inorganic compounds
LiCe9Mo16O35
aSciences Chimiques de Rennes, UMR CNRS No. 6226, Université de Rennes I - INSA Rennes, Avenue du Général Leclerc, 35042 Rennes CEDEX, France
*Correspondence e-mail: Patrick.Gougeon@univ-rennes1.fr
The structure of lithium nonacerium hexadecamolybdenum pentatridecaoxide, LiCe9Mo16O35, is isotypic with LiNd9Mo16O35 [Gougeon Gall, Cuny, Gautier, Le Polles, Delevoye & Trebosc (2011). Chem. Eur. J. 17, 13806–13813]. It is characterized by Mo16O26iO10a units (where i = inner and a = apical) containing Mo16 clusters that share some of their O atoms to form infinite molybdenum cluster chains running parallel to the b axis and separated by Li+ and Ce3+ cations. The Mo16 cluster units are centred at Wyckoff positions 2c and have point-group symmetry 2/m. The Li+ atom, in a flattened octahedron of O atoms, is in a 2a with 2/m symmetry. The Ce3+ cations have coordination numbers to the O atoms of 6, 9 or 10. Two Ce, two Mo and five O atoms lie on sites with m symmetry (Wyckoff site 4i), and one Ce and one O atom on sites with 2/m symmetry (Wyckoff sites 2b and 2d, respectively).
Related literature
For the 9Mo16O35 compound, see: Gougeon et al. (2011). For details of the i- and a-type ligand notation, see: Schäfer & von Schnering (1964). For compounds containing Mo10 clusters, see: Hibble et al. (1988); Dronskowski & Simon (1989); Gougeon et al. (1990, 1991, 2003, 2007); Dronskowski et al. (1991); Gall et al. (1993, 1995, 1999); Gall & Gougeon (1993, 1994a,b, 1998); Gougeon & Gall (2002). The oxidation states of the Mo, Ce and Li atoms were estimated using the data given by Brown & Wu (1976).
of the LiNdExperimental
Crystal data
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Refinement
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Data collection: COLLECT (Nonius, 1998); cell COLLECT; data reduction: EVALCCD (Duisenberg et al., 2003); program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Bergerhoff, 1996); software used to prepare material for publication: SHELXL97.
Supporting information
10.1107/S160053681200801X/ru2029sup1.cif
contains datablocks I, global. DOI:Structure factors: contains datablock I. DOI: 10.1107/S160053681200801X/ru2029Isup2.hkl
Single crystals of LiCe9Mo16O35 were obtained from a mixture of Li2MoO4, CeO2, MoO3, and Mo with the nominal composition Li2CeMo6O12. Before use, Mo powder was reduced under H2 flowing gas at 1273 K during 10 h in order to eliminate any trace of oxygen. The initial mixture (ca 4 g) was cold pressed and loaded into a molybdenum crucible, which was sealed under a low argon pressure using an arc welding system. The charge was heated at the rate of 300 K/h up to 2000 K, temperature which was held for 18 h, then cooled at 100 K/h down to 1373 K and finally furnace cooled.
Data collection: COLLECT (Nonius, 1998); cell
COLLECT (Nonius, 1998); data reduction: EVALCCD (Duisenberg et al., 2003); program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Bergerhoff, 1996); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).Fig. 1. View of the crystal structure of LiCe9Mo16O35 (Displacement ellipsoids are drawn at the 97% probability level). | |
Fig. 2. Plot showing the atom-numbering scheme of the Mo16O26iO10a units. Displacement ellipsoids are drawn at the 97% probability level. |
LiCe9Mo16O35 | F(000) = 2954 |
Mr = 3363.06 | Dx = 7.365 Mg m−3 |
Monoclinic, C2/m | Mo Kα radiation, λ = 0.71069 Å |
a = 18.3000 (2) Å | Cell parameters from 21270 reflections |
b = 8.6326 (1) Å | θ = 0.9–35.0° |
c = 9.8172 (1) Å | µ = 19.66 mm−1 |
β = 102.0953 (7)° | T = 293 K |
V = 1516.46 (3) Å3 | Multi-faceted fragment, black |
Z = 2 | 0.15 × 0.12 × 0.06 mm |
Nonius KappaCCD diffractometer | 3511 independent reflections |
Radiation source: fine-focus sealed tube | 3383 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.027 |
ϕ scans (κ = 0) and additional ω scans | θmax = 35.0°, θmin = 3.5° |
Absorption correction: multi-scan (PLATON; Spek, 2009) | h = −26→29 |
Tmin = 0.190, Tmax = 0.418 | k = −13→13 |
21270 measured reflections | l = −15→10 |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.016 | w = 1/[σ2(Fo2) + (0.P)2 + 6.2844P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.033 | (Δ/σ)max = 0.004 |
S = 1.29 | Δρmax = 1.13 e Å−3 |
3511 reflections | Δρmin = −1.33 e Å−3 |
158 parameters | Extinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
0 restraints | Extinction coefficient: 0.00166 (3) |
LiCe9Mo16O35 | V = 1516.46 (3) Å3 |
Mr = 3363.06 | Z = 2 |
Monoclinic, C2/m | Mo Kα radiation |
a = 18.3000 (2) Å | µ = 19.66 mm−1 |
b = 8.6326 (1) Å | T = 293 K |
c = 9.8172 (1) Å | 0.15 × 0.12 × 0.06 mm |
β = 102.0953 (7)° |
Nonius KappaCCD diffractometer | 3511 independent reflections |
Absorption correction: multi-scan (PLATON; Spek, 2009) | 3383 reflections with I > 2σ(I) |
Tmin = 0.190, Tmax = 0.418 | Rint = 0.027 |
21270 measured reflections |
R[F2 > 2σ(F2)] = 0.016 | 158 parameters |
wR(F2) = 0.033 | 0 restraints |
S = 1.29 | Δρmax = 1.13 e Å−3 |
3511 reflections | Δρmin = −1.33 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. |
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 > 2sigma(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. |
