research communications
`Pd20Sn13' revisited: of Pd6.69Sn4.31
aTechnische Universität München, Department of Chemistry, Lichtenbergstrasse 4, 85747 Garching, Germany
*Correspondence e-mail: thomas.faessler@lrz.tu-muenchen.de
The 20Sn13' [Sarah et al. (1981). 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 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 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 2. (Wyckoff letter 3a and 3b).
of the title compound was previously reported with composition `PdKeywords: crystal structure; redetermination; system Pd–Sn; defect variant of the AlB2 structure type.
CCDC reference: 1406124
1. Chemical context
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.
2. Structural commentary
The 2 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.
of the title compound can be described as a defect variant of the AlBThe 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 (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 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). 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.
4. Refinement
Crystal data, data collection and structure . 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, 1983; Parsons et al., 2013). Therefore P3221 was chosen for the current It should be noted that the value and the corresponding for the 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.
details are summarized in Table 1Supporting information
CCDC reference: 1406124
10.1107/S2056989015011366/wm5142sup1.cif
contains datablocks global, I. DOI:Structure factors: contains datablock I. DOI: 10.1107/S2056989015011366/wm5142Isup2.hkl
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.
The
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
(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
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).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.
Crystal data, data collection and structure
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, 1983; Parsons et al., 2013). Therefore P3221 was chosen for the current It should be noted that the value and the corresponding for the 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.Data collection: CrysAlis CCD (Oxford Diffraction, 2009); cell
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).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. | |
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. | |
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. |
Pd6.69Sn4.31 | Dx = 10.813 Mg m−3 |
Mr = 1223.37 | Mo Kα radiation, λ = 0.71073 Å |
Trigonal, P3221 | Cell parameters from 8247 reflections |
a = 8.77574 (17) Å | θ = 2.9–32.7° |
c = 16.9004 (4) Å | µ = 29.54 mm−1 |
V = 1127.18 (5) Å3 | T = 150 K |
Z = 6 | Fragment, black |
F(000) = 3139 | 0.16 × 0.1 × 0.08 mm |
Oxford Xcalibur 3 diffractometer | 2682 independent reflections |
Radiation source: Enhance (Mo) X-ray Source | 2001 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.041 |
Detector resolution: 16.0238 pixels mm-1 | θmax = 32.8°, θmin = 2.9° |
ω and π scans | h = −13→8 |
Absorption correction: multi-scan (CrysAlis RED; Oxford Diffraction, 2009) | k = −12→12 |
Tmin = 0.408, Tmax = 1.000 | l = −25→25 |
20534 measured reflections |
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)] = 0.028 | Δρmax = 2.66 e Å−3 |
wR(F2) = 0.076 | Δρmin = −2.52 e Å−3 |
S = 1.08 | Extinction correction: SHELXL2014 (Sheldrick, 2015), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
2682 reflections | Extinction coefficient: 0.00066 (4) |
104 parameters | Absolute structure: Flack x determined using 715 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons et al., 2013) |
0 restraints | Absolute structure parameter: −0.2 (2) |
Pd6.69Sn4.31 | Z = 6 |
Mr = 1223.37 | Mo Kα radiation |
