Download citation
Download citation
link to html
The single-crystal structure of tetratin tetracosa­molybdenum octatriaconta­oxide, Sn4.4Mo24O38, contains infinite chains of centrosymmetric dioctahedral Mo10 and centrosymmetric trioctahedral Mo14 clusters. These clusters, as well as the O atoms, the arrangement of which derives from a closest-packing with the layer sequence ...ABAC..., form sheets parallel to the ac plane of the monoclinic unit cell. The Mo-Mo distances range from 2.6225 (7) to 2.8212 (9) Å and from 2.6270 (7) to 2.8365 (7) Å in the Mo10 and Mo14 clusters, respectively. The Mo-O distances vary between 1.949 (4) and 2.151 (4) Å in the Mo10 cluster and between 1.938 (4) and 2.140 (4) Å in the Mo14 cluster. The three crystallographically independent Sn2+ ions are off the centre of distorted oxy­gen octahedra.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270199015127/br1252sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270199015127/br1252Isup2.hkl
Contains datablock I

Comment top

Finite cluster chains built up from trans edge-shared Mo6 octahedra were first discovered in In11Mo40O62 (Mattausch et al., 1986), where tetraoctahedral Mo18 and pentaoctahedral Mo22 clusters coexist in equal proportion. Subsequently, several reduced molybdenum oxides of the form Mn-xMo4n+2O6n+4 containing finite Mo4n+2 clusters (n denotes the number of trans edge-shared Mo octahedra) with n = 1 (Lii et al., 1988), n = 2 (Hibble et al., 1988), n = 3 (Dronskowski & Simon, 1991; Schimek et al., 1995), n = 4 (Schimek et al., 1994; Fais et al., 1995) and n = 5 (Dronskowski et al., 1993; Schimek & McCarley, 1994) were synthesized by either solid state reaction or fused salt electrolysis. The final member of the series corresponds to NaMo4O6 (Torardy & McCarley, 1979), in which infinite chains of trans edge-shared Mo6 octahedra occur. While in the first members of the Mn-xMo4n+2O6n+4 series, the Mo4n+2 clusters form either zigzag (n = 1) or stair-step (n = 2 or 3) infinite chains in which the shortest Mo—Mo distances between Mo4n+2 clusters vary from 2.67 to 2.80 Å, in the compounds containing larger clusters (n = 4 or 5), intercluster distances are greater than 3 Å, leading to only weak metal-metal interaction between the Mo clusters. In the early nineties, the investigation of the Sn—Mo—O system led us to the synthesis of Sn2Mo10O16 (Gougeon et al., 1990) containing infinite stair-step chains of dioctahedral Mo10 clusters (n = 2).

Recent high-resolution electron microscopy (HREM) investigations on reduced tin oxomolybdates in the SnxMo10O16—SnyMo14O22 system revealed random and ordered intergrowth of di- and trioctahedral cluster structures (Ramlau et al., 1996). In particular, ordered regions consisting of alternating layers of di- and trioctahedral clusters were observed. The resulting structure was found to be orthorhombic, with approximate cell parameters a = 10, b = 9.3 and c = 34 Å and the composition Sn4.4Mo24O38. We present here the crystal structure of a new compound having the same composition, Sn4.4Mo24O38, (I), but crystallizing in the monoclinic system. This new compound is characterized by infinite chains based on dioctahedral Mo10 and trioctahedral Mo14 clusters.

The metal-oxygen framework of the title compound consists of infinite cluster chains built up from alternating Mo10O26 and Mo14O30 cluster units (Fig. 1) which are arranged in layers parallel to the ac plane. The oxygen network can be derived from a stacking of close-packed layers with the sequence ···ABAC··· along the b direction. While the B (y ± 1/4) and C (y ± 3/4) layers are entirely occupied by O atoms and have the composition (O24), in the A layers (y ± 0.0 and ± 1/2), ten of the 24 O atoms are missing. The Sn atoms partially occupy sites close to those of some of the missing O atoms. Within the oxygen network, half of the octahedral interstices are occupied by the atoms which form di- and trioctahedral Mo10 and Mo14 clusters (Fig. 2). The interconnection between both types of cluster units within the chains is identical to that observed between the Mo10O26 units in the series of compounds M2Mo10O16 (Hibble et al., 1988). The shortest intercluster Mo—Mo distances in the title compound are 2.7704 (6) for Mo1—Mo6, 2.9854 (7) for Mo2—Mo6, 3.0244 (7) for Mo1—Mo7, 3.0614 (7) for Mo1—Mo9 and 3.0856 (7) Å for Mo4—Mo6, while the Mo—Mo distances between adjacent Mo chains are greater than 4 Å. The Mo—Mo distances within the dioctahedral Mo10 cluster range from 2.6225 (7) to 2.8212 (9) Å, with an average distance of 2.747 Å. The Mo—O distances vary from 1.949 (4) to 2.151 (4) Å (average value 2.065 Å). In the trioctahedral cluster, the Mo—Mo distances lie in about the same range [2.6270 (7)–2.8365 (7) Å], if we preclude the non-bonding apical Mo8—Mo12 distance of 2.9972 Å.

The average Mo—Mo bond distance is 2.763?Å. The Mo—O distances vary from 1.938 (4) to 2.151?(4) Å (average value 2.058?Å). The infinite chains which run parallel to the [101] direction are then interlinked through O atoms to form layers parallel to the ac plane which are shifted by c/2 with respect to each other. This leads to one-dimensional channels delimited by the Mo—O chains, where the Sn2+ cations are distributed statistically over three crystallographically independent distorted octahedral sites. The existence of compounds with n = 2, M2Mo10O16 (M = Ca, Sr, Sn, Pb, La, Ce, Pr, Nd, Sm, Eu or Gd; Gall, 1993) and n = 3, K3 - xMxMo14O22 (x = 0, x = 1.34 for M = Pb and x = 1.71 for M = Sn; Schimek et al., 1995) and Tl1.6Sn1.2 Mo14O22 (Dronskowski & Simon, 1991), containing, respectively, only Mo10 and Mo14 clusters with different electron counts, leads us to a comparative study of the Mo—Mo distances in the last two series of compounds with those in Sn4.4Mo24O38 for each cluster-type. This study clearly revealed that the different Mo—Mo distances within the Mo10 and Mo14 clusters present in Sn4.4Mo24O38 compare well with those observed in M2Mo10O16 (M is a divalent cation) for the dioctahedron cluster and with those in K1.66Pb1.34Mo14O22 for the trioctahedron. Consequently, we can roughly estimate a number of 32 and 44.3 electrons per Mo10 and Mo14 cluster, respectively. These values lead to a total of 76.3 electrons and to the hypothetical formula Sn2Mo10O16 Sn2.15Mo14O22. The excess of electrons brought by the supplementary 0.25 Sn in the investigated compound are accommodated in the intercluster bonds, as confirmed by the shorter intercluster bonds observed in the title compound compared with those in Sn2Mo10O16 and K1.66Pb1.34Mo14O22. By using the Pauling bond order (Pauling, 1960), we could estimate the excess to be about 0.7 electron, leading to 77 electrons on the Mo network. This value is close to that of 76.8 electrons based on the stoichiometry, given Sn2+ and O2-. In addition, the valences of the 12 crystallographically independent Mo atoms were calculated from the Mo—O bond lengths using the relationship of Brown & Wu (1976). This yields an average value of 2.785 and thus a total of 77 electrons on the Mo network, which is in good agreement with the previous two values.

In summary, the combination of di- and trioctahedral clusters forming infinite chains is unprecedented in reduced molybdenum oxide chemistry. This discovery suggests the synthesis of new compounds with zigzag or stair-step chains based on different types of multioctahedral Mo4n+2 clusters. Another interesting perspective would be to modify the number of electrons on the Mo10 and Mo14 clusters in this new compound. Indeed, this could lead to various electrical resistivity behaviours, as in the series M2Mo10O16 (McCarroll et al., 1998).

Experimental top

Single crystals of Sn4.4Mo24O38 were obtained from a mixture of SnO2 MoO3 and Mo, all in powder form, in the ratio 4:1:3. Before use, the Mo powder was reduced under H2 flux at 1273 K for 10 h in order to eliminate any trace of oxygen. Starting reagents were mixed, ground together in a mortar and then cold-pressed using a hand press. The pellet was then loaded in a Mo crucible which was sealed under a low argon pressure using an arc welding system. The crucible was heated at a rate of 300 K/h to 2073 K and held there for 6 h, then cooled at 100 K/h to 1300 K and finally furnace-cooled to room temperature.

Computing details top

Data collection: CAD-4 Software (Enraf-Nonius, 1989); cell refinement: CAD-4 Software; data reduction: MolEN (Fair, 1990); program(s) used to solve structure: SHELXS86 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.

