research communications\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890
Volume 71| Part 7| July 2015| Pages 807-809

`Pd20Sn13' revisited: crystal structure of Pd6.69Sn4.31

CROSSMARK_Color_square_no_text.svg

aTechnische Universität München, Department of Chemistry, Lichtenbergstrasse 4, 85747 Garching, Germany
*Correspondence e-mail: thomas.faessler@lrz.tu-muenchen.de

Edited by M. Weil, Vienna University of Technology, Austria (Received 21 March 2015; accepted 10 June 2015; online 17 June 2015)

The crystal structure of the title compound was previously reported with composition `Pd20Sn13' [Sarah et al. (1981[Sarah, N., Alasafi, K. & Schubert, K. (1981). Z. Metallkd, 72, 517-520.]). Z. Metallkd, 72, 517–520]. For the original structure model, as determined from powder X-ray data, atomic coordinates from the isostructural compound Ni13Ga3Ge6 were transferred. The present structure determination, resulting in a composition Pd6.69Sn4.31, is based on single crystal X-ray data and includes anisotropic displacement parameters for all atoms as well as standard uncertainties for the atomic coordinates, leading to higher precision and accuracy for the structure model. Single crystals of the title compound were obtained via a solid-state reaction route, starting from the elements. The crystal structure can be derived from the AlB2 type of structure after removing one eighth of the atoms at the boron positions and shifting adjacent atoms in the same layer in the direction of the voids. One atomic site is partially occupied by both elements with a Pd:Sn ratio of 0.38 (3):0.62 (3). One Sn and three Pd atoms are located on special positions with site symmetry 2. (Wyckoff letter 3a and 3b).

1. Chemical context

In the context of investigations of the binary system Pd—Sn, Nowotny et al. (1946[Nowotny, H., Schubert, K. & Dettinger, U. (1946). Z. Metallkd, 37, 137.]) observed a phase with approximate composition Pd3Sn2, which was later addressed as `Pd20Sn13' (Sarah et al., 1981[Sarah, N., Alasafi, K. & Schubert, K. (1981). Z. Metallkd, 72, 517-520.]). According to powder XRD measurements, this compound was found to be isotypical to Ni13Ga3Ge6 (Nover & Schubert, 1981[Nover, G. & Schubert, K. (1981). Z. Metallkd, 72, 26-29.]). Up to now, no further detailed structure examination has been published. In the course of our experiments, aiming at ternary Zintl phases containing tetrel elements (Hlukhyy et al., 2012[Hlukhyy, V., He, H., Jantke, L. A. & Fässler, T. F. (2012). Chem. Eur. J. 18, 12000-120007.]), single crystals of the title compound have been obtained in significant amounts and were subjected to a closer structural investigation.

2. Structural commentary

The crystal structure of the title compound can be described as a defect variant of the AlB2 structure type, where 1/8 of the boron atoms are missing. The symmetry reduction from P6/mmm to P3221 with respect to AlB2 results in 13 different crystallographic positions for the Pd and Sn atoms instead of only two, and a more complicated stacking of atomic planes including six differently packed layers for each of the former two, as shown in Fig. 1[link]. The remaining atomic sites of the B atoms in AlB2 are now substituted by seven independent atoms (Pd6, Pd7, Pd8, Sn2, Sn3, Sn4, and Sn5), the `Al' layers are substituted alternatingly by Sn1, Pd3, Pd5, (layers `Al1', `Al3', `Al5' in Fig. 1[link]), and by Pd1, Pd2, and Pd4 (`Al2', `Al4', `Al6'), respectively.

[Figure 1]
Figure 1
The crystal structure of Pd6.69Sn4.31, emphasizing the relationship to the AlB2 structure type. The `Al n' layers represent planes which are occupied by Al atoms in AlB2, the `B n' layers those with B atoms, respectively. Anisotropic displacement ellipsoids are drawn at the 90% probability level.

The layered character of the Pd6.69Sn4.31 structure is much less pronounced than in the parent AlB2 type of structure, as indicated by the mixed substitution of both the Al and B sites of the AlB2 type by Pd as well as by Sn atoms, respectively. Accordingly, there are similar, in average slightly shorter inter­atomic distances within the planes (2.6407 (19) − 2.755 (2) Å) than between them [2.7259 (18)–3.309 (2) Å]. Nevertheless, the layers are clearly distinguishable and only marginally puckered. The distorted honeycomb lattice is obvious if the voids in the `B' layer are considered (Fig. 2[link]). The distortion results from a shift of the neighbouring Sn atoms within the boron layer (Sn2, Sn3 and Sn5) in the direction of the voids.

[Figure 2]
Figure 2
The `B1' layer (see Fig. 1[link]) in Pd6.69Sn4.31. To illustrate the relationship to the AlB2 structure type, the voids are drawn as empty squares and are connected to the neighbouring Sn atoms by dashed lines. Anisotropic displacement ellipsoids are drawn at the 90% probability level.

For Sn1 a partial occupation by Pd (Pd9) was found. A full occupation of the (Sn1/Pd9) site (Fig. 3[link]a) by the element Sn would result in the composition Pd13Sn9 as suggested by the isostructural compound Ni13Ga3Ge6. However, the occupancy of this position (in contrast to all other Pd and Sn sites) deviates significantly from 100% if only Sn (refined to 96%) or Pd (refined to 107%) is considered. It has to be noticed that this site is the only one in both kinds of `Al' layers that is not close to a void in the `B' layers (Fig. 3[link]). Consequently, the coordination number (CN) of the (Sn1/Pd9) site is 14, which is higher than that of all other Sn (CN = 10) and Pd atoms (CN = 11–13) in Pd6.69Sn4.31.

[Figure 3]
Figure 3
Sections of the crystal structure of Pd6.69Sn4.31, with a) layers `B1'–`Al1'–`B6' and b) layers `B2'–`Al2'–`B1'. The voids are drawn as empty squares and are connected to the neighbouring Sn atoms by dashed lines. Shown are the surroundings of the `B' layer atoms with zero (Sn1), one (Pd4) and two voids (Pd1, Pd2, Pd3, Pd5). Anisotropic displacement ellipsoids are drawn at the 90% probability level.

In the previous structure report of `Pd20Sn13' by Sarah et al. (1981[Sarah, N., Alasafi, K. & Schubert, K. (1981). Z. Metallkd, 72, 517-520.]), the atomic parameters were adopted from the isostructural compound Ni13Ga3Ge6, and the occupation of one atomic site was fixed for Sn:Pd as 2/3:1/3. The composition `Pd20Sn13' was obviously chosen in order to get the indices as integers, however, in consequence Z = 2. Our structure refinement suggests a more precise composition Pd20.06 (5)Sn12.94 (5). With a crystallographically more appropriate number of formula units, viz. Z = 6 (indicating the asymmetric unit), the composition then refined to Pd6.69 (2)Sn4.31 (2).

3. Synthesis and crystallization

Single crystals of the title compound were obtained from experiments aiming at a ternary alloy in the chemical system K—Pd—Sn, with similar conditions as reported by Hlukhyy et al. (2012[Hlukhyy, V., He, H., Jantke, L. A. & Fässler, T. F. (2012). Chem. Eur. J. 18, 12000-120007.]). 23.4 mg K (99.9%, Riedel de Haën), 71 mg Sn (99.999%, ChemPur), and 20.6 mg of PdSn, prefabricated by arc melting of the elements, were filled into a niobium crucible, which was sealed, placed in a silica glass tube, annealed under vacuum for 20 h at 1273 K and subsequently for 72 h at 873 K, and finally quenched with liquid nitro­gen. As a by-product, K4Sn4 (Hewaidy et al., 1964[Hewaidy, I. F., Busmann, E. & Klemm, W. (1964). Z. Anorg. Allg. Chem. 328, 283-293.]) was found.

4. Refinement

Crystal data, data collection and structure refinement details are summarized in Table 1[link]. In contrast to the previously reported structure model, which was described in P3121 (based on powder X-ray data; Sarah et al., 1981[Sarah, N., Alasafi, K. & Schubert, K. (1981). Z. Metallkd, 72, 517-520.]), the crystal under investigation adopts the inverted structure, as indicated by the refined Flack parameter (Flack, 1983[Flack, H. D. (1983). Acta Cryst. A39, 876-881.]; Parsons et al., 2013[Parsons, S., Flack, H. D. & Wagner, T. (2013). Acta Cryst. B69, 249-259.]). Therefore space group P3221 was chosen for the current refinement. It should be noted that the value and the corresponding standard uncertainty for the Flack parameter are rather high. However, the cause for this behaviour remains unclear. For the Sn1 site a partial occupation by Pd (Pd9) was found, with a refined occupation of 62 (3)% Sn and 38 (3)% Pd. All atoms were refined with anisotropic displacement parameters. The remaining maximum and minimum electron densities are located 2.08 Å from Sn2 and 0.46 Å from Pd8, respectively.

