Pr16Mo21O56

Gougeon, P.; Gall, P.

doi:10.1107/S1600536811015649

Volume 67
Part 5
Pages i34-i35
May 2011

Received 12 April 2011
Accepted 26 April 2011
Online 29 April 2011

Key indicators
Single-crystal X-ray study
T = 293 K
Mean (Pr-O) = 0.002 Å
R = 0.025
wR = 0.049
Data-to-parameter ratio = 43.5
Details

Pr₁₆Mo₂₁O₅₆

Patrick Gougeon ^a ^* and Philippe Gall ^a

^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 hexadecapraseodymium henicosamolybdenum hexapentacontaoxide, Pr₁₆Mo₂₁O₅₆, is isotypic with other rare earth representatives of formula type RE₁₆Mo₂₁O₅₆ (RE = La, Ce, Nd). It is characterized by Mo₁₀O₁₈ⁱO₈^a units (where i = inner and a = apical O atoms) containing bioctahedral Mo₁₀ clusters and octahedral MoO₆ units that share some of their O atoms to form the Mo-O framework. The two independent Mo₁₀ cluster units are centred at Wyckoff positions 2b and 2c and have point-group symmetry $[\overline{1}]$ . The Mo atom of the MoO₆ unit is likewise situated at an inversion centre (2d). The eight crystallographically different Pr³⁺ cations occupy irregular voids in the framework with coordination numbers to the O atoms varying between 8 and 11.

Related literature

For previous reports on the crystal structures of RE₁₆Mo₂₁O₅₆ compounds, see: Gall & Gougeon (1993) for RE = Ce; Gall & Gougeon (1998) for RE = Nd; Gall et al. (1999) for RE = La. For details of the i- and a-type ligand notation, see: Schäfer & von Schnering (1964).

Experimental

Crystal data

Pr₁₆Mo₂₁O₅₆
M_r = 5165.30
Monoclinic, P 2₁ /c
a = 13.427 (3) Å
b = 13.3935 (16) Å
c = 13.318 (3) Å
= 100.102 (13)°
V = 2357.9 (8) Å³
Z = 2
Mo K radiation
= 21.65 mm^-1
T = 293 K
0.10 × 0.07 × 0.03 mm

Data collection

Nonius KappaCCD diffractometer
Absorption correction: multi-scan (PLATON; Spek, 2009) T_min = 0.060, T_max = 0.216
97514 measured reflections
18339 independent reflections
15545 reflections with I > 2(I)
R_int = 0.040

Refinement

R[F² > 2(F²)] = 0.025
wR(F²) = 0.049
S = 1.13
18339 reflections
422 parameters
_max = 2.19 e Å^-3
_min = -2.34 e Å^-3

Table 1
Selected bond lengths (Å)

