research communications
The layer silicate Cs2SnIVSi6O15
aInstitute for Chemical Technologies and Analytics, Division of Structural Chemistry, TU Wien, Getreidemarkt 9/164-SC, A-1060 Vienna, Austria
*Correspondence e-mail: matthias.weil@tuwien.ac.at
Single crystals of Cs2SnSi6O15, dicaesium tin(IV) hexasilicate, were serendipitously obtained from a CsCl/NaCl at 923 K, starting from mixtures of CaO, SnO and TeO2 in a closed silica ampoule. The of Cs2SnSi6O15 is constructed from {Si6O15}6– layers extending parallel to (101), and CsI cations with a of eleven as well as isolated [SnO6] octahedra situated between the silicate layers. Each of the nine different SiO4 tetrahedra in the silicate layer has a connectedness of Q3 (three bridging and one terminal O atom), which leads to the formation of five- and eight-membered rings. The same type of silicate layer is found in the of the mineral zeravshanite. Comparison with other silicates of the type Cs2MIVSi6O15 (MIV = Ti, Zr, Th, U) revealed a klassengleiche group–subgroup relationship of index 2 between Cs2ZrSi6O15 (Z = 6, C2/m) and Cs2SnSi6O15 (Z = 12, I2/c).
Keywords: crystal structure; group-subgroup relation; caesium; tin; silicates.
CCDC reference: 2130669
1. Chemical context
Calcium oxotellurate(IV), CaTeO3, is known to exist in various polymorphic forms that can be obtained either through solid-state reactions (Trömel & Ziethen-Reichenach, 1970; Stöger et al., 2009) or under hydrothermal conditions and subsequent dehydration (Poupon et al., 2015). Some of the CaTeO3 polymorphs have a non-centrosymmetric and show ferroelectric behaviour (Rai et al., 2002) or a second harmonic generation (SHG) effect (Poupon et al., 2015). These features are thought to be related to the presence of the 5s2 electron lone pair at the TeIV atom. In a current study it was attempted to incorporate SnII into CaTeO3 under formation of solid solutions (Ca1-xSnx)TeO3 in order to investigate whether the 5s2 electron lone pair at the SnII atom has any influence on the ferroelectric or SHG characteristics. For that purpose, a medium consisting of a eutectic CsCl/NaCl mixture with a melting point of 766 K (Żemcżużny & Rambach, 1909) was chosen as reaction medium in a closed silica ampoule. In comparison with conventional ceramic routes, this allows the lowering of the reaction temperatures by a simultaneous increase of the diffusion pathways. However, neither the intended (Ca1-xSnx)TeO3 solid solutions nor other calcium oxotellurates with a partial replacement of CaII by SnII could be prepared this way. One of the side products of this reaction was Cs2SnIVSi6O15, which had formed through attack of the silica glass ampoule by the molten salt mixture and concomitant oxidation of SnII to SnIV. Its along with a structural comparison with other silicates is given here.
2. Structural commentary
The 2SnSi6O15 comprises three Cs, two Sn, nine Si and twenty-three O sites. Except for one Sn site (Sn2) and one O site (O23), which are located on Wyckoff positions 4b (site symmetry ) and 4e (site symmetry 2), respectively, all atoms are on general positions. The of Cs2SnSi6O15 can be described as being built up from silicate layers extending parallel to (101). The silicate layers are linked by caesium cations and isolated [SnO6] octahedra situated between adjacent silicate layers (Fig. 1).
of CsEach of the three caesium cations exhibits a 11] polyhedra (Cs1: 3.312 Å; Cs2: 3.355 Å; Cs3: 3.342 Å) are in very good agreement with the overall mean Cs—O bond length of 3.333 (226) Å calculated from 748 bonds for 11-coordinate Cs (Gagné & Hawthorne, 2016). The two SnIV atoms show slight deviations from a regular octahedral coordination, with Sn—O bond lengths ranging from 2.031 (3) to 2.058 (3) Å. The overall mean SnIV—O bond length of 2.054 (10) Å calculated from 32 bonds (Gagné & Hawthorne, 2018) is somewhat longer than the mean values for Sn1 (2.037 Å) and Sn2 (2.047 Å).
of 11, with Cs—O bond lengths ranging from 2.951 (3) to 3.748 (3) Å. The mean Cs—O bond lengths for the three individual [CsOAll of the nine SiO4 tetrahedra in the {Si6O15}6– layer have one terminal O atom and are linked to three other SiO4 tetrahedra by common bridging O atoms. Thus, the connectedness of the silicate tetrahedra is Q3 according to the notation of Liebau (1985). The bond lengths distribution in the SiO4 tetrahedra reflects the different roles of the O atoms in the silicate layer. The Si—O bonds to terminal O atoms are shorter by about 0.03 Å (mean 1.588 Å) than those to bridging O atoms (1.621 Å). The total mean Si—O bond in Cs2SnSi6O15 has a value of 1.613 Å, which is slightly shorter than the overall mean of 1.625 (24) calculated from 9128 bonds (Gagné & Hawthorne, 2018). The connectedness of the SiO4 tetrahedra leads to the formation of a {Si6O15}6– layer comprising five- and eight-membered rings (Fig. 2). The same type of silicate layer is found in the mineral zeravshanite with composition (Cs3.80Na0.18K0.02)Na2(Zr2.73Ti0.19Sn0.04Fe0.04)(Si18O45)(H2O)2 (Uvarova et al., 2004).
Crystal-chemical features of silicates comprising the {Si6O15}6– anion were recently compiled by Wierzbicka-Wieczorek et al. (2015). A topological classification of zirconosilicates and their analogues, where the simplest structure units are [MO6] octahedra and TO4 tetrahedra united by vertices, was reported some time ago by Ilyushin & Blatov (2002). Since the same structure elements are also present in Cs2SnSi6O15 in the form of [SnO6] octahedra and SiO4 tetrahedra, a similar analysis can be made. With respect to the concept of the polyhedral microensemble (PME) introduced by Ilyushin & Blatov (2002), Cs2SnSi6O15 conforms to the PME type C-1. A comparison of the unit-cell parameters of Cs2SnSi6O15 with those of the other reported Cs2MIVSi6O15 (MIV = Ti, Zr, Th, U) compounds (Table 1) revealed a close relationship between the Sn- and Zr-containing phases. The a and b axes and the β angle in the two structures are very similar, and the c axis of the Sn-containing compound is doubled. Indeed, there is a group–subgroup relationship between the crystal structures of Cs2ZrSi6O15 and Cs2SnSi6O15. The Sn-containing phase crystallizes in a (I2/c; Z = 12) of the Zr-containing phase (C2/m; Z = 6), defining a klassengleiche relationship of index 2 (Müller, 2013).
3. Synthesis and crystallization
1.2 mmol of CaO (0.067 g), 0.13 mmol SnO (0.018 g) and 1.3 mmol of TeO2 (0.207 g) were intimately mixed with 1 g of an NaCl (35 mol%):CsCl (65 mol%) mixture and filled in a silica ampoule that was subsequently evacuated and torch-sealed. The ampoule was then heated at 923 K for 2 d before the power of the furnace was switched off. The silica ampoule showed a severe attack from the halide but was still intact. After washing the recrystallized with several portions of warm water and drying the remaining solid in air, a few lath-shaped crystals of the title compound could be isolated under a polarizing microscope. Single-crystal diffraction of other selected crystals revealed α-CaTeO3 (Stöger et al., 2009), CaTe2O5 (Weil & Stöger, 2008) and Ca4Te5O14 (Weil, 2004) as products. Powder X-ray diffraction of the bulk showed the reflections of these phases together with those of SnO2 and also some reflections of non-assignable phase(s).
4. Refinement
Crystal data, data collection and structure . For better comparison of Cs2SnSi6O15 with the of Cs2ZrSi6O15, the unconventional setting I2/c of type C2/c (No. 15) was chosen, so that unit-cell parameters a, b, c and β of the Sn-containing phase correspond to a, b, 2c and β of the Zr-containing phase (Jolicart et al., 1996; Table 1). The Cs3 atom in Cs2SnSi6O15 was found to be disordered over two sites in a 0.934 (5):0.066 ratio and was refined with common displacement parameters for the two sites (A and B).