Table 1
Experimental details

Crystal data
Chemical formula Pd6.69Sn4.31
Mr 1223.37
Crystal system, space group Trigonal, P3221
Temperature (K) 150
a, c (Å) 8.77574 (17), 16.9004 (4)
V3) 1127.18 (5)
Z 6
Radiation type Mo Kα
μ (mm−1) 29.54
Crystal size (mm) 0.16 × 0.1 × 0.08
 
Data collection
Diffractometer Oxford Xcalibur 3
Absorption correction Multi-scan (CrysAlis RED; Oxford Diffraction, 2009[Oxford Diffraction (2009). CrysAlis CCD and CrysAlis RED. Agilent Technologies UK Ltd, Yarnton, Oxfordshire, England.])
Tmin, Tmax 0.408, 1.000
No. of measured, independent and observed [I > 2σ(I)] reflections 20534, 2682, 2001
Rint 0.041
(sin θ/λ)max−1) 0.762
 
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.028, 0.076, 1.08
No. of reflections 2682
No. of parameters 104
Δρmax, Δρmin (e Å−3) 2.66, −2.52
Absolute structure Flack x determined using 715 quotients [(I+) − (I)]/[(I+) + (I)] (Parsons et al., 2013[Parsons, S., Flack, H. D. & Wagner, T. (2013). Acta Cryst. B69, 249-259.])
Absolute structure parameter −0.2 (2)
Computer programs: CrysAlis CCD and CrysAlis RED (Oxford Diffraction, 2009[Oxford Diffraction (2009). CrysAlis CCD and CrysAlis RED. Agilent Technologies UK Ltd, Yarnton, Oxfordshire, England.]), SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]), SHELXL2014 (Sheldrick, 2015[Sheldrick, G. M. (2015). Acta Cryst. C71, 3-8.]) and DIAMOND (Brandenburg, 2012[Brandenburg, K. (2012). DIAMOND. Crystal Impact GbR, Bonn, Germany.]).

Supporting information


Chemical context top

In the context of investigations of the binary system Pd—Sn, Nowotny et al. (1946) observed a phase with approximate composition Pd3Sn2, which was later addressed as `Pd20Sn13' (Sarah et al., 1981). According to powder XRD measurements, this compound was found to be isotypical to Ni13Ga3Ge6 (Nover & Schubert, 1981). Up to now, no further detailed structure examination has been published. In the course of our experiments, aiming at ternary Zintl phases containing tetrel elements (Hlukhyy et al., 2012), single crystals of the title compound have been obtained in significant amounts and were subjected to a closer structural investigation.

Structural commentary top

The crystal structure of the title compound can be described as a defect variant of the AlB2 structure type, where 1/8 of the boron atoms are missing. The symmetry reduction from P6/mmm to P3221 with respect to AlB2 results in 13 different crystallographic positions for the Pd and Sn atoms instead of only two, and a more complicated stacking of atomic planes including six differently packed layers for each of the former two, as shown in Fig. 1. The remaining atomic sites of the B atoms in AlB2 are now substituted by seven independent atoms (Pd6, Pd7, Pd8, Sn2, Sn3, Sn4, and Sn5), the `Al' layers are substituted alternatingly by Sn1, Pd3, Pd5, (layers `Al1', `Al3', `Al5' in Fig. 1), and by Pd1, Pd2, and Pd4 (`Al2', `Al4', `Al6'), respectively.

The layered character of the Pd6.69Sn4.31 structure is much less pronounced than in the parent AlB2 type of structure, as indicated by the mixed substitution of both the Al and B sites of the AlB2 type by Pd as well as by Sn atoms, respectively. Accordingly, there are similar, in average slightly shorter inter­atomic distances within the planes (2.6407 (19) - 2.755 (2) Å) than between them [2.7259 (18)–3.309 (2) Å]. Nevertheless, the layers are clearly distinguishable and only marginally puckered. The distorted honeycomb lattice is obvious if the voids in the `B' layer are considered (Fig. 2). The distortion results from a shift of the neighbouring Sn atoms within the boron layer (Sn2, Sn3 and Sn5) in the direction of the voids.

For Sn1 a partial occupation by Pd (Pd9) was found. A full occupation of the (Sn1/Pd9) site (Fig. 3a) by the element Sn would result in the composition Pd13Sn9 as suggested by the isostructural compound Ni13Ga3Ge6. However, the occupancy of this position (in contrast to all other Pd and Sn sites) deviates significantly from 100% if only Sn (refined to 96 %) or Pd (refined to `107 %') is considered. It has to be noticed that this site is the only one in both kinds of `Al' layers that is not close to a void in the `B' layers (Fig. 3). Consequently, the coordination number (CN) of the (Sn1/Pd9) site is 14, which is higher than that of all other Sn (CN = 10) and Pd atoms (CN = 11–13) in Pd6.69Sn4.31.

In the previous structure report of `Pd20Sn13' by Sarah et al. (1981), the atomic parameters were adopted from the isostructural compound Ni13Ga3Ge6, and the occupation of one atomic site was fixed for Sn:Pd as 2/3:1/3. The composition `Pd20Sn13' was obviously chosen in order to get the indices as integers, however, in consequence Z = 2. Our structure refinement suggests a more precise composition Pd20.06 (5)Sn12.94 (5). With a crystallographically more appropriate number of formula units, viz. Z = 6 (indicating the asymmetric unit), the composition then refined to Pd6.69 (2)Sn4.31 (2).

Synthesis and crystallization top

Single crystals of the title compound were obtained from experiments aiming at a ternary alloy in the chemical system K—Pd—Sn, with similar conditions as reported by Hlukhyy et al. (2012). 23.4 mg K (99.9%, Riedel de Haën), 71 mg Sn (99.999%, ChemPur), and 20.6 mg of PdSn, prefabricated by arc melting of the elements, were filled into a niobium crucible, which was sealed, placed in a silica glass tube, annealed under vacuum for 20 h at 1273 K and subsequently for 72 h at 873 K, and finally quenched with liquid nitro­gen. As a by-product, K4Sn4 (Hewaidy et al., 1964) was found.

Refinement top

Crystal data, data collection and structure refinement details are summarized in Table 1. In contrast to the previously reported structure model, which was described in P3121 (based on powder X-ray data; Sarah et al., 1981), the crystal under investigation adopts the inverted structure, as indicated by the refined Flack parameter (Flack, 1983; Parsons et al., 2013). Therefore space group P3221 was chosen for the current refinement. It should be noted that the value and the corresponding standard uncertainty for the Flack parameter are rather high. However, the cause for this behaviour remains unclear. For the Sn1 site a partial occupation by Pd (Pd9) was found, with a refined occupation of 62 (3)% Sn and 38 (3)% Pd. All atoms were refined with anisotropic displacement parameters. The remaining maximum and minimum electron densities are located 2.08 Å from Sn2 and 0.46 Å from Pd8, respectively.

Computing details top

Data collection: CrysAlis CCD (Oxford Diffraction, 2009); cell refinement: CrysAlis RED (Oxford Diffraction, 2009); data reduction: CrysAlis RED (Oxford Diffraction, 2009); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL2014 (Sheldrick, 2015); molecular graphics: DIAMOND (Brandenburg, 2012); software used to prepare material for publication: SHELXL2014 (Sheldrick, 2015).

