Abstract
Single crystals of the title compound, dipotassium aluminium tin(IV) tris[phosphate(V)], K2AlSn(PO4)3, were synthesized by a high temperature reaction in a platinum crucible. In the structure, the AlIII and SnIV atoms occupy the same site on a threefold rotation axis with occupational disorder in a 1:1 ratio. In the three-dimensional structure, Al/SnO6 octahedra and PO4 tetrahedra are interconnected via their vertices, yielding a [Al/SnP3O12]n framework. The K atoms (site symmetry 3) reside in the large cavities delimited by the [Al/SnP3O12]n framework, and are surrounded by 12 O atoms.
Related literature
For the mineral langbeinite, K2Mg2(SO4)3, see: Zemann & Zemann (1957 ▶). For related langbeinite-type compounds, see: Aatiq et al. (2006 ▶); Norberg (2002 ▶); Ogorodnyk et al. (2006 ▶); Orlova et al. (2003 ▶); Zatovsky et al. (2007 ▶); Zhao et al. (2009 ▶).
Experimental
Crystal data
K2AlSn(PO4)3
M r = 508.78
Cubic,
a = 9.7980 (8) Å
V = 940.62 (13) Å3
Z = 4
Mo Kα radiation
μ = 4.28 mm−1
T = 296 K
0.15 × 0.05 × 0.05 mm
Data collection
Bruker APEXII CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T min = 0.566, T max = 0.815
6146 measured reflections
811 independent reflections
782 reflections with I > 2σ(I)
R int = 0.065
Refinement
R[F 2 > 2σ(F 2)] = 0.029
wR(F 2) = 0.074
S = 1.18
811 reflections
59 parameters
Δρmax = 0.53 e Å−3
Δρmin = −0.60 e Å−3
Absolute structure: Flack (1983 ▶), 340 Friedel pairs
Flack parameter: −0.05 (7)
Data collection: APEX2 (Bruker, 2008 ▶); cell refinement: SAINT (Bruker, 2008 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: SHELXTL (Sheldrick, 2008 ▶); software used to prepare material for publication: SHELXTL.
Supplementary Material
Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536811037263/fi2112sup1.cif
Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536811037263/fi2112Isup2.hkl
Additional supplementary materials: crystallographic information; 3D view; checkCIF report
Acknowledgments
The authors acknowledge the Doctoral Foundation of Henan Polytechnic University (grant No. B2010–92, 648483).
supplementary crystallographic information
Comment
Langbeinite-type (K2Mg2(SO4)3, Zemann & Zemann, 1957) compounds with the simplest generic formula A2B2(XO4)3 are an important and well studied family of inorganic solids with respect to minerals. Among Langbeinite-based phosphates, whose coordination networks are based on [M2(PO4)3] fragments, may result in diverse structure types due to the 'M2' sites occupied by various types of tetravalent and bi- or trivalent metal pairs. For example, the structures K2MTi(PO4)3(M = Y, Yb, Er) (Norberg, 2002), K2FeZr(PO4)3 (Orlova et al., 2003), K2MSn(PO4)3 (M = Fe, Yb) (Aatiq et al., 2006), K2AlTi(PO4)3 (Zhao et al., 2009), K2FeSn(PO4)3 (Zatovsky et al., 2007) and K2Mn0.5Ti1.5(PO4)3 (Ogorodnyk et al., 2006), have been reported. Herein we report the single-crystal growth and structure investigation of title compound K2AlSn(PO4)3.
In the structure of title compound, K, Al and Sn atoms lie on the 3-fold rotation axes in 4a positions, while P and O atoms are located at general 12b positions. Due to the similar ionic radii of Al and Sn atoms, they occupy the same sites in a substituent disordered manner, denoted as M atoms. The three-dimensional structure contains MO6 octahedra and PO4 tetrahedra which are connected via vertices. Two nearest [MO6] octahedra are joined to each other by three bridging orthophosphate tetrahedra forming [Al/SnP3O12]n framework, which penetrate with large closed cavities. Two independent potassium atoms are located in each cavity. K1 and K2 atoms are 12-coordinated by O atoms.