Figures top
[Figure 1] Fig. 1. View of (a) the Mo10 and (b) the Mo14 clusters with their oxygen environment. Displacement ellipsoids are drawn at the 97% probability level [symmetry code: (i) -x, 1/2 + y, 1/2 - z].
[Figure 2] Fig. 2. A projection of the Mo network and Sn atoms (unconnected ellipsoids) on the ac plane (O atoms omitted for clarity). Clusters whose centre lies in the plane y = 0 are represented by black lines, those whose centre is at y = 0.5 by a light grey line. Only Mo—Mo bonds of less than 2.9 Å are drawn. Sn atoms at y ~0 and ~0.5 are represented as black and grey ellipsoids, respectively (97% probability level).
tetratintetracosamolybdenumoctatriacontaoxide top
Crystal data top
Sn4.4Mo24O38F(000) = 3064
Mr = 3433.04Dx = 7.243 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
a = 17.806 (2) ÅCell parameters from 25 reflections
b = 9.2562 (6) Åθ = 10–27°
c = 9.9337 (13) ŵ = 12.72 mm1
β = 105.955 (6)°T = 293 K
V = 1574.2 (3) Å3Irregular, black
Z = 20.14 × 0.12 × 0.08 mm
Data collection top
Enraf-Nonius CAD-4
diffractometer
4519 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.021
Graphite monochromatorθmax = 32.0°, θmin = 1.2°
θ–2θ scansh = 2625
Absorption correction: ψ-scan
(North et al., 1968)
k = 130
Tmin = 0.260, Tmax = 0.361l = 014
5726 measured reflections3 standard reflections every 60 min
5446 independent reflections intensity decay: <1
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.032Calculated w = 1/[σ2(Fo2) + (0.0169P)2 + 28.2165P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.077(Δ/σ)max = 0.001
S = 1.25Δρmax = 2.90 e Å3
5446 reflectionsΔρmin = 2.08 e Å3
216 parametersExtinction correction: SHELXL97 (Sheldrick, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction coefficient: 0.00116 (3)
Crystal data top
Sn4.4Mo24O38V = 1574.2 (3) Å3
Mr = 3433.04Z = 2
Monoclinic, P21/cMo Kα radiation
a = 17.806 (2) ŵ = 12.72 mm1
b = 9.2562 (6) ÅT = 293 K
c = 9.9337 (13) Å0.14 × 0.12 × 0.08 mm
β = 105.955 (6)°
Data collection top
Enraf-Nonius CAD-4
diffractometer
4519 reflections with I > 2σ(I)
Absorption correction: ψ-scan
(North et al., 1968)
Rint = 0.021
Tmin = 0.260, Tmax = 0.3613 standard reflections every 60 min
5726 measured reflections intensity decay: <1
5446 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.032216 parameters
wR(F2) = 0.0770 restraints
S = 1.25Δρmax = 2.90 e Å3
5446 reflectionsΔρmin = 2.08 e Å3
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Data were corrected for Lorentz and polarization effects. An absorption correction was applied using Ψ scans of nine reflections (North et al., 1968). The structure was solved with SHELXS86 (Sheldrick, 1990) and subsequent difference Fourier syntheses. Calculations were performed on a Digital Pentium Celebris 590 FP for SHELXL97 (Sheldrick, 1997) and on a Digital MicroVAX 3100 for the MolEN (Fair, 1989) programs. 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) top
xyzUiso*/UeqOcc. (<1)
Sn10.79339 (3)0.52148 (5)0.85716 (5)0.01178 (14)0.915 (3)
Sn20.60513 (4)0.01963 (7)0.09937 (6)0.0231 (2)0.866 (3)
Sn30.98697 (12)0.9909 (2)0.52331 (19)0.0407 (6)0.420 (3)
Mo10.33782 (3)0.38492 (5)0.83826 (5)0.00293 (9)
Mo20.65798 (3)0.38322 (5)0.99570 (5)0.00279 (9)
Mo30.42064 (3)0.36899 (5)0.11544 (5)0.00252 (9)
Mo40.42631 (3)0.62177 (5)0.80189 (5)0.00270 (9)
Mo50.49956 (2)0.37854 (5)0.91403 (4)0.00258 (9)
Mo60.75381 (3)0.38678 (5)0.29398 (5)0.00289 (9)
Mo70.75665 (3)0.61683 (5)0.46555 (5)0.00296 (9)
Mo80.83073 (3)0.36824 (5)0.56910 (5)0.00358 (9)
Mo90.84082 (3)0.62321 (5)0.26114 (5)0.00364 (9)
Mo100.91739 (2)0.37789 (5)0.37531 (5)0.00291 (9)
Mo110.91831 (3)0.61348 (5)0.54475 (5)0.00295 (9)
Mo120.99423 (3)0.62794 (5)0.34119 (5)0.00460 (9)
O10.7500 (2)0.2456 (4)0.7967 (4)0.0052 (7)*
O20.2454 (2)0.9976 (5)0.3893 (4)0.0058 (7)*
O30.2509 (2)0.2450 (4)0.5486 (4)0.0047 (7)*
O40.6668 (2)0.2437 (4)0.0085 (4)0.0048 (7)*
O50.3339 (2)0.9952 (5)0.6672 (4)0.0055 (7)*
O60.3388 (2)0.4993 (4)0.6554 (4)0.0048 (7)*
O70.3350 (2)0.2436 (4)0.3364 (4)0.0051 (7)*
O80.4166 (2)0.2515 (4)0.7883 (4)0.0046 (7)*
O90.5840 (2)0.2519 (4)0.8740 (4)0.0050 (7)*
O100.4979 (2)0.2672 (4)0.4295 (4)0.0047 (7)*
O110.5059 (2)0.5019 (4)0.7413 (4)0.0053 (7)*
O120.7513 (2)0.9923 (4)0.1256 (4)0.0054 (7)*
O130.1686 (2)0.2527 (4)0.7526 (4)0.0051 (7)*
O140.8328 (2)0.2588 (5)0.5891 (4)0.0060 (7)*
O150.0832 (2)0.2419 (5)0.4625 (4)0.0061 (7)*
O160.9153 (2)0.4834 (5)0.7088 (4)0.0056 (7)*
O170.9195 (2)0.0014 (5)0.6999 (4)0.0056 (7)*
O180.9148 (2)0.2651 (5)0.8891 (4)0.0054 (7)*
O190.0022 (2)0.2530 (4)0.3311 (4)0.0060 (7)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sn10.0129 (2)0.0130 (2)0.0103 (2)0.00053 (16)0.00465 (16)0.00035 (16)
Sn20.0403 (4)0.0192 (3)0.0106 (3)0.0008 (2)0.0084 (2)0.0008 (2)
Sn30.0536 (12)0.0392 (10)0.0394 (11)0.0020 (8)0.0299 (8)0.0019 (8)