Figures top
[Figure 1] Fig. 1. The crystal structure of Pd6.69Sn4.31, emphasizing the relationship to the AlB2 structure type. The `Al n' layers represent planes which are occupied by Al atoms in AlB2, the `B n' layers those with B atoms, respectively. Anisotropic displacement ellipsoids are drawn at the 90% probability level.
[Figure 2] Fig. 2. The `B1' layer (see Fig. 1) in Pd6.69Sn4.31. To illustrate the relationship to the AlB2 structure type, the voids are drawn as empty squares and are connected to the neighbouring Sn atoms by dashed lines. Anisotropic displacement ellipsoids are drawn at the 90% probability level.
[Figure 3] Fig. 3. Sections of the crystal structure of Pd6.69Sn4.31, with a) layers `B1'–`Al1'–`B6' and b) layers `B2'–`Al2'–`B1'. The voids are drawn as empty squares and are connected to the neighbouring Sn atoms by dashed lines. Shown are the surroundings of the `B' layer atoms with zero (Sn1), one (Pd4) and two voids (Pd1, Pd2, Pd3, Pd5). Anisotropic displacement ellipsoids are drawn at the 90% probability level.
Heptapalladium tetratin top
Crystal data top
Pd6.69Sn4.31Dx = 10.813 Mg m3
Mr = 1223.37Mo Kα radiation, λ = 0.71073 Å
Trigonal, P3221Cell parameters from 8247 reflections
a = 8.77574 (17) Åθ = 2.9–32.7°
c = 16.9004 (4) ŵ = 29.54 mm1
V = 1127.18 (5) Å3T = 150 K
Z = 6Fragment, black
F(000) = 31390.16 × 0.1 × 0.08 mm
Data collection top
Oxford Xcalibur 3
diffractometer
2682 independent reflections
Radiation source: Enhance (Mo) X-ray Source2001 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.041
Detector resolution: 16.0238 pixels mm-1θmax = 32.8°, θmin = 2.9°
ω and π scansh = 138
Absorption correction: multi-scan
(CrysAlis RED; Oxford Diffraction, 2009)
k = 1212
Tmin = 0.408, Tmax = 1.000l = 2525
20534 measured reflections
Refinement top
Refinement on F2 w = 1/[σ2(Fo2) + (0.0364P)2 + 1.004P]
where P = (Fo2 + 2Fc2)/3
Least-squares matrix: full(Δ/σ)max < 0.001
R[F2 > 2σ(F2)] = 0.028Δρmax = 2.66 e Å3
wR(F2) = 0.076Δρmin = 2.52 e Å3
S = 1.08Extinction correction: SHELXL2014 (Sheldrick, 2015), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
2682 reflectionsExtinction coefficient: 0.00066 (4)
104 parametersAbsolute structure: Flack x determined using 715 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons et al., 2013)
0 restraintsAbsolute structure parameter: 0.2 (2)
Crystal data top
Pd6.69Sn4.31Z = 6
Mr = 1223.37Mo Kα radiation
Trigonal, P3221µ = 29.54 mm1
a = 8.77574 (17) ÅT = 150 K
c = 16.9004 (4) Å0.16 × 0.1 × 0.08 mm
V = 1127.18 (5) Å3
Data collection top
Oxford Xcalibur 3
diffractometer
2682 independent reflections
Absorption correction: multi-scan
(CrysAlis RED; Oxford Diffraction, 2009)
2001 reflections with I > 2σ(I)
Tmin = 0.408, Tmax = 1.000Rint = 0.041
20534 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0280 restraints
wR(F2) = 0.076Δρmax = 2.66 e Å3
S = 1.08Δρmin = 2.52 e Å3
2682 reflectionsAbsolute structure: Flack x determined using 715 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons et al., 2013)
104 parametersAbsolute structure parameter: 0.2 (2)
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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Pd10.0002 (5)0.00000.16670.0083 (2)
Pd20.4990 (2)0.00000.16670.00772 (19)
Pd30.0010 (5)0.0010 (5)0.00000.0100 (2)
Pd40.5041 (2)0.5072 (3)0.16345 (4)0.01021 (19)
Pd50.4963 (2)0.0035 (5)0.00092 (4)0.00921 (17)
Pd60.6556 (3)0.3385 (3)0.07906 (6)0.0124 (2)
Pd70.6590 (3)0.82039 (16)0.07559 (5)0.00882 (17)
Pd80.18110 (16)0.3394 (3)0.08142 (5)0.00947 (16)
Pd90.4997 (2)0.4997 (2)0.00000.0071 (3)0.37 (4)
Sn10.4997 (2)0.4997 (2)0.00000.0071 (3)0.63 (4)
Sn20.3048 (2)0.11037 (11)0.08285 (5)0.00898 (19)
Sn30.3030 (3)0.6900 (3)0.08831 (5)0.0083 (2)
Sn40.83212 (15)0.16829 (14)0.08857 (4)0.00861 (14)
Sn50.88531 (10)0.6896 (2)0.08862 (5)0.0084 (2)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pd10.0096 (8)0.0087 (14)0.0063 (5)0.0044 (7)0.0006 (5)0.0012 (11)
Pd20.0096 (7)0.0076 (14)0.0052 (4)0.0038 (7)0.0002 (5)0.0003 (10)
Pd30.0104 (7)0.0104 (7)0.0062 (5)0.0028 (13)0.0005 (6)0.0005 (6)
Pd40.0100 (8)0.0122 (6)0.0072 (3)0.0046 (8)0.0002 (6)0.0011 (4)
Pd50.0143 (8)0.0093 (7)0.0060 (3)0.0074 (5)0.0004 (5)0.0002 (6)
Pd60.0116 (8)0.0116 (8)0.0137 (4)0.0056 (5)0.0001 (6)0.0005 (6)
Pd70.0087 (7)0.0089 (5)0.0096 (3)0.0049 (6)0.0004 (6)0.0007 (4)
Pd80.0091 (5)0.0101 (7)0.0099 (3)0.0053 (6)0.0008 (4)0.0005 (6)
Pd90.0070 (6)0.0070 (6)0.0060 (4)0.0026 (11)0.0003 (5)0.0003 (5)
Sn10.0070 (6)0.0070 (6)0.0060 (4)0.0026 (11)0.0003 (5)0.0003 (5)
Sn20.0081 (7)0.0138 (4)0.0076 (3)0.0074 (7)0.0014 (5)0.0019 (3)
Sn30.0080 (7)0.0069 (7)0.0070 (4)0.0015 (3)0.0001 (5)0.0004 (5)
Sn40.0079 (4)0.0072 (4)0.0081 (3)0.0018 (4)0.0002 (3)0.0001 (3)
Sn50.0123 (4)0.0089 (7)0.0065 (3)0.0070 (7)0.0009 (2)0.0008 (5)
