metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890
Volume 65| Part 12| December 2009| Pages m1698-m1699

A new hybrid Dawson-type molybdenum arsenate derivative: (H2bpy)3[As2Mo18O62] (bpy = 4,4′-bi­pyridine)

aCollege of Chemical Engineering, North-East Dianli University, Jilin 132012, People's Republic of China, bThe Academy of Fundamental and Interdisciplinary Sciences, Harbin Institute of Technology, Rm 403, Bldg 2G, 2 Yikuang St, Nangang District, Harbin 150080, People's Republic of China, cJilin Institute of Chemical Technology, Jilin 132012, People's Republic of China, and dCollege of Chemistry and State Key Laboratory of Inorganic Synthesis and Preparative Chemistry, Jilin University, Changchun 130023, People's Republic of China
*Correspondence e-mail: yhhhhyhhy@163.com

(Received 15 September 2009; accepted 23 November 2009; online 28 November 2009)

The title compound, tris­(4,4′-bipyridinium) diarsenoocta­deca­molybdate(VI), (C10H10N2)3[As2Mo18O62], featuring protonated bipyridine mol­ecules and a classical Dawson-type polyoxo-anion, has been synthesized under hydro­thermal conditions. The polyoxoanions are linked together via the bipyridyl cations, acting as hydrogen-bond donors, generating a two-dimensional supra­molecular network. The asymmetric unit contains 1.5 4,4′-bipyridinium (H2bpy) units, with an inversion centre in the central bond of the second H2bpy unit. The site symmetry of the anion is [\overline{1}].

Related literature

For the use of polyoxometalates in the construction of functional materials, see: Haushalter et al. (1989[Haushalter, R. C., Strohmaier, K. G. & Lai, F. W. (1989). Science, 246, 1289-1291.]); Pope & Müller (1991[Pope, M. T. & Müller, A. (1991). Angew. Chem. Int. Ed. Engl. 30, 34-38.]). For A/Mo/P/O compounds where A is an organic or inorganic cation, see: Rao et al. (2001[Rao, C. N. R., Natarahab, S., Houdhury, A. C., Neeraj, S. & Ayi, A. A. (2001). Acc. Chem. Res. 34, 80-???.]); Cheetham et al. (1999[Cheetham, A. K., Ferey, G. & Loiseau, T. (1999). Angew. Chem. Int. Ed. 38, 3268-3290.]); Thomas & Raja (2001[Thomas, J. M. & Raja, R. (2001). Aust. J. Chem. 54, 551-555.]); Xiao et al. (1999[Xiao, F. S., Qiu, S., Pang, W. & Xu, R. (1999). Adv. Mater. 11, 1091-1095.]). For Dawson-type polyoxometalates, see: Wang et al. (2004[Wang, J. P., Zhao, J. W. & Niu, J. Y. (2004). J. Mol. Struct. 697, 191-198.]).

[Scheme 1]

Experimental

Crystal data
  • (C10H10N2)3[As2Mo18O62]

  • Mr = 3343.36

  • Triclinic, [P \overline 1]

  • a = 11.2671 (17) Å

  • b = 12.1365 (19) Å

  • c = 13.871 (2) Å

  • α = 108.023 (2)°

  • β = 94.243 (2)°

  • γ = 107.166 (2)°

  • V = 1694.6 (4) Å3

  • Z = 1

  • Mo Kα radiation

  • μ = 4.30 mm−1

  • T = 293 K

  • 0.29 × 0.22 × 0.20 mm

Data collection
  • Rigaku R-AXIS RAPID diffractometer

  • Absorption correction: multi-scan (ABSCOR; Higashi, 1995[Higashi, T. (1995). ABSCOR. Rigaku Corporation, Tokyo, Japan.]) Tmin = 0.504, Tmax = 0.625

  • 14379 measured reflections

  • 6545 independent reflections

  • 4986 reflections with I > 2σ(I)

  • Rint = 0.042

Refinement
  • R[F2 > 2σ(F2)] = 0.047

  • wR(F2) = 0.128

  • S = 1.06

  • 6545 reflections

  • 532 parameters

  • H-atom parameters constrained

  • Δρmax = 3.42 e Å−3

  • Δρmin = −1.79 e Å−3

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A DA D—H⋯A
N1—H1A⋯O14 0.86 1.99 2.851 (10) 174
N2—H2B⋯O29i 0.86 2.32 2.805 (12) 116
N3—H3B⋯O10ii 0.86 2.56 3.291 (9) 143
N3—H3B⋯O7ii 0.86 2.60 3.336 (10) 145
Symmetry codes: (i) x-1, y+1, z; (ii) x-1, y, z.

Data collection: RAPID-AUTO (Rigaku, 1998[Rigaku (1998). PROCESS-AUTO. Rigaku Corporation, Tokyo, Japan.]); cell refinement: RAPID-AUTO; data reduction: RAPID-AUTO; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: ORTEP-3 (Burnett & Johnson, 1996[Burnett, M. N. & Johnson, C. K. (1996). ORTEPIII. Report ORNL-6895. Oak Ridge National Laboratory, Tennessee, USA.]); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]).

Supporting information


Comment top

POMs (polyoxometalates), as a class of metal oxide clusters, possess an enormous structural variety and interesting electronic properties. They have therefore been extensively employed in the construction of functional materials (Haushalter et al., 1989; Pope & Müller, 1991). The A/Mo/P/O system as an important part of this family of compounds has been synthesized and structurally characterized, where A is an organic or inorganic cation. In contrast to the rich structural chemistry of molybdenum phosphates, the Mo/As/O system remains relatively scarcely developed.(Rao et al., 2001; Cheetham et al., 1999; Xiao et al., 1999; Thomas & Raja 2001.) On the basis of these facts, we have hydrothermally synthesized and characterised a new arsenate compound (H2bpy)3[As2Mo18O62], which is described here.

The structure of compound consists of a discrete polyoxoanion [As2Mo18O62]6- and three bipyridine molecules (Fig 1). The centrosymmetric polyoxoanion is classical α-Dawson isomer [α-As2Mo18O62]6-. The parent anion [α-As2Mo18O62]6-consisting of two central AsO4 tetrahedra which are surrounded by six vertex-sharing Mo3O13 trimers, also may be described as two [α-AsMo9O31]3- units, generated from the well known [α-AsMo12O40]3- by removal of a set of three corner-sharing MoO6 octahedra and fused into a clusterof virtual D3h symmetry. In the Dawson type POM, there are two structurally distinct types of Mo atoms: six 'cap' atoms on vertical mirror-planes and grouped in two sets of three, and twelve equatorial Mo atoms are grouped in two sets of six, but do not lie on mirror-planes (Wang et al., 2004).

The unusual feature of the title compound is that it exhibits a 2-D supramolecular layer-like structure formed by the discrete Dawson-type anions and 4,4'-bpy molecules via multi-point N—H···O hydrogen-bonding interactions (Fig. 2). As a fundamental building unit, each of the polyoxoanion [As2Mo18O62]6- acting as a hexa-dentate ligand furnishes four two-bridging and two terminal oxygen atoms to connect to six adjacent 4,4'-bipy molecules via N—H···O hydrogen-bonding interactions. In particular, oxygen atoms (O14, O26i, O29 and O12i; symmetry code: (i) x - 1, 1 + y, z) connect adjacent four 4,4'-bipy molecules to form a 1-D "double-bridge" chain (chain A), respectively. The oxygen atoms (O7, O10, O7i and O10i) link two 4,4'-bpy molecules to construct an undulated chain (chain B). The chains A and B further link each other to forma novel 2-D layer-like structure with 1-D rhombic channel.

Related literature top

For the use of polyoxometalates in the construction of functional materials, see: Haushalter et al. (1989); Pope & Müller (1991). For A/Mo/P/O componds where A is an organic or inorganic cation, see: Rao et al. (2001); Cheetham et al. (1999); Thomas & Raja (2001); Xiao et al. (1999). For Dawson-type polyoxometalates, see: Wang et al. (2004).

Experimental top

The title compound was hydrothermally synthesized under autogenous pressure. A mixture of FeCl3.6H2O (0.41 g, 2.5 mmol), As2O3(0.5 g, 2.5 mmol), MoO3.2H2O(0.9 g, 5 mmol), 4,4'-bipy.2H2O (0.32 g, 1.7 mmol) and 18 ml water was stirred for 30 min in air; it was adjusted to pH=5–6 with 2M KOH, and was heated in a 25 ml stainless steel reactor with a Teflon-liner at180°C for 8 days, and then cooled to room temperature. The resulting product consisting of brown block-shaped crystals was isolated by filtration, washed with distilled water, and dried at ambient temperature (75% yield based on Mo). Elemental analysis for 1: Anal. Calcd: C, 10.77; H, 0.8970; N, 2.52; found: C, 10.96; H, 0.923; N, 2.50. F T-IRdate: (KBr pellet, ν/cm-1): 3096(w),3069(w), 1621(m),1596(m), 1546(m), 1488(m), 1418(w), 1349(w), 1204(w), 950 (m), 930 (m), 888(s), 842 (s), 776(s), 724 (s).