details are summarized in Table 2
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Supporting information
CCDC reference: 2130669
https://doi.org/10.1107/S2056989021013554/pk2660sup1.cif
contains datablock I. DOI:Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S2056989021013554/pk2660Isup2.hkl
Data collection: APEX3 (Bruker, 2018); cell
SAINT (Bruker, 2018); data reduction: SAINT (Bruker, 2018); program(s) used to solve structure: SHELXT (Sheldrick, 2015a); program(s) used to refine structure: SHELXL2018/3 (Sheldrick, 2015b); molecular graphics: ATOMS (Dowty, 2006); software used to prepare material for publication: publCIF (Westrip, 2010).Cs2SnSi6O15 | F(000) = 4368 |
Mr = 793.05 | Dx = 3.668 Mg m−3 |
Monoclinic, I2/c | Mo Kα radiation, λ = 0.71073 Å |
a = 26.3434 (10) Å | Cell parameters from 4399 reflections |
b = 7.4805 (3) Å | θ = 2.8–32.4° |
c = 22.9137 (7) Å | µ = 7.36 mm−1 |
β = 107.4020 (7)° | T = 296 K |
V = 4308.7 (3) Å3 | Lath, colourless |
Z = 12 | 0.12 × 0.03 × 0.01 mm |
Bruker APEXII CCD diffractometer | 5013 reflections with I > 2σ(I) |
ω– and φ–scans | Rint = 0.077 |
Absorption correction: multi-scan (SADABS; Krause et al., 2015). | θmax = 33.3°, θmin = 2.8° |
Tmin = 0.539, Tmax = 0.747 | h = −40→40 |
51032 measured reflections | k = −11→11 |
8282 independent reflections | l = −35→35 |
Refinement on F2 | 331 parameters |
Least-squares matrix: full | 0 restraints |
R[F2 > 2σ(F2)] = 0.037 | w = 1/[σ2(Fo2) + (0.0259P)2] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.082 | (Δ/σ)max = 0.002 |
S = 1.00 | Δρmax = 1.84 e Å−3 |
8282 reflections | Δρmin = −1.48 e Å−3 |
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Cs1 | 0.39755 (2) | −0.01953 (4) | 0.18693 (2) | 0.01982 (7) | |
Cs2 | 0.57484 (2) | −0.51580 (4) | 0.00767 (2) | 0.02128 (7) | |
Cs3A | 0.74609 (2) | −0.98408 (7) | 0.32160 (8) | 0.02213 (18) | 0.934 (5) |
Cs3B | 0.7514 (3) | −0.9776 (11) | 0.3439 (8) | 0.02213 (18) | 0.066 (5) |
Sn1 | 0.67822 (2) | −0.49735 (4) | −0.17784 (2) | 0.00700 (6) | |
Sn2 | 0.500000 | 0.000000 | 0.000000 | 0.00681 (7) | |
Si1 | 0.62500 (5) | −0.70216 (15) | 0.18853 (6) | 0.0075 (2) | |
Si2 | 0.63425 (5) | −0.30679 (15) | 0.18719 (6) | 0.0091 (2) | |
Si3 | 0.69676 (5) | −0.70648 (15) | −0.04744 (6) | 0.0077 (2) | |
Si4 | 0.63589 (4) | −0.99872 (15) | −0.00070 (5) | 0.0067 (2) | |
Si5 | 0.81053 (5) | −0.81223 (15) | 0.04445 (6) | 0.0086 (2) | |
Si6 | 0.68624 (4) | −0.99635 (15) | 0.13636 (5) | 0.0078 (2) | |
Si7 | 0.50782 (5) | −0.80838 (15) | 0.13301 (6) | 0.0080 (2) | |
Si8 | 0.51736 (5) | −0.20099 (15) | 0.13222 (6) | 0.0081 (2) | |
Si9 | 0.45804 (4) | −0.50114 (15) | 0.18261 (5) | 0.0066 (2) | |
O1 | 0.65897 (13) | −0.7024 (4) | 0.25901 (15) | 0.0129 (7) | |
O2 | 0.56382 (13) | −0.7463 (4) | 0.18108 (15) | 0.0167 (7) | |
O3 | 0.64737 (13) | −0.8469 (4) | 0.15066 (16) | 0.0199 (8) | |
O4 | 0.62794 (13) | −0.5077 (4) | 0.15681 (13) | 0.0140 (6) | |
O5 | 0.66980 (12) | −0.3096 (4) | 0.25683 (15) | 0.0115 (6) | |
O6 | 0.66307 (13) | −0.1918 (4) | 0.14653 (15) | 0.0162 (7) | |
O7 | 0.57564 (13) | −0.2302 (4) | 0.18125 (15) | 0.0170 (7) | |
O8 | 0.70020 (13) | −0.6982 (4) | −0.11572 (15) | 0.0119 (7) | |
O9 | 0.75309 (13) | −0.7544 (5) | 0.00067 (17) | 0.0187 (7) | |
O10 | 0.65155 (12) | −0.8509 (4) | −0.04422 (15) | 0.0134 (7) | |
O11 | 0.67790 (13) | −0.5157 (4) | −0.02671 (14) | 0.0144 (6) | |
O12 | 0.57747 (12) | −0.9680 (4) | 0.00220 (15) | 0.0144 (7) | |
O13 | 0.68113 (12) | −0.9797 (4) | 0.06475 (13) | 0.0123 (6) | |
O14 | 0.85664 (13) | −0.6934 (4) | 0.02893 (16) | 0.0147 (7) | |
O15 | 0.81334 (13) | −0.7987 (4) | 0.11477 (14) | 0.0125 (7) | |
O16 | 0.74525 (12) | −0.9636 (4) | 0.17887 (14) | 0.0136 (7) | |
O17 | 0.50824 (13) | −0.7996 (4) | 0.06370 (15) | 0.0127 (7) | |
O18 | 0.46185 (12) | −0.6903 (4) | 0.14849 (15) | 0.0129 (7) | |
O19 | 0.49642 (12) | −0.0117 (4) | 0.15154 (14) | 0.0119 (6) | |
O20 | 0.51978 (13) | −0.1991 (4) | 0.06375 (15) | 0.0121 (7) | |
O21 | 0.47656 (13) | −0.3514 (4) | 0.14152 (16) | 0.0171 (7) | |
O22 | 0.39930 (12) | −0.4614 (4) | 0.18260 (15) | 0.0149 (7) | |
O23 | 0.500000 | −0.5021 (6) | 0.250000 | 0.0193 (10) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Cs1 | 0.01741 (15) | 0.02075 (15) | 0.02457 (17) | −0.00118 (12) | 0.01126 (13) | −0.00080 (13) |
Cs2 | 0.01832 (15) | 0.02304 (15) | 0.02465 (17) | −0.00150 (14) | 0.00974 (13) | −0.00107 (14) |
Cs3A | 0.01454 (17) | 0.02048 (16) | 0.0320 (5) | 0.00139 (14) | 0.0080 (2) | 0.0013 (2) |
Cs3B | 0.01454 (17) | 0.02048 (16) | 0.0320 (5) | 0.00139 (14) | 0.0080 (2) | 0.0013 (2) |
Sn1 | 0.00705 (12) | 0.00726 (12) | 0.00620 (13) | 0.00027 (11) | 0.00124 (10) | 0.00007 (12) |
Sn2 | 0.00707 (17) | 0.00700 (17) | 0.00653 (18) | 0.00038 (16) | 0.00229 (14) | 0.00016 (17) |
Si1 | 0.0074 (6) | 0.0074 (5) | 0.0069 (6) | −0.0006 (4) | 0.0011 (5) | −0.0018 (4) |