Geometric parameters (Å, º) top
Pd1—Sn5i2.7259 (18)Pd5—Pd8ix2.933 (3)
Pd1—Sn5ii2.7259 (18)Pd5—Sn42.967 (2)
Pd1—Sn2iii2.741 (4)Pd6—Sn42.6407 (19)
Pd1—Sn22.741 (4)Pd6—Sn22.707 (2)
Pd1—Pd32.8168 (1)Pd6—Sn52.715 (2)
Pd1—Pd3iv2.8168 (1)Pd6—Pd92.7553 (13)
Pd1—Sn4v2.875 (3)Pd6—Sn3viii2.8242 (13)
Pd1—Sn4vi2.875 (3)Pd6—Sn3ix2.8782 (13)
Pd1—Pd82.9563 (18)Pd6—Pd5xv2.910 (4)
Pd1—Pd8iii2.9563 (18)Pd6—Pd4viii3.017 (4)
Pd1—Pd7ii3.015 (4)Pd7—Sn4xvi2.6532 (16)
Pd1—Pd7i3.015 (4)Pd7—Sn32.746 (3)
Pd2—Sn3vii2.7264 (19)Pd7—Pd92.7515 (19)
Pd2—Sn3viii2.7264 (19)Pd7—Sn52.755 (2)
Pd2—Sn2iii2.738 (2)Pd7—Sn5ix2.8188 (11)
Pd2—Sn22.738 (2)Pd7—Sn4ii2.8603 (9)
Pd2—Pd52.8325 (7)Pd7—Pd5xvi2.882 (3)
Pd2—Pd5iii2.8325 (7)Pd7—Pd3xvii2.884 (4)
Pd2—Sn4iii2.8554 (19)Pd7—Pd2xvi3.006 (2)
Pd2—Sn42.8554 (19)Pd7—Pd1xvii3.014 (4)
Pd2—Pd62.9705 (19)Pd8—Sn4vi2.6552 (18)
Pd2—Pd6iii2.9705 (19)Pd8—Sn32.708 (3)
Pd2—Pd7vii3.006 (2)Pd8—Sn22.720 (2)
Pd2—Pd7viii3.006 (2)Pd8—Sn5ii2.7802 (11)
Pd3—Sn22.738 (3)Pd8—Pd92.7853 (18)
Pd3—Sn2ix2.738 (3)Pd8—Sn2ix2.8279 (11)
Pd3—Sn5x2.811 (3)Pd8—Pd5ix2.933 (3)
Pd3—Sn5i2.811 (3)Pd8—Pd4ii2.973 (2)
Pd3—Pd1xi2.8167 (1)Pd9—Pd7ix2.7515 (19)
Pd3—Pd7x2.884 (4)Pd9—Pd6ix2.7553 (13)
Pd3—Pd7i2.884 (4)Pd9—Pd4ix2.7630 (7)
Pd3—Pd8ix2.932 (4)Pd9—Pd8ix2.7853 (18)
Pd3—Pd82.932 (4)Pd9—Sn23.2738 (16)
Pd3—Sn4vi2.9611 (11)Pd9—Sn2ix3.2738 (16)
Pd3—Sn4xii2.9611 (11)Sn2—Pd8ix2.8279 (11)
Pd4—Sn3viii2.732 (4)Sn2—Sn2iii3.2924 (15)
Pd4—Sn5ii2.742 (2)Sn3—Pd2xvi2.7263 (19)
Pd4—Pd92.7629 (7)Sn3—Pd4ii2.732 (4)
Pd4—Pd72.805 (3)Sn3—Pd5ix2.781 (4)
Pd4—Pd82.820 (2)Sn3—Pd5xvi2.797 (4)
Pd4—Pd62.821 (3)Sn3—Pd6ii2.8242 (13)
Pd4—Sn4ii2.823 (2)Sn3—Pd6ix2.8783 (13)
Pd4—Pd5xiii2.8558 (9)Sn4—Pd7vii2.6531 (16)
Pd4—Pd8viii2.973 (2)Sn4—Pd8xviii2.6552 (18)
Pd4—Pd6ii3.017 (4)Sn4—Pd4viii2.823 (2)
Pd4—Sn53.1621 (19)Sn4—Pd7viii2.8604 (9)
Pd5—Sn22.740 (3)Sn4—Pd1xviii2.875 (3)
Pd5—Sn5xii2.772 (3)Sn4—Pd5xv2.900 (2)
Pd5—Sn3ix2.781 (4)Sn4—Pd3xviii2.9611 (11)
Pd5—Sn3vii2.797 (4)Sn5—Pd1xvii2.7258 (18)
Pd5—Pd4xiv2.8557 (9)Sn5—Pd4viii2.742 (2)
Pd5—Pd7vii2.882 (3)Sn5—Pd5xv2.772 (3)
Pd5—Sn4xii2.900 (2)Sn5—Pd8viii2.7803 (11)
Pd5—Pd6xii2.910 (4)Sn5—Pd3xvii2.811 (3)
Pd5—Pd62.932 (4)Sn5—Pd7ix2.8188 (11)
Sn5i—Pd1—Sn5ii164.96 (17)Sn2—Pd6—Pd5xv151.78 (6)
Sn5i—Pd1—Sn2iii83.14 (7)Sn5—Pd6—Pd5xv58.92 (6)
Sn5ii—Pd1—Sn2iii84.84 (8)Pd9—Pd6—Pd5xv101.06 (7)
Sn5i—Pd1—Sn284.84 (8)Pd4—Pd6—Pd5xv128.45 (10)
Sn5ii—Pd1—Sn283.14 (7)Sn3viii—Pd6—Pd5xv123.49 (7)
Sn2iii—Pd1—Sn273.82 (12)Sn3ix—Pd6—Pd5xv57.78 (6)
Sn5i—Pd1—Pd360.92 (7)Sn4—Pd6—Pd564.09 (5)
Sn5ii—Pd1—Pd3119.10 (9)Sn2—Pd6—Pd557.98 (6)
Sn2iii—Pd1—Pd3121.12 (13)Sn5—Pd6—Pd5153.21 (6)
Sn2—Pd1—Pd359.00 (9)Pd9—Pd6—Pd5101.37 (7)
Sn5i—Pd1—Pd3iv119.10 (9)Pd4—Pd6—Pd5131.43 (10)
Sn5ii—Pd1—Pd3iv60.91 (7)Sn3viii—Pd6—Pd5113.13 (8)
Sn2iii—Pd1—Pd3iv59.00 (9)Sn3ix—Pd6—Pd557.19 (6)
Sn2—Pd1—Pd3iv121.11 (13)Pd5xv—Pd6—Pd597.37 (4)
Pd3—Pd1—Pd3iv179.9 (2)Sn4—Pd6—Pd260.84 (6)
Sn5i—Pd1—Sn4v86.43 (6)Sn2—Pd6—Pd257.45 (7)
Sn5ii—Pd1—Sn4v105.28 (8)Sn5—Pd6—Pd2144.58 (5)
Sn2iii—Pd1—Sn4v103.97 (3)Pd9—Pd6—Pd2130.92 (9)
Sn2—Pd1—Sn4v171.20 (4)Pd4—Pd6—Pd299.73 (7)
Pd3—Pd1—Sn4v117.20 (15)Sn3viii—Pd6—Pd256.06 (5)
Pd3iv—Pd1—Sn4v62.69 (4)Sn3ix—Pd6—Pd2113.74 (8)
Sn5i—Pd1—Sn4vi105.27 (8)Pd5xv—Pd6—Pd2123.60 (8)
Sn5ii—Pd1—Sn4vi86.43 (6)Pd5—Pd6—Pd257.35 (5)
Sn2iii—Pd1—Sn4vi171.20 (4)Sn4—Pd6—Pd4viii59.42 (5)
Sn2—Pd1—Sn4vi103.97 (3)Sn2—Pd6—Pd4viii145.74 (7)
Pd3—Pd1—Sn4vi62.69 (4)Sn5—Pd6—Pd4viii56.86 (6)
Pd3iv—Pd1—Sn4vi117.20 (15)Pd9—Pd6—Pd4viii130.73 (10)
Sn4v—Pd1—Sn4vi79.49 (11)Pd4—Pd6—Pd4viii97.46 (5)
Sn5i—Pd1—Pd8120.98 (4)Sn3viii—Pd6—Pd4viii65.93 (5)
Sn5ii—Pd1—Pd858.42 (3)Sn3ix—Pd6—Pd4viii114.46 (8)
Sn2iii—Pd1—Pd8119.43 (12)Pd5xv—Pd6—Pd4viii57.57 (6)
Sn2—Pd1—Pd856.89 (5)Pd5—Pd6—Pd4viii123.51 (7)
Pd3—Pd1—Pd860.99 (8)Pd2—Pd6—Pd4viii93.11 (6)
Pd3iv—Pd1—Pd8119.01 (8)Sn4xvi—Pd7—Sn3110.53 (8)
Sn4v—Pd1—Pd8129.67 (13)Sn4xvi—Pd7—Pd9157.08 (4)
Sn4vi—Pd1—Pd854.16 (4)Sn3—Pd7—Pd973.74 (5)
Sn5i—Pd1—Pd8iii58.42 (3)Sn4xvi—Pd7—Sn5110.81 (8)
Sn5ii—Pd1—Pd8iii120.98 (4)Sn3—Pd7—Sn5136.65 (6)
Sn2iii—Pd1—Pd8iii56.89 (5)Pd9—Pd7—Sn573.41 (4)
Sn2—Pd1—Pd8iii119.43 (12)Sn4xvi—Pd7—Pd4143.30 (5)
Pd3—Pd1—Pd8iii119.01 (8)Sn3—Pd7—Pd469.96 (7)
Pd3iv—Pd1—Pd8iii60.99 (8)Pd9—Pd7—Pd459.62 (4)
Sn4v—Pd1—Pd8iii54.15 (4)Sn5—Pd7—Pd469.31 (7)
Sn4vi—Pd1—Pd8iii129.67 (13)Sn4xvi—Pd7—Sn5ix84.66 (4)
Pd8—Pd1—Pd8iii176.07 (17)Sn3—Pd7—Sn5ix97.76 (7)
Sn5i—Pd1—Pd7ii137.27 (13)Pd9—Pd7—Sn5ix72.42 (3)
Sn5ii—Pd1—Pd7ii57.09 (5)Sn5—Pd7—Sn5ix98.45 (7)
Sn2iii—Pd1—Pd7ii117.33 (4)Pd4—Pd7—Sn5ix132.04 (6)
Sn2—Pd1—Pd7ii135.21 (3)Sn4xvi—Pd7—Sn4ii83.53 (4)
Pd3—Pd1—Pd7ii120.73 (11)Sn3—Pd7—Sn4ii86.01 (5)
Pd3iv—Pd1—Pd7ii59.16 (10)Pd9—Pd7—Sn4ii119.39 (5)
Sn4v—Pd1—Pd7ii53.49 (7)Sn5—Pd7—Sn4ii86.17 (5)
Sn4vi—Pd1—Pd7ii58.06 (7)Pd4—Pd7—Sn4ii59.77 (4)
Pd8—Pd1—Pd7ii83.04 (6)Sn5ix—Pd7—Sn4ii168.19 (6)
Pd8iii—Pd1—Pd7ii99.87 (7)Sn4xvi—Pd7—Pd5xvi64.68 (7)
