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

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890
Volume 66| Part 8| August 2010| Page m1000
https://doi.org/10.1107/S1600536810028801

Tris(2-meth­­oxy­ethanaminium) dodeca­molybdophosphate trihydrate

Akbar Raissi Shabari,a* Sara Kharaghania and Mehrdad Pourayoubib

aFaculty of Chemistry, Islamic Azad University-North Tehran Branch, Tehran, Iran, and bDepartment of Chemistry, Ferdowsi University of Mashhad, Mashhad, 91779, Iran
*Correspondence e-mail: a_raissi.shabari@yahoo.com

(Received 30 June 2010; accepted 19 July 2010; online 24 July 2010)

The asymmetric unit of the polyoxidometalate-based organic–inorganic hybrid title compound, (C3H10NO)3[PMo12O40]·3H2O, consists of one α-Keggin-type [PMo12O40]3− polyoxido­anion, three independent [CH3–O–CH2–CH2–NH3]+ cations and three solvent water mol­ecules. The polyoxidoanion shows characteristic features with respect to bond lengths and angles. In the crystal structure, extensive inter­molecular N—H⋯O and O—H⋯O hydrogen bonding between the organic cations, inorganic anions and solvent water mol­ecules leads to a three-dimensional supra­molecular network.

Related literature

For background information on polyoxometalate-based organic–inorganic hybrid materials, see: Pourayoubi & Mahjoub (2007[Pourayoubi, M. & Mahjoub, A. R. (2007). Acta Cryst. E63, m2622-m2623.], 2010[Pourayoubi, M. & Mahjoub, A. R. (2010). J. Iran. Chem. Soc. Accepted.]); Raissi Shabari et al. (2009[Raissi Shabari, A., Pourayoubi, M. & Ghamari, D. (2009). Acta Cryst. E65, m1586.]). For related structures, see: Gong et al. (2006[Gong, Y., Hu, C., Li, H., Tang, W., Huang, K. & Hou, W. (2006). J. Mol. Struct. 784, 228-238.]); Han et al. (2005[Han, Z., Zhao, Y., Peng, J., Tian, A., Feng, Y. & Liu, Q. (2005). J. Solid State Chem. 178, 1386-1394.]).

[Scheme 1]

Experimental

Crystal data

  • (C3H10NO)3[PMo12O40]·3H2O

  • Mr = 2104.66

  • Monoclinic, P 21 /n

  • a = 12.7806 (2) Å

  • b = 27.0489 (4) Å

  • c = 14.6360 (2) Å

  • β = 114.876 (1)°

  • V = 4590.24 (12) Å3

  • Z = 4

  • Mo Kα radiation

  • μ = 3.32 mm−1

  • T = 100 K

  • 0.10 × 0.05 × 0.03 mm
Data collection

  • Bruker SMART APEXII CCD area-detector diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2005[Bruker (2005). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.820, Tmax = 0.907

  • 100492 measured reflections

  • 12174 independent reflections

  • 10404 reflections with I > 2σ(I)

  • Rint = 0.042
Refinement

  • R[F2 > 2σ(F2)] = 0.022

  • wR(F2) = 0.052

  • S = 1.00

  • 12174 reflections

  • 646 parameters

  • H-atom parameters constrained

  • Δρmax = 0.66 e Å−3

  • Δρmin = −0.69 e Å−3

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A D⋯A D—H⋯A
O1W—H1WA⋯O2W 0.75 2.00 2.726 (5) 161
O1W—H1WB⋯O31i 0.85 2.14 2.936 (4) 157
O2W—H2WB⋯O15 0.83 1.99 2.807 (3) 167
O2W—H2WA⋯O22ii 0.90 2.03 2.780 (3) 140
O3W—H3WA⋯O40iii 0.88 2.05 2.904 (3) 162
O3W—H3WB⋯O10iv 0.84 1.97 2.772 (3) 159
N1S—H1NA⋯O3W 0.91 1.93 2.812 (4) 164
N1S—H1NB⋯O2Sv 0.91 2.59 3.182 (4) 123
N1S—H1NB⋯O9v 0.91 2.24 2.949 (4) 134
N1S—H1NC⋯O1S 0.91 2.31 2.731 (4) 108
N1S—H1NC⋯O31v 0.91 2.48 3.110 (4) 127
N1S—H1NC⋯O35ii 0.91 2.28 2.887 (3) 124
N2S—H2NA⋯O2S 0.91 2.42 2.814 (5) 106
N2S—H2NA⋯O8 0.91 1.94 2.811 (3) 159
N2S—H2NB⋯O1W 0.91 1.83 2.629 (5) 145
N2S—H2NC⋯O3S 0.91 1.93 2.798 (5) 158
N3S—H3NA⋯O23ii 0.91 2.31 3.110 (4) 146
N3S—H3NB⋯O34iv 0.91 2.08 2.955 (4) 161
N3S—H3NC⋯O2W 0.91 1.96 2.822 (4) 158
Symmetry codes: (i) -x, -y+1, -z+1; (ii) -x+1, -y+1, -z+1; (iii) x+1, y, z+1; (iv) [x+{\script{1\over 2}}, -y+{\script{3\over 2}}, z+{\script{1\over 2}}]; (v) x+1, y, z.

Data collection: APEX2 (Bruker, 2005[Bruker (2005). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2005[Bruker (2005). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Supporting information

Crystal structure: contains datablocks I, global. DOI: https://doi.org/10.1107/S1600536810028801/lh5078sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536810028801/lh5078Isup2.hkl

checkCIF report


Comment top

Keggin-type polyoxoanions have been used as the inorganic building blocks to construct polyoxometalate-based organic-inorganic hybrid materials containing the organic cations such as protonated-amino acid (Raissi Shabari et al., 2009), heterocyclic base (Pourayoubi & Mahjoub, 2007) and amide (Pourayoubi & Mahjoub, 2010).

We report here on the synthesis and crystal structure of a new POM-based hybrid material containing a protonated aminoether.

The title polyoxometalate-based organic-inorganic hybrid compound consists of one [PMo12O40]3- polyoxoanion, three symmetrically independent CH3–O–CH2–CH2–NH3+ cations and three solvent water molecules. The inorganic anion shows a classical α-Keggin structure (Fig. 1) with 4 different types of O atoms. This includes 12 terminal O atoms, 4 O atoms which are bonded to P and Mo, 12 MoO6 octahedra corner-shared and 12 MoO6 octahedra edge-shared oxygen atoms.

The central PO4 tetrahedron is slightly distorted and is surrounded by 12 distorted MoO6 octahedra. The P—O bond lengths range from 1.534 (2) to 1.539 (2) Å, and the O—P—O angles are in the range of 109.20 (11)–109.66 (11)°.

All three organic cations (Fig. 2) show slight differences in bond lengths, angles and torsion angles. They are involved in an extensive hydrogen bonding. Several N–H···O (N···O distances are in the range of 2.629 (5) to 3.182 (4) Å) and O–H···O (O···O distances are in the range from 2.726 (5) to 2.936 (4) Å) hydrogen bonds between the organic cations, inorganic anions and crystal water molecules lead to a 3-D supramolecular network.