Si2 | 0.0098 (6) | 0.0086 (5) | 0.0082 (7) | −0.0011 (4) | 0.0013 (5) | 0.0012 (4) |
Si3 | 0.0086 (6) | 0.0076 (5) | 0.0064 (7) | 0.0007 (4) | 0.0016 (5) | 0.0012 (4) |
Si4 | 0.0063 (5) | 0.0065 (5) | 0.0079 (5) | −0.0005 (4) | 0.0031 (4) | 0.0001 (5) |
Si5 | 0.0093 (6) | 0.0071 (5) | 0.0091 (7) | 0.0004 (4) | 0.0021 (5) | 0.0010 (4) |
Si6 | 0.0077 (5) | 0.0091 (5) | 0.0065 (5) | 0.0003 (5) | 0.0020 (4) | −0.0002 (5) |
Si7 | 0.0086 (6) | 0.0063 (5) | 0.0091 (7) | −0.0002 (4) | 0.0025 (5) | −0.0012 (4) |
Si8 | 0.0089 (6) | 0.0072 (5) | 0.0086 (7) | 0.0011 (4) | 0.0031 (5) | 0.0020 (4) |
Si9 | 0.0068 (5) | 0.0064 (5) | 0.0071 (5) | −0.0012 (5) | 0.0029 (4) | −0.0004 (5) |
O1 | 0.0160 (17) | 0.0111 (15) | 0.0096 (18) | 0.0011 (12) | 0.0008 (14) | −0.0006 (12) |
O2 | 0.0086 (16) | 0.0259 (18) | 0.0147 (19) | −0.0032 (13) | 0.0020 (14) | −0.0048 (14) |
O3 | 0.0168 (18) | 0.0198 (17) | 0.022 (2) | 0.0065 (14) | 0.0036 (16) | −0.0121 (14) |
O4 | 0.0229 (17) | 0.0077 (13) | 0.0097 (15) | −0.0037 (13) | 0.0026 (13) | −0.0007 (12) |
O5 | 0.0119 (16) | 0.0099 (14) | 0.0110 (18) | −0.0009 (12) | 0.0011 (14) | 0.0037 (12) |
O6 | 0.0219 (19) | 0.0129 (15) | 0.0154 (19) | −0.0034 (13) | 0.0079 (16) | 0.0028 (13) |
O7 | 0.0102 (17) | 0.0242 (18) | 0.0131 (19) | 0.0048 (13) | −0.0019 (14) | 0.0041 (14) |
O8 | 0.0164 (17) | 0.0092 (14) | 0.0105 (18) | 0.0016 (12) | 0.0049 (14) | 0.0024 (12) |
O9 | 0.0121 (16) | 0.0264 (17) | 0.0146 (17) | 0.0030 (13) | −0.0005 (13) | 0.0072 (13) |
O10 | 0.0129 (17) | 0.0145 (15) | 0.0105 (17) | −0.0063 (12) | 0.0001 (14) | 0.0045 (12) |
O11 | 0.0209 (17) | 0.0096 (14) | 0.0175 (17) | −0.0002 (13) | 0.0131 (14) | −0.0014 (13) |
O12 | 0.0071 (15) | 0.0177 (15) | 0.0203 (18) | −0.0010 (12) | 0.0068 (13) | −0.0010 (13) |
O13 | 0.0134 (15) | 0.0193 (16) | 0.0030 (14) | −0.0020 (13) | 0.0006 (12) | 0.0005 (12) |
O14 | 0.0124 (17) | 0.0131 (15) | 0.018 (2) | −0.0025 (12) | 0.0042 (15) | 0.0036 (13) |
O15 | 0.0196 (18) | 0.0097 (14) | 0.0070 (17) | 0.0016 (12) | 0.0022 (14) | 0.0007 (12) |
O16 | 0.0083 (15) | 0.0237 (17) | 0.0081 (16) | −0.0012 (12) | 0.0013 (12) | −0.0024 (13) |
O17 | 0.0195 (18) | 0.0111 (14) | 0.0072 (18) | −0.0012 (13) | 0.0036 (14) | −0.0039 (12) |
O18 | 0.0117 (16) | 0.0096 (14) | 0.0178 (19) | 0.0030 (12) | 0.0052 (14) | −0.0048 (12) |
O19 | 0.0146 (15) | 0.0106 (14) | 0.0132 (15) | 0.0011 (13) | 0.0084 (13) | 0.0002 (13) |
O20 | 0.0162 (17) | 0.0106 (14) | 0.0107 (18) | 0.0033 (12) | 0.0060 (14) | 0.0009 (12) |
O21 | 0.0201 (19) | 0.0143 (16) | 0.017 (2) | −0.0077 (13) | 0.0064 (16) | 0.0061 (13) |
O22 | 0.0081 (15) | 0.0155 (15) | 0.0211 (18) | 0.0013 (12) | 0.0042 (14) | −0.0025 (13) |
O23 | 0.020 (2) | 0.025 (2) | 0.011 (2) | 0.000 | 0.0024 (19) | 0.000 |
Cs1—O19 | 2.951 (3) | Sn1—O22iii | 2.036 (3) |
Cs1—O1i | 3.237 (3) | Sn1—O1x | 2.036 (3) |
Cs1—O18ii | 3.256 (3) | Sn1—O15vi | 2.038 (3) |
Cs1—O10iii | 3.282 (3) | Sn1—O16vi | 2.039 (3) |
Cs1—O7iv | 3.291 (3) | Sn1—O5x | 2.044 (3) |
Cs1—O5iv | 3.299 (3) | Sn2—O12iii | 2.040 (3) |
Cs1—O22 | 3.308 (3) | Sn2—O12ii | 2.040 (3) |
Cs1—O15v | 3.336 (3) | Sn2—O20 | 2.042 (3) |
Cs1—O8iii | 3.352 (3) | Sn2—O20xi | 2.042 (3) |
Cs1—O2i | 3.538 (3) | Sn2—O17iii | 2.058 (3) |
Cs1—O21 | 3.588 (3) | Sn2—O17ii | 2.058 (3) |
Cs1—Cs3Ai | 3.7396 (5) | Si1—O1 | 1.595 (4) |
Cs2—O11 | 3.045 (3) | Si1—O2 | 1.604 (3) |
Cs2—O20 | 3.238 (3) | Si1—O3 | 1.606 (3) |
Cs2—O17 | 3.253 (3) | Si1—O4 | 1.638 (3) |
Cs2—O14vi | 3.268 (3) | Si2—O5 | 1.590 (3) |
Cs2—O4 | 3.283 (3) | Si2—O7 | 1.614 (3) |
Cs2—O17iii | 3.300 (3) | Si2—O6 | 1.615 (3) |
Cs2—O20iii | 3.316 (3) | Si2—O4 | 1.644 (3) |
Cs2—O12 | 3.387 (3) | Si3—O8 | 1.595 (3) |
Cs2—O21iii | 3.426 (4) | Si3—O9 | 1.602 (4) |
Cs2—O10 | 3.636 (3) | Si3—O10 | 1.626 (3) |
Cs2—O18iii | 3.748 (3) | Si3—O11 | 1.628 (3) |
Cs2—Cs2iii | 3.8598 (6) | Si4—O12 | 1.577 (3) |
Cs3A—O1 | 3.129 (3) | Si4—O13 | 1.619 (3) |
Cs3A—O8vii | 3.195 (3) | Si4—O10 | 1.623 (3) |
Cs3A—O4viii | 3.206 (3) | Si4—O14xii | 1.629 (3) |
Cs3A—O5ix | 3.223 (3) | Si5—O15 | 1.594 (3) |
Cs3A—O15viii | 3.227 (3) | Si5—O9 | 1.605 (4) |
Cs3A—O16 | 3.268 (3) | Si5—O11xii | 1.628 (3) |
Cs3A—O6viii | 3.331 (3) | Si5—O14 | 1.628 (3) |
Cs3A—O16viii | 3.357 (3) | Si6—O16 | 1.587 (3) |
Cs3A—Si2viii | 3.5783 (13) | Si6—O13 | 1.611 (3) |
Cs3A—O5viii | 3.592 (3) | Si6—O3 | 1.615 (3) |
Cs3A—O3viii | 3.653 (3) | Si6—O6ix | 1.628 (3) |
Cs3B—O15viii | 3.007 (10) | Si7—O17 | 1.593 (3) |
Cs3B—O8vii | 3.050 (9) | Si7—O18 | 1.622 (3) |
Cs3B—O4viii | 3.186 (8) | Si7—O2 | 1.623 (4) |
Cs3B—O6viii | 3.308 (8) | Si7—O19ix | 1.631 (3) |
Cs3B—O1 | 3.334 (12) | Si8—O20 | 1.589 (3) |
Cs3B—O16viii | 3.347 (9) | Si8—O21 | 1.614 (3) |
Cs3B—O5ix | 3.494 (13) | Si8—O7 | 1.623 (4) |
Cs3B—O3viii | 3.580 (8) | Si8—O19 | 1.629 (3) |
Cs3B—Si2viii | 3.670 (8) | Si9—O22 | 1.576 (3) |
Cs3B—O16 | 3.738 (18) | Si9—O23 | 1.6078 (12) |
Cs3B—Si1viii | 3.796 (8) | Si9—O21 | 1.629 (3) |