Sn5i—Pd1—Pd7i57.09 (5)Sn3—Pd7—Pd5xvi59.54 (7)
Sn5ii—Pd1—Pd7i137.27 (13)Pd9—Pd7—Pd5xvi101.87 (7)
Sn2iii—Pd1—Pd7i135.21 (3)Sn5—Pd7—Pd5xvi155.91 (5)
Sn2—Pd1—Pd7i117.33 (4)Pd4—Pd7—Pd5xvi129.46 (10)
Pd3—Pd1—Pd7i59.16 (10)Sn5ix—Pd7—Pd5xvi58.18 (5)
Pd3iv—Pd1—Pd7i120.73 (11)Sn4ii—Pd7—Pd5xvi115.64 (7)
Sn4v—Pd1—Pd7i58.06 (7)Sn4xvi—Pd7—Pd3xvii64.50 (7)
Sn4vi—Pd1—Pd7i53.49 (7)Sn3—Pd7—Pd3xvii156.01 (5)
Pd8—Pd1—Pd7i99.87 (7)Pd9—Pd7—Pd3xvii102.03 (6)
Pd8iii—Pd1—Pd7i83.04 (6)Sn5—Pd7—Pd3xvii59.74 (6)
Pd7ii—Pd1—Pd7i86.07 (12)Pd4—Pd7—Pd3xvii129.03 (9)
Sn3vii—Pd2—Sn3viii164.85 (10)Sn5ix—Pd7—Pd3xvii59.05 (6)
Sn3vii—Pd2—Sn2iii83.18 (5)Sn4ii—Pd7—Pd3xvii115.50 (7)
Sn3viii—Pd2—Sn2iii84.72 (4)Pd5xvi—Pd7—Pd3xvii99.51 (4)
Sn3vii—Pd2—Sn284.73 (4)Sn4xvi—Pd7—Pd2xvi60.21 (4)
Sn3viii—Pd2—Sn283.18 (5)Sn3—Pd7—Pd2xvi56.36 (6)
Sn2iii—Pd2—Sn273.91 (8)Pd9—Pd7—Pd2xvi129.97 (8)
Sn3vii—Pd2—Pd560.38 (8)Sn5—Pd7—Pd2xvi143.17 (5)
Sn3viii—Pd2—Pd5119.57 (8)Pd4—Pd7—Pd2xvi96.79 (7)
Sn2iii—Pd2—Pd5120.80 (8)Sn5ix—Pd7—Pd2xvi114.87 (7)
Sn2—Pd2—Pd558.89 (6)Sn4ii—Pd7—Pd2xvi58.19 (4)
Sn3vii—Pd2—Pd5iii119.57 (8)Pd5xvi—Pd7—Pd2xvi57.46 (4)
Sn3viii—Pd2—Pd5iii60.38 (8)Pd3xvii—Pd7—Pd2xvi124.71 (7)
Sn2iii—Pd2—Pd5iii58.89 (6)Sn4xvi—Pd7—Pd1xvii60.56 (5)
Sn2—Pd2—Pd5iii120.80 (8)Sn3—Pd7—Pd1xvii143.39 (6)
Pd5—Pd2—Pd5iii179.68 (12)Pd9—Pd7—Pd1xvii129.46 (8)
Sn3vii—Pd2—Sn4iii86.47 (4)Sn5—Pd7—Pd1xvii56.17 (7)
Sn3viii—Pd2—Sn4iii105.28 (5)Pd4—Pd7—Pd1xvii96.32 (5)
Sn2iii—Pd2—Sn4iii103.61 (3)Sn5ix—Pd7—Pd1xvii115.31 (8)
Sn2—Pd2—Sn4iii171.07 (3)Sn4ii—Pd7—Pd1xvii58.52 (5)
Pd5—Pd2—Sn4iii117.39 (9)Pd5xvi—Pd7—Pd1xvii125.23 (7)
Pd5iii—Pd2—Sn4iii62.89 (5)Pd3xvii—Pd7—Pd1xvii57.00 (6)
Sn3vii—Pd2—Sn4105.27 (5)Pd2xvi—Pd7—Pd1xvii93.78 (5)
Sn3viii—Pd2—Sn486.47 (4)Sn4vi—Pd8—Sn3109.23 (8)
Sn2iii—Pd2—Sn4171.07 (3)Sn4vi—Pd8—Sn2110.81 (8)
Sn2—Pd2—Sn4103.61 (3)Sn3—Pd8—Sn2139.66 (6)
Pd5—Pd2—Sn462.89 (5)Sn4vi—Pd8—Sn5ii89.76 (5)
Pd5iii—Pd2—Sn4117.39 (9)Sn3—Pd8—Sn5ii92.94 (6)
Sn4iii—Pd2—Sn480.13 (7)Sn2—Pd8—Sn5ii82.52 (5)
Sn3vii—Pd2—Pd6120.09 (4)Sn4vi—Pd8—Pd9152.99 (4)
Sn3viii—Pd2—Pd659.25 (4)Sn3—Pd8—Pd973.79 (5)
Sn2iii—Pd2—Pd6119.55 (7)Sn2—Pd8—Pd972.96 (4)
Sn2—Pd2—Pd656.43 (4)Sn5ii—Pd8—Pd9117.14 (6)
Pd5—Pd2—Pd660.64 (8)Sn4vi—Pd8—Pd4147.89 (4)
Pd5iii—Pd2—Pd6119.35 (8)Sn3—Pd8—Pd470.28 (8)
Sn4iii—Pd2—Pd6130.31 (7)Sn2—Pd8—Pd473.34 (8)
Sn4—Pd2—Pd653.86 (4)Sn5ii—Pd8—Pd458.64 (5)
Sn3vii—Pd2—Pd6iii59.25 (4)Pd9—Pd8—Pd459.07 (4)
Sn3viii—Pd2—Pd6iii120.09 (4)Sn4vi—Pd8—Sn2ix81.65 (4)
Sn2iii—Pd2—Pd6iii56.43 (4)Sn3—Pd8—Sn2ix96.03 (8)
Sn2—Pd2—Pd6iii119.56 (7)Sn2—Pd8—Sn2ix94.39 (7)
Pd5—Pd2—Pd6iii119.34 (8)Sn5ii—Pd8—Sn2ix169.22 (8)
Pd5iii—Pd2—Pd6iii60.64 (8)Pd9—Pd8—Sn2ix71.35 (3)
Sn4iii—Pd2—Pd6iii53.86 (4)Pd4—Pd8—Sn2ix130.40 (5)
Sn4—Pd2—Pd6iii130.31 (7)Sn4vi—Pd8—Pd363.78 (6)
Pd6—Pd2—Pd6iii175.71 (10)Sn3—Pd8—Pd3151.91 (5)
Sn3vii—Pd2—Pd7vii56.98 (4)Sn2—Pd8—Pd357.79 (6)
Sn3viii—Pd2—Pd7vii137.49 (8)Sn5ii—Pd8—Pd3113.52 (8)
Sn2iii—Pd2—Pd7vii135.11 (4)Pd9—Pd8—Pd3100.42 (6)
Sn2—Pd2—Pd7vii117.19 (3)Pd4—Pd8—Pd3131.02 (11)
Pd5—Pd2—Pd7vii59.06 (6)Sn2ix—Pd8—Pd356.72 (6)
Pd5iii—Pd2—Pd7vii121.22 (7)Sn4vi—Pd8—Pd5ix62.28 (7)
Sn4iii—Pd2—Pd7vii58.34 (4)Sn3—Pd8—Pd5ix58.92 (7)
Sn4—Pd2—Pd7vii53.75 (5)Sn2—Pd8—Pd5ix150.35 (5)
Pd6—Pd2—Pd7vii99.52 (4)Sn5ii—Pd8—Pd5ix124.40 (6)
Pd6iii—Pd2—Pd7vii83.64 (5)Pd9—Pd8—Pd5ix100.63 (7)
Sn3vii—Pd2—Pd7viii137.49 (8)Pd4—Pd8—Pd5ix129.05 (12)
Sn3viii—Pd2—Pd7viii56.98 (4)Sn2ix—Pd8—Pd5ix56.76 (5)
Sn2iii—Pd2—Pd7viii117.19 (3)Pd3—Pd8—Pd5ix96.48 (4)
Sn2—Pd2—Pd7viii135.11 (4)Sn4vi—Pd8—Pd161.35 (9)
Pd5—Pd2—Pd7viii121.22 (7)Sn3—Pd8—Pd1146.27 (5)
Pd5iii—Pd2—Pd7viii59.06 (6)Sn2—Pd8—Pd157.57 (9)
Sn4iii—Pd2—Pd7viii53.75 (5)Sn5ii—Pd8—Pd156.64 (4)
Sn4—Pd2—Pd7viii58.35 (4)Pd9—Pd8—Pd1130.41 (10)
Pd6—Pd2—Pd7viii83.64 (5)Pd4—Pd8—Pd1100.40 (5)
Pd6iii—Pd2—Pd7viii99.52 (4)Sn2ix—Pd8—Pd1113.05 (7)
Pd7vii—Pd2—Pd7viii86.36 (9)Pd3—Pd8—Pd157.15 (5)
Sn2—Pd3—Sn2ix96.07 (14)Pd5ix—Pd8—Pd1123.62 (12)
Sn2—Pd3—Sn5x178.55 (7)Sn4vi—Pd8—Pd4ii59.90 (7)
Sn2ix—Pd3—Sn5x83.31 (2)Sn3—Pd8—Pd4ii57.26 (8)
Sn2—Pd3—Sn5i83.31 (2)Sn2—Pd8—Pd4ii146.97 (6)
Sn2ix—Pd3—Sn5i178.55 (7)Sn5ii—Pd8—Pd4ii66.59 (3)
Sn5x—Pd3—Sn5i97.34 (13)Pd9—Pd8—Pd4ii130.97 (10)
Sn2—Pd3—Pd1xi120.62 (10)Pd4—Pd8—Pd4ii98.54 (4)
Sn2ix—Pd3—Pd1xi59.12 (10)Sn2ix—Pd8—Pd4ii113.73 (7)
Sn5x—Pd3—Pd1xi57.95 (4)Pd3—Pd8—Pd4ii123.68 (10)
Sn5i—Pd3—Pd1xi122.31 (15)Pd5ix—Pd8—Pd4ii57.83 (5)
Sn2—Pd3—Pd159.12 (10)Pd1—Pd8—Pd4ii94.05 (4)
Sn2ix—Pd3—Pd1120.62 (10)Pd7—Pd9—Pd7ix80.14 (9)
Sn5x—Pd3—Pd1122.32 (15)Pd7—Pd9—Pd6ix80.90 (7)
Sn5i—Pd3—Pd157.95 (4)Pd7ix—Pd9—Pd6ix99.86 (4)
Pd1xi—Pd3—Pd1179.7 (2)Pd7—Pd9—Pd699.87 (4)
Sn2—Pd3—Pd7x121.64 (4)Pd7ix—Pd9—Pd680.90 (7)
Sn2ix—Pd3—Pd7x122.05 (4)Pd6ix—Pd9—Pd6179.02 (12)
Sn5x—Pd3—Pd7x57.85 (8)Pd7—Pd9—Pd461.16 (6)
Sn5i—Pd3—Pd7x59.33 (8)Pd7ix—Pd9—Pd4116.98 (7)
Pd1xi—Pd3—Pd7x63.84 (10)Pd6ix—Pd9—Pd4118.52 (8)
Pd1—Pd3—Pd7x116.45 (11)Pd6—Pd9—Pd461.50 (8)