Refinement top

All H atoms were placed at calculated positions (H—C = 0.93 Å), with Uiso(H) = 1.2 Ueq(C) and (H—N = 0.86 Å), with Uiso(H) =1.2Ueq(N).

Computing details top

Data collection: RAPID-AUTO (Rigaku, 1998); cell refinement: RAPID-AUTO (Rigaku, 1998); data reduction: RAPID-AUTO (Rigaku, 1998); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXTL (Sheldrick, 2008); molecular graphics: ORTEP-3 (Burnett & Johnson, 1996); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. A view ofthe molecule of (I) with displacement ellipsoids drawn at the 30% probability level. H atoms have been omitted. Second half of the anion generated by (i) 2–x, 1–y, 1–z. Second half of the second, centrosymmetric cation generated by (ii) 1–x, 1–y, –z.
[Figure 2] Fig. 2. A polyhedral representation of the supramolecular layerconstructed by "double-bridge" chain A and chain B. Symmetry codes (i) 2 – x, 1 – y, 1 – z; (ii) x – 1, y + 1, z; (iv) 1 – x, 1 – y, 1 – z.
Tris(4,4'-bipyridinium) diarsenooctadecamolybdate top
Crystal data top
(C10H10N2)3[As2Mo18O62]Z = 1
Mr = 3343.36F(000) = 1569
Triclinic, P1Dx = 3.276 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 11.2671 (17) ÅCell parameters from 4839 reflections
b = 12.1365 (19) Åθ = 3.2–26.6°
c = 13.871 (2) ŵ = 4.30 mm1
α = 108.023 (2)°T = 293 K
β = 94.243 (2)°Block, brown
γ = 107.166 (2)°0.29 × 0.22 × 0.20 mm
V = 1694.6 (4) Å3
Data collection top
Rigaku R-AXIS RAPID
diffractometer
6545 independent reflections
Radiation source: fine-focus sealed tube4986 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.042
Detector resolution: 10 pixels mm-1θmax = 26.1°, θmin = 2.2°
ω scansh = 1313
Absorption correction: multi-scan
(ABSCOR; Higashi, 1995)
k = 1514
Tmin = 0.504, Tmax = 0.625l = 1717
14379 measured reflections
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)] = 0.047Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.128H-atom parameters constrained
S = 1.06 w = 1/[σ2(Fo2) + (0.0669P)2]
where P = (Fo2 + 2Fc2)/3
6545 reflections(Δ/σ)max = 0.001
532 parametersΔρmax = 3.42 e Å3
0 restraintsΔρmin = 1.79 e Å3
Crystal data top
(C10H10N2)3[As2Mo18O62]γ = 107.166 (2)°
Mr = 3343.36V = 1694.6 (4) Å3
Triclinic, P1Z = 1
a = 11.2671 (17) ÅMo Kα radiation
b = 12.1365 (19) ŵ = 4.30 mm1
c = 13.871 (2) ÅT = 293 K
α = 108.023 (2)°0.29 × 0.22 × 0.20 mm
β = 94.243 (2)°
Data collection top
Rigaku R-AXIS RAPID
diffractometer
6545 independent reflections
Absorption correction: multi-scan
(ABSCOR; Higashi, 1995)
4986 reflections with I > 2σ(I)
Tmin = 0.504, Tmax = 0.625Rint = 0.042
14379 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0470 restraints
wR(F2) = 0.128H-atom parameters constrained
S = 1.06Δρmax = 3.42 e Å3
6545 reflectionsΔρmin = 1.79 e Å3
532 parameters
Special details top

Experimental. (See detailed section in the paper)