Sn1—O8 | 2.031 (3) | Si9—O18 | 1.634 (3) |
O19—Cs1—O1i | 129.44 (8) | O1—Si1—Cs3Aviii | 79.54 (12) |
O19—Cs1—O18ii | 48.50 (7) | O2—Si1—Cs3Aviii | 166.44 (14) |
O1i—Cs1—O18ii | 83.41 (7) | O3—Si1—Cs3Aviii | 74.38 (13) |
O19—Cs1—O10iii | 81.34 (8) | O4—Si1—Cs3Aviii | 58.51 (12) |
O1i—Cs1—O10iii | 120.55 (8) | O1—Si1—Cs3Bviii | 86.8 (3) |
O18ii—Cs1—O10iii | 92.05 (8) | O2—Si1—Cs3Bviii | 161.0 (3) |
O19—Cs1—O7iv | 107.28 (8) | O3—Si1—Cs3Bviii | 70.0 (2) |
O1i—Cs1—O7iv | 89.80 (8) | O4—Si1—Cs3Bviii | 56.05 (18) |
O18ii—Cs1—O7iv | 128.63 (8) | Cs3Aviii—Si1—Cs3Bviii | 7.4 (2) |
O10iii—Cs1—O7iv | 133.27 (8) | O1—Si1—Cs1xiii | 54.50 (11) |
O19—Cs1—O5iv | 137.94 (8) | O2—Si1—Cs1xiii | 65.38 (13) |
O1i—Cs1—O5iv | 88.26 (7) | O3—Si1—Cs1xiii | 98.41 (13) |
O18ii—Cs1—O5iv | 170.79 (7) | O4—Si1—Cs1xiii | 154.79 (12) |
O10iii—Cs1—O5iv | 95.58 (7) | Cs3Aviii—Si1—Cs1xiii | 127.81 (4) |
O7iv—Cs1—O5iv | 47.11 (8) | Cs3Bviii—Si1—Cs1xiii | 133.4 (2) |
O19—Cs1—O22 | 89.45 (8) | O1—Si1—Cs2 | 156.41 (12) |
O1i—Cs1—O22 | 139.09 (7) | O2—Si1—Cs2 | 87.35 (13) |
O18ii—Cs1—O22 | 137.29 (7) | O3—Si1—Cs2 | 75.41 (14) |
O10iii—Cs1—O22 | 71.33 (8) | O4—Si1—Cs2 | 46.31 (11) |
O7iv—Cs1—O22 | 63.12 (8) | Cs3Aviii—Si1—Cs2 | 80.71 (3) |
O5iv—Cs1—O22 | 50.83 (7) | Cs3Bviii—Si1—Cs2 | 74.0 (3) |
O19—Cs1—O15v | 111.12 (8) | Cs1xiii—Si1—Cs2 | 148.79 (3) |
O1i—Cs1—O15v | 49.69 (8) | O1—Si1—Cs3A | 36.91 (11) |
O18ii—Cs1—O15v | 69.44 (7) | O2—Si1—Cs3A | 119.24 (13) |
O10iii—Cs1—O15v | 73.23 (8) | O3—Si1—Cs3A | 74.66 (14) |
O7iv—Cs1—O15v | 136.47 (7) | O4—Si1—Cs3A | 129.29 (12) |
O5iv—Cs1—O15v | 107.90 (7) | Cs3Aviii—Si1—Cs3A | 74.28 (3) |
O22—Cs1—O15v | 135.35 (8) | Cs3Bviii—Si1—Cs3A | 79.2 (2) |
O19—Cs1—O8iii | 119.44 (8) | Cs1xiii—Si1—Cs3A | 54.428 (19) |
O1i—Cs1—O8iii | 105.87 (7) | Cs2—Si1—Cs3A | 145.09 (3) |
O18ii—Cs1—O8iii | 136.95 (8) | O5—Si2—O7 | 110.53 (17) |
O10iii—Cs1—O8iii | 46.58 (7) | O5—Si2—O6 | 110.39 (18) |
O7iv—Cs1—O8iii | 93.90 (8) | O7—Si2—O6 | 111.42 (18) |
O5iv—Cs1—O8iii | 49.56 (8) | O5—Si2—O4 | 111.56 (16) |
O22—Cs1—O8iii | 51.07 (7) | O7—Si2—O4 | 108.41 (18) |
O15v—Cs1—O8iii | 84.72 (7) | O6—Si2—O4 | 104.37 (16) |
O19—Cs1—O2i | 99.87 (8) | O5—Si2—Cs3Aviii | 77.67 (12) |
O1i—Cs1—O2i | 45.36 (8) | O7—Si2—Cs3Aviii | 170.77 (14) |
O18ii—Cs1—O2i | 75.78 (8) | O6—Si2—Cs3Aviii | 68.05 (12) |
O10iii—Cs1—O2i | 161.62 (7) | O4—Si2—Cs3Aviii | 63.62 (12) |
O7iv—Cs1—O2i | 64.15 (7) | O5—Si2—Cs3Bviii | 85.3 (3) |
O5iv—Cs1—O2i | 95.55 (7) | O7—Si2—Cs3Bviii | 163.7 (3) |
O22—Cs1—O2i | 126.86 (8) | O6—Si2—Cs3Bviii | 64.3 (2) |
O15v—Cs1—O2i | 89.43 (7) | O4—Si2—Cs3Bviii | 60.1 (2) |
O8iii—Cs1—O2i | 139.69 (7) | Cs3Aviii—Si2—Cs3Bviii | 7.6 (3) |
O19—Cs1—O21 | 45.41 (7) | O5—Si2—Cs1iv | 56.99 (11) |
O1i—Cs1—O21 | 172.30 (8) | O7—Si2—Cs1iv | 56.83 (13) |
O18ii—Cs1—O21 | 92.93 (7) | O6—Si2—Cs1iv | 112.15 (12) |
O10iii—Cs1—O21 | 66.22 (8) | O4—Si2—Cs1iv | 143.45 (12) |
O7iv—Cs1—O21 | 87.19 (8) | Cs3Aviii—Si2—Cs1iv | 132.30 (5) |
O5iv—Cs1—O21 | 94.85 (7) | Cs3Bviii—Si2—Cs1iv | 139.4 (3) |
O22—Cs1—O21 | 44.39 (7) | O5—Si2—Cs2 | 154.76 (12) |
O15v—Cs1—O21 | 135.03 (8) | O7—Si2—Cs2 | 89.01 (13) |
O8iii—Cs1—O21 | 81.42 (7) | O6—Si2—Cs2 | 74.77 (13) |
O2i—Cs1—O21 | 127.16 (8) | O4—Si2—Cs2 | 44.80 (11) |
O19—Cs1—Cs3Ai | 161.21 (7) | Cs3Aviii—Si2—Cs2 | 81.95 (4) |
O1i—Cs1—Cs3Ai | 52.70 (6) | Cs3Bviii—Si2—Cs2 | 74.7 (3) |
O18ii—Cs1—Cs3Ai | 122.16 (5) | Cs1iv—Si2—Cs2 | 145.67 (4) |
O10iii—Cs1—Cs3Ai | 82.98 (6) | O5—Si2—Cs3Aii | 38.62 (11) |
O7iv—Cs1—Cs3Ai | 91.03 (6) | O7—Si2—Cs3Aii | 107.08 (13) |
O5iv—Cs1—Cs3Ai | 54.06 (6) | O6—Si2—Cs3Aii | 77.00 (13) |
O22—Cs1—Cs3Ai | 95.29 (5) | O4—Si2—Cs3Aii | 140.89 (12) |
O15v—Cs1—Cs3Ai | 53.91 (5) | Cs3Aviii—Si2—Cs3Aii | 81.93 (4) |
O8iii—Cs1—Cs3Ai | 53.22 (5) | Cs3Bviii—Si2—Cs3Aii | 87.7 (2) |
O2i—Cs1—Cs3Ai | 91.81 (5) | Cs1iv—Si2—Cs3Aii | 54.01 (2) |
O21—Cs1—Cs3Ai | 134.39 (5) | Cs2—Si2—Cs3Aii | 151.10 (3) |
O11—Cs2—O20 | 129.98 (8) | O8—Si3—O9 | 111.77 (18) |
O11—Cs2—O17 | 136.90 (8) | O8—Si3—O10 | 109.12 (18) |
O20—Cs2—O17 | 87.84 (7) | O9—Si3—O10 | 111.11 (18) |
O11—Cs2—O14vi | 47.93 (7) | O8—Si3—O11 | 111.35 (16) |
O20—Cs2—O14vi | 84.79 (7) | O9—Si3—O11 | 107.22 (19) |
O17—Cs2—O14vi | 170.85 (8) | O10—Si3—O11 | 106.12 (16) |
O11—Cs2—O4 | 97.70 (8) | O8—Si3—Cs1iii | 55.75 (12) |
O20—Cs2—O4 | 71.06 (8) | O9—Si3—Cs1iii | 131.64 (14) |
O17—Cs2—O4 | 73.34 (8) | O10—Si3—Cs1iii | 53.45 (12) |
O14vi—Cs2—O4 | 99.06 (8) | O11—Si3—Cs1iii | 120.94 (13) |
O11—Cs2—O17iii | 112.47 (8) | O8—Si3—Cs3Bxiv | 43.6 (2) |
O20—Cs2—O17iii | 50.51 (7) | O9—Si3—Cs3Bxiv | 82.2 (2) |
O17—Cs2—O17iii | 107.82 (6) | O10—Si3—Cs3Bxiv | 92.32 (16) |
O14vi—Cs2—O17iii | 71.38 (8) | O11—Si3—Cs3Bxiv | 153.9 (2) |
O4—Cs2—O17iii | 121.04 (7) | Cs1iii—Si3—Cs3Bxiv | 56.65 (16) |
O11—Cs2—O20iii | 117.98 (7) | O8—Si3—Cs2 | 125.15 (13) |
O20—Cs2—O20iii | 107.85 (6) | O9—Si3—Cs2 | 121.49 (14) |
O17—Cs2—O20iii | 50.25 (7) | O10—Si3—Cs2 | 63.86 (12) |