Experimental
Single crystals of K2AlSn(PO4)3 have been prepared by a high-temperature method in air. A powder mixture of K2CO3, Al2O3, SnO2 and NH4H2PO4 in the molar ratio of K: Al: Sn: P = 10: 1:: 1 15 was first ground in an agate mortar and then transferred to a platinum crucible. The sample was gradually heated in air at 1173 K for 24 h. After that, the intermediate product was slowly cooled to 673 K at the rate of 2 K h-1. It was kept at 673 K for another 10 h and then quenched to room temperature. The obtained crystals were colorless with a prismatic shape.
Refinement
The atomic position and anisotropic displacement parameters of Al and Sn in the same sites were constrained to be identical, and the Al/Sn disorder with a relative occupancy of 1/1. The highest peak in the difference electron density map equals to 0.53 e/Å3 at the distance of 1.09 Å from Al2/Sn2 site while the deepest hole equals to -0.60 e/Å3 at the distance of 1.78 Å from K2 site.
Figures
Fig. 1.
A view of the asymmetric unit of K2AlSn(PO4)3 showing the coordination environments of the P and Al/Sn atoms.. Displacement ellipsoids are drawn at the 50% probability level. [Symmetry codes: (i) -x + 1, y + 1/2, -z + 1/2; (ii) z, x, y; (iii) -y + 1/2, -z + 1, x - 1/2; (iv) -z + 1/2, -x + 1, y - 1/2; (v) -y + 1, z + 1/2, -x + 1/2; (viii) y, z, x; (ix) -z, x - 1/2, -y + 1/2; (x) -y + 1/2, -z, x - 1/2; (xi) x - 1/2, -y + 1/2, -z.]
Fig. 2.
View of the crystal structure of K2AlSn(PO4)3 along [010]. PO4 and Al/SnO6 units are given in the polyhedral representation.
Crystal data
| K2AlSn(PO4)3 | Dx = 3.593 Mg m−3 |
| Mr = 508.78 | Mo Kα radiation, λ = 0.71073 Å |
| Cubic, P213 | Cell parameters from 2030 reflections |
| Hall symbol: P 2ac 2ab 3 | θ = 3.6–28.5° |
| a = 9.7980 (8) Å | µ = 4.28 mm−1 |
| V = 940.62 (13) Å3 | T = 296 K |
| Z = 4 | Prism, colourless |
| F(000) = 968 | 0.15 × 0.05 × 0.05 mm |
Data collection
| Bruker SMART APEXII CCD area-detector diffractometer | 811 independent reflections |
| Radiation source: fine-focus sealed tube | 782 reflections with I > 2σ(I) |
| graphite | Rint = 0.065 |
| Detector resolution: 83.33 pixels mm-1 | θmax = 28.5°, θmin = 2.9° |
| ω scans | h = −13→6 |
| Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | k = −12→12 |
| Tmin = 0.566, Tmax = 0.815 | l = −12→10 |
