
2757 independent reflections
Absorption correction: multi-scan
(ABSCOR; Higashi, 1995)
2053 reflections with I > 2σ(I)
Tmin = 0.503, Tmax = 1.000Rint = 0.081
11897 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0450 restraints
wR(F2) = 0.103Δρmax = 1.04 e Å3
S = 1.13Δρmin = 1.06 e Å3
2757 reflectionsAbsolute structure: Flack (1983)
121 parametersAbsolute structure parameter: 0.64 (13)
Special details top

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.

Refinement. Refined as a 2-component inversion twin.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Nb10.08230 (7)0.74603 (8)0.06349 (16)0.0193 (3)0.5889
V10.08230 (7)0.74603 (8)0.06349 (16)0.0193 (3)0.4111
Nb20.20780 (7)0.24841 (8)0.06671 (16)0.0183 (3)0.5856
V20.20780 (7)0.24841 (8)0.06671 (16)0.0183 (3)0.4144
S10.0601 (2)0.11893 (17)0.1005 (4)0.0233 (6)
S20.0647 (2)0.37577 (18)0.1107 (4)0.0258 (6)
S30.0727 (2)0.03201 (19)0.5538 (4)0.0285 (6)
S40.1930 (2)0.22558 (19)0.4241 (4)0.0284 (6)
S50.2221 (2)0.6344 (2)0.1672 (4)0.0277 (7)
S60.3292 (2)0.10963 (19)0.0949 (4)0.0284 (7)
S70.3483 (2)0.3569 (2)0.1743 (4)0.0292 (7)
S80.4267 (2)0.27029 (19)0.5806 (4)0.0284 (6)
S90.5644 (2)0.18846 (18)0.1448 (4)0.0275 (6)
S100.7986 (2)0.11500 (19)0.0879 (5)0.0275 (7)
P0.0585 (2)0.15464 (19)0.3772 (3)0.0236 (6)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Nb10.0164 (5)0.0218 (5)0.0197 (6)0.0011 (5)0.0007 (4)0.0009 (6)
V10.0164 (5)0.0218 (5)0.0197 (6)0.0011 (5)0.0007 (4)0.0009 (6)
Nb20.0145 (5)0.0214 (5)0.0192 (6)0.0012 (5)0.0009 (4)0.0013 (6)
V20.0145 (5)0.0214 (5)0.0192 (6)0.0012 (5)0.0009 (4)0.0013 (6)
S10.0206 (12)0.0257 (12)0.0238 (14)0.0001 (14)0.0004 (14)0.0006 (10)
S20.0200 (12)0.0271 (13)0.0303 (15)0.0006 (14)0.0024 (14)0.0042 (10)
S30.0256 (13)0.0319 (13)0.0281 (14)0.0039 (13)0.0051 (13)0.0078 (12)
S40.0221 (12)0.0388 (16)0.0242 (14)0.0074 (13)0.0013 (13)0.0023 (13)
S50.0234 (14)0.0301 (15)0.0296 (17)0.0041 (13)0.0029 (12)0.0047 (13)
S60.0231 (14)0.0288 (14)0.0333 (19)0.0023 (14)0.0017 (13)0.0054 (13)
S70.0267 (15)0.0326 (15)0.0283 (17)0.0050 (14)0.0009 (12)0.0067 (14)
S80.0233 (13)0.0386 (15)0.0233 (14)0.0064 (13)0.0030 (13)0.0026 (12)
S90.0248 (13)0.0334 (14)0.0243 (14)0.0014 (14)0.0004 (13)0.0023 (11)
S100.0236 (14)0.0258 (14)0.0332 (18)0.0002 (13)0.0011 (14)0.0069 (13)
P0.0223 (13)0.0283 (13)0.0202 (14)0.0001 (15)0.0013 (12)0.0036 (10)
Geometric parameters (Å, º) top
Nb1—S10i2.440 (3)Nb2—S5v2.461 (3)
Nb1—S7ii2.450 (3)Nb2—S10vi2.462 (3)
Nb1—S6ii2.458 (3)Nb2—S9vi2.540 (3)
Nb1—S52.469 (3)Nb2—S22.547 (3)
Nb1—S9ii2.533 (3)Nb2—S42.598 (3)
Nb1—S2iii2.537 (3)Nb2—S12.602 (3)
Nb1—S8iv2.585 (3)P—S12.050 (3)
Nb1—S1iii2.608 (3)P—S32.107 (3)
Nb1—Nb2ii2.8549 (13)P—S42.008 (4)
Nb2—S72.458 (3)P—S8vii2.002 (4)
Nb2—S62.459 (3)
S8vii—P—S4117.17 (16)S8vii—P—S3112.75 (17)
S8vii—P—S1106.08 (17)S4—P—S3101.85 (16)
S4—P—S1105.61 (17)S1—P—S3113.40 (15)
Symmetry codes: (i) x+1, y+1, z; (ii) x+1/2, y+1/2, z; (iii) x, y+1, z; (iv) x+1/2, y+1/2, z+1; (v) x+1/2, y1/2, z; (vi) x1/2, y+1/2, z; (vii) x1/2, y+1/2, z+1.

Experimental details

Crystal data
Chemical formulaNb1.18V0.82PS10
Mr502.97
Crystal system, space groupOrthorhombic, P21212
Temperature (K)290
a, b, c (Å)12.8472 (4), 13.6212 (4), 7.1972 (3)
V3)1259.47 (8)
Z4
Radiation typeMo Kα
µ (mm1)3.42
Crystal size (mm)0.2 × 0.02 × 0.02
Data collection
DiffractometerRigaku R-AXIS RAPID S
diffractometer
Absorption correctionMulti-scan
(ABSCOR; Higashi, 1995)
Tmin, Tmax0.503, 1.000
No. of measured, independent and
observed [I > 2σ(I)] reflections
11897, 2757, 2053
Rint0.081
(sin θ/λ)max1)0.639
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.045, 0.103, 1.13
No. of reflections2757
No. of parameters121
Δρmax, Δρmin (e Å3)1.04, 1.06
Absolute structureFlack (1983)
Absolute structure parameter0.64 (13)

Computer programs: RAPID-AUTO (Rigaku, 2006), SHELXS2013 (Sheldrick, 2008), SHELXL2013 (Sheldrick, 2015), DIAMOND (Brandenburg, 1999), WinGX (Farrugia, 2012).

 

Acknowledgements

This research was supported by the Basic Science Research Program through the National Research Foundation of Korea funded by the Ministry of Education, Science and Technology (grant No. 2011–0011309).

References

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Volume 71| Part 3| March 2015| Pages 278-280
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