O14vi—Cs2—O20iii | 137.65 (8) | O11—Si3—Cs2 | 42.26 (11) |
O4—Cs2—O20iii | 123.29 (7) | Cs1iii—Si3—Cs2 | 93.96 (3) |
O17iii—Cs2—O20iii | 85.76 (7) | Cs3Bxiv—Si3—Cs2 | 150.41 (15) |
O11—Cs2—O12 | 87.76 (7) | O8—Si3—Cs3Axiv | 38.41 (11) |
O20—Cs2—O12 | 139.65 (7) | O9—Si3—Cs3Axiv | 87.05 (14) |
O17—Cs2—O12 | 51.84 (7) | O10—Si3—Cs3Axiv | 93.01 (12) |
O14vi—Cs2—O12 | 135.12 (7) | O11—Si3—Cs3Axiv | 149.35 (12) |
O4—Cs2—O12 | 92.86 (8) | Cs1iii—Si3—Cs3Axiv | 53.629 (19) |
O17iii—Cs2—O12 | 135.53 (8) | Cs3Bxiv—Si3—Cs3Axiv | 5.5 (2) |
O20iii—Cs2—O12 | 50.21 (7) | Cs2—Si3—Cs3Axiv | 147.54 (4) |
O11—Cs2—O21iii | 81.88 (8) | O12—Si4—O13 | 113.92 (17) |
O20—Cs2—O21iii | 121.19 (8) | O12—Si4—O10 | 110.94 (17) |
O17—Cs2—O21iii | 96.07 (7) | O13—Si4—O10 | 104.91 (17) |
O14vi—Cs2—O21iii | 92.39 (8) | O12—Si4—O14xii | 112.47 (17) |
O4—Cs2—O21iii | 164.18 (7) | O13—Si4—O14xii | 107.67 (17) |
O17iii—Cs2—O21iii | 72.97 (8) | O10—Si4—O14xii | 106.39 (17) |
O20iii—Cs2—O21iii | 46.12 (7) | O12—Si4—Cs2 | 56.81 (11) |
O12—Cs2—O21iii | 71.33 (8) | O13—Si4—Cs2 | 94.11 (11) |
O11—Cs2—O10 | 44.74 (7) | O10—Si4—Cs2 | 65.92 (11) |
O20—Cs2—O10 | 173.27 (8) | O14xii—Si4—Cs2 | 158.21 (14) |
O17—Cs2—O10 | 95.59 (7) | O12—Si4—Cs1iii | 97.51 (13) |
O14vi—Cs2—O10 | 91.21 (7) | O13—Si4—Cs1iii | 146.31 (11) |
O4—Cs2—O10 | 104.34 (7) | O10—Si4—Cs1iii | 49.59 (12) |
O17iii—Cs2—O10 | 133.00 (7) | O14xii—Si4—Cs1iii | 68.28 (12) |
O20iii—Cs2—O10 | 78.73 (7) | Cs2—Si4—Cs1iii | 93.20 (2) |
O12—Cs2—O10 | 43.92 (6) | O12—Si4—Cs2ix | 75.01 (11) |
O21iii—Cs2—O10 | 64.29 (8) | O13—Si4—Cs2ix | 102.93 (11) |
O11—Cs2—O18iii | 75.42 (8) | O10—Si4—Cs2ix | 145.47 (12) |
O20—Cs2—O18iii | 93.42 (7) | O14xii—Si4—Cs2ix | 44.83 (11) |
O17—Cs2—O18iii | 129.03 (8) | Cs2—Si4—Cs2ix | 131.69 (3) |
O14vi—Cs2—O18iii | 57.05 (8) | Cs1iii—Si4—Cs2ix | 96.43 (2) |
O4—Cs2—O18iii | 153.40 (7) | O15—Si5—O9 | 111.40 (18) |
O17iii—Cs2—O18iii | 44.71 (7) | O15—Si5—O11xii | 110.88 (16) |
O20iii—Cs2—O18iii | 81.50 (7) | O9—Si5—O11xii | 107.93 (19) |
O12—Cs2—O18iii | 112.20 (7) | O15—Si5—O14 | 111.96 (18) |
O21iii—Cs2—O18iii | 41.79 (7) | O9—Si5—O14 | 110.00 (18) |
O10—Cs2—O18iii | 88.92 (6) | O11xii—Si5—O14 | 104.38 (16) |
O11—Cs2—Cs2iii | 160.41 (6) | O15—Si5—Cs2xii | 122.11 (13) |
O20—Cs2—Cs2iii | 54.87 (6) | O9—Si5—Cs2xii | 126.10 (14) |
O17—Cs2—Cs2iii | 54.48 (6) | O11xii—Si5—Cs2xii | 48.26 (11) |
O14vi—Cs2—Cs2iii | 123.98 (6) | O14—Si5—Cs2xii | 56.37 (11) |
O4—Cs2—Cs2iii | 101.49 (5) | O15—Si5—Cs3Bviii | 39.9 (2) |
O17iii—Cs2—Cs2iii | 53.35 (5) | O9—Si5—Cs3Bviii | 76.6 (2) |
O20iii—Cs2—Cs2iii | 52.98 (5) | O11xii—Si5—Cs3Bviii | 143.06 (18) |
O12—Cs2—Cs2iii | 95.13 (5) | O14—Si5—Cs3Bviii | 108.28 (16) |
O21iii—Cs2—Cs2iii | 80.72 (5) | Cs2xii—Si5—Cs3Bviii | 154.58 (17) |
O10—Cs2—Cs2iii | 131.69 (5) | O15—Si5—Cs1xv | 47.65 (11) |
O18iii—Cs2—Cs2iii | 85.59 (5) | O9—Si5—Cs1xv | 121.39 (14) |
O1—Cs3A—O8vii | 112.49 (8) | O11xii—Si5—Cs1xv | 130.40 (13) |
O1—Cs3A—O4viii | 131.83 (8) | O14—Si5—Cs1xv | 64.99 (13) |
O8vii—Cs3A—O4viii | 115.45 (8) | Cs2xii—Si5—Cs1xv | 100.22 (3) |
O1—Cs3A—O5ix | 91.53 (8) | Cs3Bviii—Si5—Cs1xv | 54.65 (16) |
O8vii—Cs3A—O5ix | 51.50 (8) | O16—Si6—O13 | 112.41 (16) |
O4viii—Cs3A—O5ix | 122.05 (8) | O16—Si6—O3 | 109.44 (18) |
O1—Cs3A—O15viii | 51.50 (8) | O13—Si6—O3 | 106.76 (18) |
O8vii—Cs3A—O15viii | 89.11 (8) | O16—Si6—O6ix | 113.01 (18) |
O4viii—Cs3A—O15viii | 124.22 (9) | O13—Si6—O6ix | 107.14 (17) |
O5ix—Cs3A—O15viii | 112.54 (8) | O3—Si6—O6ix | 107.78 (18) |
O1—Cs3A—O16 | 74.06 (8) | O16—Si6—Cs3Bviii | 59.0 (2) |
O8vii—Cs3A—O16 | 126.48 (9) | O13—Si6—Cs3Bviii | 87.2 (3) |
O4viii—Cs3A—O16 | 81.50 (8) | O3—Si6—Cs3Bviii | 67.37 (17) |
O5ix—Cs3A—O16 | 75.98 (8) | O6ix—Si6—Cs3Bviii | 165.6 (3) |
O15viii—Cs3A—O16 | 124.23 (8) | O16—Si6—Cs3Aviii | 55.21 (12) |
O1—Cs3A—O6viii | 166.14 (10) | O13—Si6—Cs3Aviii | 94.08 (11) |
O8vii—Cs3A—O6viii | 72.76 (8) | O3—Si6—Cs3Aviii | 65.97 (13) |
O4viii—Cs3A—O6viii | 46.33 (7) | O6ix—Si6—Cs3Aviii | 158.73 (13) |
O5ix—Cs3A—O6viii | 81.91 (8) | Cs3Bviii—Si6—Cs3Aviii | 6.9 (2) |
O15viii—Cs3A—O6viii | 142.36 (10) | O16—Si6—Cs3A | 49.66 (11) |
O16—Cs3A—O6viii | 92.45 (8) | O13—Si6—Cs3A | 161.93 (12) |
O1—Cs3A—O16viii | 50.82 (8) | O3—Si6—Cs3A | 81.01 (14) |
O8vii—Cs3A—O16viii | 141.13 (8) | O6ix—Si6—Cs3A | 85.16 (13) |
O4viii—Cs3A—O16viii | 87.21 (7) | Cs3Bviii—Si6—Cs3A | 80.7 (3) |
O5ix—Cs3A—O16viii | 141.80 (8) | Cs3Aviii—Si6—Cs3A | 73.88 (3) |
O15viii—Cs3A—O16viii | 52.43 (7) | O16—Si6—Cs3Bxvi | 78.5 (2) |
O16—Cs3A—O16viii | 86.00 (8) | O13—Si6—Cs3Bxvi | 95.3 (3) |
O6viii—Cs3A—O16viii | 132.99 (8) | O3—Si6—Cs3Bxvi | 150.6 (2) |
O1—Cs3A—Si2viii | 143.72 (7) | O6ix—Si6—Cs3Bxvi | 45.60 (15) |
O8vii—Cs3A—Si2viii | 99.10 (6) | Cs3Bviii—Si6—Cs3Bxvi | 134.4 (2) |
O4viii—Cs3A—Si2viii | 27.34 (5) | Cs3Aviii—Si6—Cs3Bxvi | 132.72 (14) |
O5ix—Cs3A—Si2viii | 94.72 (6) | Cs3A—Si6—Cs3Bxvi | 83.8 (2) |