Sn2—Pd3—Pd7i122.05 (4)Pd7—Pd9—Pd4ix116.98 (7)
Sn2ix—Pd3—Pd7i121.64 (4)Pd7ix—Pd9—Pd4ix61.16 (6)
Sn5x—Pd3—Pd7i59.33 (8)Pd6ix—Pd9—Pd4ix61.50 (8)
Sn5i—Pd3—Pd7i57.85 (8)Pd6—Pd9—Pd4ix118.52 (8)
Pd1xi—Pd3—Pd7i116.45 (11)Pd4—Pd9—Pd4ix177.85 (12)
Pd1—Pd3—Pd7i63.84 (10)Pd7—Pd9—Pd8ix178.02 (4)
Pd7x—Pd3—Pd7i75.79 (12)Pd7ix—Pd9—Pd8ix98.94 (3)
Sn2—Pd3—Pd8ix59.72 (8)Pd6ix—Pd9—Pd8ix97.57 (4)
Sn2ix—Pd3—Pd8ix57.22 (8)Pd6—Pd9—Pd8ix81.68 (7)
Sn5x—Pd3—Pd8ix118.91 (4)Pd4—Pd9—Pd8ix120.78 (8)
Sn5i—Pd3—Pd8ix123.33 (4)Pd4ix—Pd9—Pd8ix61.08 (5)
Pd1xi—Pd3—Pd8ix61.85 (5)Pd7—Pd9—Pd898.94 (3)
Pd1—Pd3—Pd8ix117.85 (15)Pd7ix—Pd9—Pd8178.02 (4)
Pd7x—Pd3—Pd8ix103.57 (3)Pd6ix—Pd9—Pd881.69 (7)
Pd7i—Pd3—Pd8ix178.21 (6)Pd6—Pd9—Pd897.57 (4)
Sn2—Pd3—Pd857.22 (8)Pd4—Pd9—Pd861.08 (5)
Sn2ix—Pd3—Pd859.72 (8)Pd4ix—Pd9—Pd8120.78 (8)
Sn5x—Pd3—Pd8123.32 (4)Pd8ix—Pd9—Pd882.03 (9)
Sn5i—Pd3—Pd8118.91 (4)Pd7—Pd9—Sn2127.01 (2)
Pd1xi—Pd3—Pd8117.85 (15)Pd7ix—Pd9—Sn2126.63 (6)
Pd1—Pd3—Pd861.85 (5)Pd6ix—Pd9—Sn2126.54 (8)
Pd7x—Pd3—Pd8178.21 (6)Pd6—Pd9—Sn252.49 (6)
Pd7i—Pd3—Pd8103.57 (3)Pd4—Pd9—Sn265.85 (6)
Pd8ix—Pd3—Pd877.12 (11)Pd4ix—Pd9—Sn2116.00 (6)
Sn2—Pd3—Sn4vi101.81 (8)Pd8ix—Pd9—Sn254.93 (4)
Sn2ix—Pd3—Sn4vi77.90 (6)Pd8—Pd9—Sn252.61 (5)
Sn5x—Pd3—Sn4vi79.35 (6)Pd7—Pd9—Sn2ix126.63 (6)
Sn5i—Pd3—Sn4vi100.92 (7)Pd7ix—Pd9—Sn2ix127.01 (2)
Pd1xi—Pd3—Sn4vi120.39 (7)Pd6ix—Pd9—Sn2ix52.49 (6)
Pd1—Pd3—Sn4vi59.61 (7)Pd6—Pd9—Sn2ix126.54 (8)
Pd7x—Pd3—Sn4vi126.43 (14)Pd4—Pd9—Sn2ix116.00 (6)
Pd7i—Pd3—Sn4vi53.97 (4)Pd4ix—Pd9—Sn2ix65.85 (6)
Pd8ix—Pd3—Sn4vi126.04 (13)Pd8ix—Pd9—Sn2ix52.61 (5)
Pd8—Pd3—Sn4vi53.55 (4)Pd8—Pd9—Sn2ix54.93 (4)
Sn2—Pd3—Sn4xii77.90 (6)Sn2—Pd9—Sn2ix76.90 (7)
Sn2ix—Pd3—Sn4xii101.81 (8)Pd6—Sn2—Pd8100.35 (4)
Sn5x—Pd3—Sn4xii100.92 (7)Pd6—Sn2—Pd3143.25 (7)
Sn5i—Pd3—Sn4xii79.35 (6)Pd8—Sn2—Pd364.99 (7)
Pd1xi—Pd3—Sn4xii59.61 (7)Pd6—Sn2—Pd266.12 (6)
Pd1—Pd3—Sn4xii120.39 (7)Pd8—Sn2—Pd2144.55 (4)
Pd7x—Pd3—Sn4xii53.97 (4)Pd3—Sn2—Pd2144.15 (7)
Pd7i—Pd3—Sn4xii126.43 (14)Pd6—Sn2—Pd565.14 (8)
Pd8ix—Pd3—Sn4xii53.56 (4)Pd8—Sn2—Pd5144.00 (6)
Pd8—Pd3—Sn4xii126.04 (13)Pd3—Sn2—Pd5106.02 (4)
Sn4vi—Pd3—Sn4xii179.59 (18)Pd2—Sn2—Pd562.27 (5)
Sn3viii—Pd4—Sn5ii84.03 (6)Pd6—Sn2—Pd1145.28 (4)
Sn3viii—Pd4—Pd9119.64 (12)Pd8—Sn2—Pd165.54 (7)
Sn5ii—Pd4—Pd9119.22 (7)Pd3—Sn2—Pd161.87 (6)
Sn3viii—Pd4—Pd7137.40 (9)Pd2—Sn2—Pd1106.14 (5)
Sn5ii—Pd4—Pd7136.41 (14)Pd5—Sn2—Pd1143.76 (8)
Pd9—Pd4—Pd759.22 (5)Pd6—Sn2—Pd8ix81.77 (6)
Sn3viii—Pd4—Pd8119.74 (10)Pd8—Sn2—Pd8ix82.40 (5)
Sn5ii—Pd4—Pd859.96 (5)Pd3—Sn2—Pd8ix63.56 (7)
Pd9—Pd4—Pd859.85 (5)Pd2—Sn2—Pd8ix124.61 (8)
Pd7—Pd4—Pd896.87 (7)Pd5—Sn2—Pd8ix63.55 (6)
Sn3viii—Pd4—Pd661.11 (8)Pd1—Sn2—Pd8ix124.30 (10)
Sn5ii—Pd4—Pd6119.88 (11)Pd6—Sn2—Pd953.86 (4)
Pd9—Pd4—Pd659.12 (4)Pd8—Sn2—Pd954.43 (3)
Pd7—Pd4—Pd697.00 (5)Pd3—Sn2—Pd993.51 (6)
Pd8—Pd4—Pd695.27 (6)Pd2—Sn2—Pd9119.84 (6)
Sn3viii—Pd4—Sn4ii103.82 (5)Pd5—Sn2—Pd993.67 (7)
Sn5ii—Pd4—Sn4ii103.15 (8)Pd1—Sn2—Pd9119.88 (7)
Pd9—Pd4—Sn4ii120.30 (9)Pd8ix—Sn2—Pd953.72 (3)
Pd7—Pd4—Sn4ii61.08 (6)Pd6—Sn2—Sn2iii110.29 (4)
Pd8—Pd4—Sn4ii128.95 (14)Pd8—Sn2—Sn2iii109.49 (3)
Pd6—Pd4—Sn4ii130.44 (9)Pd3—Sn2—Sn2iii106.41 (6)
Sn3viii—Pd4—Pd5xiii59.65 (9)Pd2—Sn2—Sn2iii53.05 (4)
Sn5ii—Pd4—Pd5xiii59.32 (6)Pd5—Sn2—Sn2iii106.48 (6)
Pd9—Pd4—Pd5xiii178.23 (11)Pd1—Sn2—Sn2iii53.09 (6)
Pd7—Pd4—Pd5xiii122.48 (10)Pd8ix—Sn2—Sn2iii160.33 (5)
Pd8—Pd4—Pd5xiii118.85 (9)Pd9—Sn2—Sn2iii145.95 (4)
Pd6—Pd4—Pd5xiii120.40 (14)Pd8—Sn3—Pd2xvi148.03 (5)
Sn4ii—Pd4—Pd5xiii61.40 (6)Pd8—Sn3—Pd4ii66.25 (7)
Sn3viii—Pd4—Pd8viii56.49 (6)Pd2xvi—Sn3—Pd4ii108.48 (6)
Sn5ii—Pd4—Pd8viii118.66 (5)Pd8—Sn3—Pd7101.00 (4)
Pd9—Pd4—Pd8viii120.82 (8)Pd2xvi—Sn3—Pd766.65 (7)
Pd7—Pd4—Pd8viii86.42 (5)Pd4ii—Sn3—Pd7148.98 (6)
Pd8—Pd4—Pd8viii176.19 (13)Pd8—Sn3—Pd5ix64.58 (6)
Pd6—Pd4—Pd8viii82.38 (9)Pd2xvi—Sn3—Pd5ix143.39 (7)
Sn4ii—Pd4—Pd8viii54.45 (5)Pd4ii—Sn3—Pd5ix62.39 (7)
Pd5xiii—Pd4—Pd8viii60.38 (7)Pd7—Sn3—Pd5ix139.85 (6)
Sn3viii—Pd4—Pd6ii117.94 (5)Pd8—Sn3—Pd5xvi140.76 (6)
Sn5ii—Pd4—Pd6ii56.01 (6)Pd2xvi—Sn3—Pd5xvi61.69 (6)
Pd9—Pd4—Pd6ii121.00 (11)Pd4ii—Sn3—Pd5xvi144.37 (7)
Pd7—Pd4—Pd6ii86.30 (10)Pd7—Sn3—Pd5xvi62.65 (6)
Pd8—Pd4—Pd6ii81.61 (8)Pd5ix—Sn3—Pd5xvi103.75 (3)
Pd6—Pd4—Pd6ii175.73 (7)Pd8—Sn3—Pd6ii87.24 (6)
Sn4ii—Pd4—Pd6ii53.63 (7)Pd2xvi—Sn3—Pd6ii64.69 (5)
Pd5xiii—Pd4—Pd6ii59.33 (9)Pd4ii—Sn3—Pd6ii61.01 (6)
Pd8viii—Pd4—Pd6ii100.58 (5)Pd7—Sn3—Pd6ii91.36 (5)
Sn3viii—Pd4—Sn584.60 (8)Pd5ix—Sn3—Pd6ii123.02 (9)
Sn5ii—Pd4—Sn5168.62 (12)Pd5xvi—Sn3—Pd6ii126.05 (9)
Pd9—Pd4—Sn567.09 (5)Pd8—Sn3—Pd6ix80.82 (6)
Pd7—Pd4—Sn554.59 (5)Pd2xvi—Sn3—Pd6ix122.33 (9)
Pd8—Pd4—Sn5126.91 (3)Pd4ii—Sn3—Pd6ix123.59 (10)
Pd6—Pd4—Sn553.61 (7)Pd7—Sn3—Pd6ix78.84 (6)
Sn4ii—Pd4—Sn579.51 (5)Pd5ix—Sn3—Pd6ix62.38 (7)
Pd5xiii—Pd4—Sn5114.16 (9)Pd5xvi—Sn3—Pd6ix61.68 (7)
Pd8viii—Pd4—Sn553.79 (4)Pd6ii—Sn3—Pd6ix162.73 (5)
Pd6ii—Pd4—Sn5130.65 (9)Pd8—Sn3—Pd456.50 (5)