Mo10.00315 (18)0.00318 (19)0.00212 (18)0.00039 (14)0.00017 (14)0.00051 (14)
Mo20.00260 (18)0.00319 (19)0.00227 (18)0.00048 (14)0.00015 (14)0.00011 (14)
Mo30.00273 (17)0.00285 (18)0.00173 (18)0.00020 (14)0.00021 (13)0.00031 (14)
Mo40.00281 (18)0.00315 (19)0.00172 (18)0.00001 (14)0.00007 (13)0.00049 (14)
Mo50.00279 (18)0.00294 (19)0.00178 (18)0.00004 (14)0.00023 (14)0.00028 (14)
Mo60.00290 (18)0.00318 (19)0.00226 (18)0.00023 (14)0.00013 (14)0.00038 (14)
Mo70.00289 (18)0.00311 (19)0.00257 (18)0.00012 (14)0.00024 (14)0.00019 (14)
Mo80.00493 (18)0.00332 (19)0.00251 (18)0.00061 (15)0.00107 (14)0.00028 (14)
Mo90.00537 (19)0.0033 (2)0.00199 (18)0.00049 (14)0.00058 (14)0.00025 (14)
Mo100.00295 (18)0.0035 (2)0.00201 (18)0.00028 (14)0.00019 (14)0.00005 (14)
Mo110.00309 (18)0.00324 (19)0.00217 (18)0.00001 (14)0.00015 (14)0.00003 (14)
Mo120.0079 (2)0.0032 (2)0.00293 (19)0.00013 (15)0.00179 (15)0.00048 (15)
Geometric parameters (Å, º) top
Sn1—O5i2.217 (4)Mo9—O1xv2.083 (4)
Sn1—O12ii2.231 (4)Mo9—O14xv2.093 (4)
Sn1—O1iii2.313 (4)Mo9—O2xviii2.140 (4)
Sn2—O5iv2.286 (4)Mo9—Mo122.6270 (7)
Sn2—O7v2.444 (4)Mo9—Mo102.7297 (7)
Sn2—O12iii2.545 (4)Mo9—Mo112.7770 (7)
Sn2—O11vi2.551 (4)Mo9—Mo1xiii3.0614 (7)
Sn3—Sn3vii0.759 (3)Mo10—O19xx2.044 (4)
Sn3—O17viii2.384 (4)Mo10—O15ix2.047 (4)
Sn3—O15iv2.514 (5)Mo10—O13ix2.057 (4)
Mo1—O4ix2.025 (4)Mo10—O17xv2.079 (4)
Mo1—O82.030 (4)Mo10—Mo112.7519 (7)
Mo1—O6iii2.114 (4)Mo10—Mo122.7566 (7)
Mo1—O2ii2.124 (4)Mo10—Mo11xix2.8140 (7)
Mo1—O1x2.133 (4)Mo10—Mo12xix2.8238 (7)
Mo1—Mo2xi2.6952 (7)Mo11—O19xiii2.023 (4)
Mo1—Mo3xii2.7469 (7)Mo11—O162.038 (4)
Mo1—Mo52.7698 (7)Mo11—O14iii2.069 (4)
Mo1—Mo6xiii2.7704 (6)Mo11—O18xv2.077 (4)
Mo1—Mo42.7807 (7)Mo11—Mo122.7270 (7)
Mo1—Mo7xiii3.0244 (7)Mo11—Mo12xix2.7807 (7)
Mo1—Mo9xiii3.0614 (7)Mo11—Mo10xix2.8140 (7)
Mo2—O91.949 (4)Mo12—O17xv2.037 (4)
Mo2—O5i2.008 (4)Mo12—O18xv2.051 (4)
Mo2—O7x2.015 (4)Mo12—O19v2.081 (4)
Mo2—O2i2.098 (4)Mo12—O16xix2.084 (4)
Mo2—O3x2.151 (4)Mo12—O15xxi2.089 (4)
Mo2—Mo1xi2.6952 (7)Mo12—Mo11xix2.7807 (7)
Mo2—Mo52.7127 (7)Mo12—Mo10xix2.8238 (7)
Mo2—Mo3xiii2.7550 (7)Mo12—Mo8xix2.9972 (7)
Mo2—Mo4xi2.8207 (7)O1—Mo7xvii2.034 (4)
Mo2—Mo6xii2.9854 (7)O1—Mo9xvii2.083 (4)
Mo3—O11ix2.056 (4)O1—Mo1xxii2.133 (4)
Mo3—O4xiv2.057 (4)O1—Sn1viii2.313 (4)
Mo3—O10v2.061 (4)O2—Mo2xxiii2.098 (4)
Mo3—O8xv2.065 (4)O2—Mo6xxiv2.115 (4)
Mo3—O5vi2.110 (4)O2—Mo1vi2.124 (4)
Mo3—Mo4xiii2.6225 (7)O2—Mo9xxiv2.140 (4)
Mo3—Mo5xvi2.7443 (7)O3—Mo8ix1.962 (4)
Mo3—Mo1xvi2.7469 (7)O3—Mo6ix2.061 (4)
Mo3—Mo2xiii2.7550 (7)O3—Mo2xxii2.151 (4)
Mo3—Mo5xiii2.7919 (7)O4—Mo1ix2.025 (4)
Mo4—O11iii2.037 (4)O4—Mo3xiv2.057 (4)
Mo4—O10xvii2.038 (4)O4—Mo7xv2.121 (4)
Mo4—O7xvii2.082 (4)O5—Mo2xxiii2.008 (4)
Mo4—O9x2.088 (4)O5—Mo3ii2.110 (4)
Mo4—O6iii2.134 (4)O5—Sn1xxiii2.217 (4)
Mo4—Mo3xiii2.6225 (7)O5—Sn2iv2.286 (4)
Mo4—Mo52.6855 (7)O6—Mo7ix2.096 (4)
Mo4—Mo5xi2.7673 (7)O6—Mo1viii2.114 (4)
Mo4—Mo2xi2.8207 (7)O6—Mo6ix2.124 (4)
Mo4—Mo6xiii3.0856 (7)O6—Mo4viii2.134 (4)
Mo5—O82.028 (4)O7—Mo2xxii2.015 (4)
Mo5—O92.030 (4)O7—Mo4xv2.082 (4)
Mo5—O10x2.049 (4)O7—Mo6xxv2.123 (4)
Mo5—O11iii2.071 (4)O7—Sn2xxv2.444 (4)
Mo5—Mo3xii2.7443 (7)O8—Mo3xvii2.065 (4)
Mo5—Mo4xi2.7673 (7)O9—Mo4xxii2.088 (4)
Mo5—Mo3xiii2.7919 (7)O10—Mo4xv2.038 (4)
Mo5—Mo5xi2.8212 (9)O10—Mo5xxii2.049 (4)
Mo6—O13ix2.003 (4)O10—Mo3xxv2.061 (4)
Mo6—O3ix2.061 (4)O11—Mo4viii2.037 (4)
Mo6—O2xviii2.115 (4)O11—Mo3ix2.056 (4)
Mo6—O7v2.123 (4)O11—Mo5viii2.071 (4)
Mo6—O6ix2.124 (4)O11—Sn2ii2.551 (4)
Mo6—Mo82.7049 (7)O12—Mo7vi1.987 (4)
Mo6—Mo72.7192 (7)O12—Mo8vi2.018 (4)
Mo6—Mo92.7520 (7)O12—Sn1vi2.231 (4)
Mo6—Mo1xiii2.7704 (6)O12—Sn2viii2.545 (4)
Mo6—Mo102.8016 (7)O13—Mo6ix2.003 (4)
Mo6—Mo2xvi2.9854 (7)O13—Mo10ix2.057 (4)
Mo6—Mo4xiii3.0856 (7)O13—Mo8xxii2.093 (4)
Mo7—O14iii1.938 (4)O14—Mo7viii1.938 (4)
Mo7—O12ii1.987 (4)O14—Mo11viii2.069 (4)
Mo7—O1xv2.034 (4)O14—Mo9xvii2.093 (4)
Mo7—O6ix2.096 (4)O15—Mo8ix2.020 (4)
Mo7—O4xvii2.121 (4)O15—Mo10ix2.047 (4)
Mo7—Mo82.7105 (7)O15—Mo12xxvi2.089 (4)
Mo7—Mo112.7679 (7)O15—Sn3iv2.514 (5)
Mo7—Mo92.8365 (7)O16—Mo12xix2.084 (4)
Mo7—Mo1xiii3.0244 (7)O17—Mo9xvii2.032 (4)
Mo8—O3ix1.962 (4)O17—Mo12xvii2.037 (4)
Mo8—O12ii2.018 (4)O17—Mo10xvii2.079 (4)
Mo8—O15ix2.020 (4)O17—Sn3iii2.384 (4)
Mo8—O162.044 (4)O18—Mo9xvii2.038 (4)
Mo8—O13x2.093 (4)O18—Mo12xvii2.051 (4)
Mo8—Mo102.7798 (7)O18—Mo11xvii2.077 (4)
Mo8—Mo112.8019 (7)O19—Mo11xiii2.023 (4)
Mo8—Mo12xix2.9972 (7)O19—Mo10xxvii2.044 (4)
Mo9—O17xv2.032 (4)O19—Mo12xxv2.081 (4)
Mo9—O18xv2.038 (4)
O5i—Sn1—O12ii80.52 (14)O4xvii—Mo7—Mo11137.09 (11)
O5i—Sn1—O1iii77.18 (15)Mo8—Mo7—Mo1161.509 (17)
O12ii—Sn1—O1iii81.47 (15)Mo6—Mo7—Mo1190.462 (19)
O5iv—Sn2—O7v76.83 (14)O14iii—Mo7—Mo991.47 (12)
O5iv—Sn2—O12iii72.82 (13)O12ii—Mo7—Mo9137.39 (12)
O7v—Sn2—O12iii69.65 (13)O1xv—Mo7—Mo947.17 (11)
O5iv—Sn2—O11vi68.96 (13)O6ix—Mo7—Mo996.05 (11)
O7v—Sn2—O11vi103.40 (13)O4xvii—Mo7—Mo9135.15 (11)