| 6146 measured reflections |
Refinement
| Refinement on F2 | Secondary atom site location: difference Fourier map |
| Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.0208P)2 + 3.2535P] where P = (Fo2 + 2Fc2)/3 |
| R[F2 > 2σ(F2)] = 0.029 | (Δ/σ)max < 0.001 |
| wR(F2) = 0.074 | Δρmax = 0.53 e Å−3 |
| S = 1.18 | Δρmin = −0.60 e Å−3 |
| 811 reflections | Extinction correction: SHELXTL (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
| 59 parameters | Extinction coefficient: 0.0076 (10) |
| 0 restraints | Absolute structure: Flack (1983), 340 Friedel pairs |
| Primary atom site location: structure-invariant direct methods | Flack parameter: −0.05 (7) |
Special details
| Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
| Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2)
| x | y | z | Uiso*/Ueq | Occ. (<1) | |
| Sn1 | 0.39682 (6) | 0.60318 (6) | 0.10318 (6) | 0.0091 (2) | 0.50 |
| Sn2 | 0.16412 (6) | 0.16412 (6) | 0.16412 (6) | 0.0104 (2) | 0.50 |
| Al1 | 0.39682 (6) | 0.60318 (6) | 0.10318 (6) | 0.0091 (2) | 0.50 |
| Al2 | 0.16412 (6) | 0.16412 (6) | 0.16412 (6) | 0.0104 (2) | 0.50 |
| P1 | 0.47928 (15) | 0.29006 (15) | 0.12495 (15) | 0.0133 (3) | |
| K1 | 0.18221 (14) | 0.81779 (14) | 0.31779 (14) | 0.0268 (5) | |
| K2 | 0.54175 (17) | −0.04175 (17) | 0.04175 (17) | 0.0305 (6) | |
| O1 | 0.3329 (4) | 0.2484 (4) | 0.1004 (5) | 0.0231 (9) | |
| O2 | 0.4861 (4) | 0.4378 (4) | 0.1734 (5) | 0.0198 (9) | |
| O3 | 0.5491 (5) | 0.1991 (4) | 0.2297 (4) | 0.0214 (9) | |
| O4 | 0.5569 (5) | 0.2684 (5) | −0.0094 (5) | 0.0276 (11) |
Atomic displacement parameters (Å2)
| U11 | U22 | U33 | U12 | U13 | U23 | |
| Sn1 | 0.0091 (2) | 0.0091 (2) | 0.0091 (2) | 0.0000 (2) | 0.0000 (2) | 0.0000 (2) |
| Sn2 | 0.0104 (2) | 0.0104 (2) | 0.0104 (2) | −0.0010 (2) | −0.0010 (2) | −0.0010 (2) |
| Al1 | 0.0091 (2) | 0.0091 (2) | 0.0091 (2) | 0.0000 (2) | 0.0000 (2) | 0.0000 (2) |
| Al2 | 0.0104 (2) | 0.0104 (2) | 0.0104 (2) | −0.0010 (2) | −0.0010 (2) | −0.0010 (2) |
| P1 | 0.0142 (7) | 0.0131 (7) | 0.0126 (7) | 0.0002 (5) | −0.0001 (5) | 0.0010 (5) |
| K1 | 0.0268 (5) | 0.0268 (5) | 0.0268 (5) | 0.0031 (6) | 0.0031 (6) | −0.0031 (6) |
| K2 | 0.0305 (6) | 0.0305 (6) | 0.0305 (6) | 0.0013 (6) | −0.0013 (6) | 0.0013 (6) |