Trigonal, P3221 | µ = 29.54 mm−1 |
a = 8.77574 (17) Å | T = 150 K |
c = 16.9004 (4) Å | 0.16 × 0.1 × 0.08 mm |
V = 1127.18 (5) Å3 |
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 = 1.000 | Rint = 0.041 |
20534 measured reflections |
R[F2 > 2σ(F2)] = 0.028 | 0 restraints |
wR(F2) = 0.076 | Δρmax = 2.66 e Å−3 |
S = 1.08 | Δρmin = −2.52 e Å−3 |
2682 reflections | Absolute structure: Flack x determined using 715 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons et al., 2013) |
104 parameters | Absolute structure parameter: −0.2 (2) |
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. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Pd1 | −0.0002 (5) | 0.0000 | 0.1667 | 0.0083 (2) | |
Pd2 | 0.4990 (2) | 0.0000 | 0.1667 | 0.00772 (19) | |
Pd3 | −0.0010 (5) | −0.0010 (5) | 0.0000 | 0.0100 (2) | |
Pd4 | 0.5041 (2) | 0.5072 (3) | 0.16345 (4) | 0.01021 (19) | |
Pd5 | 0.4963 (2) | −0.0035 (5) | −0.00092 (4) | 0.00921 (17) | |
Pd6 | 0.6556 (3) | 0.3385 (3) | 0.07906 (6) | 0.0124 (2) | |
Pd7 | 0.6590 (3) | 0.82039 (16) | 0.07559 (5) | 0.00882 (17) | |
Pd8 | 0.18110 (16) | 0.3394 (3) | 0.08142 (5) | 0.00947 (16) | |
Pd9 | 0.4997 (2) | 0.4997 (2) | 0.0000 | 0.0071 (3) | 0.37 (4) |
Sn1 | 0.4997 (2) | 0.4997 (2) | 0.0000 | 0.0071 (3) | 0.63 (4) |
Sn2 | 0.3048 (2) | 0.11037 (11) | 0.08285 (5) | 0.00898 (19) | |
Sn3 | 0.3030 (3) | 0.6900 (3) | 0.08831 (5) | 0.0083 (2) | |
Sn4 | 0.83212 (15) | 0.16829 (14) | 0.08857 (4) | 0.00861 (14) | |
Sn5 | 0.88531 (10) | 0.6896 (2) | 0.08862 (5) | 0.0084 (2) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Pd1 | 0.0096 (8) | 0.0087 (14) | 0.0063 (5) | 0.0044 (7) | 0.0006 (5) | 0.0012 (11) |
Pd2 | 0.0096 (7) | 0.0076 (14) | 0.0052 (4) | 0.0038 (7) | −0.0002 (5) | −0.0003 (10) |
Pd3 | 0.0104 (7) | 0.0104 (7) | 0.0062 (5) | 0.0028 (13) | 0.0005 (6) | −0.0005 (6) |
Pd4 | 0.0100 (8) | 0.0122 (6) | 0.0072 (3) | 0.0046 (8) | 0.0002 (6) | 0.0011 (4) |
Pd5 | 0.0143 (8) | 0.0093 (7) | 0.0060 (3) | 0.0074 (5) | −0.0004 (5) | −0.0002 (6) |
Pd6 | 0.0116 (8) | 0.0116 (8) | 0.0137 (4) | 0.0056 (5) | 0.0001 (6) | 0.0005 (6) |
Pd7 | 0.0087 (7) | 0.0089 (5) | 0.0096 (3) | 0.0049 (6) | 0.0004 (6) | 0.0007 (4) |
Pd8 | 0.0091 (5) | 0.0101 (7) | 0.0099 (3) | 0.0053 (6) | −0.0008 (4) | 0.0005 (6) |
Pd9 | 0.0070 (6) | 0.0070 (6) | 0.0060 (4) | 0.0026 (11) | −0.0003 (5) | 0.0003 (5) |
Sn1 | 0.0070 (6) | 0.0070 (6) | 0.0060 (4) | 0.0026 (11) | −0.0003 (5) | 0.0003 (5) |
Sn2 | 0.0081 (7) | 0.0138 (4) | 0.0076 (3) | 0.0074 (7) | 0.0014 (5) | 0.0019 (3) |
Sn3 | 0.0080 (7) | 0.0069 (7) | 0.0070 (4) | 0.0015 (3) | 0.0001 (5) | −0.0004 (5) |
Sn4 | 0.0079 (4) | 0.0072 (4) | 0.0081 (3) | 0.0018 (4) | 0.0002 (3) | −0.0001 (3) |
Sn5 | 0.0123 (4) | 0.0089 (7) | 0.0065 (3) | 0.0070 (7) | −0.0009 (2) | −0.0008 (5) |
Pd1—Sn5i | 2.7259 (18) | Pd5—Pd8ix | 2.933 (3) |
Pd1—Sn5ii | 2.7259 (18) | Pd5—Sn4 | 2.967 (2) |
Pd1—Sn2iii | 2.741 (4) | Pd6—Sn4 | 2.6407 (19) |
Pd1—Sn2 | 2.741 (4) | Pd6—Sn2 | 2.707 (2) |
Pd1—Pd3 | 2.8168 (1) | Pd6—Sn5 | 2.715 (2) |
Pd1—Pd3iv | 2.8168 (1) | Pd6—Pd9 | 2.7553 (13) |
Pd1—Sn4v | 2.875 (3) | Pd6—Sn3viii | 2.8242 (13) |
Pd1—Sn4vi | 2.875 (3) | Pd6—Sn3ix | 2.8782 (13) |
Pd1—Pd8 | 2.9563 (18) | Pd6—Pd5xv | 2.910 (4) |
Pd1—Pd8iii | 2.9563 (18) | Pd6—Pd4viii | 3.017 (4) |
Pd1—Pd7ii | 3.015 (4) | Pd7—Sn4xvi | 2.6532 (16) |
Pd1—Pd7i | 3.015 (4) | Pd7—Sn3 | 2.746 (3) |
Pd2—Sn3vii | 2.7264 (19) | Pd7—Pd9 | 2.7515 (19) |
Pd2—Sn3viii | 2.7264 (19) | Pd7—Sn5 | 2.755 (2) |
Pd2—Sn2iii | 2.738 (2) | Pd7—Sn5ix | 2.8188 (11) |
Pd2—Sn2 | 2.738 (2) | Pd7—Sn4ii | 2.8603 (9) |
Pd2—Pd5 | 2.8325 (7) | Pd7—Pd5xvi | 2.882 (3) |
Pd2—Pd5iii | 2.8325 (7) | Pd7—Pd3xvii | 2.884 (4) |
Pd2—Sn4iii | 2.8554 (19) | Pd7—Pd2xvi | 3.006 (2) |
Pd2—Sn4 | 2.8554 (19) | Pd7—Pd1xvii | 3.014 (4) |
Pd2—Pd6 | 2.9705 (19) | Pd8—Sn4vi | 2.6552 (18) |