O12iii—Sn2—O11vi141.70 (13)Mo8—Mo7—Mo989.515 (19)
Sn3vii—Sn3—O17viii163.5 (4)Mo6—Mo7—Mo959.340 (16)
Sn3vii—Sn3—O15iv128.3 (3)Mo11—Mo7—Mo959.391 (17)
O17viii—Sn3—O15iv68.00 (14)O14iii—Mo7—Mo1xiii137.35 (13)
O4ix—Mo1—O887.97 (16)O12ii—Mo7—Mo1xiii131.25 (12)
O4ix—Mo1—O6iii170.08 (16)O1xv—Mo7—Mo1xiii44.77 (12)
O8—Mo1—O6iii85.91 (16)O6ix—Mo7—Mo1xiii44.31 (11)
O4ix—Mo1—O2ii86.76 (16)O4xvii—Mo7—Mo1xiii87.72 (11)
O8—Mo1—O2ii171.77 (16)Mo8—Mo7—Mo1xiii116.96 (2)
O6iii—Mo1—O2ii98.41 (16)Mo6—Mo7—Mo1xiii57.381 (16)
O4ix—Mo1—O1x86.15 (16)Mo11—Mo7—Mo1xiii122.23 (2)
O8—Mo1—O1x86.45 (15)Mo9—Mo7—Mo1xiii62.883 (18)
O6iii—Mo1—O1x85.68 (15)O3ix—Mo8—O12ii92.01 (16)
O2ii—Mo1—O1x86.91 (15)O3ix—Mo8—O15ix92.32 (16)
O4ix—Mo1—Mo2xi93.10 (12)O12ii—Mo8—O15ix173.08 (16)
O8—Mo1—Mo2xi136.82 (11)O3ix—Mo8—O16174.09 (17)
O6iii—Mo1—Mo2xi96.70 (11)O12ii—Mo8—O1687.50 (16)
O2ii—Mo1—Mo2xi49.90 (11)O15ix—Mo8—O1687.64 (16)
O1x—Mo1—Mo2xi136.72 (11)O3ix—Mo8—O13x91.38 (16)
O4ix—Mo1—Mo3xii48.19 (12)O12ii—Mo8—O13x84.84 (16)
O8—Mo1—Mo3xii89.76 (11)O15ix—Mo8—O13x89.66 (16)
O6iii—Mo1—Mo3xii139.44 (11)O16—Mo8—O13x82.71 (16)
O2ii—Mo1—Mo3xii91.41 (11)O3ix—Mo8—Mo649.31 (12)
O1x—Mo1—Mo3xii134.31 (11)O12ii—Mo8—Mo692.63 (11)
Mo2xi—Mo1—Mo3xii60.817 (17)O15ix—Mo8—Mo694.29 (12)
O4ix—Mo1—Mo592.05 (11)O16—Mo8—Mo6136.59 (12)
O8—Mo1—Mo546.91 (11)O13x—Mo8—Mo6140.57 (11)
O6iii—Mo1—Mo589.47 (10)O3ix—Mo8—Mo793.65 (12)
O2ii—Mo1—Mo5139.60 (11)O12ii—Mo8—Mo746.93 (11)
O1x—Mo1—Mo5133.35 (11)O15ix—Mo8—Mo7138.03 (12)
Mo2xi—Mo1—Mo589.933 (19)O16—Mo8—Mo790.32 (12)
Mo3xii—Mo1—Mo559.661 (16)O13x—Mo8—Mo7131.62 (11)
O4ix—Mo1—Mo6xiii135.12 (11)Mo6—Mo8—Mo760.281 (17)
O8—Mo1—Mo6xiii134.78 (11)O3ix—Mo8—Mo1093.86 (12)
O6iii—Mo1—Mo6xiii49.35 (11)O12ii—Mo8—Mo10137.68 (12)
O2ii—Mo1—Mo6xiii49.06 (11)O15ix—Mo8—Mo1047.28 (12)
O1x—Mo1—Mo6xiii84.23 (11)O16—Mo8—Mo1090.45 (11)
Mo2xi—Mo1—Mo6xiii66.199 (18)O13x—Mo8—Mo10136.75 (11)
Mo3xii—Mo1—Mo6xiii126.88 (2)Mo6—Mo8—Mo1061.417 (18)
Mo5—Mo1—Mo6xiii125.31 (2)Mo7—Mo8—Mo1090.848 (19)
O4ix—Mo1—Mo4138.42 (12)O3ix—Mo8—Mo11139.33 (12)
O8—Mo1—Mo489.63 (11)O12ii—Mo8—Mo1190.71 (12)
O6iii—Mo1—Mo449.43 (11)O15ix—Mo8—Mo1189.52 (12)
O2ii—Mo1—Mo498.50 (11)O16—Mo8—Mo1146.57 (11)
O1x—Mo1—Mo4135.11 (11)O13x—Mo8—Mo11129.26 (11)
Mo2xi—Mo1—Mo461.985 (17)Mo6—Mo8—Mo1190.036 (19)
Mo3xii—Mo1—Mo490.304 (19)Mo7—Mo8—Mo1160.254 (17)
Mo5—Mo1—Mo457.871 (16)Mo10—Mo8—Mo1159.078 (16)
Mo6xiii—Mo1—Mo467.538 (18)O3ix—Mo8—Mo12xix136.38 (12)
O4ix—Mo1—Mo7xiii128.34 (12)O12ii—Mo8—Mo12xix131.45 (11)
O8—Mo1—Mo7xiii89.13 (11)O15ix—Mo8—Mo12xix44.08 (12)
O6iii—Mo1—Mo7xiii43.85 (11)O16—Mo8—Mo12xix43.98 (11)
O2ii—Mo1—Mo7xiii89.20 (11)O13x—Mo8—Mo12xix89.51 (11)
O1x—Mo1—Mo7xiii42.19 (11)Mo6—Mo8—Mo12xix119.74 (2)
Mo2xi—Mo1—Mo7xiii121.95 (2)Mo7—Mo8—Mo12xix117.43 (2)
Mo3xii—Mo1—Mo7xiii176.41 (2)Mo10—Mo8—Mo12xix58.380 (17)
Mo5—Mo1—Mo7xiii121.51 (2)Mo11—Mo8—Mo12xix57.188 (16)
Mo6xiii—Mo1—Mo7xiii55.764 (15)O17xv—Mo9—O18xv99.90 (16)
Mo4—Mo1—Mo7xiii93.106 (19)O17xv—Mo9—O1xv172.14 (16)
O4ix—Mo1—Mo9xiii88.48 (11)O18xv—Mo9—O1xv86.72 (16)
O8—Mo1—Mo9xiii129.24 (11)O17xv—Mo9—O14xv89.65 (16)
O6iii—Mo1—Mo9xiii89.35 (11)O18xv—Mo9—O14xv90.58 (16)
O2ii—Mo1—Mo9xiii44.32 (11)O1xv—Mo9—O14xv86.02 (16)
O1x—Mo1—Mo9xiii42.80 (11)O17xv—Mo9—O2xviii85.15 (16)
Mo2xi—Mo1—Mo9xiii93.930 (18)O18xv—Mo9—O2xviii171.37 (16)
Mo3xii—Mo1—Mo9xiii123.09 (2)O1xv—Mo9—O2xviii87.77 (16)
Mo5—Mo1—Mo9xiii176.07 (2)O14xv—Mo9—O2xviii82.41 (16)
Mo6xiii—Mo1—Mo9xiii56.047 (15)O17xv—Mo9—Mo1249.87 (11)
Mo4—Mo1—Mo9xiii123.58 (2)O18xv—Mo9—Mo1250.24 (11)
Mo7xiii—Mo1—Mo9xiii55.557 (15)O1xv—Mo9—Mo12136.96 (11)
O9—Mo2—O5i92.05 (17)O14xv—Mo9—Mo1293.97 (11)
O9—Mo2—O7x91.60 (17)O2xviii—Mo9—Mo12134.98 (11)
O5i—Mo2—O7x172.46 (16)O17xv—Mo9—Mo1049.13 (11)
O9—Mo2—O2i168.23 (16)O18xv—Mo9—Mo1096.52 (12)
O5i—Mo2—O2i85.06 (16)O1xv—Mo9—Mo10134.77 (11)
O7x—Mo2—O2i90.04 (16)O14xv—Mo9—Mo10138.78 (11)
O9—Mo2—O3x87.02 (16)O2xviii—Mo9—Mo1092.08 (11)
O5i—Mo2—O3x85.34 (16)Mo12—Mo9—Mo1061.906 (17)
O7x—Mo2—O3x88.27 (16)O17xv—Mo9—Mo692.33 (12)
O2i—Mo2—O3x81.39 (15)O18xv—Mo9—Mo6136.63 (12)
O9—Mo2—Mo1xi140.94 (12)O1xv—Mo9—Mo685.62 (11)
O5i—Mo2—Mo1xi92.91 (12)O14xv—Mo9—Mo6131.23 (11)
O7x—Mo2—Mo1xi88.40 (12)O2xviii—Mo9—Mo649.32 (11)
O2i—Mo2—Mo1xi50.75 (11)Mo12—Mo9—Mo6123.35 (2)
O3x—Mo2—Mo1xi132.00 (11)Mo10—Mo9—Mo661.472 (17)
O9—Mo2—Mo548.28 (12)O17xv—Mo9—Mo1195.41 (11)
O5i—Mo2—Mo593.86 (11)O18xv—Mo9—Mo1148.14 (12)
O7x—Mo2—Mo593.49 (11)O1xv—Mo9—Mo1192.17 (11)
O2i—Mo2—Mo5143.21 (11)O14xv—Mo9—Mo11138.69 (12)
O3x—Mo2—Mo5135.28 (11)O2xviii—Mo9—Mo11138.82 (11)
Mo1xi—Mo2—Mo592.717 (19)Mo12—Mo9—Mo1160.536 (17)
O9—Mo2—Mo3xiii95.05 (12)Mo10—Mo9—Mo1159.959 (16)
O5i—Mo2—Mo3xiii49.61 (12)Mo6—Mo9—Mo1189.593 (19)
O7x—Mo2—Mo3xiii136.51 (12)O17xv—Mo9—Mo7138.21 (12)
O2i—Mo2—Mo3xiii91.75 (11)O18xv—Mo9—Mo786.87 (11)
O3x—Mo2—Mo3xiii134.92 (11)O1xv—Mo9—Mo745.74 (11)
Mo1xi—Mo2—Mo3xiii60.519 (18)O14xv—Mo9—Mo7131.76 (11)
