The title compound, tetramolybdenum(VI) diterbate(III), was prepared by pyrolysis of Tb2(H2O)12Mo8O27·6H2O at 1023 K for 2 h in air. The structure consists of trigonal bipyramidal MoO5, tetrahedral MoO4, and monocapped trigonal prismatic TbO7 units. The two MoO5 and two MoO4 units are corner-shared, to form a Mo4O15 group.
Supporting information
Key indicators
- Single-crystal X-ray study
- T = 296 K
- Mean (Mo-O) = 0.004 Å
- R factor = 0.023
- wR factor = 0.060
- Data-to-parameter ratio = 15.7
checkCIF results
No syntax errors found
ADDSYM reports no extra symmetry
Data collection: PROCESS-AUTO (Rigaku, 1998); cell refinement: PROCESS-AUTO; data reduction: TEXSAN (Molecular Structure Corporation, 2000; program(s) used to solve structure: SIR92 (Altomare et al., 1994); program(s) used to refine structure: TEXSAN; software used to prepare material for publication: TEXSAN.
Crystal data top
Mo4O15Tb2 | F(000) = 836 |
Mr = 941.60 | Dx = 4.629 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.7107 Å |
a = 6.8666 (4) Å | Cell parameters from 3943 reflections |
b = 9.6596 (3) Å | θ = 3.7–27.5° |
c = 10.5866 (5) Å | µ = 13.97 mm−1 |
β = 105.827 (2)° | T = 296 K |
V = 675.57 (6) Å3 | Block, colorless |
Z = 2 | 0.10 × 0.10 × 0.05 mm |
Data collection top
Rigaku RAXIS-RAPID Imaging Plate diffractometer | 1454 reflections with F2 > 2.0σ(F2) |
Detector resolution: 10.00 pixels mm-1 | Rint = 0.045 |
ω scans | θmax = 27.5° |
Absorption correction: numerical (Higashi, 1999a,b) | h = 0→8 |
Tmin = 0.284, Tmax = 0.512 | k = 0→12 |
6254 measured reflections | l = −13→13 |
1545 independent reflections | |
Refinement top
Refinement on F2 | w = 1/[σ2(Fo2) + (0.05000(Max(Fo2,0) + 2Fc2)/3)2] |
R[F2 > 2σ(F2)] = 0.023 | (Δ/σ)max = 0.001 |
wR(F2) = 0.060 | Δρmax = 1.82 e Å−3 |
S = 0.90 | Δρmin = −1.97 e Å−3 |
1543 reflections | Extinction correction: Zachariasen(1967) type 2 Gaussian isotropic |
98 parameters | Extinction coefficient: 0.052 (1) |
Special details top
Refinement. Refinement using reflections with F2 > -10.0 σ(F2). The
weighted R-factor (wR) and goodness of fit (S) are based
on F2. R-factor (gt) are based on F. The threshold
expression of F2 > 2.0 σ(F2) is used only for calculating
R-factor (gt). |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Tb | 0.78645 (3) | 0.02347 (2) | 0.72258 (2) | 0.00878 (8) | |
Mo1 | 0.62161 (6) | 0.40522 (4) | 0.65547 (4) | 0.0101 (1) | |
Mo2 | 0.91738 (6) | −0.24357 (4) | 0.48824 (4) | 0.0097 (1) | |
O1 | 0.5000 | 0.5000 | 0.5000 | 0.023 (1) | |
O2 | 0.7563 (5) | −0.3652 (4) | 0.3829 (3) | 0.0165 (8) | |
O3 | 0.6110 (5) | 0.2267 (4) | 0.6456 (3) | 0.0175 (8) | |
O4 | 0.7783 (6) | −0.1534 (4) | 0.5792 (4) | 0.0199 (9) | |