Sn2—Pd5—Sn5xii178.71 (10)Pd2xvi—Sn3—Pd494.42 (7)
Sn2—Pd5—Sn3ix96.39 (11)Pd4ii—Sn3—Pd495.55 (4)
Sn5xii—Pd5—Sn3ix82.57 (4)Pd7—Sn3—Pd455.90 (4)
Sn2—Pd5—Sn3vii83.37 (4)Pd5ix—Sn3—Pd4120.95 (7)
Sn5xii—Pd5—Sn3vii97.68 (11)Pd5xvi—Sn3—Pd4118.51 (7)
Sn3ix—Pd5—Sn3vii179.44 (10)Pd6ii—Sn3—Pd459.95 (5)
Sn2—Pd5—Pd258.84 (6)Pd6ix—Sn3—Pd4102.87 (5)
Sn5xii—Pd5—Pd2122.37 (9)Pd6—Sn4—Pd7vii119.05 (5)
Sn3ix—Pd5—Pd2121.51 (11)Pd6—Sn4—Pd8xviii120.96 (5)
Sn3vii—Pd5—Pd257.93 (4)Pd7vii—Sn4—Pd8xviii118.82 (5)
Sn2—Pd5—Pd4xiv120.49 (9)Pd6—Sn4—Pd4viii66.95 (7)
Sn5xii—Pd5—Pd4xiv58.30 (5)Pd7vii—Sn4—Pd4viii155.61 (4)
Sn3ix—Pd5—Pd4xiv57.96 (9)Pd8xviii—Sn4—Pd4viii65.64 (8)
Sn3vii—Pd5—Pd4xiv122.59 (15)Pd6—Sn4—Pd265.30 (6)
Pd2—Pd5—Pd4xiv179.22 (17)Pd7vii—Sn4—Pd266.04 (5)
Sn2—Pd5—Pd7vii121.49 (5)Pd8xviii—Sn4—Pd2155.06 (4)
Sn5xii—Pd5—Pd7vii59.78 (6)Pd4viii—Sn4—Pd299.92 (6)
Sn3ix—Pd5—Pd7vii121.99 (7)Pd6—Sn4—Pd7viii92.76 (6)
Sn3vii—Pd5—Pd7vii57.81 (7)Pd7vii—Sn4—Pd7viii96.47 (4)
Pd2—Pd5—Pd7vii63.48 (6)Pd8xviii—Sn4—Pd7viii91.64 (5)
Pd4xiv—Pd5—Pd7vii117.25 (10)Pd4viii—Sn4—Pd7viii59.15 (4)
Sn2—Pd5—Sn4xii78.94 (6)Pd2—Sn4—Pd7viii63.47 (5)
Sn5xii—Pd5—Sn4xii100.48 (7)Pd6—Sn4—Pd1xviii156.15 (5)
Sn3ix—Pd5—Sn4xii100.64 (6)Pd7vii—Sn4—Pd1xviii65.95 (6)
Sn3vii—Pd5—Sn4xii79.82 (8)Pd8xviii—Sn4—Pd1xviii64.49 (7)
Pd2—Pd5—Sn4xii121.13 (7)Pd4viii—Sn4—Pd1xviii99.16 (4)
Pd4xiv—Pd5—Sn4xii58.75 (6)Pd2—Sn4—Pd1xviii100.19 (5)
Pd7vii—Pd5—Sn4xii126.67 (13)Pd7viii—Sn4—Pd1xviii63.42 (6)
Sn2—Pd5—Pd6xii123.11 (9)Pd6—Sn4—Pd5xv63.17 (8)
Sn5xii—Pd5—Pd6xii57.03 (7)Pd7vii—Sn4—Pd5xv144.54 (4)
Sn3ix—Pd5—Pd6xii119.99 (5)Pd8xviii—Sn4—Pd5xv63.56 (8)
Sn3vii—Pd5—Pd6xii60.54 (8)Pd4viii—Sn4—Pd5xv59.85 (4)
Pd2—Pd5—Pd6xii117.52 (11)Pd2—Sn4—Pd5xv128.46 (9)
Pd4xiv—Pd5—Pd6xii63.11 (9)Pd7viii—Sn4—Pd5xv119.00 (5)
Pd7vii—Pd5—Pd6xii76.17 (9)Pd1xviii—Sn4—Pd5xv128.04 (10)
Sn4xii—Pd5—Pd6xii54.07 (6)Pd6—Sn4—Pd3xviii146.14 (3)
Sn2—Pd5—Pd656.88 (7)Pd7vii—Sn4—Pd3xviii61.52 (9)
Sn5xii—Pd5—Pd6122.99 (9)Pd8xviii—Sn4—Pd3xviii62.67 (9)
Sn3ix—Pd5—Pd660.43 (8)Pd4viii—Sn4—Pd3xviii128.30 (12)
Sn3vii—Pd5—Pd6119.04 (5)Pd2—Sn4—Pd3xviii127.55 (9)
Pd2—Pd5—Pd662.01 (5)Pd7viii—Sn4—Pd3xviii121.10 (6)
Pd4xiv—Pd5—Pd6117.36 (14)Pd1xviii—Sn4—Pd3xviii57.70 (4)
Pd7vii—Pd5—Pd6103.40 (5)Pd5xv—Sn4—Pd3xviii96.58 (4)
Sn4xii—Pd5—Pd6126.25 (10)Pd6—Sn4—Pd562.73 (8)
Pd6xii—Pd5—Pd6179.50 (7)Pd7vii—Sn4—Pd561.39 (8)
Sn2—Pd5—Pd8ix59.68 (6)Pd8xviii—Sn4—Pd5146.72 (4)
Sn5xii—Pd5—Pd8ix119.04 (5)Pd4viii—Sn4—Pd5129.67 (10)
Sn3ix—Pd5—Pd8ix56.50 (7)Pd2—Sn4—Pd558.18 (3)
Sn3vii—Pd5—Pd8ix123.70 (7)Pd7viii—Sn4—Pd5121.64 (6)
Pd2—Pd5—Pd8ix117.48 (10)Pd1xviii—Sn4—Pd5127.34 (9)
Pd4xiv—Pd5—Pd8ix61.79 (6)Pd5xv—Sn4—Pd596.82 (3)
Pd7vii—Pd5—Pd8ix178.43 (9)Pd3xviii—Sn4—Pd595.86 (4)
Sn4xii—Pd5—Pd8ix54.16 (5)Pd6—Sn5—Pd1xvii148.90 (6)
Pd6xii—Pd5—Pd8ix104.12 (5)Pd6—Sn5—Pd4viii67.13 (9)
Pd6—Pd5—Pd8ix76.31 (9)Pd1xvii—Sn5—Pd4viii108.52 (4)
Sn2—Pd5—Sn4100.70 (8)Pd6—Sn5—Pd7100.78 (4)
Sn5xii—Pd5—Sn479.87 (5)Pd1xvii—Sn5—Pd766.73 (10)
Sn3ix—Pd5—Sn478.91 (8)Pd4viii—Sn5—Pd7149.46 (6)
Sn3vii—Pd5—Sn4100.63 (6)Pd6—Sn5—Pd5xv64.05 (8)
Pd2—Pd5—Sn458.94 (5)Pd1xvii—Sn5—Pd5xv143.48 (12)
Pd4xiv—Pd5—Sn4121.17 (9)Pd4viii—Sn5—Pd5xv62.38 (5)
Pd7vii—Pd5—Sn453.93 (4)Pd7—Sn5—Pd5xv139.46 (6)
Sn4xii—Pd5—Sn4179.39 (14)Pd6—Sn5—Pd8viii87.99 (6)
Pd6xii—Pd5—Sn4126.50 (10)Pd1xvii—Sn5—Pd8viii64.94 (5)
Pd6—Pd5—Sn453.18 (6)Pd4viii—Sn5—Pd8viii61.40 (4)
Pd8ix—Pd5—Sn4125.24 (13)Pd7—Sn5—Pd8viii91.30 (5)
Sn4—Pd6—Sn2110.61 (9)Pd5xv—Sn5—Pd8viii123.30 (7)
Sn4—Pd6—Sn5109.00 (8)Pd6—Sn5—Pd3xvii140.17 (7)
Sn2—Pd6—Sn5139.69 (6)Pd1xvii—Sn5—Pd3xvii61.14 (6)
Sn4—Pd6—Pd9154.46 (4)Pd4viii—Sn5—Pd3xvii144.02 (11)
Sn2—Pd6—Pd973.65 (6)Pd7—Sn5—Pd3xvii62.41 (6)
Sn5—Pd6—Pd973.96 (6)Pd5xv—Sn5—Pd3xvii104.05 (4)
Sn4—Pd6—Pd4146.07 (6)Pd8viii—Sn5—Pd3xvii125.70 (8)
Sn2—Pd6—Pd473.51 (6)Pd6—Sn5—Pd7ix80.39 (6)
Sn5—Pd6—Pd469.63 (6)Pd1xvii—Sn5—Pd7ix121.86 (8)
Pd9—Pd6—Pd459.38 (5)Pd4viii—Sn5—Pd7ix123.48 (8)
Sn4—Pd6—Sn3viii88.76 (5)Pd7—Sn5—Pd7ix78.91 (5)
Sn2—Pd6—Sn3viii81.94 (5)Pd5xv—Sn5—Pd7ix62.05 (6)
Sn5—Pd6—Sn3viii91.82 (6)Pd8viii—Sn5—Pd7ix163.04 (5)
Pd9—Pd6—Sn3viii116.71 (6)Pd3xvii—Sn5—Pd7ix61.63 (7)
Pd4—Pd6—Sn3viii57.88 (6)Pd6—Sn5—Pd456.77 (6)
Sn4—Pd6—Sn3ix82.84 (4)Pd1xvii—Sn5—Pd494.62 (5)
Sn2—Pd6—Sn3ix94.90 (8)Pd4viii—Sn5—Pd495.82 (4)
Sn5—Pd6—Sn3ix97.05 (8)Pd7—Sn5—Pd456.10 (7)
Pd9—Pd6—Sn3ix71.64 (3)Pd5xv—Sn5—Pd4120.73 (11)
Pd4—Pd6—Sn3ix131.01 (6)Pd8viii—Sn5—Pd459.62 (4)
Sn3viii—Pd6—Sn3ix169.38 (7)Pd3xvii—Sn5—Pd4118.48 (10)
Sn4—Pd6—Pd5xv62.76 (5)Pd7ix—Sn5—Pd4103.49 (4)
Symmetry codes: (i) x1, y1, z; (ii) xy, y+1, z+1/3; (iii) xy, y, z+1/3; (iv) x+y, x, z+1/3; (v) xy1, y, z+1/3; (vi) x1, y, z; (vii) x, y1, z; (viii) xy+1, y+1, z+1/3; (ix) y, x, z; (x) y1, x1, z; (xi) y, xy, z1/3; (xii) y, x1, z; (xiii) x+y+1, x+1, z+1/3; (xiv) y+1, xy, z1/3; (xv) y+1, x, z; (xvi) x, y+1, z; (xvii) x+1, y+1, z; (xviii) x+1, y, z.