Mo5—Mo2—Mo3xiii61.404 (17)O2xviii—Mo9—Mo794.02 (11)
O9—Mo2—Mo4xi91.76 (12)Mo12—Mo9—Mo7119.58 (2)
O5i—Mo2—Mo4xi138.92 (12)Mo10—Mo9—Mo789.261 (19)
O7x—Mo2—Mo4xi47.49 (11)Mo6—Mo9—Mo758.207 (16)
O2i—Mo2—Mo4xi97.92 (11)Mo11—Mo9—Mo759.074 (18)
O3x—Mo2—Mo4xi135.72 (11)O17xv—Mo9—Mo1xiii129.03 (11)
Mo1xi—Mo2—Mo4xi60.497 (17)O18xv—Mo9—Mo1xiii130.78 (11)
Mo5—Mo2—Mo4xi59.977 (17)O1xv—Mo9—Mo1xiii44.08 (11)
Mo3xiii—Mo2—Mo4xi89.311 (19)O14xv—Mo9—Mo1xiii85.39 (11)
O9—Mo2—Mo6xii136.65 (12)O2xviii—Mo9—Mo1xiii43.90 (11)
O5i—Mo2—Mo6xii130.18 (12)Mo12—Mo9—Mo1xiii178.76 (2)
O7x—Mo2—Mo6xii45.29 (12)Mo10—Mo9—Mo1xiii118.01 (2)
O2i—Mo2—Mo6xii45.12 (11)Mo6—Mo9—Mo1xiii56.620 (16)
O3x—Mo2—Mo6xii87.24 (11)Mo11—Mo9—Mo1xiii120.59 (2)
Mo1xi—Mo2—Mo6xii58.109 (16)Mo7—Mo9—Mo1xiii61.560 (17)
Mo5—Mo2—Mo6xii124.11 (2)O19xx—Mo10—O15ix89.17 (16)
Mo3xiii—Mo2—Mo6xii118.52 (2)O19xx—Mo10—O13ix91.02 (16)
Mo4xi—Mo2—Mo6xii64.132 (18)O15ix—Mo10—O13ix88.61 (16)
O11ix—Mo3—O4xiv169.95 (16)O19xx—Mo10—O17xv86.51 (16)
O11ix—Mo3—O10v99.45 (16)O15ix—Mo10—O17xv174.51 (16)
O4xiv—Mo3—O10v89.27 (16)O13ix—Mo10—O17xv88.09 (16)
O11ix—Mo3—O8xv84.77 (16)O19xx—Mo10—Mo9134.06 (12)
O4xiv—Mo3—O8xv89.96 (16)O15ix—Mo10—Mo9136.76 (12)
O10v—Mo3—O8xv92.13 (16)O13ix—Mo10—Mo990.56 (12)
O11ix—Mo3—O5vi82.49 (15)O17xv—Mo10—Mo947.68 (11)
O4xiv—Mo3—O5vi88.49 (16)O19xx—Mo10—Mo11134.36 (12)
O10v—Mo3—O5vi175.82 (16)O15ix—Mo10—Mo1190.36 (12)
O8xv—Mo3—O5vi84.34 (15)O13ix—Mo10—Mo11134.59 (11)
O11ix—Mo3—Mo4xiii49.83 (11)O17xv—Mo10—Mo1195.08 (12)
O4xiv—Mo3—Mo4xiii139.12 (11)Mo9—Mo10—Mo1160.875 (18)
O10v—Mo3—Mo4xiii49.85 (11)O19xx—Mo10—Mo1291.56 (12)
O8xv—Mo3—Mo4xiii91.62 (11)O15ix—Mo10—Mo12136.32 (12)
O5vi—Mo3—Mo4xiii132.30 (11)O13ix—Mo10—Mo12135.02 (12)
O11ix—Mo3—Mo5xvi97.44 (11)O17xv—Mo10—Mo1247.31 (11)
O4xiv—Mo3—Mo5xvi92.10 (11)Mo9—Mo10—Mo1257.217 (18)
O10v—Mo3—Mo5xvi47.93 (11)Mo11—Mo10—Mo1259.346 (17)
O8xv—Mo3—Mo5xvi139.95 (11)O19xx—Mo10—Mo8135.61 (12)
O5vi—Mo3—Mo5xvi135.69 (11)O15ix—Mo10—Mo846.47 (11)
Mo4xiii—Mo3—Mo5xvi62.031 (18)O13ix—Mo10—Mo887.06 (11)
O11ix—Mo3—Mo1xvi136.54 (11)O17xv—Mo10—Mo8137.64 (11)
O4xiv—Mo3—Mo1xvi47.22 (11)Mo9—Mo10—Mo890.317 (19)
O10v—Mo3—Mo1xvi91.81 (11)Mo11—Mo10—Mo860.860 (17)
O8xv—Mo3—Mo1xvi136.92 (11)Mo12—Mo10—Mo8120.06 (2)
O5vi—Mo3—Mo1xvi89.26 (11)O19xx—Mo10—Mo6136.55 (12)
Mo4xiii—Mo3—Mo1xvi122.51 (2)O15ix—Mo10—Mo690.87 (11)
Mo5xvi—Mo3—Mo1xvi60.584 (18)O13ix—Mo10—Mo645.56 (11)
O11ix—Mo3—Mo2xiii86.32 (11)O17xv—Mo10—Mo689.95 (11)
O4xiv—Mo3—Mo2xiii90.69 (11)Mo9—Mo10—Mo659.657 (16)
O10v—Mo3—Mo2xiii137.12 (11)Mo11—Mo10—Mo689.087 (19)
O8xv—Mo3—Mo2xiii130.75 (11)Mo12—Mo10—Mo6116.85 (2)
O5vi—Mo3—Mo2xiii46.46 (11)Mo8—Mo10—Mo657.975 (17)
Mo4xiii—Mo3—Mo2xiii117.91 (2)O19xx—Mo10—Mo11xix45.90 (12)
Mo5xvi—Mo3—Mo2xiii89.233 (19)O15ix—Mo10—Mo11xix91.45 (11)
Mo1xvi—Mo3—Mo2xiii58.663 (16)O13ix—Mo10—Mo11xix136.90 (11)
O11ix—Mo3—Mo5xiii47.65 (11)O17xv—Mo10—Mo11xix87.97 (11)
O4xiv—Mo3—Mo5xiii137.10 (11)Mo9—Mo10—Mo11xix117.09 (2)
O10v—Mo3—Mo5xiii94.62 (11)Mo11—Mo10—Mo11xix88.506 (19)
O8xv—Mo3—Mo5xiii132.41 (11)Mo12—Mo10—Mo11xix59.881 (17)
O5vi—Mo3—Mo5xiii89.42 (11)Mo8—Mo10—Mo11xix122.51 (2)
Mo4xiii—Mo3—Mo5xiii59.373 (17)Mo6—Mo10—Mo11xix176.67 (2)
Mo5xvi—Mo3—Mo5xiii61.266 (19)O19xx—Mo10—Mo12xix87.78 (12)
Mo1xvi—Mo3—Mo5xiii89.910 (19)O15ix—Mo10—Mo12xix47.57 (12)
Mo2xiii—Mo3—Mo5xiii58.553 (17)O13ix—Mo10—Mo12xix136.16 (12)
O11iii—Mo4—O10xvii100.86 (16)O17xv—Mo10—Mo12xix135.47 (11)
O11iii—Mo4—O7xvii172.15 (16)Mo9—Mo10—Mo12xix120.53 (2)
O10xvii—Mo4—O7xvii85.59 (16)Mo11—Mo10—Mo12xix59.813 (17)
O11iii—Mo4—O9x89.16 (16)Mo12—Mo10—Mo12xix88.811 (19)
O10xvii—Mo4—O9x92.02 (16)Mo8—Mo10—Mo12xix64.663 (19)
O7xvii—Mo4—O9x86.11 (16)Mo6—Mo10—Mo12xix122.58 (2)
O11iii—Mo4—O6iii86.56 (16)Mo11xix—Mo10—Mo12xix57.853 (16)
O10xvii—Mo4—O6iii170.14 (16)O19xiii—Mo11—O1692.36 (16)
O7xvii—Mo4—O6iii86.55 (16)O19xiii—Mo11—O14iii87.32 (16)
O9x—Mo4—O6iii81.52 (15)O16—Mo11—O14iii89.12 (16)
O11iii—Mo4—Mo3xiii50.48 (11)O19xiii—Mo11—O18xv85.07 (16)
O10xvii—Mo4—Mo3xiii50.62 (11)O16—Mo11—O18xv172.95 (16)
O7xvii—Mo4—Mo3xiii136.20 (11)O14iii—Mo11—O18xv84.21 (16)
O9x—Mo4—Mo3xiii95.04 (11)O19xiii—Mo11—Mo1290.92 (11)
O6iii—Mo4—Mo3xiii137.03 (11)O16—Mo11—Mo12138.51 (12)
O11iii—Mo4—Mo549.72 (11)O14iii—Mo11—Mo12132.35 (12)
O10xvii—Mo4—Mo598.42 (12)O18xv—Mo11—Mo1248.25 (11)
O7xvii—Mo4—Mo5134.24 (11)O19xiii—Mo11—Mo10137.97 (12)
O9x—Mo4—Mo5138.73 (11)O16—Mo11—Mo1091.37 (12)
O6iii—Mo4—Mo591.32 (11)O14iii—Mo11—Mo10134.59 (12)
Mo3xiii—Mo4—Mo563.455 (17)O18xv—Mo11—Mo1094.94 (12)
O11iii—Mo4—Mo5xi97.20 (11)Mo12—Mo11—Mo1060.411 (17)
O10xvii—Mo4—Mo5xi47.56 (11)O19xiii—Mo11—Mo7131.67 (12)
O7xvii—Mo4—Mo5xi90.46 (11)O16—Mo11—Mo788.84 (11)
O9x—Mo4—Mo5xi139.58 (11)O14iii—Mo11—Mo744.37 (12)
O6iii—Mo4—Mo5xi138.51 (11)O18xv—Mo11—Mo787.98 (11)
Mo3xiii—Mo4—Mo5xi61.146 (17)Mo12—Mo11—Mo7118.52 (2)
Mo5—Mo4—Mo5xi62.292 (19)Mo10—Mo11—Mo790.236 (19)