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. 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*/Ueq
As10.92601 (6)0.39285 (6)0.35346 (5)0.01514 (17)
Mo10.92713 (7)0.13757 (7)0.42221 (6)0.0338 (2)
Mo21.20090 (6)0.30431 (6)0.35916 (5)0.02772 (18)
Mo30.89323 (7)0.36087 (6)0.08380 (5)0.02746 (18)
Mo40.93667 (7)0.65754 (7)0.29565 (6)0.0334 (2)
Mo50.64553 (6)0.19759 (6)0.16132 (5)0.02573 (17)
Mo60.65550 (6)0.48482 (6)0.36298 (5)0.02779 (18)
Mo70.66101 (7)0.24692 (7)0.44528 (6)0.0339 (2)
Mo81.18997 (7)0.55435 (7)0.27224 (6)0.0338 (2)
Mo90.91060 (6)0.11763 (6)0.14911 (5)0.02525 (17)
O10.8708 (5)0.0839 (5)0.2713 (4)0.0242 (11)
O20.8653 (4)0.3000 (4)0.2292 (3)0.0188 (10)
O30.8780 (5)0.5139 (4)0.1693 (4)0.0253 (12)
O40.6376 (5)0.3687 (5)0.2392 (4)0.0253 (12)
O51.0703 (5)0.4379 (4)0.1562 (4)0.0251 (12)
O60.6331 (5)0.1776 (5)0.2873 (4)0.0254 (11)
O70.9234 (5)0.2055 (4)0.0511 (4)0.0245 (11)
O81.2798 (5)0.3941 (5)0.4871 (4)0.0421 (16)
O91.3038 (5)0.2367 (5)0.3112 (4)0.0348 (14)
O101.0727 (5)0.1992 (5)0.2114 (4)0.0292 (12)
O110.7206 (5)0.0832 (5)0.1100 (4)0.0262 (12)
O120.7180 (5)0.2819 (5)0.0661 (4)0.0262 (12)
O130.7181 (5)0.3320 (6)0.5857 (4)0.0394 (15)
O140.9134 (6)0.7594 (5)0.2412 (4)0.0340 (14)
O150.9939 (6)0.2245 (5)0.5659 (4)0.0352 (14)
O160.5297 (5)0.1427 (5)0.4500 (4)0.0380 (15)
O170.4954 (5)0.1292 (5)0.0943 (4)0.0364 (14)
O180.9085 (5)0.0231 (5)0.0725 (4)0.0310 (13)
O190.9045 (5)0.3812 (5)0.0306 (4)0.0335 (13)
O200.8980 (6)0.0045 (5)0.4235 (4)0.0395 (15)
O211.3061 (5)0.6043 (5)0.2118 (4)0.0394 (15)
O220.5319 (5)0.5286 (6)0.3467 (4)0.0428 (16)
O231.0144 (6)0.3297 (6)0.4072 (5)0.0480 (16)
O240.8062 (6)0.4072 (6)0.4183 (5)0.0489 (17)
O250.7783 (7)0.1653 (9)0.4418 (5)0.079 (3)
O261.0145 (6)0.5316 (6)0.3549 (5)0.0506 (17)
O271.2249 (8)0.4323 (5)0.3085 (6)0.077 (3)
O281.1036 (7)0.6686 (7)0.2723 (6)0.073 (3)
O291.0918 (6)0.1676 (8)0.3915 (5)0.071 (3)
O300.5883 (10)0.3638 (6)0.4230 (5)0.078 (3)
O310.7859 (7)0.6060 (6)0.3357 (6)0.073 (3)
C10.6467 (10)0.8466 (8)0.1693 (8)0.047 (2)
H1B0.69240.84740.11630.056*
C20.6260 (9)0.8143 (9)0.3263 (8)0.047 (2)
H2A0.65610.79140.37870.056*
C30.5380 (9)0.8722 (7)0.1670 (7)0.038 (2)
H3A0.50850.89040.11140.046*
C40.5159 (9)0.8432 (9)0.3276 (7)0.046 (2)
H4A0.47340.84340.38260.056*
C50.1959 (12)0.9608 (10)0.3356 (10)0.061 (3)
H5A0.16030.97530.39470.074*
C60.2963 (11)0.9183 (10)0.1629 (7)0.059 (3)
H6A0.32860.90360.10210.071*
C70.1878 (11)0.9533 (10)0.1679 (8)0.063 (3)
H7A0.14840.96320.11130.075*
C80.3549 (8)0.9057 (7)0.2474 (7)0.037 (2)
C90.4693 (8)0.8718 (7)0.2464 (6)0.034 (2)
C100.3004 (10)0.9289 (9)0.3353 (8)0.048 (2)
H10A0.33700.92220.39460.058*
C110.4424 (8)0.4594 (8)0.0113 (6)0.0334 (19)
C120.4500 (10)0.3954 (11)0.0767 (9)0.058 (3)
H12A0.52920.40270.10800.070*
C130.3450 (11)0.3218 (10)0.0970 (9)0.058 (3)
H13A0.35280.27790.14010.070*
C140.2188 (8)0.3792 (10)0.0083 (7)0.045 (2)
H14A0.13910.37580.03500.054*
C150.3229 (9)0.4474 (9)0.0299 (7)0.043 (2)
H15A0.31390.48860.07500.052*
N10.6874 (8)0.8199 (7)0.2501 (7)0.055 (2)
H1A0.75770.80560.25200.066*
N20.1441 (8)0.9716 (7)0.2529 (8)0.058 (2)
H2B0.07720.99190.25530.069*
N30.2332 (8)0.3133 (7)0.0553 (6)0.049 (2)
H3B0.16710.26600.06740.059*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
As10.0152 (4)0.0145 (4)0.0146 (4)0.0032 (3)0.0002 (3)0.0058 (3)
Mo10.0392 (4)0.0272 (4)0.0504 (5)0.0167 (3)0.0194 (4)0.0265 (4)
Mo20.0216 (4)0.0246 (4)0.0324 (4)0.0105 (3)0.0006 (3)0.0024 (3)
Mo30.0343 (4)0.0240 (4)0.0177 (3)0.0009 (3)0.0001 (3)0.0100 (3)
Mo40.0420 (4)0.0319 (4)0.0445 (5)0.0213 (3)0.0178 (4)0.0275 (4)
Mo50.0186 (3)0.0259 (4)0.0233 (4)0.0030 (3)0.0013 (3)0.0012 (3)
Mo60.0231 (4)0.0267 (4)0.0315 (4)0.0119 (3)0.0024 (3)0.0057 (3)
Mo70.0224 (4)0.0394 (4)0.0444 (5)0.0028 (3)0.0076 (3)0.0277 (4)
Mo80.0262 (4)0.0404 (4)0.0415 (5)0.0063 (3)0.0129 (3)0.0263 (4)
Mo90.0255 (4)0.0198 (3)0.0254 (4)0.0084 (3)0.0012 (3)0.0016 (3)
O10.024 (3)0.026 (3)0.020 (3)0.007 (2)0.001 (2)0.007 (2)
O20.026 (3)0.017 (2)0.011 (2)0.006 (2)0.000 (2)0.0031 (19)
O30.030 (3)0.022 (3)0.022 (3)0.008 (2)0.003 (2)0.007 (2)
O40.028 (3)0.027 (3)0.019 (3)0.009 (2)0.002 (2)0.007 (2)
O50.027 (3)0.023 (3)0.022 (3)0.009 (2)0.003 (2)0.004 (2)
O60.027 (3)0.025 (3)0.022 (3)0.009 (2)0.002 (2)0.006 (2)
O70.032 (3)0.020 (3)0.019 (3)0.006 (2)0.006 (2)0.007 (2)
O80.030 (3)0.045 (4)0.036 (3)0.019 (3)0.008 (3)0.009 (3)
O90.026 (3)0.038 (3)0.034 (3)0.014 (3)0.001 (2)0.001 (3)
O100.028 (3)0.033 (3)0.025 (3)0.011 (2)0.005 (2)0.007 (2)
O110.029 (3)0.025 (3)0.020 (3)0.003 (2)0.002 (2)0.008 (2)
O120.029 (3)0.026 (3)0.019 (3)0.004 (2)0.003 (2)0.009 (2)
O130.032 (3)0.049 (4)0.021 (3)0.007 (3)0.001 (2)0.011 (3)
O140.050 (4)0.020 (3)0.031 (3)0.009 (3)0.003 (3)0.014 (2)
O150.066 (4)0.024 (3)0.022 (3)0.023 (3)0.004 (3)0.010 (2)
O160.036 (3)0.038 (3)0.027 (3)0.006 (3)0.011 (3)0.009 (3)
O170.027 (3)0.041 (3)0.033 (3)0.009 (3)0.001 (3)0.006 (3)
O180.036 (3)0.022 (3)0.028 (3)0.007 (2)0.006 (2)0.002 (2)
O190.038 (3)0.034 (3)0.019 (3)0.000 (3)0.003 (2)0.010 (2)
O200.055 (4)0.018 (3)0.037 (3)0.007 (3)0.013 (3)0.009 (3)
O210.028 (3)0.048 (4)0.024 (3)0.008 (3)0.006 (2)0.007 (3)
O220.028 (3)0.055 (4)0.040 (4)0.024 (3)0.008 (3)0.004 (3)
O230.043 (4)0.050 (4)0.051 (4)0.014 (3)0.009 (3)0.020 (3)
O240.043 (4)0.046 (4)0.051 (4)0.015 (3)0.001 (3)0.011 (3)
O250.082 (6)0.169 (9)0.035 (4)0.104 (6)0.023 (4)0.042 (5)
O260.051 (4)0.048 (4)0.053 (4)0.015 (3)0.004 (3)0.018 (3)
O270.096 (6)0.021 (3)0.085 (6)0.003 (4)0.060 (5)0.020 (4)
O280.050 (4)0.066 (5)0.068 (5)0.031 (4)0.023 (4)0.029 (4)
O290.034 (4)0.110 (7)0.032 (4)0.020 (4)0.001 (3)0.016 (4)