O15viii—Cs3A—Si2viii | 150.05 (8) | O16—Si6—Cs3Axvi | 74.65 (12) |
O16—Cs3A—Si2viii | 72.93 (6) | O13—Si6—Cs3Axvi | 101.69 (12) |
O6viii—Cs3A—Si2viii | 26.72 (5) | O3—Si6—Cs3Axvi | 146.41 (14) |
O16viii—Cs3A—Si2viii | 111.97 (5) | O6ix—Si6—Cs3Axvi | 45.44 (12) |
O1—Cs3A—O5viii | 122.52 (9) | Cs3Bviii—Si6—Cs3Axvi | 132.32 (15) |
O8vii—Cs3A—O5viii | 106.15 (7) | Cs3Aviii—Si6—Cs3Axvi | 129.68 (4) |
O4viii—Cs3A—O5viii | 45.90 (7) | Cs3A—Si6—Cs3Axvi | 77.24 (3) |
O5ix—Cs3A—O5viii | 80.67 (8) | Cs3Bxvi—Si6—Cs3Axvi | 6.6 (2) |
O15viii—Cs3A—O5viii | 164.32 (7) | O17—Si7—O18 | 115.08 (18) |
O16—Cs3A—O5viii | 48.69 (8) | O17—Si7—O2 | 112.90 (17) |
O6viii—Cs3A—O5viii | 44.49 (7) | O18—Si7—O2 | 106.40 (17) |
O16viii—Cs3A—O5viii | 111.99 (7) | O17—Si7—O19ix | 110.79 (16) |
Si2viii—Cs3A—O5viii | 25.63 (6) | O18—Si7—O19ix | 104.08 (15) |
O1—Cs3A—O3viii | 92.49 (8) | O2—Si7—O19ix | 106.91 (18) |
O8vii—Cs3A—O3viii | 143.14 (10) | O17—Si7—Cs1ix | 124.89 (13) |
O4viii—Cs3A—O3viii | 43.96 (7) | O18—Si7—Cs1ix | 57.65 (11) |
O5ix—Cs3A—O3viii | 158.91 (8) | O2—Si7—Cs1ix | 121.55 (13) |
O15viii—Cs3A—O3viii | 85.90 (7) | O19ix—Si7—Cs1ix | 46.64 (10) |
O16—Cs3A—O3viii | 85.25 (8) | O17—Si7—Cs2iii | 49.62 (12) |
O6viii—Cs3A—O3viii | 89.48 (7) | O18—Si7—Cs2iii | 66.05 (12) |
O16viii—Cs3A—O3viii | 43.53 (7) | O2—Si7—Cs2iii | 121.72 (13) |
Si2viii—Cs3A—O3viii | 70.25 (5) | O19ix—Si7—Cs2iii | 131.32 (13) |
O5viii—Cs3A—O3viii | 79.71 (7) | Cs1ix—Si7—Cs2iii | 102.84 (3) |
O1—Cs3A—Cs1xiii | 55.38 (6) | O20—Si8—O21 | 111.19 (18) |
O8vii—Cs3A—Cs1xiii | 57.17 (6) | O20—Si8—O7 | 112.06 (18) |
O4viii—Cs3A—Cs1xiii | 172.38 (6) | O21—Si8—O7 | 110.13 (18) |
O5ix—Cs3A—Cs1xiii | 55.98 (5) | O20—Si8—O19 | 112.18 (16) |
O15viii—Cs3A—Cs1xiii | 56.64 (6) | O21—Si8—O19 | 106.10 (17) |
O16—Cs3A—Cs1xiii | 104.31 (6) | O7—Si8—O19 | 104.83 (18) |
O6viii—Cs3A—Cs1xiii | 127.54 (5) | O20—Si8—Cs1 | 125.41 (13) |
O16viii—Cs3A—Cs1xiii | 98.01 (5) | O21—Si8—Cs1 | 64.70 (12) |
Si2viii—Cs3A—Cs1xiii | 149.39 (3) | O7—Si8—Cs1 | 120.29 (13) |
O5viii—Cs3A—Cs1xiii | 135.18 (6) | O19—Si8—Cs1 | 41.45 (10) |
O3viii—Cs3A—Cs1xiii | 140.35 (5) | O20—Si8—Cs2iii | 53.68 (12) |
O15viii—Cs3B—O8vii | 96.1 (3) | O21—Si8—Cs2iii | 57.85 (13) |
O15viii—Cs3B—O4viii | 133.3 (4) | O7—Si8—Cs2iii | 134.84 (13) |
O8vii—Cs3B—O4viii | 120.4 (3) | O19—Si8—Cs2iii | 120.30 (13) |
O15viii—Cs3B—O6viii | 158.8 (6) | Cs1—Si8—Cs2iii | 94.85 (3) |
O8vii—Cs3B—O6viii | 74.9 (2) | O20—Si8—Cs1iv | 141.77 (13) |
O4viii—Cs3B—O6viii | 46.66 (13) | O21—Si8—Cs1iv | 105.59 (14) |
O15viii—Cs3B—O1 | 51.35 (16) | O7—Si8—Cs1iv | 42.51 (12) |
O8vii—Cs3B—O1 | 110.8 (3) | O19—Si8—Cs1iv | 65.46 (12) |
O4viii—Cs3B—O1 | 125.0 (4) | Cs1—Si8—Cs1iv | 79.75 (2) |
O6viii—Cs3B—O1 | 149.8 (6) | Cs2iii—Si8—Cs1iv | 162.95 (3) |
O15viii—Cs3B—O16viii | 54.21 (15) | O20—Si8—Cs2 | 39.22 (11) |
O8vii—Cs3B—O16viii | 150.0 (3) | O21—Si8—Cs2 | 94.95 (13) |
O4viii—Cs3B—O16viii | 87.7 (2) | O7—Si8—Cs2 | 86.44 (12) |
O6viii—Cs3B—O16viii | 134.3 (3) | O19—Si8—Cs2 | 150.46 (11) |
O1—Cs3B—O16viii | 49.38 (16) | Cs1—Si8—Cs2 | 150.06 (4) |
O15viii—Cs3B—O5ix | 111.0 (2) | Cs2iii—Si8—Cs2 | 55.205 (18) |
O8vii—Cs3B—O5ix | 49.88 (16) | Cs1iv—Si8—Cs2 | 128.74 (3) |
O4viii—Cs3B—O5ix | 114.6 (4) | O22—Si9—O23 | 113.21 (14) |
O6viii—Cs3B—O5ix | 78.3 (2) | O22—Si9—O21 | 109.52 (18) |
O1—Cs3B—O5ix | 83.6 (3) | O23—Si9—O21 | 108.63 (19) |
O16viii—Cs3B—O5ix | 130.7 (5) | O22—Si9—O18 | 111.34 (17) |
O15viii—Cs3B—O3viii | 90.6 (2) | O23—Si9—O18 | 109.4 (2) |
O8vii—Cs3B—O3viii | 157.1 (5) | O21—Si9—O18 | 104.29 (17) |
O4viii—Cs3B—O3viii | 44.73 (12) | O22—Si9—Cs1 | 54.89 (11) |
O6viii—Cs3B—O3viii | 91.09 (19) | O23—Si9—Cs1 | 98.43 (16) |
O1—Cs3B—O3viii | 90.5 (2) | O21—Si9—Cs1 | 65.20 (12) |
O16viii—Cs3B—O3viii | 44.18 (12) | O18—Si9—Cs1 | 152.14 (13) |
O5ix—Cs3B—O3viii | 145.7 (5) | O22—Si9—Cs2iii | 95.56 (13) |
O15viii—Cs3B—Si2viii | 159.9 (3) | O23—Si9—Cs2iii | 150.37 (5) |
O8vii—Cs3B—Si2viii | 99.9 (2) | O21—Si9—Cs2iii | 51.79 (13) |
O4viii—Cs3B—Si2viii | 26.56 (9) | O18—Si9—Cs2iii | 63.31 (12) |
O6viii—Cs3B—Si2viii | 26.10 (8) | Cs1—Si9—Cs2iii | 92.24 (2) |
O1—Cs3B—Si2viii | 131.0 (5) | O22—Si9—Cs1ix | 78.16 (11) |
O16viii—Cs3B—Si2viii | 110.0 (2) | O23—Si9—Cs1ix | 97.46 (16) |
O5ix—Cs3B—Si2viii | 88.7 (3) | O21—Si9—Cs1ix | 145.97 (13) |
O3viii—Cs3B—Si2viii | 70.04 (14) | O18—Si9—Cs1ix | 44.82 (11) |
O15viii—Cs3B—O16 | 116.2 (4) | Cs1—Si9—Cs1ix | 132.96 (3) |
O8vii—Cs3B—O16 | 116.1 (4) | Cs2iii—Si9—Cs1ix | 95.20 (2) |
O4viii—Cs3B—O16 | 74.8 (3) | Si1—O1—Sn1xvii | 131.57 (17) |
O6viii—Cs3B—O16 | 84.9 (3) | Si1—O1—Cs3A | 125.27 (15) |
O1—Cs3B—O16 | 65.8 (3) | Sn1xvii—O1—Cs3A | 100.12 (12) |
O16viii—Cs3B—O16 | 79.0 (3) | Si1—O1—Cs1xiii | 101.85 (14) |
O5ix—Cs3B—O16 | 67.0 (3) | Sn1xvii—O1—Cs1xiii | 108.13 (12) |
O3viii—Cs3B—O16 | 79.8 (3) | Cs3A—O1—Cs1xiii | 71.91 (6) |
Si2viii—Cs3B—O16 | 66.8 (2) | Si1—O1—Cs3B | 133.0 (3) |