Pr1-O28ⁱ	2.320 (2)
Pr1-O22	2.358 (2)
Pr1-O3	2.489 (2)
Pr1-O2	2.497 (2)
Pr1-O6ⁱⁱ	2.599 (2)
Pr1-O10	2.628 (2)
Pr1-O4ⁱⁱ	2.695 (2)
Pr1-O9ⁱⁱ	2.897 (2)
Pr1-O17	3.012 (2)
Pr1-O19	3.212 (2)
Pr2-O13ⁱⁱ	2.313 (2)
Pr2-O26	2.382 (2)
Pr2-O28ⁱ	2.392 (2)
Pr2-O16ⁱⁱⁱ	2.461 (2)
Pr2-O15ⁱⁱⁱ	2.513 (2)
Pr2-O23ⁱⁱⁱ	2.6186 (19)
Pr2-O14	2.675 (2)
Pr2-O19	2.739 (2)
Pr2-O1ⁱⁱ	2.914 (2)
Pr3-O5ⁱⁱ	2.378 (2)
Pr3-O28ⁱ	2.396 (2)
Pr3-O6^iv	2.428 (2)
Pr3-O19ⁱ	2.497 (2)
Pr3-O21ⁱ	2.499 (2)
Pr3-O10	2.835 (2)
Pr3-O1ⁱⁱ	2.836 (2)
Pr3-O8^iv	2.854 (2)
Pr3-O22ⁱ	3.166 (2)
Pr3-O23ⁱⁱⁱ	3.225 (2)
Pr3-O4ⁱⁱ	3.253 (2)
Pr4-O18	2.360 (2)
Pr4-O26ⁱ	2.3740 (19)
Pr4-O13^iv	2.399 (2)
Pr4-O12	2.437 (2)
Pr4-O28ⁱ	2.563 (2)
Pr4-O25ⁱⁱⁱ	2.723 (2)
Pr4-O18^v	2.854 (2)
Pr4-O23ⁱⁱⁱ	3.051 (2)
Pr4-O14	3.235 (2)
Pr4-O17	3.411 (2)
Pr4-O10	3.439 (2)
Pr5-O8ⁱⁱ	2.293 (2)
Pr5-O27^vi	2.293 (2)
Pr5-O20^vii	2.364 (2)
Pr5-O2^vii	2.372 (2)
Pr5-O22^vii	2.572 (2)
Pr5-O5^vii	2.629 (2)
Pr5-O9ⁱⁱ	2.841 (2)
Pr5-O4^vii	3.005 (2)
Pr5-O17^vii	3.128 (2)
Pr6-O25ⁱⁱ	2.226 (2)
Pr6-O11^iv	2.367 (2)
Pr6-O16^viii	2.3794 (19)
Pr6-O12^iv	2.485 (2)
Pr6-O18^viii	2.602 (2)
Pr6-O14^viii	2.752 (2)
Pr6-O27^ix	2.753 (2)
Pr6-O13	2.797 (2)
Pr7-O12	2.331 (2)
Pr7-O26^x	2.352 (2)
Pr7-O15	2.442 (2)
Pr7-O25^xi	2.465 (2)
Pr7-O27ⁱ	2.474 (2)
Pr7-O24^xi	2.598 (2)
Pr7-O18	2.675 (2)
Pr7-O17	2.810 (2)
Pr7-O7	3.128 (2)
Pr8-O27^ix	2.309 (2)
Pr8-O21^vii	2.384 (2)
Pr8-O9ⁱⁱ	2.389 (2)
Pr8-O3	2.442 (2)
Pr8-O7ⁱⁱ	2.509 (2)
Pr8-O20^vii	2.700 (2)
Pr8-O24^vii	2.708 (2)
Pr8-O4ⁱⁱ	3.235 (2)
Pr8-O1	3.360 (2)
Mo1-O1	1.939 (2)
Mo1-O4	2.004 (2)
Mo1-O3	2.009 (2)
Mo1-O2	2.046 (2)
Mo1-O5	2.175 (2)
Mo1-Mo2	2.6435 (5)
Mo1-Mo4	2.7048 (6)
Mo1-Mo5	2.7050 (4)
Mo1-Mo3	2.8049 (7)
Mo2-O7	1.973 (2)
Mo2-O8	1.979 (2)
Mo2-O4	2.008 (2)
Mo2-O6	2.019 (2)
Mo2-O9	2.159 (2)
Mo2-Mo5^iv	2.7076 (5)
Mo2-Mo3	2.7191 (4)
Mo2-Mo4	2.7525 (5)
Mo3-O12	2.032 (2)
Mo3-O2	2.0508 (19)
Mo3-O7	2.077 (2)
Mo3-O10	2.095 (2)
Mo3-O11	2.0981 (19)
Mo3-Mo4^iv	2.6477 (4)
Mo3-Mo5	2.7423 (5)
Mo3-Mo5^iv	2.7819 (6)
Mo4-O13	1.963 (2)
Mo4-O1	2.083 (2)
Mo4-O11^iv	2.088 (2)
Mo4-O6	2.088 (2)
Mo4-O10^iv	2.0982 (19)
Mo4-Mo3^iv	2.6477 (4)
Mo4-Mo5^iv	2.7530 (6)
Mo4-Mo5	2.7756 (4)
Mo5-O8^iv	2.018 (2)
Mo5-O11^iv	2.045 (2)
Mo5-O3	2.0506 (19)
Mo5-O10	2.061 (2)
Mo5-Mo2^iv	2.7076 (5)
Mo5-Mo4^iv	2.7530 (6)
Mo5-Mo3^iv	2.7819 (6)
Mo5-Mo5^iv	2.8260 (6)
Mo6-O14	1.955 (2)
Mo6-O17	1.987 (2)
Mo6-O15	2.016 (2)
Mo6-O16	2.025 (2)
Mo6-O18	2.143 (2)
Mo6-Mo7	2.6087 (6)
Mo6-Mo9	2.7077 (4)
Mo6-Mo10^xii	2.7396 (6)