x | y | z | Uiso*/Ueq | ||
Li | −0.5000 | −0.5000 | 1.0000 | 0.038 (4) | |
Ce1 | −0.345982 (8) | −0.273486 (15) | 0.201055 (12) | 0.00556 (3) | |
Ce2 | −0.191529 (11) | −0.5000 | 0.071345 (17) | 0.00625 (4) | |
Ce3 | −0.298077 (11) | 0.0000 | 0.534154 (17) | 0.00582 (4) | |
Ce4 | 0.0000 | −0.5000 | 0.0000 | 0.00664 (5) | |
Mo1 | −0.290730 (16) | −0.5000 | 0.74596 (2) | 0.00368 (5) | |
Mo2 | −0.401044 (12) | −0.33869 (2) | 0.828637 (17) | 0.00338 (4) | |
Mo3 | −0.388827 (11) | −0.34166 (2) | 0.551746 (17) | 0.00319 (4) | |
Mo4 | −0.000772 (11) | −0.31629 (2) | 0.357312 (17) | 0.00311 (4) | |
Mo5 | −0.490663 (16) | −0.5000 | 0.35678 (2) | 0.00316 (5) | |
O1 | −0.17701 (15) | −0.5000 | 0.8112 (2) | 0.0070 (4) | |
O2 | −0.28523 (11) | −0.3349 (2) | 0.88711 (16) | 0.0064 (3) | |
O3 | −0.10014 (11) | −0.6759 (2) | 0.02198 (16) | 0.0062 (3) | |
O4 | −0.27246 (11) | −0.3355 (2) | 0.60863 (16) | 0.0059 (3) | |
O5 | −0.38352 (11) | −0.1616 (2) | 0.69257 (16) | 0.0051 (3) | |
O6 | 0.00695 (16) | −0.5000 | 0.2346 (2) | 0.0066 (4) | |
O7 | −0.40015 (16) | −0.5000 | 0.9860 (2) | 0.0067 (4) | |
O8 | −0.38482 (10) | −0.1769 (2) | 0.40574 (15) | 0.0050 (3) | |
O9 | 0.0000 | −0.5000 | 0.5000 | 0.0059 (6) | |
O10 | −0.51815 (10) | −0.33622 (19) | 0.79643 (16) | 0.0050 (3) | |
O11 | −0.37455 (15) | −0.5000 | 0.3998 (2) | 0.0052 (4) | |
O12 | −0.26903 (15) | −0.5000 | 0.2327 (2) | 0.0063 (4) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Li | 0.007 (6) | 0.070 (12) | 0.037 (7) | 0.000 | 0.005 (5) | 0.000 |
Ce1 | 0.00563 (6) | 0.00466 (5) | 0.00630 (5) | 0.00095 (4) | 0.00106 (4) | 0.00077 (3) |
Ce2 | 0.00587 (9) | 0.00703 (8) | 0.00639 (6) | 0.000 | 0.00251 (5) | 0.000 |
Ce3 | 0.00568 (9) | 0.00564 (7) | 0.00553 (6) | 0.000 | −0.00025 (5) | 0.000 |
Ce4 | 0.00575 (12) | 0.00932 (11) | 0.00530 (9) | 0.000 | 0.00216 (7) | 0.000 |
Mo1 | 0.00269 (12) | 0.00349 (10) | 0.00447 (9) | 0.000 | −0.00012 (7) | 0.000 |
Mo2 | 0.00339 (9) | 0.00276 (7) | 0.00372 (6) | 0.00000 (6) | 0.00011 (5) | −0.00036 (5) |
Mo3 | 0.00291 (9) | 0.00265 (7) | 0.00385 (6) | −0.00007 (6) | 0.00036 (5) | 0.00014 (5) |
Mo4 | 0.00306 (9) | 0.00221 (7) | 0.00386 (6) | −0.00005 (6) | 0.00029 (5) | −0.00010 (5) |
Mo5 | 0.00309 (12) | 0.00254 (10) | 0.00372 (9) | 0.000 | 0.00047 (7) | 0.000 |
O1 | 0.0034 (11) | 0.0067 (10) | 0.0095 (9) | 0.000 | −0.0014 (7) | 0.000 |
O2 | 0.0061 (8) | 0.0056 (7) | 0.0068 (6) | 0.0004 (6) | −0.0004 (5) | −0.0021 (5) |
O3 | 0.0073 (8) | 0.0050 (7) | 0.0063 (6) | 0.0000 (6) | 0.0010 (5) | 0.0013 (5) |
O4 | 0.0038 (8) | 0.0062 (7) | 0.0077 (6) | −0.0006 (6) | 0.0010 (5) | 0.0006 (5) |
O5 | 0.0044 (8) | 0.0043 (7) | 0.0062 (6) | −0.0001 (6) | 0.0006 (5) | 0.0000 (5) |
O6 | 0.0110 (12) | 0.0039 (10) | 0.0047 (8) | 0.000 | 0.0013 (7) | 0.000 |
O7 | 0.0089 (12) | 0.0051 (10) | 0.0058 (8) | 0.000 | 0.0011 (7) | 0.000 |
O8 | 0.0039 (8) | 0.0051 (7) | 0.0055 (6) | −0.0001 (6) | 0.0000 (5) | 0.0009 (5) |
O9 | 0.0100 (17) | 0.0036 (13) | 0.0041 (11) | 0.000 | 0.0014 (10) | 0.000 |
O10 | 0.0037 (8) | 0.0041 (7) | 0.0073 (6) | −0.0001 (6) | 0.0013 (5) | 0.0000 (5) |
O11 | 0.0046 (11) | 0.0060 (10) | 0.0053 (8) | 0.000 | 0.0017 (7) | 0.000 |
O12 | 0.0063 (12) | 0.0063 (10) | 0.0060 (8) | 0.000 | 0.0002 (7) | 0.000 |
Li—O7i | 1.861 (3) | Mo3—O11 | 2.0795 (16) |
Li—O7 | 1.861 (3) | Mo3—O4 | 2.0860 (19) |
Li—O10ii | 2.4135 (16) | Mo3—Mo3ii | 2.7338 (4) |
Li—O10iii | 2.4135 (16) | Mo3—Mo4v | 2.7375 (3) |
Li—O10i | 2.4135 (16) | Mo3—Mo5 | 2.7405 (3) |
Li—O10 | 2.4135 (16) | Mo3—Mo4xv | 2.8391 (3) |
Ce1—O3iv | 2.3603 (16) | Mo3—Mo5xiv | 2.8928 (3) |
Ce1—O12 | 2.3916 (16) | Mo4—O6 | 2.0145 (14) |
Ce1—O1v | 2.4055 (5) | Mo4—O8xvi | 2.0758 (19) |
Ce1—O8 | 2.4159 (16) | Mo4—O5v | 2.0797 (19) |
Ce1—O10vi | 2.5499 (19) | Mo4—O10v | 2.0857 (16) |
Ce1—O4v | 2.7161 (18) | Mo4—O9 | 2.1141 (2) |
Ce1—O2v | 2.874 (2) | Mo4—Mo2v | 2.6412 (3) |
Ce1—O11 | 2.8865 (16) | Mo4—Mo5xvii | 2.7367 (2) |
Ce1—O7vii | 2.8959 (17) | Mo4—Mo3v | 2.7375 (3) |
Ce2—O12 | 2.337 (3) | Mo4—Mo4xviii | 2.7958 (3) |
Ce2—O3ii | 2.3829 (19) | Mo4—Mo3xvi | 2.8391 (3) |
Ce2—O3 | 2.3829 (19) | Mo4—Mo4ii | 3.1718 (4) |
Ce2—O1vii | 2.622 (2) | Mo5—O11 | 2.078 (3) |
Ce2—O2viii | 2.6352 (17) | Mo5—O10xiv | 2.0950 (16) |
Ce2—O2vii | 2.6352 (17) | Mo5—O10vi | 2.0950 (16) |
Ce2—O5v | 2.8054 (16) | Mo5—Mo4xix | 2.7367 (2) |
Ce2—O5ix | 2.8054 (16) | Mo5—Mo4xv | 2.7367 (2) |
Ce2—O2ix | 2.9625 (17) | Mo5—Mo3ii | 2.7405 (3) |
Ce2—O2v | 2.9625 (17) | Mo5—Mo2xiv | 2.7691 (3) |
Ce3—O12v | 2.360 (2) | Mo5—Mo2vi | 2.7691 (3) |
Ce3—O8 | 2.3670 (17) | Mo5—Mo3xiv | 2.8928 (3) |
Ce3—O8x | 2.3670 (17) | Mo5—Mo3vi | 2.8928 (3) |
Ce3—O4v | 2.5309 (18) | Mo5—Mo5xiv | 2.9030 (5) |
Ce3—O4xi | 2.5309 (18) | O1—Ce1v | 2.4055 (5) |
Ce3—O5x | 2.7980 (17) | O1—Ce1ix | 2.4055 (5) |
Ce3—O5 | 2.7980 (17) | O1—Ce2xx | 2.622 (2) |
Ce3—O4x | 3.0001 (17) | O1—Ce3v | 3.325 (2) |
Ce3—O4 | 3.0001 (17) | O2—Ce2xx | 2.6352 (17) |
Ce3—O11v | 3.089 (3) | O2—Ce1v | 2.874 (2) |
Ce4—O6xii | 2.280 (2) | O2—Ce2v | 2.9625 (17) |
Ce4—O6 | 2.280 (2) | O3—Mo2ix | 2.0277 (16) |
Ce4—O3 | 2.4244 (19) | O3—Ce1xxi | 2.3603 (16) |
Ce4—O3xii | 2.4244 (19) | O4—Ce3v | 2.5309 (18) |
Ce4—O3ii | 2.4244 (19) | O4—Ce1v | 2.7161 (18) |
Ce4—O3xiii | 2.4244 (19) | O5—Mo4v | 2.0797 (19) |