O5 | 0.8769 (5) | 0.4423 (4) | 0.6818 (4) | 0.0192 (8) | |
O6 | 1.0193 (6) | −0.1280 (4) | 0.3965 (4) | 0.0200 (9) | |
O7 | 0.5571 (6) | 0.4720 (4) | 0.7922 (4) | 0.0188 (9) | |
O8 | 1.1158 (6) | −0.3305 (4) | 0.5992 (3) | 0.0208 (9) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Tb | 0.0097 (2) | 0.0078 (2) | 0.0091 (2) | 0.00022 (7) | 0.00296 (9) | 0.00045 (7) |
Mo1 | 0.0090 (2) | 0.0097 (2) | 0.0111 (2) | 0.0008 (1) | 0.0016 (1) | 0.0003 (1) |
Mo2 | 0.0123 (2) | 0.0090 (2) | 0.0083 (2) | −0.0015 (1) | 0.0034 (1) | −0.0001 (1) |
O1 | 0.017 (3) | 0.029 (3) | 0.023 (2) | 0.006 (2) | 0.004 (2) | 0.019 (2) |
O2 | 0.015 (2) | 0.019 (2) | 0.014 (2) | −0.002 (1) | 0.002 (1) | −0.007 (1) |
O3 | 0.015 (2) | 0.010 (1) | 0.024 (2) | 0.004 (1) | 0.000 (1) | 0.000 (1) |
O4 | 0.024 (2) | 0.017 (2) | 0.023 (2) | −0.005 (1) | 0.013 (1) | −0.013 (1) |
O5 | 0.011 (1) | 0.024 (2) | 0.022 (2) | −0.003 (1) | 0.004 (1) | −0.006 (2) |
O6 | 0.020 (2) | 0.019 (2) | 0.025 (2) | 0.001 (1) | 0.013 (1) | 0.007 (1) |
O7 | 0.014 (2) | 0.025 (2) | 0.017 (2) | 0.000 (1) | 0.004 (1) | −0.010 (1) |
O8 | 0.021 (2) | 0.021 (2) | 0.017 (2) | −0.001 (1) | −0.002 (1) | 0.007 (1) |
Geometric parameters (Å, º) top
Tb—O4 | 2.276 (3) | Mo1—O7 | 1.749 (3) |
Tb—O6i | 2.303 (3) | Mo1—O1 | 1.8695 (3) |
Tb—O8ii | 2.304 (3) | Mo1—O2vi | 2.544 (3) |
Tb—O3 | 2.331 (3) | Mo2—O6 | 1.747 (3) |
Tb—O2iii | 2.335 (3) | Mo2—O8 | 1.752 (4) |
Tb—O7iv | 2.374 (4) | Mo2—O4 | 1.760 (3) |
Tb—O5v | 2.389 (3) | Mo2—O2 | 1.782 (3) |
Mo1—O3 | 1.728 (4) | Mo2—O5i | 3.211 (4) |
Mo1—O5 | 1.736 (3) | | |
| | | |
O4—Tb—O6i | 82.9 (1) | O2iii—Tb—O5v | 75.2 (1) |
O4—Tb—O8ii | 162.6 (1) | O7iv—Tb—O5v | 142.1 (1) |
O4—Tb—O3 | 118.9 (1) | O3—Mo1—O5 | 103.9 (2) |
O4—Tb—O2iii | 90.2 (1) | O3—Mo1—O7 | 113.7 (2) |
O4—Tb—O7iv | 87.5 (1) | O3—Mo1—O1 | 115.7 (1) |
O4—Tb—O5v | 83.2 (1) | O3—Mo1—O2vi | 79.3 (1) |
O6i—Tb—O8ii | 95.6 (1) | O5—Mo1—O7 | 105.3 (2) |
O6i—Tb—O3 | 76.2 (1) | O5—Mo1—O1 | 103.3 (1) |
O6i—Tb—O2iii | 149.8 (1) | O5—Mo1—O2vi | 176.8 (2) |
O6i—Tb—O7iv | 140.3 (1) | O7—Mo1—O1 | 113.3 (1) |
O6i—Tb—O5v | 74.8 (1) | O7—Mo1—O2vi | 73.2 (1) |
O8ii—Tb—O3 | 77.2 (1) | O1—Mo1—O2vi | 75.07 (8) |
O8ii—Tb—O2iii | 82.5 (1) | O6—Mo2—O8 | 108.8 (2) |
O8ii—Tb—O7iv | 104.1 (1) | O6—Mo2—O4 | 110.3 (2) |
O8ii—Tb—O5v | 79.8 (1) | O6—Mo2—O2 | 110.4 (2) |
O3—Tb—O2iii | 131.7 (1) | O8—Mo2—O4 | 108.0 (2) |
O3—Tb—O7iv | 75.1 (1) | O8—Mo2—O2 | 109.9 (2) |
O3—Tb—O5v | 140.6 (1) | O4—Mo2—O2 | 109.4 (2) |
O2iii—Tb—O7iv | 68.1 (1) | | |
Symmetry codes: (i) −x+2, −y, −z+1; (ii) −x+2, y+1/2, −z+3/2; (iii) x, −y−1/2, z+1/2; (iv) −x+1, y−1/2, −z+3/2; (v) −x+2, y−1/2, −z+3/2; (vi) −x+1, −y, −z+1. |