O11iii—Mo4—Mo193.45 (12)O19xiii—Mo11—Mo9131.92 (12)
O10xvii—Mo4—Mo1136.03 (12)O16—Mo11—Mo9135.65 (11)
O7xvii—Mo4—Mo184.82 (11)O14iii—Mo11—Mo990.45 (12)
O9x—Mo4—Mo1129.86 (11)O18xv—Mo11—Mo946.98 (11)
O6iii—Mo4—Mo148.79 (11)Mo12—Mo11—Mo957.009 (18)
Mo3xiii—Mo4—Mo1124.20 (2)Mo10—Mo11—Mo959.166 (17)
Mo5—Mo4—Mo160.860 (18)Mo7—Mo11—Mo961.535 (17)
Mo5xi—Mo4—Mo189.723 (19)O19xiii—Mo11—Mo12xix91.32 (12)
O11iii—Mo4—Mo2xi138.68 (12)O16—Mo11—Mo12xix48.29 (11)
O10xvii—Mo4—Mo2xi86.09 (11)O14iii—Mo11—Mo12xix137.32 (12)
O7xvii—Mo4—Mo2xi45.52 (11)O18xv—Mo11—Mo12xix138.19 (11)
O9x—Mo4—Mo2xi131.62 (11)Mo12—Mo11—Mo12xix90.31 (2)
O6iii—Mo4—Mo2xi92.62 (11)Mo10—Mo11—Mo12xix61.378 (18)
Mo3xiii—Mo4—Mo2xi119.21 (2)Mo7—Mo11—Mo12xix123.16 (2)
Mo5—Mo4—Mo2xi89.055 (19)Mo9—Mo11—Mo12xix120.39 (2)
Mo5xi—Mo4—Mo2xi58.076 (17)O19xiii—Mo11—Mo8139.02 (12)
Mo1—Mo4—Mo2xi57.518 (16)O16—Mo11—Mo846.75 (11)
O11iii—Mo4—Mo6xiii129.99 (11)O14iii—Mo11—Mo889.14 (12)
O10xvii—Mo4—Mo6xiii128.90 (11)O18xv—Mo11—Mo8135.10 (11)
O7xvii—Mo4—Mo6xiii43.32 (11)Mo12—Mo11—Mo8120.32 (2)
O9x—Mo4—Mo6xiii84.94 (11)Mo10—Mo11—Mo860.061 (17)
O6iii—Mo4—Mo6xiii43.44 (11)Mo7—Mo11—Mo858.236 (17)
Mo3xiii—Mo4—Mo6xiii179.52 (2)Mo9—Mo11—Mo888.896 (19)
Mo5—Mo4—Mo6xiii116.85 (2)Mo12xix—Mo11—Mo864.942 (18)
Mo5xi—Mo4—Mo6xiii118.60 (2)O19xiii—Mo11—Mo10xix46.52 (11)
Mo1—Mo4—Mo6xiii56.071 (15)O16—Mo11—Mo10xix92.59 (11)
Mo2xi—Mo4—Mo6xiii60.527 (17)O14iii—Mo11—Mo10xix133.85 (12)
O8—Mo5—O989.89 (16)O18xv—Mo11—Mo10xix90.40 (11)
O8—Mo5—O10x86.91 (16)Mo12—Mo11—Mo10xix61.254 (18)
O9—Mo5—O10x84.57 (16)Mo10—Mo11—Mo10xix91.494 (19)
O8—Mo5—O11iii89.75 (16)Mo7—Mo11—Mo10xix177.73 (2)
O9—Mo5—O11iii86.23 (16)Mo9—Mo11—Mo10xix118.26 (2)
O10x—Mo5—O11iii170.21 (16)Mo12xix—Mo11—Mo10xix59.034 (17)
O8—Mo5—Mo492.40 (12)Mo8—Mo11—Mo10xix123.97 (2)
O9—Mo5—Mo4134.76 (12)O17xv—Mo12—O18xv99.33 (16)
O10x—Mo5—Mo4140.68 (11)O17xv—Mo12—O19v85.53 (16)
O11iii—Mo5—Mo448.63 (11)O18xv—Mo12—O19v91.42 (16)
O8—Mo5—Mo2135.67 (11)O17xv—Mo12—O16xix86.95 (16)
O9—Mo5—Mo245.78 (11)O18xv—Mo12—O16xix171.34 (16)
O10x—Mo5—Mo288.81 (11)O19v—Mo12—O16xix83.07 (16)
O11iii—Mo5—Mo287.16 (11)O17xv—Mo12—O15xxi170.03 (16)
Mo4—Mo5—Mo2117.21 (2)O18xv—Mo12—O15xxi88.35 (16)
O8—Mo5—Mo3xii89.89 (11)O19v—Mo12—O15xxi87.94 (16)
O9—Mo5—Mo3xii132.81 (12)O16xix—Mo12—O15xxi84.79 (16)
O10x—Mo5—Mo3xii48.31 (11)O17xv—Mo12—Mo949.72 (11)
O11iii—Mo5—Mo3xii140.96 (11)O18xv—Mo12—Mo949.82 (11)
Mo4—Mo5—Mo3xii92.395 (19)O19v—Mo12—Mo991.39 (11)
Mo2—Mo5—Mo3xii118.76 (2)O16xix—Mo12—Mo9136.65 (11)
O8—Mo5—Mo4xi133.65 (11)O15xxi—Mo12—Mo9138.15 (11)
O9—Mo5—Mo4xi91.60 (12)O17xv—Mo12—Mo1196.83 (11)
O10x—Mo5—Mo4xi47.23 (11)O18xv—Mo12—Mo1149.06 (12)
O11iii—Mo5—Mo4xi136.58 (11)O19v—Mo12—Mo11140.37 (11)
Mo4—Mo5—Mo4xi117.708 (19)O16xix—Mo12—Mo11136.50 (11)
Mo2—Mo5—Mo4xi61.947 (17)O15xxi—Mo12—Mo1193.01 (11)
Mo3xii—Mo5—Mo4xi56.823 (18)Mo9—Mo12—Mo1162.455 (18)
O8—Mo5—Mo146.98 (11)O17xv—Mo12—Mo1048.60 (11)
O9—Mo5—Mo1136.87 (11)O18xv—Mo12—Mo1095.40 (12)
O10x—Mo5—Mo191.42 (11)O19v—Mo12—Mo10134.13 (11)
O11iii—Mo5—Mo193.02 (11)O16xix—Mo12—Mo1093.23 (12)
Mo4—Mo5—Mo161.268 (17)O15xxi—Mo12—Mo10137.44 (12)
Mo2—Mo5—Mo1177.35 (2)Mo9—Mo12—Mo1060.876 (17)
Mo3xii—Mo5—Mo159.755 (17)Mo11—Mo12—Mo1060.243 (17)
Mo4xi—Mo5—Mo1116.49 (2)O17xv—Mo12—Mo11xix89.72 (12)
O8—Mo5—Mo3xiii136.59 (11)O18xv—Mo12—Mo11xix138.38 (12)
O9—Mo5—Mo3xiii92.12 (11)O19v—Mo12—Mo11xix129.93 (11)
O10x—Mo5—Mo3xiii136.45 (11)O16xix—Mo12—Mo11xix46.89 (11)
O11iii—Mo5—Mo3xiii47.21 (11)O15xxi—Mo12—Mo11xix88.70 (12)
Mo4—Mo5—Mo3xiii57.173 (18)Mo9—Mo12—Mo11xix121.95 (2)
Mo2—Mo5—Mo3xiii60.043 (16)Mo11—Mo12—Mo11xix89.69 (2)
Mo3xii—Mo5—Mo3xiii118.734 (19)Mo10—Mo12—Mo11xix61.085 (18)
Mo4xi—Mo5—Mo3xiii89.653 (18)O17xv—Mo12—Mo10xix139.07 (12)
Mo1—Mo5—Mo3xiii118.34 (2)O18xv—Mo12—Mo10xix90.65 (11)
O8—Mo5—Mo5xi135.80 (11)O19v—Mo12—Mo10xix134.11 (11)
O9—Mo5—Mo5xi134.23 (12)O16xix—Mo12—Mo10xix88.43 (11)
O10x—Mo5—Mo5xi94.03 (12)O15xxi—Mo12—Mo10xix46.31 (11)
O11iii—Mo5—Mo5xi94.78 (12)Mo9—Mo12—Mo10xix123.34 (2)
Mo4—Mo5—Mo5xi60.28 (2)Mo11—Mo12—Mo10xix60.893 (18)
Mo2—Mo5—Mo5xi88.50 (2)Mo10—Mo12—Mo10xix91.189 (19)
Mo3xii—Mo5—Mo5xi60.199 (18)Mo11xix—Mo12—Mo10xix58.809 (16)
Mo4xi—Mo5—Mo5xi57.432 (18)O17xv—Mo12—Mo8xix129.87 (11)
Mo1—Mo5—Mo5xi88.85 (2)O18xv—Mo12—Mo8xix130.59 (12)
Mo3xiii—Mo5—Mo5xi58.535 (19)O19v—Mo12—Mo8xix88.50 (11)
O13ix—Mo6—O3ix87.44 (16)O16xix—Mo12—Mo8xix42.93 (11)
O13ix—Mo6—O2xviii86.95 (16)O15xxi—Mo12—Mo8xix42.26 (11)
O3ix—Mo6—O2xviii170.62 (16)Mo9—Mo12—Mo8xix179.58 (2)
O13ix—Mo6—O7v87.28 (16)Mo11—Mo12—Mo8xix117.84 (2)
O3ix—Mo6—O7v85.51 (15)Mo10—Mo12—Mo8xix118.95 (2)
O2xviii—Mo6—O7v86.72 (16)Mo11xix—Mo12—Mo8xix57.870 (16)
O13ix—Mo6—O6ix171.00 (16)Mo10xix—Mo12—Mo8xix56.957 (16)
O3ix—Mo6—O6ix86.33 (15)Mo7xvii—O1—Mo9xvii87.09 (16)
O2xviii—Mo6—O6ix98.33 (16)Mo7xvii—O1—Mo1xxii93.04 (16)
O7v—Mo6—O6ix85.76 (15)Mo9xvii—O1—Mo1xxii93.12 (16)