Mo1—O2 | 1.9759 (16) | O5—Ce2v | 2.8054 (16) |
Mo1—O2ii | 1.9759 (16) | O6—Mo4ii | 2.0145 (14) |
Mo1—O4ii | 2.0332 (17) | O7—Mo2ii | 2.0773 (16) |
Mo1—O4 | 2.0332 (17) | O7—Ce1xx | 2.8959 (17) |
Mo1—O1 | 2.045 (3) | O7—Ce1xxii | 2.8959 (17) |
Mo1—Mo3ii | 2.7003 (3) | O8—Mo4xv | 2.0758 (19) |
Mo1—Mo3 | 2.7003 (3) | O9—Mo4ii | 2.1141 (2) |
Mo1—Mo2ii | 2.7129 (3) | O9—Mo4xviii | 2.1141 (2) |
Mo1—Mo2 | 2.7129 (3) | O9—Mo4xxiii | 2.1141 (2) |
Mo2—O3xi | 2.0277 (16) | O9—Ce3v | 3.6397 (2) |
Mo2—O2 | 2.077 (2) | O9—Ce3xxiv | 3.6397 (2) |
Mo2—O7 | 2.0773 (16) | O10—Mo4v | 2.0857 (16) |
Mo2—O5 | 2.0985 (16) | O10—Mo5xiv | 2.0950 (16) |
Mo2—O10 | 2.0997 (19) | O10—Ce1vi | 2.5499 (19) |
Mo2—Mo4v | 2.6412 (3) | O11—Mo3ii | 2.0795 (16) |
Mo2—Mo5xiv | 2.7691 (3) | O11—Ce1ii | 2.8865 (16) |
Mo2—Mo3 | 2.7739 (2) | O11—Ce3v | 3.089 (3) |
Mo2—Mo2ii | 2.7851 (4) | O12—Ce3v | 2.360 (2) |
Mo3—O8 | 2.0315 (16) | O12—Ce1ii | 2.3916 (16) |
Mo3—O5 | 2.0688 (16) | ||
O7i—Li—O7 | 180.0 | O2ii—Mo1—Mo2 | 95.29 (6) |
O7i—Li—O10ii | 95.41 (7) | O4ii—Mo1—Mo2 | 142.46 (6) |
O7—Li—O10ii | 84.59 (7) | O4—Mo1—Mo2 | 94.36 (5) |
O7i—Li—O10iii | 84.59 (7) | O1—Mo1—Mo2 | 132.72 (5) |
O7—Li—O10iii | 95.41 (7) | Mo3ii—Mo1—Mo2 | 92.568 (10) |
O10ii—Li—O10iii | 180.0 | Mo3—Mo1—Mo2 | 61.651 (7) |
O7i—Li—O10i | 84.59 (7) | Mo2ii—Mo1—Mo2 | 61.767 (10) |
O7—Li—O10i | 95.41 (7) | O2—Mo1—Ce2xx | 52.36 (5) |
O10ii—Li—O10i | 108.28 (8) | O2ii—Mo1—Ce2xx | 52.36 (5) |
O10iii—Li—O10i | 71.72 (8) | O4ii—Mo1—Ce2xx | 120.27 (5) |
O7i—Li—O10 | 95.41 (7) | O4—Mo1—Ce2xx | 120.27 (5) |
O7—Li—O10 | 84.59 (7) | O1—Mo1—Ce2xx | 52.01 (7) |
O10ii—Li—O10 | 71.72 (8) | Mo3ii—Mo1—Ce2xx | 145.707 (6) |
O10iii—Li—O10 | 108.28 (8) | Mo3—Mo1—Ce2xx | 145.707 (6) |
O10i—Li—O10 | 180.000 (1) | Mo2ii—Mo1—Ce2xx | 90.187 (8) |
O7i—Li—Mo2 | 138.20 (5) | Mo2—Mo1—Ce2xx | 90.187 (8) |
O7—Li—Mo2 | 41.80 (5) | O2—Mo1—Ce1v | 57.59 (6) |
O10ii—Li—Mo2 | 78.79 (4) | O2ii—Mo1—Ce1v | 117.78 (5) |
O10iii—Li—Mo2 | 101.21 (4) | O4ii—Mo1—Ce1v | 111.62 (5) |
O10i—Li—Mo2 | 136.78 (4) | O4—Mo1—Ce1v | 53.03 (5) |
O10—Li—Mo2 | 43.22 (4) | O1—Mo1—Ce1v | 44.290 (8) |
O7i—Li—Mo2i | 41.80 (5) | Mo3ii—Mo1—Ce1v | 144.943 (9) |
O7—Li—Mo2i | 138.20 (5) | Mo3—Mo1—Ce1v | 96.635 (6) |
O10ii—Li—Mo2i | 101.21 (4) | Mo2ii—Mo1—Ce1v | 151.707 (9) |
O10iii—Li—Mo2i | 78.79 (4) | Mo2—Mo1—Ce1v | 99.651 (5) |
O10i—Li—Mo2i | 43.22 (4) | Ce2xx—Mo1—Ce1v | 67.487 (5) |
O10—Li—Mo2i | 136.78 (4) | O2—Mo1—Ce1ix | 117.78 (5) |
Mo2—Li—Mo2i | 180.000 (6) | O2ii—Mo1—Ce1ix | 57.59 (6) |
O7i—Li—Mo2ii | 138.20 (5) | O4ii—Mo1—Ce1ix | 53.03 (5) |
O7—Li—Mo2ii | 41.80 (5) | O4—Mo1—Ce1ix | 111.62 (5) |
O10ii—Li—Mo2ii | 43.22 (4) | O1—Mo1—Ce1ix | 44.290 (8) |
O10iii—Li—Mo2ii | 136.78 (4) | Mo3ii—Mo1—Ce1ix | 96.635 (6) |
O10i—Li—Mo2ii | 101.21 (4) | Mo3—Mo1—Ce1ix | 144.943 (9) |
O10—Li—Mo2ii | 78.79 (4) | Mo2ii—Mo1—Ce1ix | 99.651 (5) |
Mo2—Li—Mo2ii | 54.260 (7) | Mo2—Mo1—Ce1ix | 151.707 (9) |
Mo2i—Li—Mo2ii | 125.740 (7) | Ce2xx—Mo1—Ce1ix | 67.487 (5) |
O7i—Li—Mo2iii | 41.80 (5) | Ce1v—Mo1—Ce1ix | 87.964 (8) |
O7—Li—Mo2iii | 138.20 (5) | O3xi—Mo2—O2 | 86.18 (7) |
O10ii—Li—Mo2iii | 136.78 (4) | O3xi—Mo2—O7 | 85.95 (6) |
O10iii—Li—Mo2iii | 43.22 (4) | O2—Mo2—O7 | 87.51 (9) |
O10i—Li—Mo2iii | 78.79 (4) | O3xi—Mo2—O5 | 88.61 (7) |
O10—Li—Mo2iii | 101.21 (4) | O2—Mo2—O5 | 83.17 (7) |
Mo2—Li—Mo2iii | 125.740 (7) | O7—Mo2—O5 | 169.50 (9) |
Mo2i—Li—Mo2iii | 54.260 (7) | O3xi—Mo2—O10 | 87.58 (7) |
Mo2ii—Li—Mo2iii | 180.0 | O2—Mo2—O10 | 172.63 (6) |
O7i—Li—Ce1xx | 128.23 (5) | O7—Mo2—O10 | 88.14 (9) |
O7—Li—Ce1xx | 51.77 (5) | O5—Mo2—O10 | 100.61 (7) |
O10ii—Li—Ce1xx | 135.89 (4) | O3xi—Mo2—Mo4v | 92.95 (5) |
O10iii—Li—Ce1xx | 44.11 (4) | O2—Mo2—Mo4v | 133.64 (5) |
O10i—Li—Ce1xx | 84.80 (4) | O7—Mo2—Mo4v | 138.74 (8) |
O10—Li—Ce1xx | 95.20 (4) | O5—Mo2—Mo4v | 50.48 (5) |
Mo2—Li—Ce1xx | 64.780 (4) | O10—Mo2—Mo4v | 50.64 (4) |
Mo2i—Li—Ce1xx | 115.220 (4) | O3xi—Mo2—Mo1 | 132.54 (6) |
Mo2ii—Li—Ce1xx | 93.573 (4) | O2—Mo2—Mo1 | 46.41 (5) |
Mo2iii—Li—Ce1xx | 86.427 (4) | O7—Mo2—Mo1 | 89.31 (7) |
O7i—Li—Ce1xiv | 51.77 (5) | O5—Mo2—Mo1 | 87.76 (5) |
O7—Li—Ce1xiv | 128.23 (5) | O10—Mo2—Mo1 | 139.47 (5) |
O10ii—Li—Ce1xiv | 44.11 (4) | Mo4v—Mo2—Mo1 | 119.623 (9) |
O10iii—Li—Ce1xiv | 135.89 (4) | O3xi—Mo2—Mo5xiv | 136.18 (6) |
O10i—Li—Ce1xiv | 95.20 (4) | O2—Mo2—Mo5xiv | 137.57 (5) |
O10—Li—Ce1xiv | 84.80 (4) | O7—Mo2—Mo5xiv | 92.57 (6) |
Mo2—Li—Ce1xiv | 115.220 (4) | O5—Mo2—Mo5xiv | 97.57 (5) |
Mo2i—Li—Ce1xiv | 64.780 (4) | O10—Mo2—Mo5xiv | 48.62 (4) |
Mo2ii—Li—Ce1xiv | 86.427 (4) | Mo4v—Mo2—Mo5xiv | 60.718 (6) |
Mo2iii—Li—Ce1xiv | 93.573 (4) | Mo1—Mo2—Mo5xiv | 91.153 (9) |
Ce1xx—Li—Ce1xiv | 180.000 (3) | O3xi—Mo2—Mo3 | 136.41 (5) |
O3iv—Ce1—O12 | 122.15 (7) | O2—Mo2—Mo3 | 89.08 (4) |
O3iv—Ce1—O1v | 69.32 (7) | O7—Mo2—Mo3 | 137.13 (4) |
O12—Ce1—O1v | 134.79 (8) | O5—Mo2—Mo3 | 47.81 (4) |
O3iv—Ce1—O8 | 120.66 (6) | O10—Mo2—Mo3 | 98.15 (4) |
O12—Ce1—O8 | 116.24 (7) | Mo4v—Mo2—Mo3 | 60.674 (7) |
O1v—Ce1—O8 | 77.76 (7) | Mo1—Mo2—Mo3 | 58.951 (7) |
O3iv—Ce1—O10vi | 82.31 (6) | Mo5xiv—Mo2—Mo3 | 62.917 (8) |
O12—Ce1—O10vi | 111.96 (7) | O3xi—Mo2—Mo2ii | 133.86 (5) |
O1v—Ce1—O10vi | 112.96 (7) | O2—Mo2—Mo2ii | 90.91 (5) |
O8—Ce1—O10vi | 66.91 (6) | O7—Mo2—Mo2ii | 47.91 (4) |