O300.168 (9)0.038 (4)0.032 (4)0.039 (5)0.019 (5)0.012 (3)
O310.068 (5)0.033 (4)0.080 (5)0.018 (3)0.050 (4)0.007 (4)
C10.050 (6)0.035 (5)0.052 (6)0.013 (5)0.017 (5)0.010 (5)
C20.045 (6)0.052 (6)0.047 (6)0.014 (5)0.001 (5)0.028 (5)
C30.049 (6)0.028 (4)0.034 (5)0.011 (4)0.010 (4)0.008 (4)
C40.036 (5)0.063 (7)0.036 (5)0.005 (5)0.001 (4)0.025 (5)
C50.076 (8)0.051 (7)0.080 (9)0.032 (6)0.045 (7)0.037 (6)
C60.073 (8)0.062 (7)0.029 (5)0.028 (6)0.008 (5)0.005 (5)
C70.076 (8)0.067 (8)0.039 (6)0.046 (7)0.018 (6)0.004 (5)
C80.029 (5)0.026 (4)0.041 (5)0.003 (4)0.006 (4)0.007 (4)
C90.037 (5)0.022 (4)0.035 (5)0.005 (4)0.004 (4)0.014 (4)
C100.050 (6)0.049 (6)0.056 (6)0.013 (5)0.016 (5)0.035 (5)
C110.040 (5)0.042 (5)0.020 (4)0.021 (4)0.000 (4)0.006 (4)
C120.042 (6)0.085 (8)0.070 (7)0.030 (6)0.011 (5)0.050 (7)
C130.063 (7)0.073 (8)0.078 (8)0.047 (6)0.030 (6)0.054 (7)
C140.031 (5)0.077 (7)0.033 (5)0.028 (5)0.009 (4)0.016 (5)
C150.042 (5)0.071 (7)0.032 (5)0.034 (5)0.013 (4)0.023 (5)
N10.038 (5)0.031 (4)0.081 (7)0.011 (4)0.004 (5)0.002 (4)
N20.046 (5)0.031 (5)0.080 (7)0.012 (4)0.001 (5)0.002 (5)
N30.046 (5)0.049 (5)0.054 (5)0.017 (4)0.029 (4)0.016 (4)
Geometric parameters (Å, º) top
As1—O261.678 (7)Mo8—O211.671 (5)
As1—O231.682 (7)Mo8—O271.837 (6)
As1—O21.696 (4)Mo8—O51.885 (5)
As1—O241.698 (7)Mo8—O281.915 (7)
Mo1—O201.664 (5)Mo8—O13i2.007 (5)
Mo1—O251.829 (6)Mo8—O262.347 (7)
Mo1—O291.889 (7)Mo9—O181.701 (5)
Mo1—O151.913 (5)Mo9—O101.798 (5)
Mo1—O11.981 (5)Mo9—O11.917 (5)
Mo1—O232.329 (7)Mo9—O71.960 (5)
Mo2—O91.673 (5)Mo9—O112.052 (5)
Mo2—O81.768 (5)Mo9—O22.371 (5)
Mo2—O271.854 (6)O8—Mo6i2.066 (5)
Mo2—O291.950 (7)O13—Mo8i2.007 (5)
Mo2—O102.185 (5)O15—Mo4i1.941 (5)
Mo2—O232.327 (6)C1—N11.345 (13)
Mo3—O191.687 (5)C1—C31.350 (13)
Mo3—O121.882 (5)C1—H1B0.9300
Mo3—O31.934 (5)C2—N11.313 (13)
Mo3—O71.936 (5)C2—C41.385 (14)
Mo3—O51.971 (5)C2—H2A0.9300
Mo3—O22.365 (5)C3—C91.393 (12)
Mo3—Mo53.3719 (10)C3—H3A0.9300
Mo3—Mo93.3976 (10)C4—C91.387 (12)
Mo4—O141.705 (5)C4—H4A0.9300
Mo4—O311.820 (6)C5—N21.307 (14)
Mo4—O281.905 (8)C5—C101.344 (15)
Mo4—O15i1.941 (5)C5—H5A0.9300
Mo4—O31.951 (5)C6—C81.375 (13)
Mo4—O262.290 (7)C6—C71.408 (15)
Mo4—Mo83.4372 (11)C6—H6A0.9300
Mo5—O171.695 (5)C7—N21.293 (14)
Mo5—O111.823 (5)C7—H7A0.9300
Mo5—O61.847 (5)C8—C101.393 (13)
Mo5—O121.991 (5)C8—C91.465 (13)
Mo5—O42.055 (5)C10—H10A0.9300
Mo5—O22.383 (5)C11—C151.371 (12)
Mo5—Mo93.4021 (10)C11—C121.377 (13)
Mo6—O221.655 (5)C11—C11ii1.501 (17)
Mo6—O41.805 (5)C12—C131.363 (14)
Mo6—O311.901 (6)C12—H12A0.9300
Mo6—O301.902 (7)C13—N31.308 (12)
Mo6—O8i2.066 (5)C13—H13A0.9300
Mo6—O242.358 (7)C14—C151.335 (13)
Mo6—Mo73.4319 (11)C14—N31.391 (12)
Mo7—O161.659 (5)C14—H14A0.9300
Mo7—O131.858 (5)C15—H15A0.9300
Mo7—O251.866 (6)N1—H1A0.8600
Mo7—O301.923 (8)N2—H2B0.8600
Mo7—O62.051 (5)N3—H3B0.8600
Mo7—O242.294 (7)
O26—As1—O23110.6 (3)O25—Mo7—O2490.9 (3)
O26—As1—O2108.6 (3)O30—Mo7—O2467.5 (3)
O23—As1—O2108.6 (3)O6—Mo7—O2481.1 (2)
O26—As1—O24109.5 (3)O16—Mo7—Mo6122.1 (2)
O23—As1—O24110.1 (3)O13—Mo7—Mo6100.1 (2)
O2—As1—O24109.4 (3)O25—Mo7—Mo6131.3 (3)
O20—Mo1—O25103.2 (4)O30—Mo7—Mo626.0 (3)
O20—Mo1—O2999.3 (4)O6—Mo7—Mo673.78 (14)
O25—Mo1—O29157.2 (4)O24—Mo7—Mo643.18 (16)
O20—Mo1—O1598.0 (2)O21—Mo8—O27105.2 (4)
O25—Mo1—O1589.7 (3)O21—Mo8—O598.7 (2)
O29—Mo1—O1591.0 (3)O27—Mo8—O591.5 (2)
O20—Mo1—O194.4 (2)O21—Mo8—O2898.9 (4)
O25—Mo1—O189.3 (2)O27—Mo8—O28155.5 (4)
O29—Mo1—O185.1 (2)O5—Mo8—O2888.8 (2)
O15—Mo1—O1167.5 (2)O21—Mo8—O13i95.4 (2)
O20—Mo1—O23165.5 (3)O27—Mo8—O13i86.3 (3)
O25—Mo1—O2391.1 (4)O5—Mo8—O13i165.8 (2)
O29—Mo1—O2366.2 (3)O28—Mo8—O13i87.4 (3)
O15—Mo1—O2384.1 (2)O21—Mo8—O26164.4 (3)
O1—Mo1—O2383.4 (2)O27—Mo8—O2690.2 (4)
O9—Mo2—O8102.4 (3)O5—Mo8—O2683.3 (2)
O9—Mo2—O27103.9 (4)O28—Mo8—O2665.5 (3)
O8—Mo2—O2797.3 (3)O13i—Mo8—O2682.7 (2)
O9—Mo2—O2997.4 (3)O21—Mo8—Mo4123.5 (2)
O8—Mo2—O2996.4 (3)O27—Mo8—Mo4131.2 (3)
O27—Mo2—O29151.5 (3)O5—Mo8—Mo478.21 (15)
O9—Mo2—O1087.7 (2)O28—Mo8—Mo425.8 (3)
O8—Mo2—O10169.5 (2)O13i—Mo8—Mo492.66 (19)
O27—Mo2—O1082.8 (2)O26—Mo8—Mo441.54 (16)
O29—Mo2—O1079.3 (2)O18—Mo9—O10105.1 (2)
O9—Mo2—O23160.7 (3)O18—Mo9—O1100.4 (2)
O8—Mo2—O2388.9 (2)O10—Mo9—O190.3 (2)
O27—Mo2—O2389.9 (3)O18—Mo9—O7101.4 (2)
O29—Mo2—O2365.5 (3)O10—Mo9—O792.7 (2)
O10—Mo2—O2380.6 (2)O1—Mo9—O7156.3 (2)
O19—Mo3—O12100.9 (2)O18—Mo9—O1195.5 (2)
O19—Mo3—O3102.6 (2)O10—Mo9—O11159.4 (2)
O12—Mo3—O390.6 (2)O1—Mo9—O1185.6 (2)
O19—Mo3—O798.9 (2)O7—Mo9—O1183.3 (2)
O12—Mo3—O791.5 (2)O18—Mo9—O2165.9 (2)
O3—Mo3—O7157.6 (2)O10—Mo9—O288.3 (2)
O19—Mo3—O5101.8 (2)O1—Mo9—O283.47 (19)
O12—Mo3—O5157.3 (2)O7—Mo9—O273.19 (18)
O3—Mo3—O583.1 (2)O11—Mo9—O271.19 (18)
O7—Mo3—O586.5 (2)O18—Mo9—Mo3129.50 (19)
O19—Mo3—O2171.3 (2)O10—Mo9—Mo391.20 (17)
O12—Mo3—O275.12 (19)O1—Mo9—Mo3127.42 (15)
O3—Mo3—O285.29 (19)O7—Mo9—Mo329.11 (14)
O7—Mo3—O273.75 (18)O11—Mo9—Mo375.51 (14)
O5—Mo3—O282.58 (19)O2—Mo9—Mo344.08 (11)
O19—Mo3—Mo5130.11 (18)O18—Mo9—Mo5122.26 (18)
O12—Mo3—Mo530.39 (15)O10—Mo9—Mo5132.63 (17)
O3—Mo3—Mo591.13 (16)O1—Mo9—Mo582.16 (15)
O7—Mo3—Mo579.64 (15)O7—Mo9—Mo578.56 (15)
O5—Mo3—Mo5127.55 (15)O11—Mo9—Mo526.80 (14)
O2—Mo3—Mo544.97 (11)O2—Mo9—Mo544.45 (11)
O19—Mo3—Mo9128.2 (2)Mo3—Mo9—Mo559.46 (2)
O12—Mo3—Mo983.42 (16)Mo9—O1—Mo1144.0 (3)
O3—Mo3—Mo9129.06 (15)As1—O2—Mo3125.2 (2)
O7—Mo3—Mo929.52 (14)As1—O2—Mo9123.6 (2)
O5—Mo3—Mo983.73 (15)Mo3—O2—Mo991.69 (16)
O2—Mo3—Mo944.24 (11)As1—O2—Mo5124.5 (2)
Mo5—Mo3—Mo960.34 (2)Mo3—O2—Mo590.51 (16)
O14—Mo4—O31101.5 (4)Mo9—O2—Mo591.38 (16)
O14—Mo4—O2898.9 (3)Mo3—O3—Mo4149.4 (3)
O31—Mo4—O28159.5 (4)Mo6—O4—Mo5146.6 (3)
O14—Mo4—O15i96.6 (2)Mo8—O5—Mo3148.9 (3)