| O1 | 0.016 (2) | 0.024 (2) | 0.030 (2) | −0.0048 (18) | −0.006 (2) | 0.0024 (19) |
| O2 | 0.021 (2) | 0.014 (2) | 0.025 (2) | −0.0009 (16) | −0.0065 (19) | −0.0067 (17) |
| O3 | 0.025 (2) | 0.021 (2) | 0.018 (2) | −0.0001 (18) | −0.0077 (18) | 0.0088 (18) |
| O4 | 0.038 (3) | 0.028 (3) | 0.017 (2) | 0.007 (2) | 0.011 (2) | 0.003 (2) |
Geometric parameters (Å, °)
| Sn1—O3i | 1.961 (4) | K1—O4xii | 3.011 (6) |
| Sn1—O3ii | 1.961 (4) | K1—O4xi | 3.011 (6) |
| Sn1—O3iii | 1.961 (4) | K1—O4ii | 3.208 (5) |
| Sn1—O2iv | 1.966 (4) | K1—O4i | 3.208 (5) |
| Sn1—O2v | 1.966 (4) | K1—O4iii | 3.208 (5) |
| Sn1—O2 | 1.966 (4) | K2—O2xiii | 2.811 (5) |
| Sn2—O1 | 1.951 (4) | K2—O2xiv | 2.811 (5) |
| Sn2—O1ii | 1.951 (4) | K2—O2xv | 2.811 (5) |
| Sn2—O1vi | 1.951 (4) | K2—O3ix | 2.994 (5) |
| Sn2—O4vii | 1.960 (5) | K2—O3xvi | 2.994 (5) |
| Sn2—O4viii | 1.960 (5) | K2—O3 | 2.994 (5) |
| Sn2—O4ix | 1.960 (5) | K2—O4xvi | 3.084 (5) |
| P1—O1 | 1.511 (4) | K2—O4ix | 3.084 (5) |
| P1—O2 | 1.525 (4) | K2—O4 | 3.084 (5) |
| P1—O3 | 1.521 (4) | O1—K1xvii | 2.847 (5) |
| P1—O4 | 1.535 (5) | O2—K2xviii | 2.811 (5) |
| K1—O1x | 2.847 (5) | O3—Al1vi | 1.961 (4) |
| K1—O1xi | 2.847 (5) | O3—Sn1vi | 1.961 (4) |
| K1—O1xii | 2.847 (5) | O3—K1vi | 2.915 (5) |
| K1—O3ii | 2.916 (5) | O4—Al2xvi | 1.960 (5) |
| K1—O3iii | 2.916 (5) | O4—Sn2xvi | 1.960 (5) |
| K1—O3i | 2.916 (5) | O4—K1xvii | 3.011 (6) |
| K1—O4x | 3.011 (6) | O4—K1vi | 3.208 (5) |
| O3i—Sn1—O3ii | 87.42 (19) | O4x—K1—O4xii | 86.48 (14) |
| O3i—Sn1—O3iii | 87.42 (19) | O1x—K1—O4xi | 52.14 (13) |
| O3ii—Sn1—O3iii | 87.42 (19) | O1xi—K1—O4xi | 49.38 (13) |
| O3i—Sn1—O2iv | 175.0 (2) | O1xii—K1—O4xi | 114.88 (15) |
| O3ii—Sn1—O2iv | 89.00 (17) | O3ii—K1—O4xi | 132.86 (13) |
| O3iii—Sn1—O2iv | 88.90 (18) | O3iii—K1—O4xi | 95.45 (12) |
| O3i—Sn1—O2v | 88.90 (19) | O3i—K1—O4xi | 140.66 (13) |
| O3ii—Sn1—O2v | 175.0 (2) | O4x—K1—O4xi | 86.48 (14) |
| O3iii—Sn1—O2v | 89.00 (17) | O4xii—K1—O4xi | 86.48 (14) |
| O2iv—Sn1—O2v | 94.46 (18) | O1x—K1—O4ii | 156.33 (13) |
| O3i—Sn1—O2 | 88.99 (17) | O1xi—K1—O4ii | 55.82 (12) |
| O3ii—Sn1—O2 | 88.90 (18) | O1xii—K1—O4ii | 86.26 (12) |
| O3iii—Sn1—O2 | 175.0 (2) | O3ii—K1—O4ii | 46.65 (11) |
| O2iv—Sn1—O2 | 94.46 (18) | O3iii—K1—O4ii | 88.29 (13) |
| O2v—Sn1—O2 | 94.45 (18) | O3i—K1—O4ii | 100.74 (13) |