O3iv—Ce1—O4v | 129.24 (6) | O5—Mo2—Mo2ii | 136.76 (4) |
O12—Ce1—O4v | 80.26 (6) | O10—Mo2—Mo2ii | 90.58 (5) |
O1v—Ce1—O4v | 64.64 (7) | Mo4v—Mo2—Mo2ii | 120.433 (6) |
O8—Ce1—O4v | 68.88 (6) | Mo1—Mo2—Mo2ii | 59.117 (5) |
O10vi—Ce1—O4v | 134.92 (5) | Mo5xiv—Mo2—Mo2ii | 59.809 (5) |
O3iv—Ce1—O2v | 79.48 (6) | Mo3—Mo2—Mo2ii | 89.470 (5) |
O12—Ce1—O2v | 78.39 (7) | O3xi—Mo2—Li | 80.52 (5) |
O1v—Ce1—O2v | 59.97 (7) | O2—Mo2—Li | 122.93 (5) |
O8—Ce1—O2v | 123.24 (5) | O7—Mo2—Li | 36.66 (8) |
O10vi—Ce1—O2v | 161.79 (5) | O5—Mo2—Li | 150.49 (5) |
O4v—Ce1—O2v | 59.85 (5) | O10—Mo2—Li | 51.92 (4) |
O3iv—Ce1—O11 | 140.28 (7) | Mo4v—Mo2—Li | 102.456 (8) |
O12—Ce1—O11 | 62.84 (7) | Mo1—Mo2—Li | 119.677 (7) |
O1v—Ce1—O11 | 139.21 (6) | Mo5xiv—Mo2—Li | 72.991 (7) |
O8—Ce1—O11 | 62.94 (5) | Mo3—Mo2—Li | 135.603 (8) |
O10vi—Ce1—O11 | 62.26 (6) | Mo2ii—Mo2—Li | 62.870 (4) |
O4v—Ce1—O11 | 90.07 (6) | O3xi—Mo2—Ce2v | 43.12 (5) |
O2v—Ce1—O11 | 134.84 (6) | O2—Mo2—Ce2v | 59.43 (5) |
O3iv—Ce1—O7vii | 63.38 (5) | O7—Mo2—Ce2v | 115.69 (5) |
O12—Ce1—O7vii | 69.19 (7) | O5—Mo2—Ce2v | 55.05 (4) |
O1v—Ce1—O7vii | 131.52 (6) | O10—Mo2—Ce2v | 117.60 (5) |
O8—Ce1—O7vii | 136.39 (7) | Mo4v—Mo2—Ce2v | 89.410 (7) |
O10vi—Ce1—O7vii | 71.23 (7) | Mo1—Mo2—Ce2v | 99.782 (8) |
O4v—Ce1—O7vii | 146.86 (6) | Mo5xiv—Mo2—Ce2v | 149.571 (7) |
O2v—Ce1—O7vii | 100.38 (6) | Mo3—Mo2—Ce2v | 98.774 (7) |
O11—Ce1—O7vii | 87.29 (5) | Mo2ii—Mo2—Ce2v | 148.794 (4) |
O3iv—Ce1—Mo1v | 92.59 (5) | Li—Mo2—Ce2v | 123.174 (6) |
O12—Ce1—Mo1v | 98.83 (5) | O8—Mo3—O5 | 86.67 (6) |
O1v—Ce1—Mo1v | 36.42 (6) | O8—Mo3—O11 | 85.73 (6) |
O8—Ce1—Mo1v | 88.19 (4) | O5—Mo3—O11 | 167.88 (8) |
O10vi—Ce1—Mo1v | 146.49 (4) | O8—Mo3—O4 | 89.16 (7) |
O4v—Ce1—Mo1v | 36.73 (4) | O5—Mo3—O4 | 84.24 (7) |
O2v—Ce1—Mo1v | 35.48 (3) | O11—Mo3—O4 | 86.22 (9) |
O11—Ce1—Mo1v | 126.78 (5) | O8—Mo3—Mo1 | 137.36 (5) |
O7vii—Ce1—Mo1v | 135.15 (5) | O5—Mo3—Mo1 | 88.70 (5) |
O3iv—Ce1—Mo4xv | 96.09 (5) | O11—Mo3—Mo1 | 90.50 (6) |
O12—Ce1—Mo4xv | 128.25 (6) | O4—Mo3—Mo1 | 48.20 (5) |
O1v—Ce1—Mo4xv | 88.36 (6) | O8—Mo3—Mo3ii | 134.44 (5) |
O8—Ce1—Mo4xv | 34.03 (4) | O5—Mo3—Mo3ii | 138.70 (4) |
O10vi—Ce1—Mo4xv | 34.97 (4) | O11—Mo3—Mo3ii | 48.91 (4) |
O4v—Ce1—Mo4xv | 102.68 (4) | O4—Mo3—Mo3ii | 91.45 (5) |
O2v—Ce1—Mo4xv | 147.69 (3) | Mo1—Mo3—Mo3ii | 59.590 (5) |
O11—Ce1—Mo4xv | 65.48 (4) | O8—Mo3—Mo4v | 91.12 (5) |
O7vii—Ce1—Mo4xv | 106.14 (6) | O5—Mo3—Mo4v | 48.88 (5) |
Mo1v—Ce1—Mo4xv | 114.039 (6) | O11—Mo3—Mo4v | 140.67 (7) |
O3iv—Ce1—Mo2vii | 31.40 (4) | O4—Mo3—Mo4v | 132.99 (5) |
O12—Ce1—Mo2vii | 92.04 (5) | Mo1—Mo3—Mo4v | 116.662 (9) |
O1v—Ce1—Mo2vii | 96.68 (5) | Mo3ii—Mo3—Mo4v | 119.873 (6) |
O8—Ce1—Mo2vii | 145.48 (4) | O8—Mo3—Mo5 | 88.64 (5) |
O10vi—Ce1—Mo2vii | 84.91 (3) | O5—Mo3—Mo5 | 140.47 (5) |
O4v—Ce1—Mo2vii | 139.49 (4) | O11—Mo3—Mo5 | 48.74 (7) |
O2v—Ce1—Mo2vii | 79.64 (3) | O4—Mo3—Mo5 | 134.94 (5) |
O11—Ce1—Mo2vii | 121.66 (4) | Mo1—Mo3—Mo5 | 119.660 (8) |
O7vii—Ce1—Mo2vii | 34.91 (3) | Mo3ii—Mo3—Mo5 | 60.081 (5) |
Mo1v—Ce1—Mo2vii | 107.584 (6) | Mo4v—Mo3—Mo5 | 92.056 (9) |
Mo4xv—Ce1—Mo2vii | 112.839 (6) | O8—Mo3—Mo2 | 135.01 (5) |
O12—Ce2—O3ii | 133.58 (5) | O5—Mo3—Mo2 | 48.73 (4) |
O12—Ce2—O3 | 133.58 (5) | O11—Mo3—Mo2 | 139.20 (4) |
O3ii—Ce2—O3 | 79.20 (9) | O4—Mo3—Mo2 | 91.42 (4) |
O12—Ce2—O1vii | 149.28 (9) | Mo1—Mo3—Mo2 | 59.398 (8) |
O3ii—Ce2—O1vii | 65.37 (6) | Mo3ii—Mo3—Mo2 | 90.530 (5) |
O3—Ce2—O1vii | 65.37 (6) | Mo4v—Mo3—Mo2 | 57.266 (7) |
O12—Ce2—O2viii | 93.73 (7) | Mo5—Mo3—Mo2 | 120.425 (10) |
O3ii—Ce2—O2viii | 126.07 (5) | O8—Mo3—Mo4xv | 46.92 (5) |
O3—Ce2—O2viii | 84.21 (6) | O5—Mo3—Mo4xv | 90.84 (5) |
O1vii—Ce2—O2viii | 61.04 (6) | O11—Mo3—Mo4xv | 90.85 (6) |
O12—Ce2—O2vii | 93.73 (7) | O4—Mo3—Mo4xv | 136.07 (5) |
O3ii—Ce2—O2vii | 84.21 (6) | Mo1—Mo3—Mo4xv | 175.622 (10) |
O3—Ce2—O2vii | 126.07 (5) | Mo3ii—Mo3—Mo4xv | 118.702 (5) |
O1vii—Ce2—O2vii | 61.04 (6) | Mo4v—Mo3—Mo4xv | 60.145 (7) |
O2viii—Ce2—O2vii | 65.50 (7) | Mo5—Mo3—Mo4xv | 58.713 (6) |
O12—Ce2—O5v | 72.64 (6) | Mo2—Mo3—Mo4xv | 117.351 (9) |
O3ii—Ce2—O5v | 66.93 (5) | O8—Mo3—Mo5xiv | 133.82 (5) |
O3—Ce2—O5v | 104.01 (6) | O5—Mo3—Mo5xiv | 94.57 (5) |
O1vii—Ce2—O5v | 132.27 (6) | O11—Mo3—Mo5xiv | 97.51 (6) |
O2viii—Ce2—O5v | 166.30 (5) | O4—Mo3—Mo5xiv | 136.95 (5) |
O2vii—Ce2—O5v | 115.69 (5) | Mo1—Mo3—Mo5xiv | 88.790 (9) |
O12—Ce2—O5ix | 72.64 (6) | Mo3ii—Mo3—Mo5xiv | 61.803 (5) |
O3ii—Ce2—O5ix | 104.01 (6) | Mo4v—Mo3—Mo5xiv | 58.087 (6) |
O3—Ce2—O5ix | 66.93 (5) | Mo5—Mo3—Mo5xiv | 61.970 (9) |
O1vii—Ce2—O5ix | 132.27 (6) | Mo2—Mo3—Mo5xiv | 58.461 (7) |
O2viii—Ce2—O5ix | 115.69 (5) | Mo4xv—Mo3—Mo5xiv | 86.906 (8) |
O2vii—Ce2—O5ix | 166.30 (5) | O8—Mo3—Ce3 | 42.95 (5) |
O5v—Ce2—O5ix | 59.64 (7) | O5—Mo3—Ce3 | 55.13 (5) |
O12—Ce2—O2ix | 77.39 (4) | O11—Mo3—Ce3 | 113.38 (5) |
O3ii—Ce2—O2ix | 140.99 (6) | O4—Mo3—Ce3 | 60.69 (5) |
O3—Ce2—O2ix | 62.17 (6) | Mo1—Mo3—Ce3 | 102.416 (8) |
O1vii—Ce2—O2ix | 100.42 (3) | Mo3ii—Mo3—Ce3 | 149.964 (5) |
O2viii—Ce2—O2ix | 58.34 (6) | Mo4v—Mo3—Ce3 | 89.212 (7) |
O2vii—Ce2—O2ix | 122.06 (3) | Mo5—Mo3—Ce3 | 131.587 (7) |
O5v—Ce2—O2ix | 115.54 (5) | Mo2—Mo3—Ce3 | 100.481 (7) |
O5ix—Ce2—O2ix | 57.35 (5) | Mo4xv—Mo3—Ce3 | 80.844 (7) |
O12—Ce2—O2v | 77.39 (4) | Mo5xiv—Mo3—Ce3 | 146.743 (8) |