O13ix—Mo6—Mo890.24 (12)Mo7xvii—O1—Sn1viii113.12 (18)
O3ix—Mo6—Mo846.21 (11)Mo9xvii—O1—Sn1viii109.35 (17)
O2xviii—Mo6—Mo8141.30 (11)Mo1xxii—O1—Sn1viii145.7 (2)
O7v—Mo6—Mo8131.72 (11)Mo2xxiii—O2—Mo6xxiv90.23 (16)
O6ix—Mo6—Mo890.13 (11)Mo2xxiii—O2—Mo1vi79.35 (14)
O13ix—Mo6—Mo7137.28 (12)Mo6xxiv—O2—Mo1vi81.61 (14)
O3ix—Mo6—Mo791.19 (11)Mo2xxiii—O2—Mo9xxiv168.1 (2)
O2xviii—Mo6—Mo798.04 (11)Mo6xxiv—O2—Mo9xxiv80.58 (14)
O7v—Mo6—Mo7135.19 (11)Mo1vi—O2—Mo9xxiv91.78 (16)
O6ix—Mo6—Mo749.44 (11)Mo8ix—O3—Mo6ix84.48 (15)
Mo8—Mo6—Mo759.960 (17)Mo8ix—O3—Mo2xxii132.5 (2)
O13ix—Mo6—Mo991.09 (12)Mo6ix—O3—Mo2xxii134.2 (2)
O3ix—Mo6—Mo9137.58 (11)Mo1ix—O4—Mo3xiv84.58 (15)
O2xviii—Mo6—Mo950.10 (11)Mo1ix—O4—Mo7xv134.2 (2)
O7v—Mo6—Mo9136.79 (11)Mo3xiv—O4—Mo7xv132.9 (2)
O6ix—Mo6—Mo997.90 (11)Mo2xxiii—O5—Mo3ii83.93 (15)
Mo8—Mo6—Mo991.433 (19)Mo2xxiii—O5—Sn1xxiii104.43 (17)
Mo7—Mo6—Mo962.453 (17)Mo3ii—O5—Sn1xxiii136.9 (2)
O13ix—Mo6—Mo1xiii135.78 (12)Mo2xxiii—O5—Sn2iv130.0 (2)
O3ix—Mo6—Mo1xiii134.74 (11)Mo3ii—O5—Sn2iv97.26 (16)
O2xviii—Mo6—Mo1xiii49.32 (11)Sn1xxiii—O5—Sn2iv107.68 (16)
O7v—Mo6—Mo1xiii84.33 (11)Mo7ix—O6—Mo1viii91.85 (16)
O6ix—Mo6—Mo1xiii49.01 (11)Mo7ix—O6—Mo6ix80.22 (13)
Mo8—Mo6—Mo1xiii126.59 (2)Mo1viii—O6—Mo6ix81.64 (14)
Mo7—Mo6—Mo1xiii66.855 (18)Mo7ix—O6—Mo4viii171.3 (2)
Mo9—Mo6—Mo1xiii67.333 (18)Mo1viii—O6—Mo4viii81.78 (14)
O13ix—Mo6—Mo1047.18 (12)Mo6ix—O6—Mo4viii92.87 (16)
O3ix—Mo6—Mo1091.07 (11)Mo2xxii—O7—Mo4xv86.99 (16)
O2xviii—Mo6—Mo1090.63 (11)Mo2xxii—O7—Mo6xxv92.30 (16)
O7v—Mo6—Mo10134.46 (11)Mo4xv—O7—Mo6xxv94.39 (16)
O6ix—Mo6—Mo10139.41 (11)Mo2xxii—O7—Sn2xxv112.50 (18)
Mo8—Mo6—Mo1060.608 (17)Mo4xv—O7—Sn2xxv102.98 (16)
Mo7—Mo6—Mo1090.202 (19)Mo6xxv—O7—Sn2xxv150.1 (2)
Mo9—Mo6—Mo1058.872 (17)Mo5—O8—Mo186.11 (16)
Mo1xiii—Mo6—Mo10126.11 (2)Mo5—O8—Mo3xvii129.7 (2)
O13ix—Mo6—Mo2xvi90.36 (12)Mo1—O8—Mo3xvii135.8 (2)
O3ix—Mo6—Mo2xvi127.92 (11)Mo2—O9—Mo585.94 (16)
O2xviii—Mo6—Mo2xvi44.65 (11)Mo2—O9—Mo4xxii140.1 (2)
O7v—Mo6—Mo2xvi42.41 (11)Mo5—O9—Mo4xxii126.7 (2)
O6ix—Mo6—Mo2xvi88.35 (11)Mo4xv—O10—Mo5xxii85.21 (16)
Mo8—Mo6—Mo2xvi174.05 (2)Mo4xv—O10—Mo3xxv79.53 (15)
Mo7—Mo6—Mo2xvi122.53 (2)Mo5xxii—O10—Mo3xxv83.76 (15)
Mo9—Mo6—Mo2xvi94.473 (19)Mo4viii—O11—Mo3ix79.69 (15)
Mo1xiii—Mo6—Mo2xvi55.692 (15)Mo4viii—O11—Mo5viii81.65 (14)
Mo10—Mo6—Mo2xvi123.45 (2)Mo3ix—O11—Mo5viii85.14 (15)
O13ix—Mo6—Mo4xiii129.57 (12)Mo4viii—O11—Sn2ii147.5 (2)
O3ix—Mo6—Mo4xiii87.81 (11)Mo3ix—O11—Sn2ii90.87 (14)
O2xviii—Mo6—Mo4xiii89.97 (11)Mo5viii—O11—Sn2ii128.85 (18)
O7v—Mo6—Mo4xiii42.29 (11)Mo7vi—O12—Mo8vi85.17 (15)
O6ix—Mo6—Mo4xiii43.69 (11)Mo7vi—O12—Sn1vi132.7 (2)
Mo8—Mo6—Mo4xiii120.32 (2)Mo8vi—O12—Sn1vi107.02 (17)
Mo7—Mo6—Mo4xiii92.992 (18)Mo7vi—O12—Sn2viii102.48 (16)
Mo9—Mo6—Mo4xiii123.72 (2)Mo8vi—O12—Sn2viii136.22 (19)
Mo1xiii—Mo6—Mo4xiii56.391 (16)Sn1vi—O12—Sn2viii98.94 (14)
Mo10—Mo6—Mo4xiii176.64 (2)Mo6ix—O13—Mo10ix87.26 (16)
Mo2xvi—Mo6—Mo4xiii55.341 (15)Mo6ix—O13—Mo8xxii133.1 (2)
O14iii—Mo7—O12ii90.99 (17)Mo10ix—O13—Mo8xxii130.8 (2)
O14iii—Mo7—O1xv92.63 (17)Mo7viii—O14—Mo11viii87.33 (17)
O12ii—Mo7—O1xv174.11 (16)Mo7viii—O14—Mo9xvii138.8 (2)
O14iii—Mo7—O6ix170.87 (16)Mo11viii—O14—Mo9xvii128.8 (2)
O12ii—Mo7—O6ix86.99 (16)Mo8ix—O15—Mo10ix86.25 (16)
O1xv—Mo7—O6ix88.71 (16)Mo8ix—O15—Mo12xxvi93.67 (17)
O14iii—Mo7—O4xvii88.79 (16)Mo10ix—O15—Mo12xxvi86.11 (16)
O12ii—Mo7—O4xvii87.43 (16)Mo8ix—O15—Sn3iv156.2 (2)
O1xv—Mo7—O4xvii88.01 (16)Mo10ix—O15—Sn3iv111.89 (17)
O6ix—Mo7—O4xvii82.23 (15)Mo12xxvi—O15—Sn3iv102.52 (17)
O14iii—Mo7—Mo894.67 (12)Mo11—O16—Mo886.67 (15)
O12ii—Mo7—Mo847.90 (12)Mo11—O16—Mo12xix84.82 (15)
O1xv—Mo7—Mo8136.25 (11)Mo8—O16—Mo12xix93.08 (17)
O6ix—Mo7—Mo890.58 (11)Mo9xvii—O17—Mo12xvii80.41 (15)
O4xvii—Mo7—Mo8135.17 (11)Mo9xvii—O17—Mo10xvii83.19 (15)
O14iii—Mo7—Mo6138.72 (12)Mo12xvii—O17—Mo10xvii84.08 (15)
O12ii—Mo7—Mo692.90 (12)Mo9xvii—O17—Sn3iii139.9 (2)
O1xv—Mo7—Mo687.44 (12)Mo12xvii—O17—Sn3iii99.10 (17)
O6ix—Mo7—Mo650.35 (11)Mo10xvii—O17—Sn3iii136.8 (2)
O4xvii—Mo7—Mo6132.43 (11)Mo9xvii—O18—Mo12xvii79.94 (15)
Mo8—Mo7—Mo659.758 (18)Mo9xvii—O18—Mo11xvii84.88 (16)
O14iii—Mo7—Mo1148.30 (12)Mo12xvii—O18—Mo11xvii82.70 (15)
O12ii—Mo7—Mo1192.36 (11)Mo11xiii—O19—Mo10xxvii87.58 (16)
O1xv—Mo7—Mo1193.51 (11)Mo11xiii—O19—Mo12xxv131.9 (2)
O6ix—Mo7—Mo11140.64 (11)Mo10xxvii—O19—Mo12xxv133.0 (2)
Symmetry codes: (i) x+1, y3/2, z+3/2; (ii) x, y+1/2, z+1/2; (iii) x, y1, z; (iv) x+1, y+1, z+1; (v) x+1, y1/2, z+1/2; (vi) x, y+1/2, z1/2; (vii) x+2, y+2, z+1; (viii) x, y+1, z; (ix) x+1, y, z+1; (x) x+1, y1/2, z+3/2; (xi) x+1, y1, z+2; (xii) x, y, z+1; (xiii) x+1, y1, z+1; (xiv) x+1, y, z; (xv) x, y1/2, z1/2; (xvi) x, y, z1; (xvii) x, y1/2, z+1/2; (xviii) x+1, y3/2, z+1/2; (xix) x+2, y1, z+1; (xx) x+1, y, z; (xxi) x+1, y1, z; (xxii) x+1, y+1/2, z+3/2; (xxiii) x+1, y+3/2, z+3/2; (xxiv) x+1, y+3/2, z+1/2; (xxv) x+1, y+1/2, z+1/2; (xxvi) x1, y+1, z; (xxvii) x1, y, z.