In the title hybrid compound, the position of organic cations and water molecules allows to direct interaction of one polyoxoanion with four neighboring polyoxoanions via O···O contacts [2.80-3.018 Å]. Two important O···O contacts are the O36···O6 (2.800 Å) and O32···O17 (2.814 Å) interactions, O36 and O32 are the terminal and O6 and O17 are the bridged oxygen atoms of the polyoxoanions. The less important O···O contacts are O31···O35 (3.018 Å), O29···O34 (3.012 Å), O27···O28 (2.981 Å) and O24···O40 (2.915 Å) [O31, O35, O29, O34 and O40 are terminal and O24, O27 and O28 are bridging oxygen atoms]. Similar interactions have been observed in the structure of (C5N2H7)5H[P2Mo5O23] (C5N2H7 = protonated 2-aminopyridine) reported by Gong et al. (2006) [Oterminal···Oterminal = 2.398 Å] and in the structure of (H3/4pbpy)4[PMo12O40].1.25H2O (pbpy = 5-phenyl-2-(4-pyridinyl)pyridine) reported by Han et al. (2005) [Oterminal···Oterminal and Oterminal···Obridge in the range of 2.931 to 3.001 Å].

Related literature top

For background information on polyoxometalate-based organic–inorganic hybrid materials, see: Pourayoubi & Mahjoub (2007, 2010); Raissi Shabari et al. (2009). For related structures, see: Gong et al. (2006); Han et al. (2005).

Experimental top

The title hybrid compound was obtained from mixing H3PMo12O40 and SrCl2.2H2O and then the treatment with CH3OCH2CH2NH2 in a mixture of H2O and CH3CN. 31P-NMR (DMSO-d6, p.p.m.): -4.11. IR (KBr, cm-1): 3371.4 m, 2908.7 w, 1611.7 m, 1501.6 m, 1208.2 w, 1062.1 s, 957.9 vs, 878.8 s, 783.6 vs.

Refinement top

The hydrogen atoms of NH3 groups were included in calculated positions with N-H = 0.91Å and those of the H2O molecules were found in a difference Fourier synthesis. The H(C) atom positions were placed in calculated positions with C-H = 0.98-0.99Å. All hydrogen atoms were refined in isotropic approximation in a riding-model with the Uiso(H) parameters in the range 1.2-1.5 Ueq(C,N,O).

Structure description top

Keggin-type polyoxoanions have been used as the inorganic building blocks to construct polyoxometalate-based organic-inorganic hybrid materials containing the organic cations such as protonated-amino acid (Raissi Shabari et al., 2009), heterocyclic base (Pourayoubi & Mahjoub, 2007) and amide (Pourayoubi & Mahjoub, 2010).

We report here on the synthesis and crystal structure of a new POM-based hybrid material containing a protonated aminoether.

The title polyoxometalate-based organic-inorganic hybrid compound consists of one [PMo12O40]3- polyoxoanion, three symmetrically independent CH3–O–CH2–CH2–NH3+ cations and three solvent water molecules. The inorganic anion shows a classical α-Keggin structure (Fig. 1) with 4 different types of O atoms. This includes 12 terminal O atoms, 4 O atoms which are bonded to P and Mo, 12 MoO6 octahedra corner-shared and 12 MoO6 octahedra edge-shared oxygen atoms.

The central PO4 tetrahedron is slightly distorted and is surrounded by 12 distorted MoO6 octahedra. The P—O bond lengths range from 1.534 (2) to 1.539 (2) Å, and the O—P—O angles are in the range of 109.20 (11)–109.66 (11)°.

All three organic cations (Fig. 2) show slight differences in bond lengths, angles and torsion angles. They are involved in an extensive hydrogen bonding. Several N–H···O (N···O distances are in the range of 2.629 (5) to 3.182 (4) Å) and O–H···O (O···O distances are in the range from 2.726 (5) to 2.936 (4) Å) hydrogen bonds between the organic cations, inorganic anions and crystal water molecules lead to a 3-D supramolecular network.

In the title hybrid compound, the position of organic cations and water molecules allows to direct interaction of one polyoxoanion with four neighboring polyoxoanions via O···O contacts [2.80-3.018 Å]. Two important O···O contacts are the O36···O6 (2.800 Å) and O32···O17 (2.814 Å) interactions, O36 and O32 are the terminal and O6 and O17 are the bridged oxygen atoms of the polyoxoanions. The less important O···O contacts are O31···O35 (3.018 Å), O29···O34 (3.012 Å), O27···O28 (2.981 Å) and O24···O40 (2.915 Å) [O31, O35, O29, O34 and O40 are terminal and O24, O27 and O28 are bridging oxygen atoms]. Similar interactions have been observed in the structure of (C5N2H7)5H[P2Mo5O23] (C5N2H7 = protonated 2-aminopyridine) reported by Gong et al. (2006) [Oterminal···Oterminal = 2.398 Å] and in the structure of (H3/4pbpy)4[PMo12O40].1.25H2O (pbpy = 5-phenyl-2-(4-pyridinyl)pyridine) reported by Han et al. (2005) [Oterminal···Oterminal and Oterminal···Obridge in the range of 2.931 to 3.001 Å].

For background information on polyoxometalate-based organic–inorganic hybrid materials, see: Pourayoubi & Mahjoub (2007, 2010); Raissi Shabari et al. (2009). For related structures, see: Gong et al. (2006); Han et al. (2005).

Computing details top

Data collection: APEX2 (Bruker, 2005); cell refinement: SAINT (Bruker, 2005); data reduction: SAINT (Bruker, 2005); program(s) used to solve structure: SHELXTL (Sheldrick, 2008); program(s) used to refine structure: SHELXTL (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. An ORTEP-style plot of the α-Keggin-type PMo12O403- polyoxoanion. Ellipsoids are given at the 50% probability level.
[Figure 2] Fig. 2. A view of the three symmetrically independent organic cations and the solvent water molecules. Ellipsoids are given at the 50% probability level.
Tris(2-methoxyethanaminium) dodecamolybdophosphate trihydrate top
Crystal data top
(C3H10NO)3[PMo12O40]·3H2OF(000) = 3992
Mr = 2104.66Dx = 3.045 Mg m−3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 3521 reflections
a = 12.7806 (2) Åθ = 2–25°
b = 27.0489 (4) ŵ = 3.32 mm−1
c = 14.6360 (2) ÅT = 100 K
β = 114.876 (1)°Prism, light-green
V = 4590.24 (12) Å30.10 × 0.05 × 0.03 mm
Z = 4
Data collection top
Bruker SMART APEXII CCD area-detector
diffractometer		12174 independent reflections
Radiation source: fine-focus sealed tube10404 reflections with I > 2/s(I)
Graphite monochromatorRint = 0.042
φ and ω scansθmax = 29.0°, θmin = 1.7°
Absorption correction: multi-scan
(SADABS; Bruker, 2005)		h = −17→17
Tmin = 0.820, Tmax = 0.907k = −36→36
100492 measured reflectionsl = −19→19
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)] = 0.022Hydrogen site location: mixed
wR(F2) = 0.052H-atom parameters constrained
S = 1.00 w = 1/[σ2(Fo2) + (0.026P)2 + 6.P]
where P = (Fo2 + 2Fc2)/3
12174 reflections(Δ/σ)max = 0.003
646 parametersΔρmax = 0.66 e Å−3
0 restraintsΔρmin = −0.69 e Å−3
Crystal data top
(C3H10NO)3[PMo12O40]·3H2OV = 4590.24 (12) Å3
Mr = 2104.66Z = 4
Monoclinic, P21/nMo Kα radiation
a = 12.7806 (2) ŵ = 3.32 mm−1
b = 27.0489 (4) ÅT = 100 K
c = 14.6360 (2) Å0.10 × 0.05 × 0.03 mm
β = 114.876 (1)°
Data collection top
Bruker SMART APEXII CCD area-detector
diffractometer		12174 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2005)		10404 reflections with I > 2/s(I)
Tmin = 0.820, Tmax = 0.907Rint = 0.042
100492 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0220 restraints
wR(F2) = 0.052H-atom parameters constrained
S = 1.00Δρmax = 0.66 e Å−3
12174 reflectionsΔρmin = −0.69 e Å−3
646 parameters
Special details top