O3ii—Ce2—O2v | 62.17 (6) | O6—Mo4—O8xvi | 85.31 (9) |
O3—Ce2—O2v | 140.99 (6) | O6—Mo4—O5v | 89.00 (9) |
O1vii—Ce2—O2v | 100.42 (3) | O8xvi—Mo4—O5v | 173.10 (7) |
O2viii—Ce2—O2v | 122.06 (3) | O6—Mo4—O10v | 91.20 (7) |
O2vii—Ce2—O2v | 58.34 (6) | O8xvi—Mo4—O10v | 82.35 (7) |
O5v—Ce2—O2v | 57.35 (5) | O5v—Mo4—O10v | 101.70 (7) |
O5ix—Ce2—O2v | 115.54 (5) | O6—Mo4—O9 | 79.29 (5) |
O2ix—Ce2—O2v | 154.73 (7) | O8xvi—Mo4—O9 | 87.84 (5) |
O12—Ce2—Mo1vii | 111.35 (6) | O5v—Mo4—O9 | 87.27 (4) |
O3ii—Ce2—Mo1vii | 94.00 (4) | O10v—Mo4—O9 | 166.89 (5) |
O3—Ce2—Mo1vii | 94.00 (4) | O6—Mo4—Mo2v | 96.21 (6) |
O1vii—Ce2—Mo1vii | 37.93 (6) | O8xvi—Mo4—Mo2v | 133.42 (5) |
O2viii—Ce2—Mo1vii | 36.42 (4) | O5v—Mo4—Mo2v | 51.11 (4) |
O2vii—Ce2—Mo1vii | 36.42 (4) | O10v—Mo4—Mo2v | 51.11 (5) |
O5v—Ce2—Mo1vii | 150.15 (3) | O9—Mo4—Mo2v | 138.338 (10) |
O5ix—Ce2—Mo1vii | 150.15 (3) | O6—Mo4—Mo5xvii | 140.45 (5) |
O2ix—Ce2—Mo1vii | 93.84 (3) | O8xvi—Mo4—Mo5xvii | 87.85 (5) |
O2v—Ce2—Mo1vii | 93.84 (3) | O5v—Mo4—Mo5xvii | 99.03 (5) |
O12—Ce2—Mo2v | 98.05 (3) | O10v—Mo4—Mo5xvii | 49.26 (5) |
O3ii—Ce2—Mo2v | 35.57 (4) | O9—Mo4—Mo5xvii | 139.345 (9) |
O3—Ce2—Mo2v | 106.07 (5) | Mo2v—Mo4—Mo5xvii | 61.952 (8) |
O1vii—Ce2—Mo2v | 97.73 (3) | O6—Mo4—Mo3v | 137.41 (8) |
O2viii—Ce2—Mo2v | 150.68 (4) | O8xvi—Mo4—Mo3v | 136.74 (4) |
O2vii—Ce2—Mo2v | 86.93 (4) | O5v—Mo4—Mo3v | 48.54 (5) |
O5v—Ce2—Mo2v | 37.81 (3) | O10v—Mo4—Mo3v | 99.64 (5) |
O5ix—Ce2—Mo2v | 93.48 (4) | O9—Mo4—Mo3v | 93.467 (8) |
O2ix—Ce2—Mo2v | 150.67 (3) | Mo2v—Mo4—Mo3v | 62.060 (7) |
O2v—Ce2—Mo2v | 37.12 (4) | Mo5xvii—Mo4—Mo3v | 63.801 (8) |
Mo1vii—Ce2—Mo2v | 114.434 (4) | O6—Mo4—Mo4xviii | 127.74 (5) |
O12v—Ce3—O8 | 132.16 (5) | O8xvi—Mo4—Mo4xviii | 88.58 (4) |
O12v—Ce3—O8x | 132.16 (5) | O5v—Mo4—Mo4xviii | 91.83 (4) |
O8—Ce3—O8x | 80.35 (8) | O10v—Mo4—Mo4xviii | 139.18 (4) |
O12v—Ce3—O4v | 108.37 (7) | O9—Mo4—Mo4xviii | 48.606 (5) |
O8—Ce3—O4v | 72.90 (6) | Mo2v—Mo4—Mo4xviii | 123.722 (10) |
O8x—Ce3—O4v | 115.46 (5) | Mo5xvii—Mo4—Mo4xviii | 90.884 (6) |
O12v—Ce3—O4xi | 108.37 (7) | Mo3v—Mo4—Mo4xviii | 61.730 (7) |
O8—Ce3—O4xi | 115.46 (5) | O6—Mo4—Mo3xvi | 130.47 (8) |
O8x—Ce3—O4xi | 72.90 (6) | O8xvi—Mo4—Mo3xvi | 45.63 (4) |
O4v—Ce3—O4xi | 68.25 (8) | O5v—Mo4—Mo3xvi | 139.29 (4) |
O12v—Ce3—O5x | 72.46 (7) | O10v—Mo4—Mo3xvi | 88.72 (5) |
O8—Ce3—O5x | 103.13 (6) | O9—Mo4—Mo3xvi | 90.635 (7) |
O8x—Ce3—O5x | 65.41 (5) | Mo2v—Mo4—Mo3xvi | 120.793 (9) |
O4v—Ce3—O5x | 175.45 (6) | Mo5xvii—Mo4—Mo3xvi | 58.843 (8) |
O4xi—Ce3—O5x | 115.94 (5) | Mo3v—Mo4—Mo3xvi | 91.111 (9) |
O12v—Ce3—O5 | 72.47 (7) | Mo4xviii—Mo4—Mo3xvi | 58.125 (7) |
O8—Ce3—O5 | 65.41 (5) | O6—Mo4—Mo4ii | 38.07 (5) |
O8x—Ce3—O5 | 103.13 (6) | O8xvi—Mo4—Mo4ii | 88.38 (5) |
O4v—Ce3—O5 | 115.94 (5) | O5v—Mo4—Mo4ii | 84.74 (5) |
O4xi—Ce3—O5 | 175.45 (6) | O10v—Mo4—Mo4ii | 129.14 (5) |
O5x—Ce3—O5 | 59.82 (7) | O9—Mo4—Mo4ii | 41.395 (5) |
O12v—Ce3—O4x | 74.97 (3) | Mo2v—Mo4—Mo4ii | 120.433 (6) |
O8—Ce3—O4x | 143.69 (6) | Mo5xvii—Mo4—Mo4ii | 176.099 (7) |
O8x—Ce3—O4x | 63.90 (5) | Mo3v—Mo4—Mo4ii | 119.873 (6) |
O4v—Ce3—O4x | 127.22 (4) | Mo4xviii—Mo4—Mo4ii | 90.0 |
O4xi—Ce3—O4x | 61.42 (6) | Mo3xvi—Mo4—Mo4ii | 118.702 (5) |
O5x—Ce3—O4x | 57.32 (5) | O6—Mo4—Ce1xvi | 75.70 (7) |
O5—Ce3—O4x | 115.02 (5) | O8xvi—Mo4—Ce1xvi | 40.64 (4) |
O12v—Ce3—O4 | 74.97 (3) | O5v—Mo4—Ce1xvi | 141.03 (4) |
O8—Ce3—O4 | 63.90 (5) | O10v—Mo4—Ce1xvi | 44.48 (5) |
O8x—Ce3—O4 | 143.69 (6) | O9—Mo4—Ce1xvi | 123.412 (8) |
O4v—Ce3—O4 | 61.42 (6) | Mo2v—Mo4—Ce1xvi | 94.531 (7) |
O4xi—Ce3—O4 | 127.22 (3) | Mo5xvii—Mo4—Ce1xvi | 73.927 (8) |
O5x—Ce3—O4 | 115.02 (5) | Mo3v—Mo4—Ce1xvi | 137.453 (8) |
O5—Ce3—O4 | 57.32 (5) | Mo4xviii—Mo4—Ce1xvi | 125.945 (10) |
O4x—Ce3—O4 | 149.80 (6) | Mo3xvi—Mo4—Ce1xvi | 70.101 (6) |
O12v—Ce3—O11v | 59.67 (8) | Mo4ii—Mo4—Ce1xvi | 102.511 (4) |
O8—Ce3—O11v | 130.85 (5) | O11—Mo5—O10xiv | 85.23 (7) |
O8x—Ce3—O11v | 130.85 (5) | O11—Mo5—O10vi | 85.23 (7) |
O4v—Ce3—O11v | 59.89 (5) | O10xiv—Mo5—O10vi | 84.89 (9) |
O4xi—Ce3—O11v | 59.89 (5) | O11—Mo5—Mo4xix | 93.800 (8) |
O5x—Ce3—O11v | 123.33 (5) | O10xiv—Mo5—Mo4xix | 48.96 (4) |
O5—Ce3—O11v | 123.33 (5) | O10vi—Mo5—Mo4xix | 133.64 (5) |
O4x—Ce3—O11v | 81.27 (4) | O11—Mo5—Mo4xv | 93.800 (8) |
O4—Ce3—O11v | 81.27 (4) | O10xiv—Mo5—Mo4xv | 133.64 (5) |
O12v—Ce3—O1v | 157.12 (8) | O10vi—Mo5—Mo4xv | 48.96 (4) |
O8—Ce3—O1v | 61.54 (5) | Mo4xix—Mo5—Mo4xv | 172.199 (15) |
O8x—Ce3—O1v | 61.54 (5) | O11—Mo5—Mo3 | 48.79 (4) |
O4v—Ce3—O1v | 53.99 (5) | O10xiv—Mo5—Mo3 | 134.00 (5) |
O4xi—Ce3—O1v | 53.99 (5) | O10vi—Mo5—Mo3 | 91.23 (5) |
O5x—Ce3—O1v | 126.41 (5) | Mo4xix—Mo5—Mo3 | 122.183 (10) |
O5—Ce3—O1v | 126.41 (5) | Mo4xv—Mo5—Mo3 | 62.444 (6) |
O4x—Ce3—O1v | 103.27 (3) | O11—Mo5—Mo3ii | 48.79 (4) |
O4—Ce3—O1v | 103.27 (3) | O10xiv—Mo5—Mo3ii | 91.23 (5) |
O11v—Ce3—O1v | 97.45 (6) | O10vi—Mo5—Mo3ii | 134.00 (5) |
O12v—Ce3—Mo3 | 96.37 (3) | Mo4xix—Mo5—Mo3ii | 62.444 (6) |
O8—Ce3—Mo3 | 35.79 (4) | Mo4xv—Mo5—Mo3ii | 122.183 (10) |
O8x—Ce3—Mo3 | 107.81 (4) | Mo3—Mo5—Mo3ii | 59.838 (9) |
O4v—Ce3—Mo3 | 81.55 (4) | O11—Mo5—Mo2xiv | 133.96 (4) |
O4xi—Ce3—Mo3 | 145.52 (4) | O10xiv—Mo5—Mo2xiv | 48.76 (5) |
O5x—Ce3—Mo3 | 93.92 (4) | O10vi—Mo5—Mo2xiv | 91.12 (5) |
O5—Ce3—Mo3 | 37.35 (3) | Mo4xix—Mo5—Mo2xiv | 57.330 (6) |