Pd2—Pd6iii | 2.9705 (19) | Pd8—Sn3 | 2.708 (3) |
Pd2—Pd7vii | 3.006 (2) | Pd8—Sn2 | 2.720 (2) |
Pd2—Pd7viii | 3.006 (2) | Pd8—Sn5ii | 2.7802 (11) |
Pd3—Sn2 | 2.738 (3) | Pd8—Pd9 | 2.7853 (18) |
Pd3—Sn2ix | 2.738 (3) | Pd8—Sn2ix | 2.8279 (11) |
Pd3—Sn5x | 2.811 (3) | Pd8—Pd5ix | 2.933 (3) |
Pd3—Sn5i | 2.811 (3) | Pd8—Pd4ii | 2.973 (2) |
Pd3—Pd1xi | 2.8167 (1) | Pd9—Pd7ix | 2.7515 (19) |
Pd3—Pd7x | 2.884 (4) | Pd9—Pd6ix | 2.7553 (13) |
Pd3—Pd7i | 2.884 (4) | Pd9—Pd4ix | 2.7630 (7) |
Pd3—Pd8ix | 2.932 (4) | Pd9—Pd8ix | 2.7853 (18) |
Pd3—Pd8 | 2.932 (4) | Pd9—Sn2 | 3.2738 (16) |
Pd3—Sn4vi | 2.9611 (11) | Pd9—Sn2ix | 3.2738 (16) |
Pd3—Sn4xii | 2.9611 (11) | Sn2—Pd8ix | 2.8279 (11) |
Pd4—Sn3viii | 2.732 (4) | Sn2—Sn2iii | 3.2924 (15) |
Pd4—Sn5ii | 2.742 (2) | Sn3—Pd2xvi | 2.7263 (19) |
Pd4—Pd9 | 2.7629 (7) | Sn3—Pd4ii | 2.732 (4) |
Pd4—Pd7 | 2.805 (3) | Sn3—Pd5ix | 2.781 (4) |
Pd4—Pd8 | 2.820 (2) | Sn3—Pd5xvi | 2.797 (4) |
Pd4—Pd6 | 2.821 (3) | Sn3—Pd6ii | 2.8242 (13) |
Pd4—Sn4ii | 2.823 (2) | Sn3—Pd6ix | 2.8783 (13) |
Pd4—Pd5xiii | 2.8558 (9) | Sn4—Pd7vii | 2.6531 (16) |
Pd4—Pd8viii | 2.973 (2) | Sn4—Pd8xviii | 2.6552 (18) |
Pd4—Pd6ii | 3.017 (4) | Sn4—Pd4viii | 2.823 (2) |
Pd4—Sn5 | 3.1621 (19) | Sn4—Pd7viii | 2.8604 (9) |
Pd5—Sn2 | 2.740 (3) | Sn4—Pd1xviii | 2.875 (3) |
Pd5—Sn5xii | 2.772 (3) | Sn4—Pd5xv | 2.900 (2) |
Pd5—Sn3ix | 2.781 (4) | Sn4—Pd3xviii | 2.9611 (11) |
Pd5—Sn3vii | 2.797 (4) | Sn5—Pd1xvii | 2.7258 (18) |
Pd5—Pd4xiv | 2.8557 (9) | Sn5—Pd4viii | 2.742 (2) |
Pd5—Pd7vii | 2.882 (3) | Sn5—Pd5xv | 2.772 (3) |
Pd5—Sn4xii | 2.900 (2) | Sn5—Pd8viii | 2.7803 (11) |
Pd5—Pd6xii | 2.910 (4) | Sn5—Pd3xvii | 2.811 (3) |
Pd5—Pd6 | 2.932 (4) | Sn5—Pd7ix | 2.8188 (11) |
Sn5i—Pd1—Sn5ii | 164.96 (17) | Sn2—Pd6—Pd5xv | 151.78 (6) |
Sn5i—Pd1—Sn2iii | 83.14 (7) | Sn5—Pd6—Pd5xv | 58.92 (6) |
Sn5ii—Pd1—Sn2iii | 84.84 (8) | Pd9—Pd6—Pd5xv | 101.06 (7) |
Sn5i—Pd1—Sn2 | 84.84 (8) | Pd4—Pd6—Pd5xv | 128.45 (10) |
Sn5ii—Pd1—Sn2 | 83.14 (7) | Sn3viii—Pd6—Pd5xv | 123.49 (7) |
Sn2iii—Pd1—Sn2 | 73.82 (12) | Sn3ix—Pd6—Pd5xv | 57.78 (6) |
Sn5i—Pd1—Pd3 | 60.92 (7) | Sn4—Pd6—Pd5 | 64.09 (5) |
Sn5ii—Pd1—Pd3 | 119.10 (9) | Sn2—Pd6—Pd5 | 57.98 (6) |
Sn2iii—Pd1—Pd3 | 121.12 (13) | Sn5—Pd6—Pd5 | 153.21 (6) |
Sn2—Pd1—Pd3 | 59.00 (9) | Pd9—Pd6—Pd5 | 101.37 (7) |
Sn5i—Pd1—Pd3iv | 119.10 (9) | Pd4—Pd6—Pd5 | 131.43 (10) |
Sn5ii—Pd1—Pd3iv | 60.91 (7) | Sn3viii—Pd6—Pd5 | 113.13 (8) |
Sn2iii—Pd1—Pd3iv | 59.00 (9) | Sn3ix—Pd6—Pd5 | 57.19 (6) |
Sn2—Pd1—Pd3iv | 121.11 (13) | Pd5xv—Pd6—Pd5 | 97.37 (4) |
Pd3—Pd1—Pd3iv | 179.9 (2) | Sn4—Pd6—Pd2 | 60.84 (6) |
Sn5i—Pd1—Sn4v | 86.43 (6) | Sn2—Pd6—Pd2 | 57.45 (7) |
Sn5ii—Pd1—Sn4v | 105.28 (8) | Sn5—Pd6—Pd2 | 144.58 (5) |
Sn2iii—Pd1—Sn4v | 103.97 (3) | Pd9—Pd6—Pd2 | 130.92 (9) |
Sn2—Pd1—Sn4v | 171.20 (4) | Pd4—Pd6—Pd2 | 99.73 (7) |
Pd3—Pd1—Sn4v | 117.20 (15) | Sn3viii—Pd6—Pd2 | 56.06 (5) |
Pd3iv—Pd1—Sn4v | 62.69 (4) | Sn3ix—Pd6—Pd2 | 113.74 (8) |
Sn5i—Pd1—Sn4vi | 105.27 (8) | Pd5xv—Pd6—Pd2 | 123.60 (8) |
Sn5ii—Pd1—Sn4vi | 86.43 (6) | Pd5—Pd6—Pd2 | 57.35 (5) |
Sn2iii—Pd1—Sn4vi | 171.20 (4) | Sn4—Pd6—Pd4viii | 59.42 (5) |
Sn2—Pd1—Sn4vi | 103.97 (3) | Sn2—Pd6—Pd4viii | 145.74 (7) |
Pd3—Pd1—Sn4vi | 62.69 (4) | Sn5—Pd6—Pd4viii | 56.86 (6) |
Pd3iv—Pd1—Sn4vi | 117.20 (15) | Pd9—Pd6—Pd4viii | 130.73 (10) |
Sn4v—Pd1—Sn4vi | 79.49 (11) | Pd4—Pd6—Pd4viii | 97.46 (5) |
Sn5i—Pd1—Pd8 | 120.98 (4) | Sn3viii—Pd6—Pd4viii | 65.93 (5) |
Sn5ii—Pd1—Pd8 | 58.42 (3) | Sn3ix—Pd6—Pd4viii | 114.46 (8) |
Sn2iii—Pd1—Pd8 | 119.43 (12) | Pd5xv—Pd6—Pd4viii | 57.57 (6) |
Sn2—Pd1—Pd8 | 56.89 (5) | Pd5—Pd6—Pd4viii | 123.51 (7) |
Pd3—Pd1—Pd8 | 60.99 (8) | Pd2—Pd6—Pd4viii | 93.11 (6) |
Pd3iv—Pd1—Pd8 | 119.01 (8) | Sn4xvi—Pd7—Sn3 | 110.53 (8) |
Sn4v—Pd1—Pd8 | 129.67 (13) | Sn4xvi—Pd7—Pd9 | 157.08 (4) |
Sn4vi—Pd1—Pd8 | 54.16 (4) | Sn3—Pd7—Pd9 | 73.74 (5) |