O31—Mo4—O15i89.3 (3)Mo5—O6—Mo7151.5 (3)
O28—Mo4—O15i89.5 (3)Mo3—O7—Mo9121.4 (2)
O14—Mo4—O396.2 (2)Mo2—O8—Mo6i168.5 (3)
O31—Mo4—O389.8 (3)Mo9—O10—Mo2145.1 (3)
O28—Mo4—O386.7 (2)Mo5—O11—Mo9122.7 (3)
O15i—Mo4—O3167.1 (2)Mo3—O12—Mo5121.0 (3)
O14—Mo4—O26165.8 (3)Mo7—O13—Mo8i167.9 (3)
O31—Mo4—O2692.6 (3)Mo1—O15—Mo4i168.2 (3)
O28—Mo4—O2666.9 (3)As1—O23—Mo2125.0 (3)
O15i—Mo4—O2684.4 (2)As1—O23—Mo1121.6 (3)
O3—Mo4—O2682.7 (2)Mo2—O23—Mo197.1 (2)
O14—Mo4—Mo8123.2 (2)As1—O24—Mo7124.1 (3)
O31—Mo4—Mo8134.0 (3)As1—O24—Mo6120.7 (3)
O28—Mo4—Mo825.9 (3)Mo7—O24—Mo695.1 (2)
O15i—Mo4—Mo895.15 (18)Mo1—O25—Mo7156.5 (6)
O3—Mo4—Mo876.28 (15)As1—O26—Mo4124.0 (3)
O26—Mo4—Mo842.80 (17)As1—O26—Mo8121.0 (3)
O17—Mo5—O11103.4 (2)Mo4—O26—Mo895.7 (2)
O17—Mo5—O6103.9 (3)Mo8—O27—Mo2158.2 (6)
O11—Mo5—O697.6 (2)Mo4—O28—Mo8128.3 (5)
O17—Mo5—O1297.6 (2)Mo1—O29—Mo2130.8 (5)
O11—Mo5—O1288.9 (2)Mo6—O30—Mo7127.6 (5)
O6—Mo5—O12155.4 (2)Mo4—O31—Mo6151.9 (5)
O17—Mo5—O499.2 (2)N1—C1—C3118.5 (9)
O11—Mo5—O4156.5 (2)N1—C1—H1B120.7
O6—Mo5—O483.1 (2)C3—C1—H1B120.7
O12—Mo5—O481.8 (2)N1—C2—C4119.1 (9)
O17—Mo5—O2170.2 (2)N1—C2—H2A120.4
O11—Mo5—O274.61 (19)C4—C2—H2A120.4
O6—Mo5—O285.92 (19)C1—C3—C9121.1 (9)
O12—Mo5—O272.86 (18)C1—C3—H3A119.4
O4—Mo5—O282.01 (18)C9—C3—H3A119.4
O17—Mo5—Mo3125.8 (2)C2—C4—C9119.7 (9)
O11—Mo5—Mo378.62 (16)C2—C4—H4A120.2
O6—Mo5—Mo3129.90 (16)C9—C4—H4A120.2
O12—Mo5—Mo328.57 (14)N2—C5—C10120.1 (10)
O4—Mo5—Mo382.99 (14)N2—C5—H5A119.9
O2—Mo5—Mo344.53 (11)C10—C5—H5A119.9
O17—Mo5—Mo9133.62 (19)C8—C6—C7120.3 (10)
O11—Mo5—Mo930.51 (15)C8—C6—H6A119.8
O6—Mo5—Mo991.66 (16)C7—C6—H6A119.8
O12—Mo5—Mo981.85 (15)N2—C7—C6118.5 (10)
O4—Mo5—Mo9126.19 (14)N2—C7—H7A120.7
O2—Mo5—Mo944.17 (11)C6—C7—H7A120.7
Mo3—Mo5—Mo960.21 (2)C6—C8—C10116.3 (9)
O22—Mo6—O4102.1 (3)C6—C8—C9122.2 (9)
O22—Mo6—O31102.1 (4)C10—C8—C9121.5 (8)
O4—Mo6—O3193.7 (3)C4—C9—C3117.7 (9)
O22—Mo6—O30100.3 (4)C4—C9—C8120.6 (8)
O4—Mo6—O3091.8 (3)C3—C9—C8121.6 (8)
O31—Mo6—O30155.2 (4)C5—C10—C8121.0 (10)
O22—Mo6—O8i93.8 (3)C5—C10—H10A119.5
O4—Mo6—O8i164.1 (2)C8—C10—H10A119.5
O31—Mo6—O8i82.5 (3)C15—C11—C12116.0 (9)
O30—Mo6—O8i85.6 (3)C15—C11—C11ii121.6 (9)
O22—Mo6—O24165.5 (3)C12—C11—C11ii122.3 (9)
O4—Mo6—O2484.9 (2)C13—C12—C11122.0 (9)
O31—Mo6—O2490.0 (3)C13—C12—H12A119.0
O30—Mo6—O2466.4 (3)C11—C12—H12A119.0
O8i—Mo6—O2479.7 (2)N3—C13—C12119.4 (9)
O22—Mo6—Mo7126.1 (2)N3—C13—H13A120.3
O4—Mo6—Mo781.29 (16)C12—C13—H13A120.3
O31—Mo6—Mo7131.7 (3)C15—C14—N3118.0 (8)
O30—Mo6—Mo726.4 (3)C15—C14—H14A121.0
O8i—Mo6—Mo789.71 (18)N3—C14—H14A121.0
O24—Mo6—Mo741.75 (16)C14—C15—C11122.9 (9)
O16—Mo7—O1399.1 (3)C14—C15—H15A118.5
O16—Mo7—O25102.2 (4)C11—C15—H15A118.5
O13—Mo7—O2590.9 (3)C2—N1—C1123.8 (9)
O16—Mo7—O3098.5 (4)C2—N1—H1A118.1
O13—Mo7—O3094.9 (3)C1—N1—H1A118.1
O25—Mo7—O30157.3 (4)C7—N2—C5123.8 (10)
O16—Mo7—O693.0 (2)C7—N2—H2B118.1
O13—Mo7—O6167.9 (2)C5—N2—H2B118.1
O25—Mo7—O685.7 (2)C13—N3—C14121.5 (8)
O30—Mo7—O684.0 (2)C13—N3—H3B119.3
O16—Mo7—O24165.2 (3)C14—N3—H3B119.3
O13—Mo7—O2487.4 (2)
O19—Mo3—Mo5—O177.7 (4)O5—Mo3—O3—Mo426.0 (6)
O12—Mo3—Mo5—O1710.7 (4)O2—Mo3—O3—Mo457.0 (6)
O3—Mo3—Mo5—O1799.9 (3)Mo5—Mo3—O3—Mo4101.7 (6)
O7—Mo3—Mo5—O17100.6 (3)Mo9—Mo3—O3—Mo450.1 (7)
O5—Mo3—Mo5—O17178.0 (3)O14—Mo4—O3—Mo3143.2 (6)
O2—Mo3—Mo5—O17177.9 (3)O31—Mo4—O3—Mo3115.2 (6)
Mo9—Mo3—Mo5—O17124.6 (2)O28—Mo4—O3—Mo344.6 (6)
O19—Mo3—Mo5—O1190.7 (3)O15i—Mo4—O3—Mo328.9 (15)
O12—Mo3—Mo5—O11109.1 (3)O26—Mo4—O3—Mo322.5 (6)
O3—Mo3—Mo5—O11161.7 (2)Mo8—Mo4—O3—Mo320.6 (5)
O7—Mo3—Mo5—O112.2 (2)O22—Mo6—O4—Mo5136.8 (5)
O5—Mo3—Mo5—O1179.6 (2)O31—Mo6—O4—Mo5120.0 (6)
O2—Mo3—Mo5—O1179.6 (2)O30—Mo6—O4—Mo535.9 (6)
Mo9—Mo3—Mo5—O1126.17 (16)O8i—Mo6—O4—Mo544.4 (12)
O19—Mo3—Mo5—O6179.0 (3)O24—Mo6—O4—Mo530.3 (5)
O12—Mo3—Mo5—O6160.6 (4)Mo7—Mo6—O4—Mo511.7 (5)
O3—Mo3—Mo5—O671.4 (3)O17—Mo5—O4—Mo6121.5 (5)
O7—Mo3—Mo5—O688.1 (3)O11—Mo5—O4—Mo674.6 (8)
O5—Mo3—Mo5—O610.8 (3)O6—Mo5—O4—Mo618.5 (5)
O2—Mo3—Mo5—O610.8 (3)O12—Mo5—O4—Mo6142.1 (5)
Mo9—Mo3—Mo5—O664.2 (2)O2—Mo5—O4—Mo668.3 (5)
O19—Mo3—Mo5—O1218.4 (4)Mo3—Mo5—O4—Mo6113.3 (5)
O3—Mo3—Mo5—O1289.2 (3)Mo9—Mo5—O4—Mo668.5 (6)
O7—Mo3—Mo5—O12111.3 (3)O21—Mo8—O5—Mo3139.1 (6)
O5—Mo3—Mo5—O12171.4 (4)O27—Mo8—O5—Mo3115.2 (6)
O2—Mo3—Mo5—O12171.4 (4)O28—Mo8—O5—Mo340.3 (6)
Mo9—Mo3—Mo5—O12135.3 (3)O13i—Mo8—O5—Mo334.4 (13)
O19—Mo3—Mo5—O4104.1 (3)O26—Mo8—O5—Mo325.2 (6)
O12—Mo3—Mo5—O485.7 (3)Mo4—Mo8—O5—Mo316.6 (5)
O3—Mo3—Mo5—O43.53 (18)O19—Mo3—O5—Mo8124.6 (6)
O7—Mo3—Mo5—O4163.0 (2)O12—Mo3—O5—Mo851.7 (9)
O5—Mo3—Mo5—O485.7 (2)O3—Mo3—O5—Mo823.1 (6)
O2—Mo3—Mo5—O485.7 (2)O7—Mo3—O5—Mo8137.1 (6)
Mo9—Mo3—Mo5—O4139.10 (14)O2—Mo3—O5—Mo863.1 (6)
O19—Mo3—Mo5—O2170.2 (3)Mo5—Mo3—O5—Mo863.1 (6)
O12—Mo3—Mo5—O2171.4 (4)Mo9—Mo3—O5—Mo8107.6 (6)
O3—Mo3—Mo5—O282.2 (2)O17—Mo5—O6—Mo7125.5 (6)
O7—Mo3—Mo5—O277.3 (2)O11—Mo5—O6—Mo7128.7 (6)
O5—Mo3—Mo5—O20.0 (2)O12—Mo5—O6—Mo724.7 (10)
Mo9—Mo3—Mo5—O253.38 (16)O4—Mo5—O6—Mo727.6 (6)
O19—Mo3—Mo5—Mo9116.8 (3)O2—Mo5—O6—Mo754.8 (6)
O12—Mo3—Mo5—Mo9135.3 (3)Mo3—Mo5—O6—Mo747.2 (7)
O3—Mo3—Mo5—Mo9135.57 (14)Mo9—Mo5—O6—Mo798.6 (6)
O7—Mo3—Mo5—Mo923.94 (15)O16—Mo7—O6—Mo5146.0 (6)
O5—Mo3—Mo5—Mo953.40 (18)O13—Mo7—O6—Mo537.8 (16)
O2—Mo3—Mo5—Mo953.38 (16)O25—Mo7—O6—Mo5111.9 (7)
O22—Mo6—Mo7—O1613.4 (3)O30—Mo7—O6—Mo547.8 (7)
O4—Mo6—Mo7—O1685.3 (3)O24—Mo7—O6—Mo520.3 (6)
O31—Mo6—Mo7—O16172.5 (4)Mo6—Mo7—O6—Mo523.4 (6)
O30—Mo6—Mo7—O1627.2 (5)O19—Mo3—O7—Mo9175.1 (3)
O8i—Mo6—Mo7—O16107.8 (3)O12—Mo3—O7—Mo973.8 (3)
O24—Mo6—Mo7—O16177.4 (3)O3—Mo3—O7—Mo921.2 (7)
O22—Mo6—Mo7—O1394.2 (3)O5—Mo3—O7—Mo983.5 (3)
O4—Mo6—Mo7—O13167.1 (2)O2—Mo3—O7—Mo90.2 (3)
O31—Mo6—Mo7—O1379.9 (3)Mo5—Mo3—O7—Mo945.7 (2)
O30—Mo6—Mo7—O1380.4 (5)O18—Mo9—O7—Mo3166.4 (3)
O8i—Mo6—Mo7—O130.2 (2)O10—Mo9—O7—Mo387.6 (3)