O4x—Ce3—Mo3 | 151.21 (4) | Mo4xv—Mo5—Mo2xiv | 117.621 (10) |
O4—Ce3—Mo3 | 37.32 (4) | Mo3—Mo5—Mo2xiv | 176.566 (12) |
O11v—Ce3—Mo3 | 118.510 (8) | Mo3ii—Mo5—Mo2xiv | 119.773 (6) |
O1v—Ce3—Mo3 | 95.02 (2) | O11—Mo5—Mo2vi | 133.96 (4) |
O12v—Ce3—Mo3x | 96.37 (3) | O10xiv—Mo5—Mo2vi | 91.12 (5) |
O8—Ce3—Mo3x | 107.81 (4) | O10vi—Mo5—Mo2vi | 48.76 (5) |
O8x—Ce3—Mo3x | 35.79 (4) | Mo4xix—Mo5—Mo2vi | 117.621 (10) |
O4v—Ce3—Mo3x | 145.52 (4) | Mo4xv—Mo5—Mo2vi | 57.330 (6) |
O4xi—Ce3—Mo3x | 81.55 (4) | Mo3—Mo5—Mo2vi | 119.773 (6) |
O5x—Ce3—Mo3x | 37.35 (3) | Mo3ii—Mo5—Mo2vi | 176.566 (12) |
O5—Ce3—Mo3x | 93.92 (4) | Mo2xiv—Mo5—Mo2vi | 60.381 (9) |
O4x—Ce3—Mo3x | 37.32 (4) | O11—Mo5—Mo3xiv | 138.63 (4) |
O4—Ce3—Mo3x | 151.21 (4) | O10xiv—Mo5—Mo3xiv | 94.72 (5) |
O11v—Ce3—Mo3x | 118.510 (8) | O10vi—Mo5—Mo3xiv | 136.07 (5) |
O1v—Ce3—Mo3x | 95.02 (2) | Mo4xix—Mo5—Mo3xiv | 58.113 (6) |
Mo3—Ce3—Mo3x | 119.929 (9) | Mo4xv—Mo5—Mo3xiv | 114.493 (10) |
O12v—Ce3—Mo1v | 122.20 (7) | Mo3—Mo5—Mo3xiv | 118.030 (9) |
O8—Ce3—Mo1v | 87.20 (4) | Mo3ii—Mo5—Mo3xiv | 89.919 (9) |
O8x—Ce3—Mo1v | 87.20 (4) | Mo2xiv—Mo5—Mo3xiv | 58.622 (7) |
O4v—Ce3—Mo1v | 35.35 (4) | Mo2vi—Mo5—Mo3xiv | 87.395 (10) |
O4xi—Ce3—Mo1v | 35.35 (4) | O11—Mo5—Mo3vi | 138.63 (4) |
O5x—Ce3—Mo1v | 148.03 (3) | O10xiv—Mo5—Mo3vi | 136.07 (5) |
O5—Ce3—Mo1v | 148.03 (3) | O10vi—Mo5—Mo3vi | 94.72 (5) |
O4x—Ce3—Mo1v | 96.76 (3) | Mo4xix—Mo5—Mo3vi | 114.493 (10) |
O4—Ce3—Mo1v | 96.76 (3) | Mo4xv—Mo5—Mo3vi | 58.113 (6) |
O11v—Ce3—Mo1v | 62.53 (4) | Mo3—Mo5—Mo3vi | 89.919 (9) |
O1v—Ce3—Mo1v | 34.92 (5) | Mo3ii—Mo5—Mo3vi | 118.030 (9) |
Mo3—Ce3—Mo1v | 110.725 (4) | Mo2xiv—Mo5—Mo3vi | 87.395 (10) |
Mo3x—Ce3—Mo1v | 110.725 (4) | Mo2vi—Mo5—Mo3vi | 58.622 (7) |
O12v—Ce3—O9xxv | 113.66 (7) | Mo3xiv—Mo5—Mo3vi | 56.395 (9) |
O8—Ce3—O9xxv | 52.86 (4) | O11—Mo5—Mo5xiv | 97.23 (6) |
O8x—Ce3—O9xxv | 52.86 (4) | O10xiv—Mo5—Mo5xiv | 137.55 (4) |
O4v—Ce3—O9xxv | 125.08 (4) | O10vi—Mo5—Mo5xiv | 137.55 (4) |
O4xi—Ce3—O9xxv | 125.08 (4) | Mo4xix—Mo5—Mo5xiv | 88.648 (6) |
O5x—Ce3—O9xxv | 51.42 (4) | Mo4xv—Mo5—Mo5xiv | 88.648 (6) |
O5—Ce3—O9xxv | 51.42 (4) | Mo3—Mo5—Mo5xiv | 61.593 (9) |
O4x—Ce3—O9xxv | 97.25 (4) | Mo3ii—Mo5—Mo5xiv | 61.593 (9) |
O4—Ce3—O9xxv | 97.25 (4) | Mo2xiv—Mo5—Mo5xiv | 115.053 (13) |
O11v—Ce3—O9xxv | 173.33 (4) | Mo2vi—Mo5—Mo5xiv | 115.053 (13) |
O1v—Ce3—O9xxv | 89.22 (5) | Mo3xiv—Mo5—Mo5xiv | 56.437 (9) |
Mo3—Ce3—O9xxv | 60.555 (5) | Mo3vi—Mo5—Mo5xiv | 56.437 (9) |
Mo3x—Ce3—O9xxv | 60.555 (5) | Mo1—O1—Ce1v | 99.29 (6) |
Mo1v—Ce3—O9xxv | 124.139 (7) | Mo1—O1—Ce1ix | 99.29 (6) |
O12v—Ce3—Ce1xi | 36.60 (3) | Ce1v—O1—Ce1ix | 157.89 (13) |
O8—Ce3—Ce1xi | 168.71 (4) | Mo1—O1—Ce2xx | 90.06 (9) |
O8x—Ce3—Ce1xi | 108.76 (4) | Ce1v—O1—Ce2xx | 95.93 (6) |
O4v—Ce3—Ce1xi | 107.70 (4) | Ce1ix—O1—Ce2xx | 95.93 (6) |
O4xi—Ce3—Ce1xi | 74.40 (4) | Mo1—O1—Ce3v | 76.55 (7) |
O5x—Ce3—Ce1xi | 75.73 (4) | Ce1v—O1—Ce3v | 86.38 (6) |
O5—Ce3—Ce1xi | 105.23 (3) | Ce1ix—O1—Ce3v | 86.38 (6) |
O4x—Ce3—Ce1xi | 44.87 (3) | Ce2xx—O1—Ce3v | 166.61 (11) |
O4—Ce3—Ce1xi | 106.11 (3) | Mo1—O2—Mo2 | 84.01 (7) |
O11v—Ce3—Ce1xi | 47.87 (3) | Mo1—O2—Ce2xx | 91.22 (7) |
O1v—Ce3—Ce1xi | 128.32 (4) | Mo2—O2—Ce2xx | 131.36 (8) |
Mo3—Ce3—Ce1xi | 132.947 (5) | Mo1—O2—Ce1v | 86.94 (6) |
Mo3x—Ce3—Ce1xi | 78.291 (4) | Mo2—O2—Ce1v | 142.24 (7) |
Mo1v—Ce3—Ce1xi | 99.649 (6) | Ce2xx—O2—Ce1v | 85.31 (6) |
O9xxv—Ce3—Ce1xi | 127.147 (5) | Mo1—O2—Ce2v | 144.38 (7) |
O6xii—Ce4—O6 | 180.0 | Mo2—O2—Ce2v | 83.45 (6) |
O6xii—Ce4—O3 | 101.93 (7) | Ce2xx—O2—Ce2v | 121.66 (6) |
O6—Ce4—O3 | 78.07 (7) | Ce1v—O2—Ce2v | 82.93 (5) |
O6xii—Ce4—O3xii | 78.07 (7) | Mo2ix—O3—Ce1xxi | 111.27 (8) |
O6—Ce4—O3xii | 101.93 (7) | Mo2ix—O3—Ce2 | 101.31 (7) |
O3—Ce4—O3xii | 180.00 (6) | Ce1xxi—O3—Ce2 | 103.98 (7) |
O6xii—Ce4—O3ii | 101.93 (7) | Mo2ix—O3—Ce4 | 127.21 (8) |
O6—Ce4—O3ii | 78.07 (7) | Ce1xxi—O3—Ce4 | 108.51 (6) |
O3—Ce4—O3ii | 77.58 (9) | Ce2—O3—Ce4 | 101.22 (6) |
O3xii—Ce4—O3ii | 102.42 (9) | Mo1—O4—Mo3 | 81.91 (7) |
O6xii—Ce4—O3xiii | 78.07 (7) | Mo1—O4—Ce3v | 98.59 (7) |
O6—Ce4—O3xiii | 101.93 (7) | Mo3—O4—Ce3v | 116.62 (7) |
O3—Ce4—O3xiii | 102.42 (9) | Mo1—O4—Ce1v | 90.24 (6) |
O3xii—Ce4—O3xiii | 77.58 (9) | Mo3—O4—Ce1v | 144.66 (8) |
O3ii—Ce4—O3xiii | 180.00 (6) | Ce3v—O4—Ce1v | 98.58 (6) |
O6xii—Ce4—Ce2 | 109.59 (7) | Mo1—O4—Ce3 | 142.82 (8) |
O6—Ce4—Ce2 | 70.41 (7) | Mo3—O4—Ce3 | 81.99 (6) |
O3—Ce4—Ce2 | 38.98 (4) | Ce3v—O4—Ce3 | 118.58 (6) |
O3xii—Ce4—Ce2 | 141.02 (4) | Ce1v—O4—Ce3 | 83.95 (5) |
O3ii—Ce4—Ce2 | 38.98 (4) | Mo3—O5—Mo4v | 82.58 (6) |
O3xiii—Ce4—Ce2 | 141.02 (4) | Mo3—O5—Mo2 | 83.46 (6) |
O6xii—Ce4—Ce2xii | 70.41 (7) | Mo4v—O5—Mo2 | 78.42 (6) |
O6—Ce4—Ce2xii | 109.59 (7) | Mo3—O5—Ce3 | 87.52 (6) |
O3—Ce4—Ce2xii | 141.02 (4) | Mo4v—O5—Ce3 | 125.09 (7) |
O3xii—Ce4—Ce2xii | 38.98 (4) | Mo2—O5—Ce3 | 153.48 (9) |
O3ii—Ce4—Ce2xii | 141.02 (4) | Mo3—O5—Ce2v | 150.69 (9) |
O3xiii—Ce4—Ce2xii | 38.98 (4) | Mo4v—O5—Ce2v | 122.56 (7) |
Ce2—Ce4—Ce2xii | 180.000 (1) | Mo2—O5—Ce2v | 87.13 (5) |
O6xii—Ce4—Ce1xvi | 113.22 (5) | Ce3—O5—Ce2v | 88.70 (5) |
O6—Ce4—Ce1xvi | 66.78 (5) | Mo4—O6—Mo4ii | 103.86 (10) |
O3—Ce4—Ce1xvi | 144.81 (4) | Mo4—O6—Ce4 | 127.46 (5) |
O3xii—Ce4—Ce1xvi | 35.19 (4) | Mo4ii—O6—Ce4 | 127.46 (5) |