Sn5i—Pd1—Pd8iii | 58.42 (3) | Sn4xvi—Pd7—Sn5 | 110.81 (8) |
Sn5ii—Pd1—Pd8iii | 120.98 (4) | Sn3—Pd7—Sn5 | 136.65 (6) |
Sn2iii—Pd1—Pd8iii | 56.89 (5) | Pd9—Pd7—Sn5 | 73.41 (4) |
Sn2—Pd1—Pd8iii | 119.43 (12) | Sn4xvi—Pd7—Pd4 | 143.30 (5) |
Pd3—Pd1—Pd8iii | 119.01 (8) | Sn3—Pd7—Pd4 | 69.96 (7) |
Pd3iv—Pd1—Pd8iii | 60.99 (8) | Pd9—Pd7—Pd4 | 59.62 (4) |
Sn4v—Pd1—Pd8iii | 54.15 (4) | Sn5—Pd7—Pd4 | 69.31 (7) |
Sn4vi—Pd1—Pd8iii | 129.67 (13) | Sn4xvi—Pd7—Sn5ix | 84.66 (4) |
Pd8—Pd1—Pd8iii | 176.07 (17) | Sn3—Pd7—Sn5ix | 97.76 (7) |
Sn5i—Pd1—Pd7ii | 137.27 (13) | Pd9—Pd7—Sn5ix | 72.42 (3) |
Sn5ii—Pd1—Pd7ii | 57.09 (5) | Sn5—Pd7—Sn5ix | 98.45 (7) |
Sn2iii—Pd1—Pd7ii | 117.33 (4) | Pd4—Pd7—Sn5ix | 132.04 (6) |
Sn2—Pd1—Pd7ii | 135.21 (3) | Sn4xvi—Pd7—Sn4ii | 83.53 (4) |
Pd3—Pd1—Pd7ii | 120.73 (11) | Sn3—Pd7—Sn4ii | 86.01 (5) |
Pd3iv—Pd1—Pd7ii | 59.16 (10) | Pd9—Pd7—Sn4ii | 119.39 (5) |
Sn4v—Pd1—Pd7ii | 53.49 (7) | Sn5—Pd7—Sn4ii | 86.17 (5) |
Sn4vi—Pd1—Pd7ii | 58.06 (7) | Pd4—Pd7—Sn4ii | 59.77 (4) |
Pd8—Pd1—Pd7ii | 83.04 (6) | Sn5ix—Pd7—Sn4ii | 168.19 (6) |
Pd8iii—Pd1—Pd7ii | 99.87 (7) | Sn4xvi—Pd7—Pd5xvi | 64.68 (7) |
Sn5i—Pd1—Pd7i | 57.09 (5) | Sn3—Pd7—Pd5xvi | 59.54 (7) |
Sn5ii—Pd1—Pd7i | 137.27 (13) | Pd9—Pd7—Pd5xvi | 101.87 (7) |
Sn2iii—Pd1—Pd7i | 135.21 (3) | Sn5—Pd7—Pd5xvi | 155.91 (5) |
Sn2—Pd1—Pd7i | 117.33 (4) | Pd4—Pd7—Pd5xvi | 129.46 (10) |
Pd3—Pd1—Pd7i | 59.16 (10) | Sn5ix—Pd7—Pd5xvi | 58.18 (5) |
Pd3iv—Pd1—Pd7i | 120.73 (11) | Sn4ii—Pd7—Pd5xvi | 115.64 (7) |
Sn4v—Pd1—Pd7i | 58.06 (7) | Sn4xvi—Pd7—Pd3xvii | 64.50 (7) |
Sn4vi—Pd1—Pd7i | 53.49 (7) | Sn3—Pd7—Pd3xvii | 156.01 (5) |
Pd8—Pd1—Pd7i | 99.87 (7) | Pd9—Pd7—Pd3xvii | 102.03 (6) |
Pd8iii—Pd1—Pd7i | 83.04 (6) | Sn5—Pd7—Pd3xvii | 59.74 (6) |
Pd7ii—Pd1—Pd7i | 86.07 (12) | Pd4—Pd7—Pd3xvii | 129.03 (9) |
Sn3vii—Pd2—Sn3viii | 164.85 (10) | Sn5ix—Pd7—Pd3xvii | 59.05 (6) |
Sn3vii—Pd2—Sn2iii | 83.18 (5) | Sn4ii—Pd7—Pd3xvii | 115.50 (7) |
Sn3viii—Pd2—Sn2iii | 84.72 (4) | Pd5xvi—Pd7—Pd3xvii | 99.51 (4) |
Sn3vii—Pd2—Sn2 | 84.73 (4) | Sn4xvi—Pd7—Pd2xvi | 60.21 (4) |
Sn3viii—Pd2—Sn2 | 83.18 (5) | Sn3—Pd7—Pd2xvi | 56.36 (6) |
Sn2iii—Pd2—Sn2 | 73.91 (8) | Pd9—Pd7—Pd2xvi | 129.97 (8) |
Sn3vii—Pd2—Pd5 | 60.38 (8) | Sn5—Pd7—Pd2xvi | 143.17 (5) |
Sn3viii—Pd2—Pd5 | 119.57 (8) | Pd4—Pd7—Pd2xvi | 96.79 (7) |
Sn2iii—Pd2—Pd5 | 120.80 (8) | Sn5ix—Pd7—Pd2xvi | 114.87 (7) |
Sn2—Pd2—Pd5 | 58.89 (6) | Sn4ii—Pd7—Pd2xvi | 58.19 (4) |
Sn3vii—Pd2—Pd5iii | 119.57 (8) | Pd5xvi—Pd7—Pd2xvi | 57.46 (4) |
Sn3viii—Pd2—Pd5iii | 60.38 (8) | Pd3xvii—Pd7—Pd2xvi | 124.71 (7) |
Sn2iii—Pd2—Pd5iii | 58.89 (6) | Sn4xvi—Pd7—Pd1xvii | 60.56 (5) |
Sn2—Pd2—Pd5iii | 120.80 (8) | Sn3—Pd7—Pd1xvii | 143.39 (6) |
Pd5—Pd2—Pd5iii | 179.68 (12) | Pd9—Pd7—Pd1xvii | 129.46 (8) |
Sn3vii—Pd2—Sn4iii | 86.47 (4) | Sn5—Pd7—Pd1xvii | 56.17 (7) |
Sn3viii—Pd2—Sn4iii | 105.28 (5) | Pd4—Pd7—Pd1xvii | 96.32 (5) |
Sn2iii—Pd2—Sn4iii | 103.61 (3) | Sn5ix—Pd7—Pd1xvii | 115.31 (8) |
Sn2—Pd2—Sn4iii | 171.07 (3) | Sn4ii—Pd7—Pd1xvii | 58.52 (5) |
Pd5—Pd2—Sn4iii | 117.39 (9) | Pd5xvi—Pd7—Pd1xvii | 125.23 (7) |
Pd5iii—Pd2—Sn4iii | 62.89 (5) | Pd3xvii—Pd7—Pd1xvii | 57.00 (6) |
Sn3vii—Pd2—Sn4 | 105.27 (5) | Pd2xvi—Pd7—Pd1xvii | 93.78 (5) |
Sn3viii—Pd2—Sn4 | 86.47 (4) | Sn4vi—Pd8—Sn3 | 109.23 (8) |
Sn2iii—Pd2—Sn4 | 171.07 (3) | Sn4vi—Pd8—Sn2 | 110.81 (8) |
Sn2—Pd2—Sn4 | 103.61 (3) | Sn3—Pd8—Sn2 | 139.66 (6) |
Pd5—Pd2—Sn4 | 62.89 (5) | Sn4vi—Pd8—Sn5ii | 89.76 (5) |
Pd5iii—Pd2—Sn4 | 117.39 (9) | Sn3—Pd8—Sn5ii | 92.94 (6) |
Sn4iii—Pd2—Sn4 | 80.13 (7) | Sn2—Pd8—Sn5ii | 82.52 (5) |
Sn3vii—Pd2—Pd6 | 120.09 (4) | Sn4vi—Pd8—Pd9 | 152.99 (4) |
Sn3viii—Pd2—Pd6 | 59.25 (4) | Sn3—Pd8—Pd9 | 73.79 (5) |
Sn2iii—Pd2—Pd6 | 119.55 (7) | Sn2—Pd8—Pd9 | 72.96 (4) |
Sn2—Pd2—Pd6 | 56.43 (4) | Sn5ii—Pd8—Pd9 | 117.14 (6) |
Pd5—Pd2—Pd6 | 60.64 (8) | Sn4vi—Pd8—Pd4 | 147.89 (4) |