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

Refinement. 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
Mo10.24736 (2)0.664083 (9)0.512361 (18)0.01740 (5)
Mo2−0.00825 (2)0.715144 (9)0.349457 (19)0.01756 (5)
Mo30.00282 (2)0.592678 (9)0.412826 (19)0.01770 (5)
Mo40.35509 (2)0.720875 (9)0.337823 (18)0.01669 (5)
Mo50.41688 (2)0.588865 (9)0.409766 (18)0.01740 (5)
Mo60.09067 (2)0.751816 (9)0.154478 (18)0.01716 (5)
Mo70.19104 (2)0.507896 (9)0.350528 (19)0.01738 (5)
Mo8−0.15388 (2)0.664402 (9)0.090979 (19)0.01764 (5)
Mo9−0.09683 (2)0.542448 (9)0.152746 (19)0.01797 (5)
Mo100.26798 (2)0.673700 (9)0.100035 (18)0.01724 (5)
Mo110.28028 (2)0.541453 (9)0.170021 (18)0.01750 (5)
Mo120.00156 (2)0.596892 (9)−0.005718 (18)0.01759 (5)
P10.13305 (6)0.62980 (3)0.25327 (5)0.01579 (13)
O1S0.6654 (2)0.61043 (9)0.33985 (17)0.0277 (5)
O1W0.2136 (3)0.50927 (12)0.6577 (2)0.0489 (7)
H1WA0.26500.50640.64590.059*
H1WB0.16750.49470.60460.059*
O10.10526 (17)0.64338 (7)0.34244 (15)0.0173 (4)
O20.18748 (17)0.67467 (7)0.22546 (15)0.0170 (4)
O2W0.4173 (2)0.51907 (9)0.64138 (18)0.0303 (5)
H2WB0.39940.52580.58110.036*
H2WA0.44230.48900.66800.036*
O2S0.0596 (2)0.68215 (10)0.67215 (18)0.0321 (5)
O3S0.4383 (2)0.59570 (9)0.83909 (18)0.0292 (5)
O3W0.8029 (2)0.64000 (8)0.71502 (17)0.0266 (5)
H3WA0.86250.62750.76680.032*
H3WB0.80240.66710.74300.032*
O30.21837 (17)0.58625 (7)0.28277 (15)0.0172 (4)
O40.02149 (17)0.61520 (7)0.16266 (15)0.0178 (4)
O50.30395 (17)0.70902 (7)0.43468 (15)0.0182 (4)
O60.12074 (17)0.71361 (7)0.46892 (15)0.0186 (4)
O70.33997 (18)0.61763 (8)0.49225 (15)0.0197 (4)
O80.14437 (18)0.62037 (8)0.52687 (15)0.0191 (4)
O9−0.05958 (17)0.65483 (8)0.40290 (16)0.0201 (4)
O100.24744 (18)0.76801 (8)0.26560 (15)0.0194 (4)
O110.05341 (17)0.74765 (8)0.27458 (16)0.0193 (4)
O12−0.11778 (17)0.68535 (8)0.21912 (16)0.0198 (4)
O130.42021 (17)0.65201 (8)0.36937 (15)0.0188 (4)
O14−0.08156 (18)0.57175 (8)0.28521 (16)0.0198 (4)
O150.34077 (18)0.52739 (8)0.43200 (15)0.0196 (4)
O160.12090 (18)0.54363 (8)0.41412 (16)0.0198 (4)
O170.16896 (17)0.73395 (8)0.07979 (15)0.0192 (4)
O18−0.03860 (17)0.71521 (8)0.09183 (15)0.0188 (4)
O190.37360 (17)0.70610 (8)0.21113 (15)0.0189 (4)
O200.31360 (17)0.61041 (8)0.14154 (15)0.0192 (4)
O21−0.20133 (17)0.60120 (8)0.10127 (16)0.0203 (4)
O220.42056 (17)0.55662 (8)0.30009 (16)0.0197 (4)
O230.24697 (18)0.49318 (8)0.24407 (16)0.0201 (4)
O240.04070 (18)0.51300 (8)0.23044 (16)0.0198 (4)
O25−0.11806 (17)0.63845 (8)−0.02211 (16)0.0202 (4)
O260.11346 (17)0.64344 (8)0.01772 (15)0.0198 (4)
O27−0.08159 (18)0.54429 (8)0.03363 (16)0.0208 (4)
O280.13624 (18)0.55233 (8)0.07437 (15)0.0198 (4)
O290.32331 (19)0.68249 (8)0.63240 (16)0.0230 (4)
O30−0.09283 (18)0.75731 (8)0.36978 (17)0.0234 (4)
O31−0.05393 (19)0.56240 (8)0.48270 (17)0.0231 (4)
O320.47484 (18)0.75507 (8)0.39483 (16)0.0215 (4)
O330.55037 (18)0.57974 (8)0.50144 (16)0.0221 (4)
O340.04977 (18)0.81057 (8)0.11564 (16)0.0218 (4)
O350.1858 (2)0.44995 (8)0.38943 (17)0.0239 (4)
O36−0.27941 (18)0.69254 (8)0.02173 (17)0.0233 (4)
O37−0.19494 (19)0.49750 (8)0.13432 (17)0.0251 (5)
O380.31745 (19)0.68375 (8)0.01167 (16)0.0234 (4)
O390.34656 (19)0.50846 (8)0.11232 (17)0.0234 (4)
O40−0.03200 (18)0.57955 (8)−0.12542 (16)0.0221 (4)
N1S0.8071 (2)0.64679 (10)0.5249 (2)0.0228 (5)
H1NA0.81690.64890.59010.034*
H1NB0.86940.66010.51910.034*
H1NC0.79950.61450.50570.034*
N2S0.1986 (3)0.59691 (13)0.7289 (2)0.0327 (7)
H2NA0.17130.61090.66660.049*
H2NB0.19230.56340.72260.049*
H2NC0.27400.60530.76420.049*
N3S0.5835 (2)0.59440 (11)0.7239 (2)0.0269 (6)
H3NA0.64440.57850.72030.040*
H3NB0.56060.61960.67860.040*