O3ii—Ce4—Ce1xvi | 93.18 (4) | Li—O7—Mo2ii | 101.54 (10) |
O3xiii—Ce4—Ce1xvi | 86.82 (4) | Li—O7—Mo2 | 101.54 (10) |
Ce2—Ce4—Ce1xvi | 121.134 (3) | Mo2ii—O7—Mo2 | 84.19 (8) |
Ce2xii—Ce4—Ce1xvi | 58.866 (3) | Li—O7—Ce1xx | 97.91 (7) |
O6xii—Ce4—Ce1xxi | 66.78 (5) | Mo2ii—O7—Ce1xx | 160.55 (13) |
O6—Ce4—Ce1xxi | 113.22 (5) | Mo2—O7—Ce1xx | 92.16 (3) |
O3—Ce4—Ce1xxi | 35.19 (4) | Li—O7—Ce1xxii | 97.91 (7) |
O3xii—Ce4—Ce1xxi | 144.81 (4) | Mo2ii—O7—Ce1xxii | 92.16 (3) |
O3ii—Ce4—Ce1xxi | 86.82 (4) | Mo2—O7—Ce1xxii | 160.55 (13) |
O3xiii—Ce4—Ce1xxi | 93.18 (4) | Ce1xx—O7—Ce1xxii | 84.94 (6) |
Ce2—Ce4—Ce1xxi | 58.866 (3) | Mo3—O8—Mo4xv | 87.45 (7) |
Ce2xii—Ce4—Ce1xxi | 121.134 (3) | Mo3—O8—Ce3 | 101.26 (6) |
Ce1xvi—Ce4—Ce1xxi | 180.000 (3) | Mo4xv—O8—Ce3 | 132.81 (8) |
O6xii—Ce4—Ce1xxiv | 113.22 (5) | Mo3—O8—Ce1 | 113.93 (8) |
O6—Ce4—Ce1xxiv | 66.78 (5) | Mo4xv—O8—Ce1 | 105.34 (6) |
O3—Ce4—Ce1xxiv | 93.18 (4) | Ce3—O8—Ce1 | 112.60 (7) |
O3xii—Ce4—Ce1xxiv | 86.82 (4) | Mo4ii—O9—Mo4xviii | 180.000 (11) |
O3ii—Ce4—Ce1xxiv | 144.81 (4) | Mo4ii—O9—Mo4 | 97.211 (10) |
O3xiii—Ce4—Ce1xxiv | 35.19 (4) | Mo4xviii—O9—Mo4 | 82.789 (10) |
Ce2—Ce4—Ce1xxiv | 121.134 (3) | Mo4ii—O9—Mo4xxiii | 82.789 (10) |
Ce2xii—Ce4—Ce1xxiv | 58.866 (3) | Mo4xviii—O9—Mo4xxiii | 97.211 (10) |
Ce1xvi—Ce4—Ce1xxiv | 74.878 (4) | Mo4—O9—Mo4xxiii | 180.000 (11) |
Ce1xxi—Ce4—Ce1xxiv | 105.122 (4) | Mo4ii—O9—Ce3v | 94.201 (6) |
O6xii—Ce4—Ce1xxvi | 66.78 (5) | Mo4xviii—O9—Ce3v | 85.799 (6) |
O6—Ce4—Ce1xxvi | 113.22 (5) | Mo4—O9—Ce3v | 94.201 (6) |
O3—Ce4—Ce1xxvi | 86.82 (4) | Mo4xxiii—O9—Ce3v | 85.799 (6) |
O3xii—Ce4—Ce1xxvi | 93.18 (4) | Mo4ii—O9—Ce3xxiv | 85.799 (6) |
O3ii—Ce4—Ce1xxvi | 35.19 (4) | Mo4xviii—O9—Ce3xxiv | 94.201 (6) |
O3xiii—Ce4—Ce1xxvi | 144.81 (4) | Mo4—O9—Ce3xxiv | 85.799 (6) |
Ce2—Ce4—Ce1xxvi | 58.866 (3) | Mo4xxiii—O9—Ce3xxiv | 94.201 (6) |
Ce2xii—Ce4—Ce1xxvi | 121.134 (3) | Ce3v—O9—Ce3xxiv | 180.000 (5) |
Ce1xvi—Ce4—Ce1xxvi | 105.122 (4) | Mo4v—O10—Mo5xiv | 81.78 (6) |
Ce1xxi—Ce4—Ce1xxvi | 74.878 (4) | Mo4v—O10—Mo2 | 78.26 (6) |
Ce1xxiv—Ce4—Ce1xxvi | 180.000 (3) | Mo5xiv—O10—Mo2 | 82.62 (6) |
O2—Mo1—O2ii | 92.35 (10) | Mo4v—O10—Li | 162.57 (9) |
O2—Mo1—O4ii | 167.83 (8) | Mo5xiv—O10—Li | 100.44 (7) |
O2ii—Mo1—O4ii | 88.28 (7) | Mo2—O10—Li | 84.86 (6) |
O2—Mo1—O4 | 88.28 (7) | Mo4v—O10—Ce1vi | 100.54 (7) |
O2ii—Mo1—O4 | 167.83 (8) | Mo5xiv—O10—Ce1vi | 111.85 (7) |
O4ii—Mo1—O4 | 88.58 (10) | Mo2—O10—Ce1vi | 165.29 (8) |
O2—Mo1—O1 | 83.18 (7) | Li—O10—Ce1vi | 94.68 (6) |
O2ii—Mo1—O1 | 83.18 (7) | Mo5—O11—Mo3 | 82.47 (8) |
O4ii—Mo1—O1 | 84.83 (7) | Mo5—O11—Mo3ii | 82.47 (8) |
O4—Mo1—O1 | 84.83 (7) | Mo3—O11—Mo3ii | 82.19 (8) |
O2—Mo1—Mo3ii | 142.09 (6) | Mo5—O11—Ce1ii | 100.65 (7) |
O2ii—Mo1—Mo3ii | 93.36 (5) | Mo3—O11—Ce1ii | 176.28 (11) |
O4ii—Mo1—Mo3ii | 49.89 (5) | Mo3ii—O11—Ce1ii | 96.162 (13) |
O4—Mo1—Mo3ii | 93.59 (5) | Mo5—O11—Ce1 | 100.65 (7) |
O1—Mo1—Mo3ii | 134.71 (5) | Mo3—O11—Ce1 | 96.162 (13) |
O2—Mo1—Mo3 | 93.36 (5) | Mo3ii—O11—Ce1 | 176.28 (11) |
O2ii—Mo1—Mo3 | 142.09 (6) | Ce1ii—O11—Ce1 | 85.28 (6) |
O4ii—Mo1—Mo3 | 93.59 (5) | Mo5—O11—Ce3v | 179.63 (10) |
O4—Mo1—Mo3 | 49.89 (5) | Mo3—O11—Ce3v | 97.25 (8) |
O1—Mo1—Mo3 | 134.71 (5) | Mo3ii—O11—Ce3v | 97.25 (8) |
Mo3ii—Mo1—Mo3 | 60.821 (10) | Ce1ii—O11—Ce3v | 79.62 (6) |
O2—Mo1—Mo2ii | 95.29 (6) | Ce1—O11—Ce3v | 79.62 (6) |
O2ii—Mo1—Mo2ii | 49.58 (6) | Ce2—O12—Ce3v | 113.01 (11) |
O4ii—Mo1—Mo2ii | 94.36 (5) | Ce2—O12—Ce1ii | 109.67 (6) |
O4—Mo1—Mo2ii | 142.46 (6) | Ce3v—O12—Ce1ii | 107.36 (6) |
O1—Mo1—Mo2ii | 132.72 (5) | Ce2—O12—Ce1 | 109.67 (6) |
Mo3ii—Mo1—Mo2ii | 61.651 (7) | Ce3v—O12—Ce1 | 107.36 (6) |
Mo3—Mo1—Mo2ii | 92.568 (10) | Ce1ii—O12—Ce1 | 109.69 (11) |
O2—Mo1—Mo2 | 49.58 (6) |
Symmetry codes: (i) −x−1, −y−1, −z+2; (ii) x, −y−1, z; (iii) −x−1, y, −z+2; (iv) −x−1/2, y+1/2, −z; (v) −x−1/2, −y−1/2, −z+1; (vi) −x−1, y, −z+1; (vii) x, y, z−1; (viii) x, −y−1, z−1; (ix) −x−1/2, y−1/2, −z+1; (x) x, −y, z; (xi) −x−1/2, y+1/2, −z+1; (xii) −x, −y−1, −z; (xiii) −x, y, −z; (xiv) −x−1, −y−1, −z+1; (xv) x−1/2, −y−1/2, z; (xvi) x+1/2, −y−1/2, z; (xvii) x+1/2, y+1/2, z; (xviii) −x, y, −z+1; (xix) x−1/2, y−1/2, z; (xx) x, y, z+1; (xxi) −x−1/2, y−1/2, −z; (xxii) x, −y−1, z+1; (xxiii) −x, −y−1, −z+1; (xxiv) x+1/2, y−1/2, z; (xxv) x−1/2, y+1/2, z; (xxvi) −x−1/2, −y−1/2, −z. |
Experimental details
Crystal data | |
Chemical formula | LiCe9Mo16O35 |
Mr | 3363.06 |
Crystal system, space group | Monoclinic, C2/m |
Temperature (K) | 293 |
a, b, c (Å) | 18.3000 (2), 8.6326 (1), 9.8172 (1) |
β (°) | 102.0953 (7) |
V (Å3) | 1516.46 (3) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 19.66 |
Crystal size (mm) | 0.15 × 0.12 × 0.06 |
Data collection | |
Diffractometer | Nonius KappaCCD diffractometer |
Absorption correction | Multi-scan (PLATON; Spek, 2009) |
Tmin, Tmax | 0.190, 0.418 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 21270, 3511, 3383 |
Rint | 0.027 |
(sin θ/λ)max (Å−1) | 0.807 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.016, 0.033, 1.29 |
No. of reflections | 3511 |
No. of parameters | 158 |
Δρmax, Δρmin (e Å−3) | 1.13, −1.33 |
Computer programs: COLLECT (Nonius, 1998), EVALCCD (Duisenberg et al., 2003), SIR97 (Altomare et al., 1999), SHELXL97 (Sheldrick, 2008), DIAMOND (Bergerhoff, 1996).