Pd5iii—Pd2—Pd6 | 119.35 (8) | Sn3—Pd8—Pd4 | 70.28 (8) |
Sn4iii—Pd2—Pd6 | 130.31 (7) | Sn2—Pd8—Pd4 | 73.34 (8) |
Sn4—Pd2—Pd6 | 53.86 (4) | Sn5ii—Pd8—Pd4 | 58.64 (5) |
Sn3vii—Pd2—Pd6iii | 59.25 (4) | Pd9—Pd8—Pd4 | 59.07 (4) |
Sn3viii—Pd2—Pd6iii | 120.09 (4) | Sn4vi—Pd8—Sn2ix | 81.65 (4) |
Sn2iii—Pd2—Pd6iii | 56.43 (4) | Sn3—Pd8—Sn2ix | 96.03 (8) |
Sn2—Pd2—Pd6iii | 119.56 (7) | Sn2—Pd8—Sn2ix | 94.39 (7) |
Pd5—Pd2—Pd6iii | 119.34 (8) | Sn5ii—Pd8—Sn2ix | 169.22 (8) |
Pd5iii—Pd2—Pd6iii | 60.64 (8) | Pd9—Pd8—Sn2ix | 71.35 (3) |
Sn4iii—Pd2—Pd6iii | 53.86 (4) | Pd4—Pd8—Sn2ix | 130.40 (5) |
Sn4—Pd2—Pd6iii | 130.31 (7) | Sn4vi—Pd8—Pd3 | 63.78 (6) |
Pd6—Pd2—Pd6iii | 175.71 (10) | Sn3—Pd8—Pd3 | 151.91 (5) |
Sn3vii—Pd2—Pd7vii | 56.98 (4) | Sn2—Pd8—Pd3 | 57.79 (6) |
Sn3viii—Pd2—Pd7vii | 137.49 (8) | Sn5ii—Pd8—Pd3 | 113.52 (8) |
Sn2iii—Pd2—Pd7vii | 135.11 (4) | Pd9—Pd8—Pd3 | 100.42 (6) |
Sn2—Pd2—Pd7vii | 117.19 (3) | Pd4—Pd8—Pd3 | 131.02 (11) |
Pd5—Pd2—Pd7vii | 59.06 (6) | Sn2ix—Pd8—Pd3 | 56.72 (6) |
Pd5iii—Pd2—Pd7vii | 121.22 (7) | Sn4vi—Pd8—Pd5ix | 62.28 (7) |
Sn4iii—Pd2—Pd7vii | 58.34 (4) | Sn3—Pd8—Pd5ix | 58.92 (7) |
Sn4—Pd2—Pd7vii | 53.75 (5) | Sn2—Pd8—Pd5ix | 150.35 (5) |
Pd6—Pd2—Pd7vii | 99.52 (4) | Sn5ii—Pd8—Pd5ix | 124.40 (6) |
Pd6iii—Pd2—Pd7vii | 83.64 (5) | Pd9—Pd8—Pd5ix | 100.63 (7) |
Sn3vii—Pd2—Pd7viii | 137.49 (8) | Pd4—Pd8—Pd5ix | 129.05 (12) |
Sn3viii—Pd2—Pd7viii | 56.98 (4) | Sn2ix—Pd8—Pd5ix | 56.76 (5) |
Sn2iii—Pd2—Pd7viii | 117.19 (3) | Pd3—Pd8—Pd5ix | 96.48 (4) |
Sn2—Pd2—Pd7viii | 135.11 (4) | Sn4vi—Pd8—Pd1 | 61.35 (9) |
Pd5—Pd2—Pd7viii | 121.22 (7) | Sn3—Pd8—Pd1 | 146.27 (5) |
Pd5iii—Pd2—Pd7viii | 59.06 (6) | Sn2—Pd8—Pd1 | 57.57 (9) |
Sn4iii—Pd2—Pd7viii | 53.75 (5) | Sn5ii—Pd8—Pd1 | 56.64 (4) |
Sn4—Pd2—Pd7viii | 58.35 (4) | Pd9—Pd8—Pd1 | 130.41 (10) |
Pd6—Pd2—Pd7viii | 83.64 (5) | Pd4—Pd8—Pd1 | 100.40 (5) |
Pd6iii—Pd2—Pd7viii | 99.52 (4) | Sn2ix—Pd8—Pd1 | 113.05 (7) |
Pd7vii—Pd2—Pd7viii | 86.36 (9) | Pd3—Pd8—Pd1 | 57.15 (5) |
Sn2—Pd3—Sn2ix | 96.07 (14) | Pd5ix—Pd8—Pd1 | 123.62 (12) |
Sn2—Pd3—Sn5x | 178.55 (7) | Sn4vi—Pd8—Pd4ii | 59.90 (7) |
Sn2ix—Pd3—Sn5x | 83.31 (2) | Sn3—Pd8—Pd4ii | 57.26 (8) |
Sn2—Pd3—Sn5i | 83.31 (2) | Sn2—Pd8—Pd4ii | 146.97 (6) |
Sn2ix—Pd3—Sn5i | 178.55 (7) | Sn5ii—Pd8—Pd4ii | 66.59 (3) |
Sn5x—Pd3—Sn5i | 97.34 (13) | Pd9—Pd8—Pd4ii | 130.97 (10) |
Sn2—Pd3—Pd1xi | 120.62 (10) | Pd4—Pd8—Pd4ii | 98.54 (4) |
Sn2ix—Pd3—Pd1xi | 59.12 (10) | Sn2ix—Pd8—Pd4ii | 113.73 (7) |
Sn5x—Pd3—Pd1xi | 57.95 (4) | Pd3—Pd8—Pd4ii | 123.68 (10) |
Sn5i—Pd3—Pd1xi | 122.31 (15) | Pd5ix—Pd8—Pd4ii | 57.83 (5) |
Sn2—Pd3—Pd1 | 59.12 (10) | Pd1—Pd8—Pd4ii | 94.05 (4) |
Sn2ix—Pd3—Pd1 | 120.62 (10) | Pd7—Pd9—Pd7ix | 80.14 (9) |
Sn5x—Pd3—Pd1 | 122.32 (15) | Pd7—Pd9—Pd6ix | 80.90 (7) |
Sn5i—Pd3—Pd1 | 57.95 (4) | Pd7ix—Pd9—Pd6ix | 99.86 (4) |
Pd1xi—Pd3—Pd1 | 179.7 (2) | Pd7—Pd9—Pd6 | 99.87 (4) |
Sn2—Pd3—Pd7x | 121.64 (4) | Pd7ix—Pd9—Pd6 | 80.90 (7) |
Sn2ix—Pd3—Pd7x | 122.05 (4) | Pd6ix—Pd9—Pd6 | 179.02 (12) |
Sn5x—Pd3—Pd7x | 57.85 (8) | Pd7—Pd9—Pd4 | 61.16 (6) |
Sn5i—Pd3—Pd7x | 59.33 (8) | Pd7ix—Pd9—Pd4 | 116.98 (7) |
Pd1xi—Pd3—Pd7x | 63.84 (10) | Pd6ix—Pd9—Pd4 | 118.52 (8) |
Pd1—Pd3—Pd7x | 116.45 (11) | Pd6—Pd9—Pd4 | 61.50 (8) |
Sn2—Pd3—Pd7i | 122.05 (4) | Pd7—Pd9—Pd4ix | 116.98 (7) |
Sn2ix—Pd3—Pd7i | 121.64 (4) | Pd7ix—Pd9—Pd4ix | 61.16 (6) |
Sn5x—Pd3—Pd7i | 59.33 (8) | Pd6ix—Pd9—Pd4ix | 61.50 (8) |
Sn5i—Pd3—Pd7i | 57.85 (8) | Pd6—Pd9—Pd4ix | 118.52 (8) |
Pd1xi—Pd3—Pd7i | 116.45 (11) | Pd4—Pd9—Pd4ix | 177.85 (12) |
Pd1—Pd3—Pd7i | 63.84 (10) | Pd7—Pd9—Pd8ix | 178.02 (4) |
Pd7x—Pd3—Pd7i | 75.79 (12) | Pd7ix—Pd9—Pd8ix | 98.94 (3) |
Sn2—Pd3—Pd8ix | 59.72 (8) | Pd6ix—Pd9—Pd8ix | 97.57 (4) |
Sn2ix—Pd3—Pd8ix | 57.22 (8) | Pd6—Pd9—Pd8ix | 81.68 (7) |
Sn5x—Pd3—Pd8ix | 118.91 (4) | Pd4—Pd9—Pd8ix | 120.78 (8) |
Sn5i—Pd3—Pd8ix | 123.33 (4) | Pd4ix—Pd9—Pd8ix | 61.08 (5) |