| O3i—Sn1—K1 | 52.93 (13) | O4x—K1—O4ii | 136.85 (10) |
| O3ii—Sn1—K1 | 52.93 (13) | O4xii—K1—O4ii | 53.57 (17) |
| O3iii—Sn1—K1 | 52.93 (13) | O4xi—K1—O4ii | 104.39 (2) |
| O2iv—Sn1—K1 | 122.05 (13) | O1x—K1—O4i | 86.26 (12) |
| O2v—Sn1—K1 | 122.05 (13) | O1xi—K1—O4i | 156.33 (13) |
| O2—Sn1—K1 | 122.05 (13) | O1xii—K1—O4i | 55.82 (12) |
| O3i—Sn1—K2ii | 129.38 (14) | O3ii—K1—O4i | 88.29 (13) |
| O3ii—Sn1—K2ii | 51.14 (14) | O3iii—K1—O4i | 100.74 (13) |
| O3iii—Sn1—K2ii | 66.00 (13) | O3i—K1—O4i | 46.65 (11) |
| O2iv—Sn1—K2ii | 45.73 (13) | O4x—K1—O4i | 53.57 (17) |
| O2v—Sn1—K2ii | 130.02 (13) | O4xii—K1—O4i | 104.39 (3) |
| O2—Sn1—K2ii | 114.01 (13) | O4xi—K1—O4i | 136.85 (10) |
| K1—Sn1—K2ii | 77.229 (18) | O4ii—K1—O4i | 115.74 (6) |
| O3i—Sn1—K2xix | 66.00 (13) | O1x—K1—O4iii | 55.82 (12) |
| O3ii—Sn1—K2xix | 129.38 (14) | O1xi—K1—O4iii | 86.26 (12) |
| O3iii—Sn1—K2xix | 51.14 (14) | O1xii—K1—O4iii | 156.33 (13) |
| O2iv—Sn1—K2xix | 114.01 (13) | O3ii—K1—O4iii | 100.74 (13) |
| O2v—Sn1—K2xix | 45.73 (13) | O3iii—K1—O4iii | 46.65 (11) |
| O2—Sn1—K2xix | 130.02 (13) | O3i—K1—O4iii | 88.29 (13) |
| K1—Sn1—K2xix | 77.229 (18) | O4x—K1—O4iii | 104.39 (2) |
| K2ii—Sn1—K2xix | 115.259 (13) | O4xii—K1—O4iii | 136.85 (10) |
| O3i—Sn1—K2xviii | 51.14 (14) | O4xi—K1—O4iii | 53.57 (17) |
| O3ii—Sn1—K2xviii | 66.00 (13) | O4ii—K1—O4iii | 115.74 (6) |
| O3iii—Sn1—K2xviii | 129.38 (14) | O4i—K1—O4iii | 115.74 (6) |
| O2iv—Sn1—K2xviii | 130.02 (13) | O2xiii—K2—O2xiv | 91.85 (14) |
| O2v—Sn1—K2xviii | 114.01 (13) | O2xiii—K2—O2xv | 91.85 (14) |
| O2—Sn1—K2xviii | 45.73 (13) | O2xiv—K2—O2xv | 91.85 (14) |
| K1—Sn1—K2xviii | 77.229 (18) | O2xiii—K2—O3ix | 147.18 (15) |
| K2ii—Sn1—K2xviii | 115.259 (13) | O2xiv—K2—O3ix | 56.50 (11) |
| K2xix—Sn1—K2xviii | 115.259 (13) | O2xv—K2—O3ix | 81.71 (12) |
| O1—Sn2—O1ii | 92.8 (2) | O2xiii—K2—O3xvi | 56.50 (11) |
| O1—Sn2—O1vi | 92.8 (2) | O2xiv—K2—O3xvi | 81.71 (12) |
| O1ii—Sn2—O1vi | 92.8 (2) | O2xv—K2—O3xvi | 147.18 (15) |
| O1—Sn2—O4vii | 93.7 (2) | O3ix—K2—O3xvi | 119.27 (3) |
| O1ii—Sn2—O4vii | 82.5 (2) | O2xiii—K2—O3 | 81.71 (12) |
| O1vi—Sn2—O4vii | 172.2 (2) | O2xiv—K2—O3 | 147.18 (15) |
| O1—Sn2—O4viii | 172.2 (2) | O2xv—K2—O3 | 56.50 (11) |
| O1ii—Sn2—O4viii | 93.7 (2) | O3ix—K2—O3 | 119.27 (3) |