O24—Mo6—Mo7—O1375.0 (3)O1—Mo9—O7—Mo39.4 (7)
O22—Mo6—Mo7—O25165.4 (4)O11—Mo9—O7—Mo372.1 (3)
O4—Mo6—Mo7—O2566.8 (4)O2—Mo9—O7—Mo30.2 (3)
O31—Mo6—Mo7—O2520.4 (4)Mo5—Mo9—O7—Mo345.4 (2)
O30—Mo6—Mo7—O25179.3 (6)O9—Mo2—O8—Mo6i168 (2)
O8i—Mo6—Mo7—O25100.1 (4)O27—Mo2—O8—Mo6i62 (2)
O24—Mo6—Mo7—O2525.3 (4)O29—Mo2—O8—Mo6i93 (2)
O22—Mo6—Mo7—O3013.8 (5)O10—Mo2—O8—Mo6i28 (3)
O4—Mo6—Mo7—O30112.5 (5)O23—Mo2—O8—Mo6i28 (2)
O31—Mo6—Mo7—O30160.3 (6)O18—Mo9—O10—Mo2127.2 (5)
O8i—Mo6—Mo7—O3080.6 (5)O1—Mo9—O10—Mo226.3 (5)
O24—Mo6—Mo7—O30155.4 (5)O7—Mo9—O10—Mo2130.2 (5)
O22—Mo6—Mo7—O696.5 (3)O11—Mo9—O10—Mo252.2 (9)
O4—Mo6—Mo7—O62.1 (2)O2—Mo9—O10—Mo257.2 (5)
O31—Mo6—Mo7—O689.3 (3)Mo3—Mo9—O10—Mo2101.2 (5)
O30—Mo6—Mo7—O6110.4 (5)Mo5—Mo9—O10—Mo253.3 (6)
O8i—Mo6—Mo7—O6169.0 (2)O9—Mo2—O10—Mo9143.0 (6)
O24—Mo6—Mo7—O694.2 (3)O8—Mo2—O10—Mo921.6 (18)
O22—Mo6—Mo7—O24169.3 (3)O27—Mo2—O10—Mo9112.7 (6)
O4—Mo6—Mo7—O2492.1 (3)O29—Mo2—O10—Mo945.0 (6)
O31—Mo6—Mo7—O244.9 (3)O23—Mo2—O10—Mo921.6 (5)
O30—Mo6—Mo7—O24155.4 (5)O17—Mo5—O11—Mo9173.3 (3)
O8i—Mo6—Mo7—O2474.8 (3)O6—Mo5—O11—Mo980.4 (3)
O14—Mo4—Mo8—O213.3 (3)O12—Mo5—O11—Mo975.8 (3)
O31—Mo4—Mo8—O21167.8 (4)O4—Mo5—O11—Mo99.7 (7)
O28—Mo4—Mo8—O2119.9 (5)O2—Mo5—O11—Mo93.3 (2)
O15i—Mo4—Mo8—O2198.1 (3)Mo3—Mo5—O11—Mo948.9 (2)
O3—Mo4—Mo8—O2191.8 (3)O18—Mo9—O11—Mo5178.7 (3)
O26—Mo4—Mo8—O21174.1 (3)O10—Mo9—O11—Mo51.9 (8)
O14—Mo4—Mo8—O27171.1 (3)O1—Mo9—O11—Mo581.2 (3)
O31—Mo4—Mo8—O276.5 (4)O7—Mo9—O11—Mo577.8 (3)
O28—Mo4—Mo8—O27165.8 (5)O2—Mo9—O11—Mo53.4 (3)
O15i—Mo4—Mo8—O2787.6 (3)Mo3—Mo9—O11—Mo549.3 (3)
O3—Mo4—Mo8—O2782.6 (3)O19—Mo3—O12—Mo5165.8 (3)
O26—Mo4—Mo8—O2711.5 (4)O3—Mo3—O12—Mo591.3 (3)
O14—Mo4—Mo8—O589.5 (3)O7—Mo3—O12—Mo566.5 (3)
O31—Mo4—Mo8—O575.1 (4)O5—Mo3—O12—Mo518.0 (7)
O28—Mo4—Mo8—O5112.6 (5)O2—Mo3—O12—Mo56.3 (3)
O15i—Mo4—Mo8—O5169.2 (2)Mo9—Mo3—O12—Mo538.0 (3)
O3—Mo4—Mo8—O51.0 (2)O17—Mo5—O12—Mo3171.3 (3)
O26—Mo4—Mo8—O593.1 (3)O11—Mo5—O12—Mo367.9 (3)
O14—Mo4—Mo8—O2823.1 (5)O6—Mo5—O12—Mo337.9 (7)
O31—Mo4—Mo8—O28172.3 (6)O4—Mo5—O12—Mo390.4 (3)
O15i—Mo4—Mo8—O2878.2 (5)O2—Mo5—O12—Mo36.3 (3)
O3—Mo4—Mo8—O28111.6 (5)Mo9—Mo5—O12—Mo338.1 (3)
O26—Mo4—Mo8—O28154.3 (5)O16—Mo7—O13—Mo8i179.8 (19)
O14—Mo4—Mo8—O13i101.6 (3)O25—Mo7—O13—Mo8i77.6 (19)
O31—Mo4—Mo8—O13i93.9 (4)O30—Mo7—O13—Mo8i80.4 (19)
O28—Mo4—Mo8—O13i78.4 (5)O6—Mo7—O13—Mo8i4 (3)
O15i—Mo4—Mo8—O13i0.2 (2)O24—Mo7—O13—Mo8i13.3 (19)
O3—Mo4—Mo8—O13i169.9 (2)Mo6—Mo7—O13—Mo8i54.7 (19)
O26—Mo4—Mo8—O13i75.8 (3)O20—Mo1—O15—Mo4i176.8 (18)
O14—Mo4—Mo8—O26177.4 (3)O25—Mo1—O15—Mo4i73.5 (18)
O31—Mo4—Mo8—O2618.0 (4)O29—Mo1—O15—Mo4i83.7 (18)
O28—Mo4—Mo8—O26154.3 (5)O1—Mo1—O15—Mo4i12 (3)
O15i—Mo4—Mo8—O2676.1 (3)O23—Mo1—O15—Mo4i17.7 (18)
O3—Mo4—Mo8—O2694.1 (3)O26—As1—O23—Mo253.2 (5)
O19—Mo3—Mo9—O1811.2 (3)O2—As1—O23—Mo265.9 (4)
O12—Mo3—Mo9—O1887.5 (3)O24—As1—O23—Mo2174.3 (3)
O3—Mo3—Mo9—O18172.8 (3)O26—As1—O23—Mo1179.3 (3)
O7—Mo3—Mo9—O1817.4 (4)O2—As1—O23—Mo161.6 (4)
O5—Mo3—Mo9—O18111.4 (3)O24—As1—O23—Mo158.2 (4)
O2—Mo3—Mo9—O18162.9 (3)O9—Mo2—O23—As1112.0 (8)
Mo5—Mo3—Mo9—O18108.5 (2)O8—Mo2—O23—As1121.6 (4)
O19—Mo3—Mo9—O1099.6 (3)O27—Mo2—O23—As124.4 (4)
O12—Mo3—Mo9—O10161.7 (2)O29—Mo2—O23—As1140.8 (5)
O3—Mo3—Mo9—O1076.4 (3)O10—Mo2—O23—As158.4 (4)
O7—Mo3—Mo9—O1093.4 (3)O9—Mo2—O23—Mo125.0 (9)
O5—Mo3—Mo9—O100.5 (2)O8—Mo2—O23—Mo1101.3 (3)
O2—Mo3—Mo9—O1086.3 (2)O27—Mo2—O23—Mo1161.4 (3)
Mo5—Mo3—Mo9—O10140.73 (16)O29—Mo2—O23—Mo13.8 (2)
O19—Mo3—Mo9—O1169.1 (3)O10—Mo2—O23—Mo178.7 (2)
O12—Mo3—Mo9—O170.4 (2)O20—Mo1—O23—As1137.5 (9)
O3—Mo3—Mo9—O115.0 (3)O25—Mo1—O23—As133.8 (4)
O7—Mo3—Mo9—O1175.3 (4)O29—Mo1—O23—As1142.9 (5)
O5—Mo3—Mo9—O190.8 (2)O15—Mo1—O23—As1123.4 (4)
O2—Mo3—Mo9—O15.0 (2)O1—Mo1—O23—As155.4 (4)
Mo5—Mo3—Mo9—O149.38 (18)O20—Mo1—O23—Mo21.5 (11)
O19—Mo3—Mo9—O76.2 (4)O25—Mo1—O23—Mo2172.9 (3)
O12—Mo3—Mo9—O7104.9 (3)O29—Mo1—O23—Mo23.9 (2)
O3—Mo3—Mo9—O7169.8 (4)O15—Mo1—O23—Mo297.6 (3)
O5—Mo3—Mo9—O793.9 (3)O1—Mo1—O23—Mo283.7 (2)
O2—Mo3—Mo9—O7179.7 (3)O26—As1—O24—Mo7177.6 (3)
Mo5—Mo3—Mo9—O7125.9 (3)O23—As1—O24—Mo755.8 (5)
O19—Mo3—Mo9—O1196.3 (3)O2—As1—O24—Mo763.5 (4)
O12—Mo3—Mo9—O112.4 (2)O26—As1—O24—Mo660.7 (4)
O3—Mo3—Mo9—O1187.7 (2)O23—As1—O24—Mo6177.5 (3)
O7—Mo3—Mo9—O11102.5 (3)O2—As1—O24—Mo658.2 (4)
O5—Mo3—Mo9—O11163.6 (2)O16—Mo7—O24—As1124.0 (9)
O2—Mo3—Mo9—O1177.8 (2)O13—Mo7—O24—As1119.4 (4)
Mo5—Mo3—Mo9—O1123.37 (14)O25—Mo7—O24—As128.5 (4)
O19—Mo3—Mo9—O2174.1 (3)O30—Mo7—O24—As1144.1 (5)
O12—Mo3—Mo9—O275.4 (2)O6—Mo7—O24—As157.0 (4)
O3—Mo3—Mo9—O210.0 (2)Mo6—Mo7—O24—As1132.7 (5)
O7—Mo3—Mo9—O2179.7 (3)O16—Mo7—O24—Mo68.7 (11)
O5—Mo3—Mo9—O285.8 (2)O13—Mo7—O24—Mo6107.8 (3)
Mo5—Mo3—Mo9—O254.39 (16)O25—Mo7—O24—Mo6161.3 (3)
O19—Mo3—Mo9—Mo5119.7 (2)O30—Mo7—O24—Mo611.4 (2)
O12—Mo3—Mo9—Mo521.01 (15)O6—Mo7—O24—Mo675.8 (2)
O3—Mo3—Mo9—Mo564.3 (2)O22—Mo6—O24—As1171.9 (9)
O7—Mo3—Mo9—Mo5125.9 (3)O4—Mo6—O24—As152.3 (4)
O5—Mo3—Mo9—Mo5140.18 (15)O31—Mo6—O24—As141.4 (4)
O2—Mo3—Mo9—Mo554.39 (16)O30—Mo6—O24—As1146.6 (4)
O17—Mo5—Mo9—O187.4 (4)O8i—Mo6—O24—As1123.8 (4)
O11—Mo5—Mo9—O181.5 (4)Mo7—Mo6—O24—As1135.0 (5)
O6—Mo5—Mo9—O18103.6 (3)O22—Mo6—O24—Mo736.9 (11)
O12—Mo5—Mo9—O18100.2 (3)O4—Mo6—O24—Mo782.6 (2)
O4—Mo5—Mo9—O18173.7 (3)O31—Mo6—O24—Mo7176.4 (3)
O2—Mo5—Mo9—O18173.9 (3)O30—Mo6—O24—Mo711.6 (2)
Mo3—Mo5—Mo9—O18120.1 (2)O8i—Mo6—O24—Mo7101.3 (3)
O17—Mo5—Mo9—O10172.0 (4)O20—Mo1—O25—Mo7167.3 (11)
O11—Mo5—Mo9—O10179.1 (4)O29—Mo1—O25—Mo72.7 (17)
O6—Mo5—Mo9—O1077.0 (3)O15—Mo1—O25—Mo794.6 (11)
O12—Mo5—Mo9—O1079.2 (3)O1—Mo1—O25—Mo772.9 (11)
O4—Mo5—Mo9—O105.7 (3)O23—Mo1—O25—Mo710.5 (11)
O2—Mo5—Mo9—O105.5 (3)O16—Mo7—O25—Mo1164.8 (11)
Mo3—Mo5—Mo9—O1059.3 (2)O13—Mo7—O25—Mo195.7 (11)