Pd1xi—Pd3—Pd8ix | 61.85 (5) | Pd7—Pd9—Pd8 | 98.94 (3) |
Pd1—Pd3—Pd8ix | 117.85 (15) | Pd7ix—Pd9—Pd8 | 178.02 (4) |
Pd7x—Pd3—Pd8ix | 103.57 (3) | Pd6ix—Pd9—Pd8 | 81.69 (7) |
Pd7i—Pd3—Pd8ix | 178.21 (6) | Pd6—Pd9—Pd8 | 97.57 (4) |
Sn2—Pd3—Pd8 | 57.22 (8) | Pd4—Pd9—Pd8 | 61.08 (5) |
Sn2ix—Pd3—Pd8 | 59.72 (8) | Pd4ix—Pd9—Pd8 | 120.78 (8) |
Sn5x—Pd3—Pd8 | 123.32 (4) | Pd8ix—Pd9—Pd8 | 82.03 (9) |
Sn5i—Pd3—Pd8 | 118.91 (4) | Pd7—Pd9—Sn2 | 127.01 (2) |
Pd1xi—Pd3—Pd8 | 117.85 (15) | Pd7ix—Pd9—Sn2 | 126.63 (6) |
Pd1—Pd3—Pd8 | 61.85 (5) | Pd6ix—Pd9—Sn2 | 126.54 (8) |
Pd7x—Pd3—Pd8 | 178.21 (6) | Pd6—Pd9—Sn2 | 52.49 (6) |
Pd7i—Pd3—Pd8 | 103.57 (3) | Pd4—Pd9—Sn2 | 65.85 (6) |
Pd8ix—Pd3—Pd8 | 77.12 (11) | Pd4ix—Pd9—Sn2 | 116.00 (6) |
Sn2—Pd3—Sn4vi | 101.81 (8) | Pd8ix—Pd9—Sn2 | 54.93 (4) |
Sn2ix—Pd3—Sn4vi | 77.90 (6) | Pd8—Pd9—Sn2 | 52.61 (5) |
Sn5x—Pd3—Sn4vi | 79.35 (6) | Pd7—Pd9—Sn2ix | 126.63 (6) |
Sn5i—Pd3—Sn4vi | 100.92 (7) | Pd7ix—Pd9—Sn2ix | 127.01 (2) |
Pd1xi—Pd3—Sn4vi | 120.39 (7) | Pd6ix—Pd9—Sn2ix | 52.49 (6) |
Pd1—Pd3—Sn4vi | 59.61 (7) | Pd6—Pd9—Sn2ix | 126.54 (8) |
Pd7x—Pd3—Sn4vi | 126.43 (14) | Pd4—Pd9—Sn2ix | 116.00 (6) |
Pd7i—Pd3—Sn4vi | 53.97 (4) | Pd4ix—Pd9—Sn2ix | 65.85 (6) |
Pd8ix—Pd3—Sn4vi | 126.04 (13) | Pd8ix—Pd9—Sn2ix | 52.61 (5) |
Pd8—Pd3—Sn4vi | 53.55 (4) | Pd8—Pd9—Sn2ix | 54.93 (4) |
Sn2—Pd3—Sn4xii | 77.90 (6) | Sn2—Pd9—Sn2ix | 76.90 (7) |
Sn2ix—Pd3—Sn4xii | 101.81 (8) | Pd6—Sn2—Pd8 | 100.35 (4) |
Sn5x—Pd3—Sn4xii | 100.92 (7) | Pd6—Sn2—Pd3 | 143.25 (7) |
Sn5i—Pd3—Sn4xii | 79.35 (6) | Pd8—Sn2—Pd3 | 64.99 (7) |
Pd1xi—Pd3—Sn4xii | 59.61 (7) | Pd6—Sn2—Pd2 | 66.12 (6) |
Pd1—Pd3—Sn4xii | 120.39 (7) | Pd8—Sn2—Pd2 | 144.55 (4) |
Pd7x—Pd3—Sn4xii | 53.97 (4) | Pd3—Sn2—Pd2 | 144.15 (7) |
Pd7i—Pd3—Sn4xii | 126.43 (14) | Pd6—Sn2—Pd5 | 65.14 (8) |
Pd8ix—Pd3—Sn4xii | 53.56 (4) | Pd8—Sn2—Pd5 | 144.00 (6) |
Pd8—Pd3—Sn4xii | 126.04 (13) | Pd3—Sn2—Pd5 | 106.02 (4) |
Sn4vi—Pd3—Sn4xii | 179.59 (18) | Pd2—Sn2—Pd5 | 62.27 (5) |
Sn3viii—Pd4—Sn5ii | 84.03 (6) | Pd6—Sn2—Pd1 | 145.28 (4) |
Sn3viii—Pd4—Pd9 | 119.64 (12) | Pd8—Sn2—Pd1 | 65.54 (7) |
Sn5ii—Pd4—Pd9 | 119.22 (7) | Pd3—Sn2—Pd1 | 61.87 (6) |
Sn3viii—Pd4—Pd7 | 137.40 (9) | Pd2—Sn2—Pd1 | 106.14 (5) |
Sn5ii—Pd4—Pd7 | 136.41 (14) | Pd5—Sn2—Pd1 | 143.76 (8) |
Pd9—Pd4—Pd7 | 59.22 (5) | Pd6—Sn2—Pd8ix | 81.77 (6) |
Sn3viii—Pd4—Pd8 | 119.74 (10) | Pd8—Sn2—Pd8ix | 82.40 (5) |
Sn5ii—Pd4—Pd8 | 59.96 (5) | Pd3—Sn2—Pd8ix | 63.56 (7) |
Pd9—Pd4—Pd8 | 59.85 (5) | Pd2—Sn2—Pd8ix | 124.61 (8) |
Pd7—Pd4—Pd8 | 96.87 (7) | Pd5—Sn2—Pd8ix | 63.55 (6) |
Sn3viii—Pd4—Pd6 | 61.11 (8) | Pd1—Sn2—Pd8ix | 124.30 (10) |
Sn5ii—Pd4—Pd6 | 119.88 (11) | Pd6—Sn2—Pd9 | 53.86 (4) |
Pd9—Pd4—Pd6 | 59.12 (4) | Pd8—Sn2—Pd9 | 54.43 (3) |
Pd7—Pd4—Pd6 | 97.00 (5) | Pd3—Sn2—Pd9 | 93.51 (6) |
Pd8—Pd4—Pd6 | 95.27 (6) | Pd2—Sn2—Pd9 | 119.84 (6) |
Sn3viii—Pd4—Sn4ii | 103.82 (5) | Pd5—Sn2—Pd9 | 93.67 (7) |
Sn5ii—Pd4—Sn4ii | 103.15 (8) | Pd1—Sn2—Pd9 | 119.88 (7) |
Pd9—Pd4—Sn4ii | 120.30 (9) | Pd8ix—Sn2—Pd9 | 53.72 (3) |
Pd7—Pd4—Sn4ii | 61.08 (6) | Pd6—Sn2—Sn2iii | 110.29 (4) |
Pd8—Pd4—Sn4ii | 128.95 (14) | Pd8—Sn2—Sn2iii | 109.49 (3) |
Pd6—Pd4—Sn4ii | 130.44 (9) | Pd3—Sn2—Sn2iii | 106.41 (6) |
Sn3viii—Pd4—Pd5xiii | 59.65 (9) | Pd2—Sn2—Sn2iii | 53.05 (4) |
Sn5ii—Pd4—Pd5xiii | 59.32 (6) | Pd5—Sn2—Sn2iii | 106.48 (6) |
Pd9—Pd4—Pd5xiii | 178.23 (11) | Pd1—Sn2—Sn2iii | 53.09 (6) |
Pd7—Pd4—Pd5xiii | 122.48 (10) | Pd8ix—Sn2—Sn2iii | 160.33 (5) |
Pd8—Pd4—Pd5xiii | 118.85 (9) | Pd9—Sn2—Sn2iii | 145.95 (4) |
Pd6—Pd4—Pd5xiii | 120.40 (14) | Pd8—Sn3—Pd2xvi | 148.03 (5) |
Sn4ii—Pd4—Pd5xiii | 61.40 (6) | Pd8—Sn3—Pd4ii | 66.25 (7) |
Sn3viii—Pd4—Pd8viii | 56.49 (6) | Pd2xvi—Sn3—Pd4ii | 108.48 (6) |
Sn5ii—Pd4—Pd8viii | 118.66 (5) | Pd8—Sn3—Pd7 | 101.00 (4) |
Pd9—Pd4—Pd8viii | 120.82 (8) | Pd2xvi—Sn3—Pd7 | 66.65 (7) |
Pd7—Pd4—Pd8viii | 86.42 (5) | Pd4ii—Sn3—Pd7 | 148.98 (6) |