| O1vi—Sn2—O4viii | 82.5 (2) | O3xvi—K2—O3 | 119.27 (3) |
| O4vii—Sn2—O4viii | 91.5 (2) | O2xiii—K2—O4xvi | 103.66 (12) |
| O1—Sn2—O4ix | 82.5 (2) | O2xiv—K2—O4xvi | 82.44 (13) |
| O1ii—Sn2—O4ix | 172.2 (2) | O2xv—K2—O4xvi | 163.58 (13) |
| O1vi—Sn2—O4ix | 93.7 (2) | O3ix—K2—O4xvi | 82.31 (13) |
| O4vii—Sn2—O4ix | 91.5 (2) | O3xvi—K2—O4xvi | 47.30 (12) |
| O4viii—Sn2—O4ix | 91.5 (2) | O3—K2—O4xvi | 130.38 (15) |
| O1—Sn2—K1xx | 128.15 (13) | O2xiii—K2—O4ix | 163.58 (13) |
| O1ii—Sn2—K1xx | 49.01 (14) | O2xiv—K2—O4ix | 103.66 (12) |
| O1vi—Sn2—K1xx | 118.40 (13) | O2xv—K2—O4ix | 82.44 (13) |
| O4vii—Sn2—K1xx | 53.89 (16) | O3ix—K2—O4ix | 47.30 (12) |
| O4viii—Sn2—K1xx | 59.65 (16) | O3xvi—K2—O4ix | 130.38 (15) |
| O4ix—Sn2—K1xx | 130.31 (15) | O3—K2—O4ix | 82.31 (13) |
| O1—Sn2—K1xxi | 118.40 (13) | O4xvi—K2—O4ix | 83.98 (16) |
| O1ii—Sn2—K1xxi | 128.15 (13) | O2xiii—K2—O4 | 82.44 (13) |
| O1vi—Sn2—K1xxi | 49.01 (14) | O2xiv—K2—O4 | 163.58 (13) |
| O4vii—Sn2—K1xxi | 130.31 (15) | O2xv—K2—O4 | 103.66 (12) |
| O4viii—Sn2—K1xxi | 53.89 (16) | O3ix—K2—O4 | 130.38 (15) |
| O4ix—Sn2—K1xxi | 59.65 (16) | O3xvi—K2—O4 | 82.31 (13) |
| K1xx—Sn2—K1xxi | 113.210 (15) | O3—K2—O4 | 47.30 (12) |
| O1—Sn2—K1xvii | 49.01 (14) | O4xvi—K2—O4 | 83.98 (16) |
| O1ii—Sn2—K1xvii | 118.40 (13) | O4ix—K2—O4 | 83.98 (16) |
| O1vi—Sn2—K1xvii | 128.15 (13) | O2xiii—K2—P1 | 93.94 (9) |
| O4vii—Sn2—K1xvii | 59.65 (16) | O2xiv—K2—P1 | 169.50 (10) |
| O4viii—Sn2—K1xvii | 130.31 (15) | O2xv—K2—P1 | 79.23 (9) |
| O4ix—Sn2—K1xvii | 53.89 (16) | O3ix—K2—P1 | 116.07 (10) |
| K1xx—Sn2—K1xvii | 113.210 (15) | O3xvi—K2—P1 | 108.78 (10) |
| K1xxi—Sn2—K1xvii | 113.210 (15) | O3—K2—P1 | 26.50 (8) |
| O1—P1—O2 | 110.3 (3) | O4xvi—K2—P1 | 104.63 (13) |
| O1—P1—O3 | 112.1 (3) | O4ix—K2—P1 | 69.91 (10) |
| O2—P1—O3 | 109.1 (3) | O4—K2—P1 | 26.76 (9) |
| O1—P1—O4 | 107.2 (3) | O2xiii—K2—P1ix | 169.50 (10) |
| O2—P1—O4 | 112.1 (3) | O2xiv—K2—P1ix | 79.23 (9) |
| O3—P1—O4 | 105.9 (3) | O2xv—K2—P1ix | 93.94 (9) |
| O1—P1—K1vi | 168.93 (19) | O3ix—K2—P1ix | 26.50 (8) |
| O2—P1—K1vi | 80.16 (17) | O3xvi—K2—P1ix | 116.07 (10) |
| O3—P1—K1vi | 59.55 (18) | O3—K2—P1ix | 108.78 (10) |
| O4—P1—K1vi | 70.5 (2) | O4xvi—K2—P1ix | 69.91 (10) |
| O1—P1—K2 | 82.78 (18) | O4ix—K2—P1ix | 26.76 (9) |