O17—Mo5—Mo9—O1104.8 (3)O30—Mo7—O25—Mo19.6 (17)
O11—Mo5—Mo9—O195.9 (3)O6—Mo7—O25—Mo172.7 (11)
O6—Mo5—Mo9—O16.2 (2)O24—Mo7—O25—Mo18.3 (11)
O12—Mo5—Mo9—O1162.4 (2)Mo6—Mo7—O25—Mo18.8 (13)
O4—Mo5—Mo9—O188.9 (2)O23—As1—O26—Mo4177.8 (3)
O2—Mo5—Mo9—O188.6 (2)O2—As1—O26—Mo463.1 (4)
Mo3—Mo5—Mo9—O1142.52 (15)O24—As1—O26—Mo456.3 (5)
O17—Mo5—Mo9—O788.9 (3)O23—As1—O26—Mo859.2 (5)
O11—Mo5—Mo9—O797.9 (3)O2—As1—O26—Mo859.9 (4)
O6—Mo5—Mo9—O7160.0 (2)O24—As1—O26—Mo8179.3 (3)
O12—Mo5—Mo9—O73.8 (2)O14—Mo4—O26—As1142.6 (8)
O4—Mo5—Mo9—O777.4 (2)O31—Mo4—O26—As133.4 (4)
O2—Mo5—Mo9—O777.6 (2)O28—Mo4—O26—As1145.6 (5)
Mo3—Mo5—Mo9—O723.72 (14)O15i—Mo4—O26—As1122.5 (4)
O17—Mo5—Mo9—O119.0 (4)O3—Mo4—O26—As156.1 (4)
O6—Mo5—Mo9—O11102.1 (3)Mo8—Mo4—O26—As1133.7 (5)
O12—Mo5—Mo9—O11101.7 (3)O14—Mo4—O26—Mo88.9 (11)
O4—Mo5—Mo9—O11175.2 (3)O31—Mo4—O26—Mo8167.1 (3)
O2—Mo5—Mo9—O11175.5 (3)O28—Mo4—O26—Mo811.9 (2)
Mo3—Mo5—Mo9—O11121.6 (3)O15i—Mo4—O26—Mo8103.8 (3)
O17—Mo5—Mo9—O2166.5 (3)O3—Mo4—O26—Mo877.7 (2)
O11—Mo5—Mo9—O2175.5 (3)O21—Mo8—O26—As1154.1 (7)
O6—Mo5—Mo9—O282.4 (2)O27—Mo8—O26—As135.7 (4)
O12—Mo5—Mo9—O273.8 (2)O5—Mo8—O26—As155.8 (4)
O4—Mo5—Mo9—O20.2 (2)O28—Mo8—O26—As1147.6 (5)
Mo3—Mo5—Mo9—O253.87 (16)O13i—Mo8—O26—As1121.9 (4)
O17—Mo5—Mo9—Mo3112.6 (3)Mo4—Mo8—O26—As1135.7 (5)
O11—Mo5—Mo9—Mo3121.6 (3)O21—Mo8—O26—Mo418.4 (10)
O6—Mo5—Mo9—Mo3136.29 (15)O27—Mo8—O26—Mo4171.3 (3)
O12—Mo5—Mo9—Mo319.88 (14)O5—Mo8—O26—Mo479.8 (2)
O4—Mo5—Mo9—Mo353.63 (17)O28—Mo8—O26—Mo412.0 (2)
O2—Mo5—Mo9—Mo353.87 (16)O13i—Mo8—O26—Mo4102.4 (3)
O18—Mo9—O1—Mo1126.5 (5)O21—Mo8—O27—Mo2173.5 (11)
O10—Mo9—O1—Mo121.1 (5)O5—Mo8—O27—Mo274.0 (11)
O7—Mo9—O1—Mo176.4 (7)O28—Mo8—O27—Mo216.5 (15)
O11—Mo9—O1—Mo1138.7 (5)O13i—Mo8—O27—Mo291.9 (11)
O2—Mo9—O1—Mo167.2 (5)O26—Mo8—O27—Mo29.2 (11)
Mo3—Mo9—O1—Mo170.7 (5)Mo4—Mo8—O27—Mo21.6 (13)
Mo5—Mo9—O1—Mo1112.0 (5)O9—Mo2—O27—Mo8162.0 (11)
O20—Mo1—O1—Mo9136.9 (5)O8—Mo2—O27—Mo893.3 (11)
O25—Mo1—O1—Mo9119.9 (6)O29—Mo2—O27—Mo824.8 (16)
O29—Mo1—O1—Mo937.9 (5)O10—Mo2—O27—Mo876.2 (11)
O15—Mo1—O1—Mo934.4 (14)O23—Mo2—O27—Mo84.4 (11)
O23—Mo1—O1—Mo928.7 (5)O14—Mo4—O28—Mo8160.6 (4)
O26—As1—O2—Mo32.9 (4)O31—Mo4—O28—Mo816.0 (11)
O23—As1—O2—Mo3123.3 (3)O15i—Mo4—O28—Mo8102.8 (5)
O24—As1—O2—Mo3116.5 (3)O3—Mo4—O28—Mo864.8 (4)
O26—As1—O2—Mo9117.8 (3)O26—Mo4—O28—Mo818.7 (4)
O23—As1—O2—Mo92.5 (4)O21—Mo8—O28—Mo4163.3 (4)
O24—As1—O2—Mo9122.7 (3)O27—Mo8—O28—Mo426.5 (9)
O26—As1—O2—Mo5122.8 (3)O5—Mo8—O28—Mo464.7 (5)
O23—As1—O2—Mo5116.9 (3)O13i—Mo8—O28—Mo4101.6 (5)
O24—As1—O2—Mo53.3 (4)O26—Mo8—O28—Mo418.4 (4)
O19—Mo3—O2—As1166.6 (14)O20—Mo1—O29—Mo2172.6 (4)
O12—Mo3—O2—As1129.8 (3)O25—Mo1—O29—Mo22.4 (11)
O3—Mo3—O2—As138.0 (3)O15—Mo1—O29—Mo289.2 (4)
O7—Mo3—O2—As1134.1 (3)O1—Mo1—O29—Mo278.9 (4)
O5—Mo3—O2—As145.6 (3)O23—Mo1—O29—Mo26.1 (4)
Mo5—Mo3—O2—As1134.3 (4)O9—Mo2—O29—Mo1164.7 (4)
Mo9—Mo3—O2—As1134.3 (4)O8—Mo2—O29—Mo191.9 (4)
O19—Mo3—O2—Mo932.4 (16)O27—Mo2—O29—Mo126.3 (9)
O12—Mo3—O2—Mo995.9 (2)O10—Mo2—O29—Mo178.4 (4)
O3—Mo3—O2—Mo9172.26 (19)O23—Mo2—O29—Mo16.1 (4)
O7—Mo3—O2—Mo90.14 (18)O22—Mo6—O30—Mo7168.7 (4)
O5—Mo3—O2—Mo988.62 (18)O4—Mo6—O30—Mo766.1 (5)
Mo5—Mo3—O2—Mo991.40 (16)O31—Mo6—O30—Mo736.9 (9)
O19—Mo3—O2—Mo559.0 (16)O8i—Mo6—O30—Mo798.3 (5)
O12—Mo3—O2—Mo54.50 (18)O24—Mo6—O30—Mo717.6 (4)
O3—Mo3—O2—Mo596.34 (19)O16—Mo7—O30—Mo6157.0 (4)
O7—Mo3—O2—Mo591.54 (19)O13—Mo7—O30—Mo6103.0 (5)
O5—Mo3—O2—Mo5179.98 (19)O25—Mo7—O30—Mo61.4 (11)
Mo9—Mo3—O2—Mo591.40 (16)O6—Mo7—O30—Mo664.8 (4)
O18—Mo9—O2—As1155.6 (8)O24—Mo7—O30—Mo617.9 (4)
O10—Mo9—O2—As141.9 (3)O14—Mo4—O31—Mo6149.3 (10)
O1—Mo9—O2—As148.6 (3)O28—Mo4—O31—Mo627.2 (17)
O7—Mo9—O2—As1135.2 (3)O15i—Mo4—O31—Mo6114.1 (10)
O11—Mo9—O2—As1136.2 (3)O3—Mo4—O31—Mo652.9 (10)
Mo3—Mo9—O2—As1135.4 (4)O26—Mo4—O31—Mo629.8 (11)
Mo5—Mo9—O2—As1134.1 (4)Mo8—Mo4—O31—Mo617.6 (12)
O18—Mo9—O2—Mo369.0 (9)O22—Mo6—O31—Mo4154.8 (10)
O10—Mo9—O2—Mo393.5 (2)O4—Mo6—O31—Mo451.6 (11)
O1—Mo9—O2—Mo3176.00 (19)O30—Mo6—O31—Mo450.9 (14)
O7—Mo9—O2—Mo30.14 (18)O8i—Mo6—O31—Mo4112.9 (11)
O11—Mo9—O2—Mo388.39 (19)O24—Mo6—O31—Mo433.3 (11)
Mo5—Mo9—O2—Mo390.55 (16)Mo7—Mo6—O31—Mo430.0 (12)
O18—Mo9—O2—Mo521.5 (9)N1—C1—C3—C90.4 (13)
O10—Mo9—O2—Mo5176.0 (2)N1—C2—C4—C93.0 (14)
O1—Mo9—O2—Mo585.45 (18)C8—C6—C7—N20.9 (16)
O7—Mo9—O2—Mo590.69 (19)C7—C6—C8—C100.2 (15)
O11—Mo9—O2—Mo52.16 (16)C7—C6—C8—C9178.8 (9)
Mo3—Mo9—O2—Mo590.55 (16)C2—C4—C9—C31.1 (13)
O17—Mo5—O2—As1144.7 (12)C2—C4—C9—C8178.4 (8)
O11—Mo5—O2—As1135.8 (3)C1—C3—C9—C40.5 (13)
O6—Mo5—O2—As136.8 (3)C1—C3—C9—C8176.7 (8)
O12—Mo5—O2—As1130.6 (3)C6—C8—C9—C4171.0 (9)
O4—Mo5—O2—As146.7 (3)C10—C8—C9—C410.0 (12)
Mo3—Mo5—O2—As1134.9 (4)C6—C8—C9—C311.8 (13)
Mo9—Mo5—O2—As1133.4 (4)C10—C8—C9—C3167.1 (8)
O17—Mo5—O2—Mo39.9 (14)N2—C5—C10—C80.6 (16)
O11—Mo5—O2—Mo389.3 (2)C6—C8—C10—C50.5 (14)
O6—Mo5—O2—Mo3171.70 (19)C9—C8—C10—C5179.5 (9)
O12—Mo5—O2—Mo34.31 (18)C15—C11—C12—C131.8 (16)
O4—Mo5—O2—Mo388.11 (18)C11ii—C11—C12—C13180.0 (11)
Mo9—Mo5—O2—Mo391.70 (16)C11—C12—C13—N31.7 (18)
O17—Mo5—O2—Mo981.8 (13)N3—C14—C15—C113.0 (14)
O11—Mo5—O2—Mo92.39 (18)C12—C11—C15—C140.6 (14)
O6—Mo5—O2—Mo996.60 (19)C11ii—C11—C15—C14177.6 (10)
O12—Mo5—O2—Mo996.0 (2)C4—C2—N1—C13.3 (15)
O4—Mo5—O2—Mo9179.81 (18)C3—C1—N1—C21.6 (14)
Mo3—Mo5—O2—Mo991.70 (16)C6—C7—N2—C50.9 (17)
O19—Mo3—O3—Mo4126.7 (6)C10—C5—N2—C70.2 (17)
O12—Mo3—O3—Mo4132.1 (6)C12—C13—N3—C140.9 (16)
O7—Mo3—O3—Mo436.8 (10)C15—C14—N3—C133.1 (14)
Symmetry codes: (i) x+2, y+1, z+1; (ii) x+1, y+1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1A···O140.861.992.851 (10)174
N2—H2B···O29iii0.862.322.805 (12)116
N3—H3B···O10iv0.862.563.291 (9)143
N3—H3B···O7iv0.862.603.336 (10)145
Symmetry codes: (iii) x1, y+1, z; (iv) x1, y, z.