Pd8—Pd4—Pd8viii | 176.19 (13) | Pd8—Sn3—Pd5ix | 64.58 (6) |
Pd6—Pd4—Pd8viii | 82.38 (9) | Pd2xvi—Sn3—Pd5ix | 143.39 (7) |
Sn4ii—Pd4—Pd8viii | 54.45 (5) | Pd4ii—Sn3—Pd5ix | 62.39 (7) |
Pd5xiii—Pd4—Pd8viii | 60.38 (7) | Pd7—Sn3—Pd5ix | 139.85 (6) |
Sn3viii—Pd4—Pd6ii | 117.94 (5) | Pd8—Sn3—Pd5xvi | 140.76 (6) |
Sn5ii—Pd4—Pd6ii | 56.01 (6) | Pd2xvi—Sn3—Pd5xvi | 61.69 (6) |
Pd9—Pd4—Pd6ii | 121.00 (11) | Pd4ii—Sn3—Pd5xvi | 144.37 (7) |
Pd7—Pd4—Pd6ii | 86.30 (10) | Pd7—Sn3—Pd5xvi | 62.65 (6) |
Pd8—Pd4—Pd6ii | 81.61 (8) | Pd5ix—Sn3—Pd5xvi | 103.75 (3) |
Pd6—Pd4—Pd6ii | 175.73 (7) | Pd8—Sn3—Pd6ii | 87.24 (6) |
Sn4ii—Pd4—Pd6ii | 53.63 (7) | Pd2xvi—Sn3—Pd6ii | 64.69 (5) |
Pd5xiii—Pd4—Pd6ii | 59.33 (9) | Pd4ii—Sn3—Pd6ii | 61.01 (6) |
Pd8viii—Pd4—Pd6ii | 100.58 (5) | Pd7—Sn3—Pd6ii | 91.36 (5) |
Sn3viii—Pd4—Sn5 | 84.60 (8) | Pd5ix—Sn3—Pd6ii | 123.02 (9) |
Sn5ii—Pd4—Sn5 | 168.62 (12) | Pd5xvi—Sn3—Pd6ii | 126.05 (9) |
Pd9—Pd4—Sn5 | 67.09 (5) | Pd8—Sn3—Pd6ix | 80.82 (6) |
Pd7—Pd4—Sn5 | 54.59 (5) | Pd2xvi—Sn3—Pd6ix | 122.33 (9) |
Pd8—Pd4—Sn5 | 126.91 (3) | Pd4ii—Sn3—Pd6ix | 123.59 (10) |
Pd6—Pd4—Sn5 | 53.61 (7) | Pd7—Sn3—Pd6ix | 78.84 (6) |
Sn4ii—Pd4—Sn5 | 79.51 (5) | Pd5ix—Sn3—Pd6ix | 62.38 (7) |
Pd5xiii—Pd4—Sn5 | 114.16 (9) | Pd5xvi—Sn3—Pd6ix | 61.68 (7) |
Pd8viii—Pd4—Sn5 | 53.79 (4) | Pd6ii—Sn3—Pd6ix | 162.73 (5) |
Pd6ii—Pd4—Sn5 | 130.65 (9) | Pd8—Sn3—Pd4 | 56.50 (5) |
Sn2—Pd5—Sn5xii | 178.71 (10) | Pd2xvi—Sn3—Pd4 | 94.42 (7) |
Sn2—Pd5—Sn3ix | 96.39 (11) | Pd4ii—Sn3—Pd4 | 95.55 (4) |
Sn5xii—Pd5—Sn3ix | 82.57 (4) | Pd7—Sn3—Pd4 | 55.90 (4) |
Sn2—Pd5—Sn3vii | 83.37 (4) | Pd5ix—Sn3—Pd4 | 120.95 (7) |
Sn5xii—Pd5—Sn3vii | 97.68 (11) | Pd5xvi—Sn3—Pd4 | 118.51 (7) |
Sn3ix—Pd5—Sn3vii | 179.44 (10) | Pd6ii—Sn3—Pd4 | 59.95 (5) |
Sn2—Pd5—Pd2 | 58.84 (6) | Pd6ix—Sn3—Pd4 | 102.87 (5) |
Sn5xii—Pd5—Pd2 | 122.37 (9) | Pd6—Sn4—Pd7vii | 119.05 (5) |
Sn3ix—Pd5—Pd2 | 121.51 (11) | Pd6—Sn4—Pd8xviii | 120.96 (5) |
Sn3vii—Pd5—Pd2 | 57.93 (4) | Pd7vii—Sn4—Pd8xviii | 118.82 (5) |
Sn2—Pd5—Pd4xiv | 120.49 (9) | Pd6—Sn4—Pd4viii | 66.95 (7) |
Sn5xii—Pd5—Pd4xiv | 58.30 (5) | Pd7vii—Sn4—Pd4viii | 155.61 (4) |
Sn3ix—Pd5—Pd4xiv | 57.96 (9) | Pd8xviii—Sn4—Pd4viii | 65.64 (8) |
Sn3vii—Pd5—Pd4xiv | 122.59 (15) | Pd6—Sn4—Pd2 | 65.30 (6) |
Pd2—Pd5—Pd4xiv | 179.22 (17) | Pd7vii—Sn4—Pd2 | 66.04 (5) |
Sn2—Pd5—Pd7vii | 121.49 (5) | Pd8xviii—Sn4—Pd2 | 155.06 (4) |
Sn5xii—Pd5—Pd7vii | 59.78 (6) | Pd4viii—Sn4—Pd2 | 99.92 (6) |
Sn3ix—Pd5—Pd7vii | 121.99 (7) | Pd6—Sn4—Pd7viii | 92.76 (6) |
Sn3vii—Pd5—Pd7vii | 57.81 (7) | Pd7vii—Sn4—Pd7viii | 96.47 (4) |
Pd2—Pd5—Pd7vii | 63.48 (6) | Pd8xviii—Sn4—Pd7viii | 91.64 (5) |
Pd4xiv—Pd5—Pd7vii | 117.25 (10) | Pd4viii—Sn4—Pd7viii | 59.15 (4) |
Sn2—Pd5—Sn4xii | 78.94 (6) | Pd2—Sn4—Pd7viii | 63.47 (5) |
Sn5xii—Pd5—Sn4xii | 100.48 (7) | Pd6—Sn4—Pd1xviii | 156.15 (5) |
Sn3ix—Pd5—Sn4xii | 100.64 (6) | Pd7vii—Sn4—Pd1xviii | 65.95 (6) |
Sn3vii—Pd5—Sn4xii | 79.82 (8) | Pd8xviii—Sn4—Pd1xviii | 64.49 (7) |
Pd2—Pd5—Sn4xii | 121.13 (7) | Pd4viii—Sn4—Pd1xviii | 99.16 (4) |
Pd4xiv—Pd5—Sn4xii | 58.75 (6) | Pd2—Sn4—Pd1xviii | 100.19 (5) |
Pd7vii—Pd5—Sn4xii | 126.67 (13) | Pd7viii—Sn4—Pd1xviii | 63.42 (6) |
Sn2—Pd5—Pd6xii | 123.11 (9) | Pd6—Sn4—Pd5xv | 63.17 (8) |
Sn5xii—Pd5—Pd6xii | 57.03 (7) | Pd7vii—Sn4—Pd5xv | 144.54 (4) |
Sn3ix—Pd5—Pd6xii | 119.99 (5) | Pd8xviii—Sn4—Pd5xv | 63.56 (8) |
Sn3vii—Pd5—Pd6xii | 60.54 (8) | Pd4viii—Sn4—Pd5xv | 59.85 (4) |
Pd2—Pd5—Pd6xii | 117.52 (11) | Pd2—Sn4—Pd5xv | 128.46 (9) |
Pd4xiv—Pd5—Pd6xii | 63.11 (9) | Pd7viii—Sn4—Pd5xv | 119.00 (5) |
Pd7vii—Pd5—Pd6xii | 76.17 (9) | Pd1xviii—Sn4—Pd5xv | 128.04 (10) |
Sn4xii—Pd5—Pd6xii | 54.07 (6) | Pd6—Sn4—Pd3xviii | 146.14 (3) |
Sn2—Pd5—Pd6 | 56.88 (7) | Pd7vii—Sn4—Pd3xviii | 61.52 (9) |
Sn5xii—Pd5—Pd6 | 122.99 (9) | Pd8xviii—Sn4—Pd3xviii | 62.67 (9) |
Sn3ix—Pd5—Pd6 | 60.43 (8) | Pd4viii—Sn4—Pd3xviii | 128.30 (12) |