Experimental details

Crystal data
Chemical formulaSn4.4Mo24O38
Mr3433.04
Crystal system, space groupMonoclinic, P21/c
Temperature (K)293
a, b, c (Å)17.806 (2), 9.2562 (6), 9.9337 (13)
β (°) 105.955 (6)
V3)1574.2 (3)
Z2
Radiation typeMo Kα
µ (mm1)12.72
Crystal size (mm)0.14 × 0.12 × 0.08
Data collection
DiffractometerEnraf-Nonius CAD-4
diffractometer
Absorption correctionψ-scan
(North et al., 1968)
Tmin, Tmax0.260, 0.361
No. of measured, independent and
observed [I > 2σ(I)] reflections
5726, 5446, 4519
Rint0.021
(sin θ/λ)max1)0.745
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.032, 0.077, 1.25
No. of reflections5446
No. of parameters216
Calculated w = 1/[σ2(Fo2) + (0.0169P)2 + 28.2165P]
where P = (Fo2 + 2Fc2)/3
Δρmax, Δρmin (e Å3)2.90, 2.08

Computer programs: CAD-4 Software (Enraf-Nonius, 1989), CAD-4 Software, MolEN (Fair, 1990), SHELXS86 (Sheldrick, 1990), SHELXL97 (Sheldrick, 1997), ORTEPII (Johnson, 1976), SHELXL97.

Selected bond lengths (Å) top
Sn1—O5i2.217 (4)Sn2—O12iii2.545 (4)
Sn1—O12ii2.231 (4)Sn2—O11vi2.551 (4)
Sn1—O1iii2.313 (4)Sn3—Sn3vii0.759 (3)
Sn2—O5iv2.286 (4)Sn3—O17viii2.384 (4)
Sn2—O7v2.444 (4)Sn3—O15iv2.514 (5)
Symmetry codes: (i) x+1, y3/2, z+3/2; (ii) x, y+1/2, z+1/2; (iii) x, y1, z; (iv) x+1, y+1, z+1; (v) x+1, y1/2, z+1/2; (vi) x, y+1/2, z1/2; (vii) x+2, y+2, z+1; (viii) x, y+1, z.
 

Follow Acta Cryst. C
Sign up for e-alerts
Follow Acta Cryst. on Twitter
Follow us on facebook
Sign up for RSS feeds