Experimental details

Crystal data
Chemical formula(C10H10N2)3[As2Mo18O62]
Mr3343.36
Crystal system, space groupTriclinic, P1
Temperature (K)293
a, b, c (Å)11.2671 (17), 12.1365 (19), 13.871 (2)
α, β, γ (°)108.023 (2), 94.243 (2), 107.166 (2)
V3)1694.6 (4)
Z1
Radiation typeMo Kα
µ (mm1)4.30
Crystal size (mm)0.29 × 0.22 × 0.20
Data collection
DiffractometerRigaku R-AXIS RAPID
diffractometer
Absorption correctionMulti-scan
(ABSCOR; Higashi, 1995)
Tmin, Tmax0.504, 0.625
No. of measured, independent and
observed [I > 2σ(I)] reflections
14379, 6545, 4986
Rint0.042
(sin θ/λ)max1)0.619
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.047, 0.128, 1.06
No. of reflections6545
No. of parameters532
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)3.42, 1.79

Computer programs: RAPID-AUTO (Rigaku, 1998), SHELXS97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008), ORTEP-3 (Burnett & Johnson, 1996), SHELXL97 (Sheldrick, 2008).

Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1A···O140.861.992.851 (10)173.9
N2—H2B···O29i0.862.322.805 (12)115.7
N3—H3B···O10ii0.862.563.291 (9)142.8
N3—H3B···O7ii0.862.603.336 (10)144.6
Symmetry codes: (i) x1, y+1, z; (ii) x1, y, z.
 

Acknowledgements

This work was supported by the National Natural Science Foundation of China (20571032 and20333070).

References

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Volume 65| Part 12| December 2009| Pages m1698-m1699
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