O15viii—Cs3B—Cs1xiii | 57.45 (14) | Sn1xvii—O1—Cs3B | 93.2 (3) |
O8vii—Cs3B—Cs1xiii | 57.53 (14) | Cs3A—O1—Cs3B | 7.9 (2) |
O4viii—Cs3B—Cs1xiii | 167.5 (5) | Cs1xiii—O1—Cs3B | 70.34 (15) |
O6viii—Cs3B—Cs1xiii | 126.7 (3) | Si1—O1—Cs3Aviii | 76.02 (12) |
O1—Cs3B—Cs1xiii | 53.63 (14) | Sn1xvii—O1—Cs3Aviii | 90.90 (10) |
O16viii—Cs3B—Cs1xiii | 97.3 (2) | Cs3A—O1—Cs3Aviii | 88.33 (8) |
O5ix—Cs3B—Cs1xiii | 53.71 (15) | Cs1xiii—O1—Cs3Aviii | 154.40 (9) |
O3viii—Cs3B—Cs1xiii | 141.5 (3) | Cs3B—O1—Cs3Aviii | 92.2 (2) |
Si2viii—Cs3B—Cs1xiii | 142.4 (4) | Si1—O2—Si7 | 144.3 (2) |
O16—Cs3B—Cs1xiii | 94.8 (4) | Si1—O2—Cs1xiii | 90.29 (14) |
O15viii—Cs3B—Si1viii | 114.8 (2) | Si7—O2—Cs1xiii | 112.69 (15) |
O8vii—Cs3B—Si1viii | 145.5 (3) | Si1—O3—Si6 | 159.1 (3) |
O4viii—Cs3B—Si1viii | 25.25 (8) | Si1—O3—Cs3Bviii | 85.1 (2) |
O6viii—Cs3B—Si1viii | 70.77 (15) | Si6—O3—Cs3Bviii | 88.02 (19) |
O1—Cs3B—Si1viii | 100.8 (3) | Si1—O3—Cs3Aviii | 80.57 (13) |
O16viii—Cs3B—Si1viii | 63.64 (15) | Si6—O3—Cs3Aviii | 90.22 (14) |
O5ix—Cs3B—Si1viii | 123.9 (4) | Cs3Bviii—O3—Cs3Aviii | 7.7 (3) |
O3viii—Cs3B—Si1viii | 24.92 (7) | Si1—O4—Si2 | 129.51 (19) |
Si2viii—Cs3B—Si1viii | 46.82 (10) | Si1—O4—Cs3Bviii | 98.7 (2) |
O16—Cs3B—Si1viii | 64.7 (2) | Si2—O4—Cs3Bviii | 93.4 (2) |
Cs1xiii—Cs3B—Si1viii | 153.4 (4) | Si1—O4—Cs3Aviii | 95.66 (14) |
O8—Sn1—O22iii | 89.80 (12) | Si2—O4—Cs3Aviii | 89.04 (13) |
O8—Sn1—O1x | 177.68 (12) | Cs3Bviii—O4—Cs3Aviii | 8.8 (3) |
O22iii—Sn1—O1x | 92.32 (13) | Si1—O4—Cs2 | 112.55 (14) |
O8—Sn1—O15vi | 95.43 (12) | Si2—O4—Cs2 | 114.54 (14) |
O22iii—Sn1—O15vi | 92.48 (12) | Cs3Bviii—O4—Cs2 | 96.3 (3) |
O1x—Sn1—O15vi | 85.41 (12) | Cs3Aviii—O4—Cs2 | 105.03 (9) |
O8—Sn1—O16vi | 91.37 (12) | Si2—O5—Sn1xvii | 130.27 (17) |
O22iii—Sn1—O16vi | 176.09 (13) | Si2—O5—Cs3Aii | 123.44 (14) |
O1x—Sn1—O16vi | 86.45 (12) | Sn1xvii—O5—Cs3Aii | 106.29 (13) |
O15vi—Sn1—O16vi | 91.12 (12) | Si2—O5—Cs1iv | 99.16 (13) |
O8—Sn1—O5x | 86.35 (12) | Sn1xvii—O5—Cs1iv | 97.58 (10) |
O22iii—Sn1—O5x | 88.07 (12) | Cs3Aii—O5—Cs1iv | 69.96 (6) |
O1x—Sn1—O5x | 92.80 (12) | Si2—O5—Cs3Bii | 129.9 (3) |
O15vi—Sn1—O5x | 178.14 (12) | Sn1xvii—O5—Cs3Bii | 99.8 (3) |
O16vi—Sn1—O5x | 88.28 (12) | Cs3Aii—O5—Cs3Bii | 7.0 (2) |
O8—Sn1—Cs3Bx | 122.9 (3) | Cs1iv—O5—Cs3Bii | 67.68 (14) |
O22iii—Sn1—Cs3Bx | 125.41 (13) | Si2—O5—Cs3Aviii | 76.70 (12) |
O1x—Sn1—Cs3Bx | 56.3 (3) | Sn1xvii—O5—Cs3Aviii | 96.58 (10) |
O15vi—Sn1—Cs3Bx | 47.0 (2) | Cs3Aii—O5—Cs3Aviii | 99.33 (8) |
O16vi—Sn1—Cs3Bx | 56.66 (14) | Cs1iv—O5—Cs3Aviii | 164.22 (9) |
O5x—Sn1—Cs3Bx | 131.4 (2) | Cs3Bii—O5—Cs3Aviii | 103.00 (19) |
O8—Sn1—Cs3Ax | 129.10 (9) | Si2—O6—Si6ii | 145.3 (2) |
O22iii—Sn1—Cs3Ax | 125.11 (8) | Si2—O6—Cs3Bviii | 89.6 (2) |
O1x—Sn1—Cs3Ax | 49.99 (9) | Si6ii—O6—Cs3Bviii | 113.8 (2) |
O15vi—Sn1—Cs3Ax | 52.78 (8) | Si2—O6—Cs3Aviii | 85.23 (13) |
O16vi—Sn1—Cs3Ax | 56.45 (9) | Si6ii—O6—Cs3Aviii | 114.18 (15) |
O5x—Sn1—Cs3Ax | 125.54 (8) | Cs3Bviii—O6—Cs3Aviii | 8.5 (3) |
Cs3Bx—Sn1—Cs3Ax | 7.0 (2) | Si2—O7—Si8 | 142.1 (2) |
O8—Sn1—Cs1iii | 54.30 (9) | Si2—O7—Cs1iv | 98.93 (15) |
O22iii—Sn1—Cs1iii | 53.05 (8) | Si8—O7—Cs1iv | 118.02 (15) |
O1x—Sn1—Cs1iii | 126.61 (9) | Si3—O8—Sn1 | 128.90 (17) |
O15vi—Sn1—Cs1iii | 128.78 (8) | Si3—O8—Cs3Bxiv | 115.3 (3) |
O16vi—Sn1—Cs1iii | 125.17 (9) | Sn1—O8—Cs3Bxiv | 115.8 (3) |
O5x—Sn1—Cs1iii | 52.84 (8) | Si3—O8—Cs3Axiv | 123.52 (15) |
Cs3Bx—Sn1—Cs1iii | 175.7 (2) | Sn1—O8—Cs3Axiv | 107.58 (12) |
Cs3Ax—Sn1—Cs1iii | 176.60 (2) | Cs3Bxiv—O8—Cs3Axiv | 8.6 (3) |
O8—Sn1—Cs3Axiv | 45.47 (8) | Si3—O8—Cs1iii | 101.09 (13) |
O22iii—Sn1—Cs3Axiv | 106.03 (8) | Sn1—O8—Cs1iii | 96.22 (12) |
O1x—Sn1—Cs3Axiv | 132.83 (9) | Cs3Bxiv—O8—Cs1iii | 72.34 (19) |
O15vi—Sn1—Cs3Axiv | 135.00 (9) | Cs3Axiv—O8—Cs1iii | 69.61 (6) |
O16vi—Sn1—Cs3Axiv | 72.31 (9) | Si3—O9—Si5 | 175.2 (3) |
O5x—Sn1—Cs3Axiv | 46.38 (9) | Si4—O10—Si3 | 143.6 (2) |
Cs3Bx—Sn1—Cs3Axiv | 128.32 (11) | Si4—O10—Cs1iii | 108.30 (14) |
Cs3Ax—Sn1—Cs3Axiv | 128.760 (13) | Si3—O10—Cs1iii | 103.11 (14) |
Cs1iii—Sn1—Cs3Axiv | 52.982 (8) | Si4—O10—Cs2 | 90.03 (13) |
O8—Sn1—Cs1xi | 136.49 (8) | Si3—O10—Cs2 | 92.47 (13) |
O22iii—Sn1—Cs1xi | 72.06 (8) | Cs1iii—O10—Cs2 | 115.94 (9) |
O1x—Sn1—Cs1xi | 45.31 (8) | Si5vi—O11—Si3 | 130.59 (18) |
O15vi—Sn1—Cs1xi | 48.21 (9) | Si5vi—O11—Cs2 | 108.23 (14) |
O16vi—Sn1—Cs1xi | 109.41 (9) | Si3—O11—Cs2 | 116.67 (14) |
O5x—Sn1—Cs1xi | 130.44 (9) | Si4—O12—Sn2ix | 164.45 (19) |
Cs3Bx—Sn1—Cs1xi | 53.90 (11) | Si4—O12—Cs2 | 100.26 (13) |
Cs3Ax—Sn1—Cs1xi | 53.058 (9) | Sn2ix—O12—Cs2 | 94.97 (10) |
Cs1iii—Sn1—Cs1xi | 125.031 (10) | Si6—O13—Si4 | 138.7 (2) |
Cs3Axiv—Sn1—Cs1xi | 176.69 (2) | Si5—O14—Si4vi | 139.6 (2) |
O8—Sn1—Cs3Avi | 116.76 (8) | Si5—O14—Cs2xii | 99.13 (13) |
O22iii—Sn1—Cs3Avi | 130.18 (9) | Si4vi—O14—Cs2xii | 114.59 (14) |
O1x—Sn1—Cs3Avi | 61.07 (9) | Si5—O14—Cs1xv | 92.19 (14) |
O15vi—Sn1—Cs3Avi | 123.03 (8) | Si4vi—O14—Cs1xv | 88.28 (13) |