| O2—P1—K2 | 166.53 (19) | O4—K2—P1ix | 104.63 (13) |
| O3—P1—K2 | 61.42 (18) | P1—K2—P1ix | 95.73 (6) |
| O4—P1—K2 | 64.79 (19) | O2xiii—K2—P1xvi | 79.23 (9) |
| K1vi—P1—K2 | 86.56 (5) | O2xiv—K2—P1xvi | 93.94 (9) |
| O1—P1—K1xvii | 50.43 (19) | O2xv—K2—P1xvi | 169.50 (10) |
| O2—P1—K1xvii | 124.36 (19) | O3ix—K2—P1xvi | 108.78 (10) |
| O3—P1—K1xvii | 126.57 (19) | O3xvi—K2—P1xvi | 26.50 (8) |
| O4—P1—K1xvii | 56.9 (2) | O3—K2—P1xvi | 116.07 (10) |
| K1vi—P1—K1xvii | 126.95 (5) | O4xvi—K2—P1xvi | 26.76 (9) |
| K2—P1—K1xvii | 66.07 (6) | O4ix—K2—P1xvi | 104.63 (13) |
| O1—P1—K2xviii | 102.1 (2) | O4—K2—P1xvi | 69.91 (10) |
| O2—P1—K2xviii | 45.40 (18) | P1—K2—P1xvi | 95.73 (6) |
| O3—P1—K2xviii | 71.80 (18) | P1ix—K2—P1xvi | 95.73 (6) |
| O4—P1—K2xviii | 148.7 (2) | P1—O1—Sn2 | 150.2 (3) |
| K1vi—P1—K2xviii | 82.58 (4) | P1—O1—K1xvii | 105.4 (2) |
| K2—P1—K2xviii | 130.74 (6) | Sn2—O1—K1xvii | 99.85 (17) |
| K1xvii—P1—K2xviii | 149.53 (5) | P1—O2—Sn1 | 130.9 (3) |
| O1x—K1—O1xi | 100.53 (12) | P1—O2—K2xviii | 111.9 (2) |
| O1x—K1—O1xii | 100.53 (12) | Sn1—O2—K2xviii | 104.22 (16) |
| O1xi—K1—O1xii | 100.53 (12) | P1—O3—Al1vi | 164.9 (3) |
| O1x—K1—O3ii | 149.59 (14) | P1—O3—Sn1vi | 164.9 (3) |
| O1xi—K1—O3ii | 96.38 (13) | Al1vi—O3—Sn1vi | 0.00 (5) |
| O1xii—K1—O3ii | 100.99 (13) | P1—O3—K1vi | 93.7 (2) |
| O1x—K1—O3iii | 96.38 (13) | Al1vi—O3—K1vi | 94.60 (17) |
| O1xi—K1—O3iii | 100.99 (13) | Sn1vi—O3—K1vi | 94.60 (17) |
| O1xii—K1—O3iii | 149.59 (14) | P1—O3—K2 | 92.1 (2) |
| O3ii—K1—O3iii | 55.40 (14) | Al1vi—O3—K2 | 98.18 (17) |
| O1x—K1—O3i | 100.99 (13) | Sn1vi—O3—K2 | 98.18 (17) |
| O1xi—K1—O3i | 149.59 (14) | K1vi—O3—K2 | 103.77 (14) |
| O1xii—K1—O3i | 96.38 (13) | P1—O4—Al2xvi | 152.0 (3) |
| O3ii—K1—O3i | 55.40 (14) | P1—O4—Sn2xvi | 152.0 (3) |
| O3iii—K1—O3i | 55.40 (14) | Al2xvi—O4—Sn2xvi | 0.000 (18) |
| O1x—K1—O4x | 49.38 (13) | P1—O4—K1xvii | 97.8 (2) |
| O1xi—K1—O4x | 114.88 (15) | Al2xvi—O4—K1xvii | 94.39 (18) |
| O1xii—K1—O4x | 52.14 (13) | Sn2xvi—O4—K1xvii | 94.39 (18) |
| O3ii—K1—O4x | 140.66 (13) | P1—O4—K2 | 88.5 (2) |
| O3iii—K1—O4x | 132.86 (13) | Al2xvi—O4—K2 | 118.9 (2) |
| O3i—K1—O4x | 95.45 (12) | Sn2xvi—O4—K2 | 118.9 (2) |
| O1x—K1—O4xii | 114.88 (15) | K1xvii—O4—K2 | 77.14 (14) |
| O1xi—K1—O4xii | 52.14 (13) | P1—O4—K1vi | 82.7 (2) |