H3NC0.52420.57280.70970.040*
C1S0.6294 (3)0.59620 (15)0.2376 (3)0.0326 (7)
H1SA0.63490.56020.23350.049*
H1SB0.67910.61200.21030.049*
H1SC0.54940.60660.19850.049*
C2S0.6681 (3)0.66261 (12)0.3497 (2)0.0249 (6)
H2SA0.59150.67670.30720.030*
H2SB0.72530.67680.32780.030*
C3S0.7011 (3)0.67455 (12)0.4591 (2)0.0247 (6)
H3SA0.71520.71050.47020.030*
H3SB0.63690.66560.47690.030*
C4S0.0660 (3)0.73358 (14)0.6557 (3)0.0363 (8)
H4SA0.01850.74130.58480.054*
H4SB0.14630.74280.67290.054*
H4SC0.03770.75220.69820.054*
C5S0.1207 (4)0.67011 (17)0.7758 (3)0.0407 (9)
H5SA0.07860.68260.81450.049*
H5SB0.19830.68530.80340.049*
C6S0.1303 (3)0.61496 (16)0.7831 (3)0.0385 (9)
H6SA0.16840.60490.85470.046*
H6SB0.05230.60000.75310.046*
C7S0.4675 (3)0.57169 (17)0.9337 (3)0.0417 (9)
H7SA0.41260.54490.92530.063*
H7SB0.46410.59570.98260.063*
H7SC0.54560.55810.95810.063*
C8S0.5176 (3)0.63418 (12)0.8428 (3)0.0278 (7)
H8SA0.54580.65090.90900.033*
H8SB0.47660.65900.79010.033*
C9S0.6185 (3)0.61453 (13)0.8273 (2)0.0266 (6)
H9SA0.67530.64140.83900.032*
H9SB0.65630.58810.87710.032*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mo10.01831 (11)0.01785 (11)0.01572 (11)−0.00033 (9)0.00683 (9)−0.00083 (8)
Mo20.01774 (11)0.01614 (11)0.01939 (11)0.00003 (9)0.00838 (9)−0.00108 (9)
Mo30.01888 (11)0.01722 (11)0.01885 (11)−0.00036 (9)0.00974 (9)−0.00019 (9)
Mo40.01548 (10)0.01697 (11)0.01635 (11)−0.00128 (8)0.00544 (8)−0.00015 (8)
Mo50.01689 (11)0.01780 (11)0.01664 (11)0.00086 (9)0.00619 (9)0.00099 (8)
Mo60.01651 (11)0.01596 (11)0.01729 (11)−0.00057 (8)0.00542 (9)0.00140 (8)
Mo70.01957 (11)0.01499 (11)0.01857 (11)0.00056 (9)0.00898 (9)0.00065 (8)
Mo80.01530 (10)0.01735 (11)0.01846 (11)−0.00049 (9)0.00533 (9)−0.00002 (9)
Mo90.01790 (11)0.01625 (11)0.01958 (11)−0.00236 (9)0.00771 (9)−0.00150 (9)
Mo100.01738 (11)0.01835 (11)0.01584 (11)−0.00129 (9)0.00684 (9)0.00073 (9)
Mo110.01854 (11)0.01715 (11)0.01760 (11)0.00070 (9)0.00836 (9)−0.00062 (9)
Mo120.01766 (11)0.01825 (11)0.01574 (11)−0.00166 (9)0.00593 (9)−0.00113 (9)
P10.0158 (3)0.0156 (3)0.0156 (3)−0.0006 (2)0.0062 (3)−0.0002 (2)
O1S0.0344 (12)0.0269 (12)0.0223 (11)−0.0018 (10)0.0125 (10)−0.0006 (9)
O1W0.0467 (17)0.0505 (18)0.0548 (19)−0.0057 (14)0.0266 (15)−0.0035 (15)
O10.0180 (9)0.0169 (9)0.0174 (9)−0.0008 (7)0.0079 (8)−0.0004 (7)
O20.0174 (9)0.0163 (9)0.0173 (9)−0.0004 (7)0.0071 (8)0.0000 (7)
O2W0.0351 (13)0.0253 (12)0.0232 (11)−0.0023 (10)0.0052 (10)0.0055 (9)
O2S0.0340 (13)0.0372 (14)0.0241 (12)−0.0010 (11)0.0113 (10)−0.0041 (10)
O3S0.0255 (11)0.0328 (13)0.0287 (12)−0.0039 (10)0.0108 (9)−0.0011 (10)
O3W0.0318 (12)0.0215 (11)0.0229 (11)0.0059 (9)0.0079 (9)−0.0016 (9)
O30.0171 (9)0.0179 (10)0.0167 (9)0.0000 (7)0.0071 (7)0.0005 (7)
O40.0180 (9)0.0177 (10)0.0166 (9)−0.0012 (8)0.0065 (8)−0.0014 (7)
O50.0187 (9)0.0171 (10)0.0189 (10)−0.0007 (8)0.0081 (8)−0.0004 (8)
O60.0195 (9)0.0170 (10)0.0194 (10)−0.0011 (8)0.0082 (8)−0.0016 (8)
O70.0209 (10)0.0198 (10)0.0192 (10)0.0004 (8)0.0094 (8)0.0019 (8)
O80.0210 (10)0.0186 (10)0.0189 (10)−0.0007 (8)0.0094 (8)−0.0006 (8)
O90.0196 (10)0.0208 (10)0.0213 (10)−0.0005 (8)0.0098 (8)−0.0005 (8)
O100.0198 (9)0.0171 (10)0.0199 (10)−0.0007 (8)0.0069 (8)0.0013 (8)
O110.0185 (9)0.0182 (10)0.0212 (10)−0.0013 (8)0.0085 (8)−0.0008 (8)
O120.0199 (10)0.0180 (10)0.0210 (10)−0.0013 (8)0.0079 (8)−0.0008 (8)
O130.0185 (9)0.0193 (10)0.0188 (10)−0.0014 (8)0.0081 (8)−0.0003 (8)
O140.0217 (10)0.0181 (10)0.0210 (10)−0.0009 (8)0.0104 (8)−0.0010 (8)
O150.0207 (10)0.0185 (10)0.0194 (10)0.0016 (8)0.0080 (8)0.0021 (8)
O160.0213 (10)0.0202 (10)0.0199 (10)0.0010 (8)0.0106 (8)0.0006 (8)