O16vi—Sn1—Cs3Avi | 46.12 (9) | Cs2xii—O14—Cs1xv | 122.15 (10) |
O5x—Sn1—Cs3Avi | 55.46 (8) | Si5—O15—Sn1xii | 129.25 (17) |
Cs3Bx—Sn1—Cs3Avi | 76.1 (2) | Si5—O15—Cs3Bviii | 120.2 (4) |
Cs3Ax—Sn1—Cs3Avi | 70.79 (2) | Sn1xii—O15—Cs3Bviii | 103.3 (3) |
Cs1iii—Sn1—Cs3Avi | 108.007 (10) | Si5—O15—Cs3Aviii | 128.03 (16) |
Cs3Axiv—Sn1—Cs3Avi | 74.36 (3) | Sn1xii—O15—Cs3Aviii | 97.02 (10) |
Cs1xi—Sn1—Cs3Avi | 104.687 (12) | Cs3Bviii—O15—Cs3Aviii | 8.1 (3) |
O12iii—Sn2—O12ii | 180.00 (18) | Si5—O15—Cs1xv | 111.68 (14) |
O12iii—Sn2—O20 | 88.36 (12) | Sn1xii—O15—Cs1xv | 104.69 (12) |
O12ii—Sn2—O20 | 91.64 (12) | Cs3Bviii—O15—Cs1xv | 73.1 (2) |
O12iii—Sn2—O20xi | 91.64 (12) | Cs3Aviii—O15—Cs1xv | 69.45 (6) |
O12ii—Sn2—O20xi | 88.36 (12) | Si6—O16—Sn1xii | 139.84 (18) |
O20—Sn2—O20xi | 180.0 | Si6—O16—Cs3A | 108.61 (13) |
O12iii—Sn2—O17iii | 90.26 (12) | Sn1xii—O16—Cs3A | 107.16 (12) |
O12ii—Sn2—O17iii | 89.74 (12) | Si6—O16—Cs3Bviii | 97.1 (3) |
O20—Sn2—O17iii | 85.77 (12) | Sn1xii—O16—Cs3Bviii | 92.74 (16) |
O20xi—Sn2—O17iii | 94.23 (12) | Cs3A—O16—Cs3Bviii | 102.1 (3) |
O12iii—Sn2—O17ii | 89.74 (12) | Si6—O16—Cs3Aviii | 101.94 (14) |
O12ii—Sn2—O17ii | 90.26 (12) | Sn1xii—O16—Cs3Aviii | 93.15 (10) |
O20—Sn2—O17ii | 94.23 (12) | Cs3A—O16—Cs3Aviii | 94.00 (8) |
O20xi—Sn2—O17ii | 85.77 (12) | Cs3Bviii—O16—Cs3Aviii | 8.4 (3) |
O17iii—Sn2—O17ii | 180.00 (18) | Si6—O16—Cs3B | 110.77 (18) |
O12iii—Sn2—Cs2iii | 55.33 (8) | Sn1xii—O16—Cs3B | 105.33 (17) |
O12ii—Sn2—Cs2iii | 124.67 (8) | Cs3A—O16—Cs3B | 2.28 (13) |
O20—Sn2—Cs2iii | 53.35 (9) | Cs3Bviii—O16—Cs3B | 101.0 (3) |
O20xi—Sn2—Cs2iii | 126.65 (9) | Cs3Aviii—O16—Cs3B | 92.79 (14) |
O17iii—Sn2—Cs2iii | 51.61 (8) | Si7—O17—Sn2ix | 130.26 (17) |
O17ii—Sn2—Cs2iii | 128.39 (8) | Si7—O17—Cs2 | 125.86 (15) |
O12iii—Sn2—Cs2ii | 124.67 (8) | Sn2ix—O17—Cs2 | 98.65 (10) |
O12ii—Sn2—Cs2ii | 55.33 (8) | Si7—O17—Cs2iii | 108.81 (14) |
O20—Sn2—Cs2ii | 126.65 (9) | Sn2ix—O17—Cs2iii | 104.82 (12) |
O20xi—Sn2—Cs2ii | 53.35 (9) | Cs2—O17—Cs2iii | 72.17 (6) |
O17iii—Sn2—Cs2ii | 128.39 (8) | Si7—O18—Si9 | 137.1 (2) |
O17ii—Sn2—Cs2ii | 51.61 (8) | Si7—O18—Cs1ix | 97.47 (13) |
Cs2iii—Sn2—Cs2ii | 180.0 | Si9—O18—Cs1ix | 114.47 (14) |
O12iii—Sn2—Cs2 | 109.74 (8) | Si7—O18—Cs2iii | 90.66 (13) |
O12ii—Sn2—Cs2 | 70.26 (8) | Si9—O18—Cs2iii | 93.76 (13) |
O20—Sn2—Cs2 | 45.77 (8) | Cs1ix—O18—Cs2iii | 124.26 (10) |
O20xi—Sn2—Cs2 | 134.23 (8) | Si8—O19—Si7ii | 129.52 (18) |
O17iii—Sn2—Cs2 | 47.71 (9) | Si8—O19—Cs1 | 117.12 (14) |
O17ii—Sn2—Cs2 | 132.29 (9) | Si7ii—O19—Cs1 | 109.67 (13) |
Cs2iii—Sn2—Cs2 | 54.535 (8) | Si8—O20—Sn2 | 129.48 (17) |
Cs2ii—Sn2—Cs2 | 125.465 (8) | Si8—O20—Cs2 | 122.70 (15) |
O12iii—Sn2—Cs2xi | 70.26 (8) | Sn2—O20—Cs2 | 107.37 (11) |
O12ii—Sn2—Cs2xi | 109.74 (8) | Si8—O20—Cs2iii | 103.61 (14) |
O20—Sn2—Cs2xi | 134.23 (8) | Sn2—O20—Cs2iii | 97.05 (12) |
O20xi—Sn2—Cs2xi | 45.77 (8) | Cs2—O20—Cs2iii | 72.15 (6) |
O17iii—Sn2—Cs2xi | 132.29 (9) | Si8—O21—Si9 | 151.9 (3) |
O17ii—Sn2—Cs2xi | 47.71 (9) | Si8—O21—Cs2iii | 98.65 (14) |
Cs2iii—Sn2—Cs2xi | 125.466 (8) | Si9—O21—Cs2iii | 106.27 (15) |
Cs2ii—Sn2—Cs2xi | 54.534 (8) | Si8—O21—Cs1 | 91.31 (13) |
Cs2—Sn2—Cs2xi | 180.0 | Si9—O21—Cs1 | 90.47 (13) |
O1—Si1—O2 | 110.44 (18) | Cs2iii—O21—Cs1 | 113.55 (10) |
O1—Si1—O3 | 111.15 (18) | Si9—O22—Sn1iii | 160.20 (19) |
O2—Si1—O3 | 108.86 (18) | Si9—O22—Cs1 | 102.17 (14) |
O1—Si1—O4 | 111.33 (16) | Sn1iii—O22—Cs1 | 97.49 (10) |
O2—Si1—O4 | 108.37 (18) | Si9iv—O23—Si9 | 179.5 (3) |
O3—Si1—O4 | 106.57 (18) |
Symmetry codes: (i) −x+1, y+1, −z+1/2; (ii) x, y+1, z; (iii) −x+1, −y−1, −z; (iv) −x+1, y, −z+1/2; (v) x−1/2, −y−1/2, z; (vi) −x+3/2, y+1/2, −z; (vii) x, −y−2, z+1/2; (viii) −x+3/2, −y−3/2, −z+1/2; (ix) x, y−1, z; (x) x, −y−1, z−1/2; (xi) −x+1, −y, −z; (xii) −x+3/2, y−1/2, −z; (xiii) −x+1, y−1, −z+1/2; (xiv) x, −y−2, z−1/2; (xv) x+1/2, −y−1/2, z; (xvi) −x+3/2, −y−5/2, −z+1/2; (xvii) x, −y−1, z+1/2. |
M | Ti (single-crystal data)a | Ti (powder data)b | Zrc | Th (173 K data)d | Th (293 K data)e | Uf |
Space group | C2/c | Cc | C2/m | Pca21 | Cmc21 | Cmc21 |
Z | 4 | 4 | 6 | 4 | 4 | 4 |
a | 13.386 (5) | 12.988 (2) | 26.610 (10) | 16.2920 (10) | 7.2813 (15) | 7.2717 (3) |
b | 7.423 (3) | 7.5014 (3) | 7.506 (2) | 7.2154 (6) | 16.420 (3) | 16.3061 (7) |
c | 15.134 (5) | 15.156 (3) | 11.602 (4) | 13.6800 (10) | 13.591 (3) | 13.4983 (6) |
β | 107.71 (3) | 105.80 (3) | 107.43 (2) | 90 | 90 | 90 |
V | 1432.51 | 1420.83 | 2210.92 | 1608.13 | 1624.92 | 1600.53 |
References: (a) Grey et al. (1997); (b) Nyman et al. (2000); (c) Jolicart et al. (1996); (d) Woodward et al. (2005); (e) Mann et al. (2015); (f) Liu & Lii (2011). |
Acknowledgements
The X-ray centre of the Vienna University of Technology is acknowledged for financial support and for providing access to the single-crystal and powder diffractometers.
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