Mo6-Mo8	2.7987 (5)
Mo7-O17	1.980 (2)
Mo7-O20	1.991 (2)
Mo7-O19	1.991 (2)
Mo7-O21	2.0146 (19)
Mo7-O22	2.133 (2)
Mo7-Mo10	2.7151 (6)
Mo7-Mo9	2.7257 (5)
Mo7-Mo8	2.7514 (4)
Mo8-O25	2.025 (2)
Mo8-O15	2.0509 (19)
Mo8-O20	2.075 (2)
Mo8-O24	2.0843 (19)
Mo8-O23	2.088 (2)
Mo8-Mo9^xii	2.6006 (6)
Mo8-Mo10^xii	2.7556 (5)
Mo8-Mo10	2.7648 (4)
Mo9-O26	1.955 (2)
Mo9-O19	2.064 (2)
Mo9-O14	2.084 (2)
Mo9-O23^xii	2.0935 (19)
Mo9-O24^xii	2.105 (2)
Mo9-Mo8^xii	2.6006 (6)
Mo9-Mo10	2.7168 (5)
Mo9-Mo10^xii	2.7422 (4)
Mo10-O16^xii	2.0182 (19)
Mo10-O21	2.062 (2)
Mo10-O23^xii	2.066 (2)
Mo10-O24	2.086 (2)
Mo10-Mo6^xii	2.7396 (6)
Mo10-Mo9^xii	2.7422 (4)
Mo10-Mo8^xii	2.7556 (5)
Mo10-Mo10^xii	2.8525 (7)
Mo11-O5^vii	2.024 (2)
Mo11-O5	2.024 (2)
Mo11-O9^xiii	2.027 (2)
Mo11-O9ⁱⁱ	2.027 (2)
Mo11-O22	2.048 (2)
Mo11-O22^vii	2.048 (2)
Symmetry codes: (i) $[x, -y+{\script{1\over 2}}, z-{\script{1\over 2}}]$ ; (ii) $[-x+1, y+{\script{1\over 2}}, -z+{\script{1\over 2}}]$ ; (iii) $[-x, y+{\script{1\over 2}}, -z+{\script{1\over 2}}]$ ; (iv) -x+1, -y, -z; (v) -x, -y, -z; (vi) $[-x+1, y-{\script{1\over 2}}, -z+{\script{3\over 2}}]$ ; (vii) -x+1, -y, -z+1; (viii) x+1, y, z; (ix) -x+1, -y+1, -z+1; (x) $[-x, y-{\script{1\over 2}}, -z+{\script{1\over 2}}]$ ; (xi) $[x, -y-{\script{1\over 2}}, z-{\script{1\over 2}}]$ ; (xii) -x, -y, -z+1; (xiii) $[x, -y-{\script{1\over 2}}, z+{\script{1\over 2}}]$ .

Data collection: COLLECT (Nonius, 1998); cell refinement: 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.

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: WM2479 ).

Acknowledgements

Intensity data were collected on the Nonius KappaCCD X-ray diffactometer system of the Centre de diffractométrie de l'Université de Rennes I (www.cdifx.univ-rennes1.fr).

References

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Bergerhoff, G. (1996). DIAMOND. University of Bonn, Germany.
Duisenberg, A. J. M., Kroon-Batenburg, L. M. J. & Schreurs, A. M. M. (2003). J. Appl. Cryst. 36, 220-229.
Gall, P., Gautier, R., Halet, J. F. & Gougeon, P. (1999). Inorg. Chem. 38, 4455-4461.
Gall, P. & Gougeon, P. (1993). Acta Cryst. C49, 659-663.
Gall, P. & Gougeon, P. (1998). Z. Kristallogr. New Cryst. Struct. 213, 1-2.
Nonius (1998). COLLECT. Nonius BV, Delft, The Netherlands.
Schäfer, H. & von Schnering, H. G. (1964). Angew. Chem. 76, 833-845.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Spek, A. L. (2009). Acta Cryst. D65, 148-155.

inorganic compounds