O170.0168 (9)0.0214 (10)0.0186 (10)−0.0004 (8)0.0065 (8)0.0029 (8)
O180.0163 (9)0.0206 (10)0.0176 (9)−0.0014 (8)0.0051 (8)0.0005 (8)
O190.0188 (9)0.0197 (10)0.0180 (9)−0.0020 (8)0.0076 (8)0.0005 (8)
O200.0181 (9)0.0194 (10)0.0208 (10)0.0006 (8)0.0088 (8)0.0010 (8)
O210.0184 (9)0.0199 (10)0.0226 (10)0.0001 (8)0.0085 (8)−0.0006 (8)
O220.0191 (9)0.0209 (10)0.0199 (10)0.0008 (8)0.0090 (8)−0.0002 (8)
O230.0217 (10)0.0177 (10)0.0210 (10)0.0001 (8)0.0091 (8)0.0006 (8)
O240.0217 (10)0.0178 (10)0.0205 (10)−0.0007 (8)0.0097 (8)−0.0023 (8)
O250.0187 (9)0.0200 (10)0.0197 (10)−0.0009 (8)0.0057 (8)0.0004 (8)
O260.0194 (10)0.0198 (10)0.0193 (10)−0.0005 (8)0.0073 (8)0.0003 (8)
O270.0203 (10)0.0196 (10)0.0212 (10)−0.0029 (8)0.0073 (8)−0.0024 (8)
O280.0207 (10)0.0187 (10)0.0190 (10)−0.0011 (8)0.0075 (8)−0.0013 (8)
O290.0244 (10)0.0248 (11)0.0183 (10)−0.0006 (9)0.0075 (8)−0.0020 (8)
O300.0213 (10)0.0219 (11)0.0282 (11)0.0025 (8)0.0115 (9)−0.0019 (9)
O310.0256 (11)0.0216 (11)0.0269 (11)−0.0005 (8)0.0157 (9)0.0024 (8)
O320.0183 (10)0.0225 (11)0.0211 (10)−0.0040 (8)0.0059 (8)−0.0004 (8)
O330.0217 (10)0.0218 (11)0.0221 (10)0.0018 (8)0.0085 (8)0.0024 (8)
O340.0219 (10)0.0189 (10)0.0229 (11)−0.0001 (8)0.0077 (8)0.0033 (8)
O350.0298 (11)0.0168 (10)0.0279 (11)0.0022 (8)0.0149 (9)0.0029 (8)
O360.0190 (10)0.0212 (11)0.0265 (11)−0.0005 (8)0.0062 (9)−0.0001 (8)
O370.0242 (11)0.0232 (11)0.0277 (11)−0.0046 (9)0.0109 (9)−0.0001 (9)
O380.0259 (11)0.0267 (11)0.0191 (10)−0.0017 (9)0.0109 (9)0.0017 (8)
O390.0253 (11)0.0231 (11)0.0233 (11)0.0012 (9)0.0118 (9)−0.0018 (8)
O400.0227 (10)0.0235 (11)0.0187 (10)−0.0033 (8)0.0073 (8)−0.0034 (8)
N1S0.0259 (13)0.0211 (12)0.0238 (13)0.0005 (10)0.0127 (10)0.0000 (10)
N2S0.0269 (14)0.0486 (19)0.0234 (14)−0.0049 (13)0.0114 (11)0.0059 (13)
N3S0.0269 (13)0.0286 (14)0.0244 (13)−0.0044 (11)0.0101 (11)−0.0024 (11)
C1S0.0325 (17)0.043 (2)0.0225 (16)−0.0023 (15)0.0119 (13)−0.0041 (14)
C2S0.0230 (14)0.0254 (15)0.0270 (16)0.0038 (12)0.0111 (12)0.0035 (12)
C3S0.0207 (14)0.0240 (15)0.0280 (16)0.0030 (11)0.0088 (12)−0.0005 (12)
C4S0.042 (2)0.0353 (19)0.0350 (19)0.0091 (16)0.0193 (16)−0.0045 (15)
C5S0.043 (2)0.054 (3)0.0225 (17)−0.0019 (18)0.0113 (15)−0.0006 (16)
C6S0.0352 (19)0.056 (2)0.0312 (18)−0.0004 (17)0.0205 (16)0.0061 (17)
C7S0.036 (2)0.052 (2)0.040 (2)0.0060 (18)0.0195 (17)0.0121 (18)
C8S0.0264 (15)0.0236 (16)0.0283 (16)−0.0030 (12)0.0065 (13)−0.0038 (12)
C9S0.0253 (15)0.0278 (16)0.0241 (15)−0.0052 (12)0.0078 (12)−0.0017 (12)
Geometric parameters (Å, º) top
Mo1—O291.686 (2)Mo11—O231.857 (2)
Mo1—O71.833 (2)Mo11—O201.996 (2)
Mo1—O81.847 (2)Mo11—O222.033 (2)
Mo1—O61.988 (2)Mo11—O32.432 (2)
Mo1—O51.996 (2)Mo12—O401.686 (2)
Mo1—O12.449 (2)Mo12—O261.826 (2)
Mo2—O301.682 (2)Mo12—O251.830 (2)
Mo2—O111.822 (2)Mo12—O272.000 (2)
Mo2—O61.831 (2)Mo12—O282.023 (2)
Mo2—O122.000 (2)Mo12—O42.420 (2)
Mo2—O92.034 (2)P1—O11.534 (2)
Mo2—O12.451 (2)P1—O41.535 (2)
Mo3—O311.693 (2)P1—O21.537 (2)
Mo3—O141.810 (2)P1—O31.539 (2)
Mo3—O91.840 (2)O1S—C2S1.417 (4)
Mo3—O162.003 (2)O1S—C1S1.421 (4)
Mo3—O82.020 (2)O1W—H1WA0.7499
Mo3—O12.406 (2)O1W—H1WB0.8499
Mo4—O321.679 (2)O2W—H2WB0.8334
Mo4—O51.822 (2)O2W—H2WA0.8998
Mo4—O101.847 (2)O2S—C4S1.420 (5)
Mo4—O192.006 (2)O2S—C5S1.421 (4)
Mo4—O132.013 (2)O3S—C7S1.430 (5)
Mo4—O22.427 (2)O3S—C8S1.437 (4)
Mo5—O331.687 (2)O3W—H3WA0.8844
Mo5—O131.814 (2)O3W—H3WB0.8416
Mo5—O221.845 (2)N1S—C3S1.493 (4)
Mo5—O72.007 (2)N1S—H1NA0.9100
Mo5—O152.021 (2)N1S—H1NB0.9100
Mo5—O32.435 (2)N1S—H1NC0.9100
Mo6—O341.695 (2)N2S—C6S1.488 (5)
Mo6—O181.810 (2)N2S—H2NA0.9100
Mo6—O171.830 (2)N2S—H2NB0.9100
Mo6—O112.009 (2)N2S—H2NC0.9100