| O1xii—K1—O4xii | 49.38 (13) | Al2xvi—O4—K1vi | 88.54 (19) |
| O3ii—K1—O4xii | 95.45 (12) | Sn2xvi—O4—K1vi | 88.54 (19) |
| O3iii—K1—O4xii | 140.66 (13) | K1xvii—O4—K1vi | 172.37 (18) |
| O3i—K1—O4xii | 132.86 (12) | K2—O4—K1vi | 95.27 (14) |
Symmetry codes: (i) −x+1, y+1/2, −z+1/2; (ii) z, x, y; (iii) −y+1/2, −z+1, x−1/2; (iv) −z+1/2, −x+1, y−1/2; (v) −y+1, z+1/2, −x+1/2; (vi) y, z, x; (vii) x−1/2, −y+1/2, −z; (viii) −z, x−1/2, −y+1/2; (ix) −y+1/2, −z, x−1/2; (x) y, z+1, x; (xi) −z, x+1/2, −y+1/2; (xii) −x+1/2, −y+1, z+1/2; (xiii) −z+1, x−1/2, −y+1/2; (xiv) −y+1, z−1/2, −x+1/2; (xv) −x+1, y−1/2, −z+1/2; (xvi) z+1/2, −x+1/2, −y; (xvii) z, x, y−1; (xviii) −z+1/2, −x+1, y+1/2; (xix) x, y+1, z; (xx) y−1, z, x; (xxi) x, y−1, z.
Footnotes
Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: FI2112).
References
- Aatiq, A., Haggouch, B., Bakri, R., Lakhdar, Y. & Saadoune, I. (2006). Powder Diffr. 21, 214–219.
- Bruker (2008). APEX2 and SAINT Bruker AXS Inc., Madison, Wisconsin, USA.
- Flack, H. D. (1983). Acta Cryst. A39, 876–881.
- Norberg, S. T. (2002). Acta Cryst. B58, 743–749. [DOI] [PMC free article] [PubMed]
- Ogorodnyk, I. V., Zatovsky, I. V., Slobodyanik, N. S., Baumer, V. N. & Shishkin, O. V. (2006). J. Solid State Chem. 179, 3461–3466.
- Orlova, A. I., Trubach, I. G., Kurazhkovskaya, V. S., Pertierra, P., Salvado, M. A., Garcia-Granda, S., Khainakov, S. A. & Garcia, J. R. (2003). J. Solid State Chem. 173, 314–318.
- Sheldrick, G. M. (1996). SADABS University of Göttingen, Germany.
- Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. [DOI] [PubMed]
- Zatovsky, I. V., Yatskin, M. M., Baumer, V. N., Slobodyanik, N. S. & Shishkin, O. V. (2007). Acta Cryst. E63, i199.
- Zemann, A. & Zemann, J. (1957). Acta Cryst. 10, 409–413.
- Zhao, D., Zhang, H., Huang, S. P., Zhang, W. L., Yang, S. L. & Cheng, W. D. (2009). J. Alloys Compd, 477, 795–799.
Associated Data
This section collects any data citations, data availability statements, or supplementary materials included in this article.
Supplementary Materials
Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536811037263/fi2112sup1.cif
Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536811037263/fi2112Isup2.hkl
Additional supplementary materials: crystallographic information; 3D view; checkCIF report