Experimental details

Crystal data
Chemical formulaPd6.69Sn4.31
Mr1223.37
Crystal system, space groupTrigonal, P3221
Temperature (K)150
a, c (Å)8.77574 (17), 16.9004 (4)
V3)1127.18 (5)
Z6
Radiation typeMo Kα
µ (mm1)29.54
Crystal size (mm)0.16 × 0.1 × 0.08
Data collection
DiffractometerOxford Xcalibur 3
diffractometer
Absorption correctionMulti-scan
(CrysAlis RED; Oxford Diffraction, 2009)
Tmin, Tmax0.408, 1.000
No. of measured, independent and
observed [I > 2σ(I)] reflections
20534, 2682, 2001
Rint0.041
(sin θ/λ)max1)0.762
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.028, 0.076, 1.08
No. of reflections2682
No. of parameters104
Δρmax, Δρmin (e Å3)2.66, 2.52
Absolute structureFlack x determined using 715 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons et al., 2013)
Absolute structure parameter0.2 (2)

Computer programs: CrysAlis CCD (Oxford Diffraction, 2009), CrysAlis RED (Oxford Diffraction, 2009), SHELXS97 (Sheldrick, 2008), SHELXL2014 (Sheldrick, 2015), DIAMOND (Brandenburg, 2012).

 

Acknowledgements

This work was supported by the German Research Foundation (DFG) and the Technische Universität München within the funding programme Open Access Publishing.

References

First citationBrandenburg, K. (2012). DIAMOND. Crystal Impact GbR, Bonn, Germany.  Google Scholar
First citationFlack, H. D. (1983). Acta Cryst. A39, 876–881.  CrossRef CAS Web of Science IUCr Journals Google Scholar
First citationHewaidy, I. F., Busmann, E. & Klemm, W. (1964). Z. Anorg. Allg. Chem. 328, 283–293.  CrossRef CAS Google Scholar
First citationHlukhyy, V., He, H., Jantke, L. A. & Fässler, T. F. (2012). Chem. Eur. J. 18, 12000–120007.  CrossRef CAS PubMed Google Scholar
First citationNover, G. & Schubert, K. (1981). Z. Metallkd, 72, 26–29.  CAS Google Scholar
First citationNowotny, H., Schubert, K. & Dettinger, U. (1946). Z. Metallkd, 37, 137.  Google Scholar
First citationOxford Diffraction (2009). CrysAlis CCD and CrysAlis RED. Agilent Technologies UK Ltd, Yarnton, Oxfordshire, England.  Google Scholar
First citationParsons, S., Flack, H. D. & Wagner, T. (2013). Acta Cryst. B69, 249–259.  Web of Science CrossRef CAS IUCr Journals Google Scholar
First citationSarah, N., Alasafi, K. & Schubert, K. (1981). Z. Metallkd, 72, 517–520.  CAS Google Scholar
First citationSheldrick, G. M. (2008). Acta Cryst. A64, 112–122.  Web of Science CrossRef CAS IUCr Journals Google Scholar
First citationSheldrick, G. M. (2015). Acta Cryst. C71, 3–8.  Web of Science CrossRef IUCr Journals Google Scholar

This is an open-access article distributed under the terms of the Creative Commons Attribution (CC-BY) Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890
Volume 71| Part 7| July 2015| Pages 807-809
Follow Acta Cryst. E
Sign up for e-alerts
Follow Acta Cryst. on Twitter
Follow us on facebook
Sign up for RSS feeds