Mo6—O102.027 (2)N3S—C9S1.488 (4)
Mo6—O22.425 (2)N3S—H3NA0.9100
Mo7—O351.679 (2)N3S—H3NB0.9100
Mo7—O161.818 (2)N3S—H3NC0.9100
Mo7—O151.855 (2)C1S—H1SA0.9800
Mo7—O241.990 (2)C1S—H1SB0.9800
Mo7—O232.009 (2)C1S—H1SC0.9800
Mo7—O32.427 (2)C2S—C3S1.510 (5)
Mo8—O361.677 (2)C2S—H2SA0.9900
Mo8—O121.823 (2)C2S—H2SB0.9900
Mo8—O211.841 (2)C3S—H3SA0.9900
Mo8—O182.011 (2)C3S—H3SB0.9900
Mo8—O252.020 (2)C4S—H4SA0.9800
Mo8—O42.432 (2)C4S—H4SB0.9800
Mo9—O371.685 (2)C4S—H4SC0.9800
Mo9—O241.826 (2)C5S—C6S1.497 (6)
Mo9—O271.834 (2)C5S—H5SA0.9900
Mo9—O212.008 (2)C5S—H5SB0.9900
Mo9—O142.026 (2)C6S—H6SA0.9900
Mo9—O42.449 (2)C6S—H6SB0.9900
Mo10—O381.684 (2)C7S—H7SA0.9800
Mo10—O201.828 (2)C7S—H7SB0.9800
Mo10—O191.841 (2)C7S—H7SC0.9800
Mo10—O262.005 (2)C8S—C9S1.498 (5)
Mo10—O172.007 (2)C8S—H8SA0.9900
Mo10—O22.453 (2)C8S—H8SB0.9900
Mo11—O391.682 (2)C9S—H9SA0.9900
Mo11—O281.808 (2)C9S—H9SB0.9900
O29—Mo1—O7104.01 (10)O39—Mo11—O2298.35 (10)
O29—Mo1—O8101.25 (10)O28—Mo11—O22154.40 (9)
O7—Mo1—O896.84 (9)O23—Mo11—O2285.63 (9)
O29—Mo1—O699.71 (10)O20—Mo11—O2279.95 (8)
O7—Mo1—O6154.74 (9)O39—Mo11—O3168.89 (9)
O8—Mo1—O686.82 (9)O28—Mo11—O385.89 (8)
O29—Mo1—O5103.06 (10)O23—Mo11—O374.60 (8)
O7—Mo1—O585.00 (9)O20—Mo11—O380.51 (8)
O8—Mo1—O5154.40 (9)O22—Mo11—O371.02 (7)
O6—Mo1—O581.30 (8)O40—Mo12—O26102.94 (10)
O29—Mo1—O1169.06 (9)O40—Mo12—O25101.61 (10)
O7—Mo1—O186.18 (8)O26—Mo12—O2598.40 (9)
O8—Mo1—O173.17 (8)O40—Mo12—O2799.65 (10)
O6—Mo1—O170.92 (7)O26—Mo12—O27154.86 (9)
O5—Mo1—O181.51 (7)O25—Mo12—O2787.64 (9)
O30—Mo2—O11104.59 (10)O40—Mo12—O28102.65 (10)
O30—Mo2—O6103.53 (10)O26—Mo12—O2883.90 (9)
O11—Mo2—O698.15 (9)O25—Mo12—O28154.44 (9)
O30—Mo2—O12101.41 (10)O27—Mo12—O2880.50 (8)
O11—Mo2—O1285.81 (9)O40—Mo12—O4170.84 (9)
O6—Mo2—O12152.80 (9)O26—Mo12—O485.92 (8)
O30—Mo2—O998.09 (10)O25—Mo12—O474.46 (8)
O11—Mo2—O9155.42 (9)O27—Mo12—O472.14 (8)
O6—Mo2—O985.47 (9)O28—Mo12—O480.35 (8)
O12—Mo2—O980.45 (8)O1—P1—O4109.46 (11)
O30—Mo2—O1168.59 (9)O1—P1—O2109.20 (11)
O11—Mo2—O186.77 (8)O4—P1—O2109.50 (11)
O6—Mo2—O173.20 (8)O1—P1—O3109.56 (11)
O12—Mo2—O180.22 (8)O4—P1—O3109.66 (11)
O9—Mo2—O170.93 (8)O2—P1—O3109.44 (11)
O31—Mo3—O14104.55 (10)C2S—O1S—C1S111.1 (3)
O31—Mo3—O9102.01 (10)H1WA—O1W—H1WB94.4
O14—Mo3—O998.86 (9)P1—O1—Mo3126.16 (11)
O31—Mo3—O16100.74 (10)P1—O1—Mo1125.48 (11)
O14—Mo3—O1685.53 (9)Mo3—O1—Mo190.01 (7)
O9—Mo3—O16154.89 (9)P1—O1—Mo2125.31 (11)
O31—Mo3—O898.20 (10)Mo3—O1—Mo289.72 (7)
O14—Mo3—O8155.00 (9)Mo1—O1—Mo288.60 (7)
O9—Mo3—O886.23 (9)P1—O2—Mo6125.93 (11)
O16—Mo3—O880.12 (8)P1—O2—Mo4126.59 (11)
O31—Mo3—O1169.32 (9)Mo6—O2—Mo489.60 (7)
O14—Mo3—O186.09 (8)P1—O2—Mo10124.67 (11)
O9—Mo3—O175.01 (8)Mo6—O2—Mo1089.29 (7)
O16—Mo3—O180.68 (8)Mo4—O2—Mo1089.09 (6)
O8—Mo3—O171.51 (8)H2WB—O2W—H2WA123.0
O32—Mo4—O5105.11 (10)C4S—O2S—C5S111.1 (3)
O32—Mo4—O10102.00 (10)C7S—O3S—C8S113.6 (3)
O5—Mo4—O1098.17 (9)H3WA—O3W—H3WB95.5
O32—Mo4—O1997.57 (9)P1—O3—Mo7125.21 (11)
O5—Mo4—O19154.78 (9)P1—O3—Mo11125.83 (11)
O10—Mo4—O1987.57 (9)Mo7—O3—Mo1189.20 (7)
O32—Mo4—O13101.14 (9)P1—O3—Mo5125.44 (11)
O5—Mo4—O1384.70 (9)Mo7—O3—Mo589.79 (7)
O10—Mo4—O13155.02 (9)Mo11—O3—Mo590.03 (7)
O19—Mo4—O1380.19 (8)P1—O4—Mo12126.44 (11)
O32—Mo4—O2168.64 (9)P1—O4—Mo8125.75 (11)
O5—Mo4—O286.18 (8)Mo12—O4—Mo889.40 (7)
O10—Mo4—O274.64 (8)P1—O4—Mo9125.73 (11)
O19—Mo4—O271.62 (7)Mo12—O4—Mo988.70 (6)
O13—Mo4—O280.85 (7)Mo8—O4—Mo988.86 (7)
O33—Mo5—O13104.03 (10)Mo4—O5—Mo1152.24 (12)
O33—Mo5—O22103.62 (10)Mo2—O6—Mo1127.27 (11)
O13—Mo5—O2298.57 (9)Mo1—O7—Mo5151.06 (12)
O33—Mo5—O799.53 (9)Mo1—O8—Mo3125.19 (11)
O13—Mo5—O785.16 (9)Mo3—O9—Mo2124.34 (11)
O22—Mo5—O7154.82 (9)Mo4—O10—Mo6123.83 (11)