Li—O7 | 1.861 (3) | Mo1—O2 | 1.9759 (16) |
Li—O10 | 2.4135 (16) | Mo1—O2v | 1.9759 (16) |
Ce1—O3i | 2.3603 (16) | Mo1—O4v | 2.0332 (17) |
Ce1—O12 | 2.3916 (16) | Mo1—O4 | 2.0332 (17) |
Ce1—O1ii | 2.4055 (5) | Mo1—O1 | 2.045 (3) |
Ce1—O8 | 2.4159 (16) | Mo1—Mo3 | 2.7003 (3) |
Ce1—O10iii | 2.5499 (19) | Mo1—Mo2 | 2.7129 (3) |
Ce1—O4ii | 2.7161 (18) | Mo2—O3ix | 2.0277 (16) |
Ce1—O2ii | 2.874 (2) | Mo2—O2 | 2.077 (2) |
Ce1—O11 | 2.8865 (16) | Mo2—O7 | 2.0773 (16) |
Ce1—O7iv | 2.8959 (17) | Mo2—O5 | 2.0985 (16) |
Ce2—O12 | 2.337 (3) | Mo2—O10 | 2.0997 (19) |
Ce2—O3v | 2.3829 (19) | Mo2—Mo4ii | 2.6412 (3) |
Ce2—O3 | 2.3829 (19) | Mo2—Mo5xii | 2.7691 (3) |
Ce2—O1iv | 2.622 (2) | Mo2—Mo3 | 2.7739 (2) |
Ce2—O2vi | 2.6352 (17) | Mo2—Mo2v | 2.7851 (4) |
Ce2—O2iv | 2.6352 (17) | Mo3—O8 | 2.0315 (16) |
Ce2—O5ii | 2.8054 (16) | Mo3—O5 | 2.0688 (16) |
Ce2—O5vii | 2.8054 (16) | Mo3—O11 | 2.0795 (16) |
Ce2—O2vii | 2.9625 (17) | Mo3—O4 | 2.0860 (19) |
Ce2—O2ii | 2.9625 (17) | Mo3—Mo3v | 2.7338 (4) |
Ce3—O8 | 2.3670 (17) | Mo3—Mo4ii | 2.7375 (3) |
Ce3—O8viii | 2.3670 (17) | Mo3—Mo5 | 2.7405 (3) |
Ce3—O4ii | 2.5309 (18) | Mo3—Mo4xiii | 2.8391 (3) |
Ce3—O4ix | 2.5309 (18) | Mo3—Mo5xii | 2.8928 (3) |
Ce3—O5viii | 2.7980 (17) | Mo4—O6 | 2.0145 (14) |
Ce3—O5 | 2.7980 (17) | Mo4—O8xiv | 2.0758 (19) |
Ce3—O4viii | 3.0001 (17) | Mo4—O5ii | 2.0797 (19) |
Ce3—O4 | 3.0001 (17) | Mo4—O10ii | 2.0857 (16) |
Ce3—O11ii | 3.089 (3) | Mo4—O9 | 2.1141 (2) |
Ce4—O6x | 2.280 (2) | Mo4—Mo4xv | 2.7958 (3) |
Ce4—O6 | 2.280 (2) | Mo5—O11 | 2.078 (3) |
Ce4—O3 | 2.4244 (19) | Mo5—O10xii | 2.0950 (16) |
Ce4—O3x | 2.4244 (19) | Mo5—O10iii | 2.0950 (16) |
Ce4—O3v | 2.4244 (19) | Mo5—Mo5xii | 2.9030 (5) |
Ce4—O3xi | 2.4244 (19) |
Symmetry codes: (i) −x−1/2, y+1/2, −z; (ii) −x−1/2, −y−1/2, −z+1; (iii) −x−1, y, −z+1; (iv) x, y, z−1; (v) x, −y−1, z; (vi) x, −y−1, z−1; (vii) −x−1/2, y−1/2, −z+1; (viii) x, −y, z; (ix) −x−1/2, y+1/2, −z+1; (x) −x, −y−1, −z; (xi) −x, y, −z; (xii) −x−1, −y−1, −z+1; (xiii) x−1/2, −y−1/2, z; (xiv) x+1/2, −y−1/2, z; (xv) −x, y, −z+1. |
Acknowledgements
Intensity data were collected on the Nonius KappaCCD X-ray diffactometer system of the `Centre de diffractométrie de l'Université de Rennes I'.
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LiCe9Mo16O35 is isotopic with the LiNd9Mo16O35 (Gougeon et al., 2011) structure type. The crystal structure (Fig. 1) is based on Mo16O26iO10a cluster units (Fig. 2) sharing two Oi or four Oa ligands (for details of the i- and a-type ligand notation, see Schäfer & von Schnering (1964)) to form infinite molybdenum cluster chains running parallel to the b axis. The Mo16 core of the Mo16O26iO10a unit can be seen as resulting of the fusion of two bioctahedral Mo10 clusters through the sharing of three edges per Mo10 cluster. The Mo10 cluster results itself from metal edge-sharing of two Mo6 octahedra and was first observed forming infinite chains in the MMo5O8 (M = Ca, Sr, Sn, Pb, La–Gd) compounds (Hibble et al., 1988; Dronskowski & Simon, 1989; Gougeon et al., 1990, 1991, 2003, 2007; Dronskowski et al., 1991; Gall et al., 1993, 1995; Gall & Gougeon, 1994a,b; Gougeon & Gall, 2002) and more later as isolated cluster in the R16Mo21O56 (R = La, Ce, Pr, and Nd) series (Gall & Gougeon, 1993, 1998; Gall et al., 1999). The Mo16O26iO10a cluster is centered on 2b position and thus has point-group symmetry 2/m. The Mo—Mo distances lie between 2.6412 (3) and 2.9030 (5) Å compared to 2.725 Å in the Mo metal and the Mo—O distances between 1.9759 (16) and 2.11407 (18) Å. The Mo—O chains, which have the connectivity formula Mo16O24iO2/2i-iO6aO4/2a-a are separated by the Li+ and Ce3+ cations. The Li+ cation occupies a highly tetragonally distorted octahedral site of O atoms of symmetry 2/m centered at the origin of the unit cell. The Li—O distances in the equatorial plane are 2.4135 (16) Å [Li—O10] and the two trans Li—O7 bonds are 1.861 (3) Å. The coordination numbers of the Ce ions are 6, 9 or 10 with Ce—O distances spreading over a wide range [2.280 (2) to 3.089 (3) Å]. By using the bond-length–bond-strength formula (Brown & Wu, 1976) for the Mo—O, Ce—O and Li—O bonds (s = [d(Mo—O)/1.882]-6, s = [d(Ce—O)/2.160]-6.5 and s = [d(Li—O)/1.378]-4.065), an assignment of oxidation states to the Mo, Ce and Li atoms was made. The valence of each independent Mo atom was determined as follows: Mo(1) +3.36, Mo(2) +2.78, Mo(3) +2.29, Mo(4) + 2.81, and Mo(5) + 1.6. From these values, we could deduce an average Mo oxidation state of + 2.60 which is close to that based on the stoichiometry, + 2.625, when considering all the Ce ions as trivalent and the Li ion monovalent. Bond-valence sums of the Ce—O bonds was +3.08, +3.11, +3.09, and +3.30 for Ce1, Ce2, Ce3, and Ce4, respectively. For the Li atom, a value of +1.00 was found. It is interesting to note that for the total valence sum Σ(Mo—O) + Σ(Ce—O) + Σ(Li—O), we obtained a value of 70.5 per formula unit, which is in very good agreement with the theoretical value of 70 based on the 35 O atoms.