Sn3vii—Pd5—Pd6 | 119.04 (5) | Pd2—Sn4—Pd3xviii | 127.55 (9) |
Pd2—Pd5—Pd6 | 62.01 (5) | Pd7viii—Sn4—Pd3xviii | 121.10 (6) |
Pd4xiv—Pd5—Pd6 | 117.36 (14) | Pd1xviii—Sn4—Pd3xviii | 57.70 (4) |
Pd7vii—Pd5—Pd6 | 103.40 (5) | Pd5xv—Sn4—Pd3xviii | 96.58 (4) |
Sn4xii—Pd5—Pd6 | 126.25 (10) | Pd6—Sn4—Pd5 | 62.73 (8) |
Pd6xii—Pd5—Pd6 | 179.50 (7) | Pd7vii—Sn4—Pd5 | 61.39 (8) |
Sn2—Pd5—Pd8ix | 59.68 (6) | Pd8xviii—Sn4—Pd5 | 146.72 (4) |
Sn5xii—Pd5—Pd8ix | 119.04 (5) | Pd4viii—Sn4—Pd5 | 129.67 (10) |
Sn3ix—Pd5—Pd8ix | 56.50 (7) | Pd2—Sn4—Pd5 | 58.18 (3) |
Sn3vii—Pd5—Pd8ix | 123.70 (7) | Pd7viii—Sn4—Pd5 | 121.64 (6) |
Pd2—Pd5—Pd8ix | 117.48 (10) | Pd1xviii—Sn4—Pd5 | 127.34 (9) |
Pd4xiv—Pd5—Pd8ix | 61.79 (6) | Pd5xv—Sn4—Pd5 | 96.82 (3) |
Pd7vii—Pd5—Pd8ix | 178.43 (9) | Pd3xviii—Sn4—Pd5 | 95.86 (4) |
Sn4xii—Pd5—Pd8ix | 54.16 (5) | Pd6—Sn5—Pd1xvii | 148.90 (6) |
Pd6xii—Pd5—Pd8ix | 104.12 (5) | Pd6—Sn5—Pd4viii | 67.13 (9) |
Pd6—Pd5—Pd8ix | 76.31 (9) | Pd1xvii—Sn5—Pd4viii | 108.52 (4) |
Sn2—Pd5—Sn4 | 100.70 (8) | Pd6—Sn5—Pd7 | 100.78 (4) |
Sn5xii—Pd5—Sn4 | 79.87 (5) | Pd1xvii—Sn5—Pd7 | 66.73 (10) |
Sn3ix—Pd5—Sn4 | 78.91 (8) | Pd4viii—Sn5—Pd7 | 149.46 (6) |
Sn3vii—Pd5—Sn4 | 100.63 (6) | Pd6—Sn5—Pd5xv | 64.05 (8) |
Pd2—Pd5—Sn4 | 58.94 (5) | Pd1xvii—Sn5—Pd5xv | 143.48 (12) |
Pd4xiv—Pd5—Sn4 | 121.17 (9) | Pd4viii—Sn5—Pd5xv | 62.38 (5) |
Pd7vii—Pd5—Sn4 | 53.93 (4) | Pd7—Sn5—Pd5xv | 139.46 (6) |
Sn4xii—Pd5—Sn4 | 179.39 (14) | Pd6—Sn5—Pd8viii | 87.99 (6) |
Pd6xii—Pd5—Sn4 | 126.50 (10) | Pd1xvii—Sn5—Pd8viii | 64.94 (5) |
Pd6—Pd5—Sn4 | 53.18 (6) | Pd4viii—Sn5—Pd8viii | 61.40 (4) |
Pd8ix—Pd5—Sn4 | 125.24 (13) | Pd7—Sn5—Pd8viii | 91.30 (5) |
Sn4—Pd6—Sn2 | 110.61 (9) | Pd5xv—Sn5—Pd8viii | 123.30 (7) |
Sn4—Pd6—Sn5 | 109.00 (8) | Pd6—Sn5—Pd3xvii | 140.17 (7) |
Sn2—Pd6—Sn5 | 139.69 (6) | Pd1xvii—Sn5—Pd3xvii | 61.14 (6) |
Sn4—Pd6—Pd9 | 154.46 (4) | Pd4viii—Sn5—Pd3xvii | 144.02 (11) |
Sn2—Pd6—Pd9 | 73.65 (6) | Pd7—Sn5—Pd3xvii | 62.41 (6) |
Sn5—Pd6—Pd9 | 73.96 (6) | Pd5xv—Sn5—Pd3xvii | 104.05 (4) |
Sn4—Pd6—Pd4 | 146.07 (6) | Pd8viii—Sn5—Pd3xvii | 125.70 (8) |
Sn2—Pd6—Pd4 | 73.51 (6) | Pd6—Sn5—Pd7ix | 80.39 (6) |
Sn5—Pd6—Pd4 | 69.63 (6) | Pd1xvii—Sn5—Pd7ix | 121.86 (8) |
Pd9—Pd6—Pd4 | 59.38 (5) | Pd4viii—Sn5—Pd7ix | 123.48 (8) |
Sn4—Pd6—Sn3viii | 88.76 (5) | Pd7—Sn5—Pd7ix | 78.91 (5) |
Sn2—Pd6—Sn3viii | 81.94 (5) | Pd5xv—Sn5—Pd7ix | 62.05 (6) |
Sn5—Pd6—Sn3viii | 91.82 (6) | Pd8viii—Sn5—Pd7ix | 163.04 (5) |
Pd9—Pd6—Sn3viii | 116.71 (6) | Pd3xvii—Sn5—Pd7ix | 61.63 (7) |
Pd4—Pd6—Sn3viii | 57.88 (6) | Pd6—Sn5—Pd4 | 56.77 (6) |
Sn4—Pd6—Sn3ix | 82.84 (4) | Pd1xvii—Sn5—Pd4 | 94.62 (5) |
Sn2—Pd6—Sn3ix | 94.90 (8) | Pd4viii—Sn5—Pd4 | 95.82 (4) |
Sn5—Pd6—Sn3ix | 97.05 (8) | Pd7—Sn5—Pd4 | 56.10 (7) |
Pd9—Pd6—Sn3ix | 71.64 (3) | Pd5xv—Sn5—Pd4 | 120.73 (11) |
Pd4—Pd6—Sn3ix | 131.01 (6) | Pd8viii—Sn5—Pd4 | 59.62 (4) |
Sn3viii—Pd6—Sn3ix | 169.38 (7) | Pd3xvii—Sn5—Pd4 | 118.48 (10) |
Sn4—Pd6—Pd5xv | 62.76 (5) | Pd7ix—Sn5—Pd4 | 103.49 (4) |
Symmetry codes: (i) x−1, y−1, z; (ii) x−y, −y+1, −z+1/3; (iii) x−y, −y, −z+1/3; (iv) −x+y, −x, z+1/3; (v) x−y−1, −y, −z+1/3; (vi) x−1, y, z; (vii) x, y−1, z; (viii) x−y+1, −y+1, −z+1/3; (ix) y, x, −z; (x) y−1, x−1, −z; (xi) −y, x−y, z−1/3; (xii) y, x−1, −z; (xiii) −x+y+1, −x+1, z+1/3; (xiv) −y+1, x−y, z−1/3; (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 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) |
V (Å3) | 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 diffractometer |
Absorption correction | Multi-scan (CrysAlis RED; Oxford Diffraction, 2009) |
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 (Å−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) |
Absolute structure parameter | −0.2 (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.
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