O33—Mo5—O1598.38 (9)Mo2—O11—Mo6151.05 (12)
O13—Mo5—O15155.00 (9)Mo8—O12—Mo2151.53 (12)
O22—Mo5—O1586.63 (9)Mo5—O13—Mo4151.88 (12)
O7—Mo5—O1580.29 (9)Mo3—O14—Mo9152.28 (12)
O33—Mo5—O3169.49 (9)Mo7—O15—Mo5124.51 (11)
O13—Mo5—O386.47 (8)Mo7—O16—Mo3151.50 (12)
O22—Mo5—O373.85 (8)Mo6—O17—Mo10126.53 (11)
O7—Mo5—O381.59 (8)Mo6—O18—Mo8152.52 (12)
O15—Mo5—O371.42 (7)Mo10—O19—Mo4125.71 (11)
O34—Mo6—O18104.83 (10)Mo10—O20—Mo11151.44 (12)
O34—Mo6—O17102.49 (10)Mo8—O21—Mo9125.14 (11)
O18—Mo6—O1799.49 (9)Mo5—O22—Mo11125.09 (11)
O34—Mo6—O11101.12 (10)Mo11—O23—Mo7123.85 (11)
O18—Mo6—O1184.88 (9)Mo9—O24—Mo7154.04 (12)
O17—Mo6—O11153.95 (9)Mo12—O25—Mo8124.81 (11)
O34—Mo6—O1097.34 (9)Mo12—O26—Mo10152.86 (12)
O18—Mo6—O10155.24 (9)Mo9—O27—Mo12125.08 (11)
O17—Mo6—O1086.11 (9)Mo11—O28—Mo12152.48 (12)
O11—Mo6—O1080.11 (8)C3S—N1S—H1NA109.5
O34—Mo6—O2168.59 (9)C3S—N1S—H1NB109.5
O18—Mo6—O286.49 (8)H1NA—N1S—H1NB109.5
O17—Mo6—O273.75 (8)C3S—N1S—H1NC109.5
O11—Mo6—O280.96 (8)H1NA—N1S—H1NC109.5
O10—Mo6—O271.84 (7)H1NB—N1S—H1NC109.5
O35—Mo7—O16102.95 (10)C6S—N2S—H2NA109.5
O35—Mo7—O15103.01 (10)C6S—N2S—H2NB109.5
O16—Mo7—O1596.73 (9)H2NA—N2S—H2NB109.5
O35—Mo7—O24101.70 (10)C6S—N2S—H2NC109.5
O16—Mo7—O2485.09 (9)H2NA—N2S—H2NC109.5
O15—Mo7—O24154.13 (9)H2NB—N2S—H2NC109.5
O35—Mo7—O2398.99 (10)C9S—N3S—H3NA109.5
O16—Mo7—O23156.27 (9)C9S—N3S—H3NB109.5
O15—Mo7—O2386.99 (9)H3NA—N3S—H3NB109.5
O24—Mo7—O2381.67 (8)C9S—N3S—H3NC109.5
O35—Mo7—O3170.87 (9)H3NA—N3S—H3NC109.5
O16—Mo7—O386.08 (8)H3NB—N3S—H3NC109.5
O15—Mo7—O374.20 (8)O1S—C1S—H1SA109.5
O24—Mo7—O380.21 (8)O1S—C1S—H1SB109.5
O23—Mo7—O372.35 (8)H1SA—C1S—H1SB109.5
O36—Mo8—O12104.15 (10)O1S—C1S—H1SC109.5
O36—Mo8—O21101.92 (10)H1SA—C1S—H1SC109.5
O12—Mo8—O2198.86 (9)H1SB—C1S—H1SC109.5
O36—Mo8—O18101.87 (9)O1S—C2S—C3S107.7 (3)
O12—Mo8—O1885.04 (9)O1S—C2S—H2SA110.2
O21—Mo8—O18154.12 (9)C3S—C2S—H2SA110.2
O36—Mo8—O2598.71 (10)O1S—C2S—H2SB110.2
O12—Mo8—O25154.77 (9)C3S—C2S—H2SB110.2
O21—Mo8—O2586.58 (9)H2SA—C2S—H2SB108.5
O18—Mo8—O2579.89 (8)N1S—C3S—C2S110.5 (3)
O36—Mo8—O4169.30 (9)N1S—C3S—H3SA109.6
O12—Mo8—O486.43 (8)C2S—C3S—H3SA109.6
O21—Mo8—O474.47 (8)N1S—C3S—H3SB109.6
O18—Mo8—O480.30 (8)C2S—C3S—H3SB109.6
O25—Mo8—O471.21 (7)H3SA—C3S—H3SB108.1
O37—Mo9—O24103.97 (10)O2S—C4S—H4SA109.5
O37—Mo9—O27103.70 (10)O2S—C4S—H4SB109.5
O24—Mo9—O2798.31 (9)H4SA—C4S—H4SB109.5
O37—Mo9—O21100.27 (10)O2S—C4S—H4SC109.5
O24—Mo9—O21153.26 (9)H4SA—C4S—H4SC109.5
O27—Mo9—O2186.66 (9)H4SB—C4S—H4SC109.5
O37—Mo9—O14101.59 (10)O2S—C5S—C6S107.2 (3)
O24—Mo9—O1483.96 (9)O2S—C5S—H5SA110.3
O27—Mo9—O14153.20 (9)C6S—C5S—H5SA110.3
O21—Mo9—O1480.25 (8)O2S—C5S—H5SB110.3
O37—Mo9—O4171.45 (9)C6S—C5S—H5SB110.3
O24—Mo9—O484.55 (8)H5SA—C5S—H5SB108.5
O27—Mo9—O474.02 (8)N2S—C6S—C5S109.7 (3)
O21—Mo9—O471.51 (8)N2S—C6S—H6SA109.7
O14—Mo9—O479.66 (7)C5S—C6S—H6SA109.7
O38—Mo10—O20103.66 (10)N2S—C6S—H6SB109.7
O38—Mo10—O19103.23 (10)C5S—C6S—H6SB109.7
O20—Mo10—O1998.02 (9)H6SA—C6S—H6SB108.2
O38—Mo10—O26101.40 (10)O3S—C7S—H7SA109.5
O20—Mo10—O2685.02 (9)O3S—C7S—H7SB109.5
O19—Mo10—O26153.67 (9)H7SA—C7S—H7SB109.5
O38—Mo10—O1799.94 (10)O3S—C7S—H7SC109.5
O20—Mo10—O17154.49 (9)H7SA—C7S—H7SC109.5
O19—Mo10—O1785.78 (9)H7SB—C7S—H7SC109.5
O26—Mo10—O1780.93 (8)O3S—C8S—C9S112.0 (3)
O38—Mo10—O2169.86 (9)O3S—C8S—H8SA109.2
O20—Mo10—O286.39 (8)C9S—C8S—H8SA109.2
O19—Mo10—O273.53 (8)O3S—C8S—H8SB109.2
O26—Mo10—O280.61 (8)C9S—C8S—H8SB109.2
O17—Mo10—O270.43 (7)H8SA—C8S—H8SB107.9
O39—Mo11—O28105.16 (10)N3S—C9S—C8S112.0 (3)
O39—Mo11—O23101.97 (10)N3S—C9S—H9SA109.2
O28—Mo11—O2399.07 (9)C8S—C9S—H9SA109.2
O39—Mo11—O20101.20 (10)N3S—C9S—H9SB109.2
O28—Mo11—O2085.61 (9)C8S—C9S—H9SB109.2
O23—Mo11—O20154.21 (9)H9SA—C9S—H9SB107.9
O4—P1—O1—Mo353.93 (16)O29—Mo1—O7—Mo5−132.4 (2)
O2—P1—O1—Mo3173.79 (12)O8—Mo1—O7—Mo5124.2 (2)
O3—P1—O1—Mo3−66.36 (15)O6—Mo1—O7—Mo527.1 (4)
O4—P1—O1—Mo1175.34 (12)O5—Mo1—O7—Mo5−30.2 (2)
O2—P1—O1—Mo1−64.80 (15)O1—Mo1—O7—Mo551.6 (2)
O3—P1—O1—Mo155.05 (16)O33—Mo5—O7—Mo1134.2 (2)
O4—P1—O1—Mo2−66.75 (15)O13—Mo5—O7—Mo130.8 (2)
O2—P1—O1—Mo253.11 (16)O22—Mo5—O7—Mo1−69.1 (4)
O3—P1—O1—Mo2172.96 (12)O15—Mo5—O7—Mo1−128.8 (3)
O31—Mo3—O1—P1149.9 (4)O3—Mo5—O7—Mo1−56.3 (2)
O14—Mo3—O1—P1−34.78 (14)O29—Mo1—O8—Mo3167.10 (13)
O9—Mo3—O1—P1−135.04 (15)O7—Mo1—O8—Mo3−87.09 (13)
O16—Mo3—O1—P151.33 (14)O6—Mo1—O8—Mo367.82 (13)
O8—Mo3—O1—P1133.95 (15)O5—Mo1—O8—Mo35.6 (3)
O31—Mo3—O1—Mo113.9 (5)O1—Mo1—O8—Mo3−3.21 (11)
O14—Mo3—O1—Mo1−170.75 (8)O31—Mo3—O8—Mo1−173.76 (13)
O9—Mo3—O1—Mo188.99 (8)O14—Mo3—O8—Mo130.8 (3)
O16—Mo3—O1—Mo1−84.65 (8)O9—Mo3—O8—Mo1−72.15 (14)
O8—Mo3—O1—Mo1−2.03 (7)O16—Mo3—O8—Mo186.68 (13)
O31—Mo3—O1—Mo2−74.7 (5)O1—Mo3—O8—Mo13.29 (11)
O14—Mo3—O1—Mo2100.65 (8)O31—Mo3—O9—Mo2168.88 (13)
O9—Mo3—O1—Mo20.39 (7)O14—Mo3—O9—Mo2−84.07 (13)
O16—Mo3—O1—Mo2−173.25 (8)O16—Mo3—O9—Mo214.4 (3)
O8—Mo3—O1—Mo2−90.63 (8)O8—Mo3—O9—Mo271.29 (13)
O29—Mo1—O1—P1165.2 (4)O1—Mo3—O9—Mo2−0.57 (11)
O7—Mo1—O1—P1−35.90 (14)O30—Mo2—O9—Mo3−176.26 (13)
O8—Mo1—O1—P1−134.24 (16)O11—Mo2—O9—Mo326.5 (3)
O6—Mo1—O1—P1133.28 (15)O6—Mo2—O9—Mo3−73.21 (13)
O5—Mo1—O1—P149.60 (14)O12—Mo2—O9—Mo383.44 (13)
O29—Mo1—O1—Mo3−58.4 (5)O1—Mo2—O9—Mo30.57 (11)
O7—Mo1—O1—Mo3100.54 (8)O32—Mo4—O10—Mo6166.04 (13)
O8—Mo1—O1—Mo32.20 (8)O5—Mo4—O10—Mo6−86.52 (13)
O6—Mo1—O1—Mo3−90.28 (8)O19—Mo4—O10—Mo668.81 (13)
O5—Mo1—O1—Mo3−173.96 (8)O13—Mo4—O10—Mo68.5 (3)
O29—Mo1—O1—Mo231.4 (5)O2—Mo4—O10—Mo6−2.80 (11)
O7—Mo1—O1—Mo2−169.74 (8)O34—Mo6—O10—Mo4−173.43 (13)
O8—Mo1—O1—Mo291.92 (8)O18—Mo6—O10—Mo433.0 (3)
O6—Mo1—O1—Mo2−0.56 (7)O17—Mo6—O10—Mo4−71.32 (13)
O5—Mo1—O1—Mo2−84.24 (7)O11—Mo6—O10—Mo486.49 (13)
O30—Mo2—O1—P1151.7 (4)O2—Mo6—O10—Mo42.84 (11)
O11—Mo2—O1—P1−33.84 (14)O30—Mo2—O11—Mo6−130.3 (2)
O6—Mo2—O1—P1−133.36 (15)O6—Mo2—O11—Mo6123.3 (2)
O12—Mo2—O1—P152.46 (14)O12—Mo2—O11—Mo6−29.6 (2)
O9—Mo2—O1—P1135.66 (15)O9—Mo2—O11—Mo626.4 (4)
O30—Mo2—O1—Mo315.7 (5)O1—Mo2—O11—Mo650.8 (2)
O11—Mo2—O1—Mo3−169.86 (8)O34—Mo6—O11—Mo2134.8 (2)
O6—Mo2—O1—Mo390.62 (8)O18—Mo6—O11—Mo230.7 (2)
O12—Mo2—O1—Mo3−83.56 (8)O17—Mo6—O11—Mo2−70.5 (3)
O9—Mo2—O1—Mo3−0.36 (7)O10—Mo6—O11—Mo2−129.5 (3)
O30—Mo2—O1—Mo1−74.3 (5)O2—Mo6—O11—Mo2−56.6 (2)
O11—Mo2—O1—Mo1100.12 (8)O36—Mo8—O12—Mo2−128.3 (2)
O6—Mo2—O1—Mo10.60 (7)O21—Mo8—O12—Mo2126.9 (2)
O12—Mo2—O1—Mo1−173.57 (8)O18—Mo8—O12—Mo2−27.3 (2)
O9—Mo2—O1—Mo1−90.38 (8)O25—Mo8—O12—Mo226.0 (4)
O1—P1—O2—Mo6−67.43 (15)O4—Mo8—O12—Mo253.3 (2)
O4—P1—O2—Mo652.41 (16)O30—Mo2—O12—Mo8132.5 (3)
O3—P1—O2—Mo6172.64 (12)O11—Mo2—O12—Mo828.4 (3)
O1—P1—O2—Mo454.39 (16)O6—Mo2—O12—Mo8−71.3 (3)
O4—P1—O2—Mo4174.23 (12)O9—Mo2—O12—Mo8−131.1 (3)
O3—P1—O2—Mo4−65.54 (16)O1—Mo2—O12—Mo8−59.0 (2)
O1—P1—O2—Mo10173.70 (11)O33—Mo5—O13—Mo4−128.7 (2)
O4—P1—O2—Mo10−66.46 (15)O22—Mo5—O13—Mo4124.8 (2)
O3—P1—O2—Mo1053.77 (15)O7—Mo5—O13—Mo4−30.1 (2)
O34—Mo6—O2—P1154.2 (4)O15—Mo5—O13—Mo424.3 (4)
O18—Mo6—O2—P1−32.65 (14)O3—Mo5—O13—Mo451.7 (2)
O17—Mo6—O2—P1−133.60 (15)O32—Mo4—O13—Mo5135.1 (2)
O11—Mo6—O2—P152.71 (14)O5—Mo4—O13—Mo530.7 (2)
O10—Mo6—O2—P1135.19 (15)O10—Mo4—O13—Mo5−67.2 (4)
O34—Mo6—O2—Mo417.2 (5)O19—Mo4—O13—Mo5−129.0 (3)
O18—Mo6—O2—Mo4−169.64 (8)O2—Mo4—O13—Mo5−56.2 (2)
O17—Mo6—O2—Mo489.42 (8)O31—Mo3—O14—Mo9−127.3 (3)
O11—Mo6—O2—Mo4−84.27 (7)O9—Mo3—O14—Mo9127.7 (3)
O10—Mo6—O2—Mo4−1.80 (7)O16—Mo3—O14—Mo9−27.4 (3)
O34—Mo6—O2—Mo10−71.9 (5)O8—Mo3—O14—Mo927.6 (4)
O18—Mo6—O2—Mo10101.27 (8)O1—Mo3—O14—Mo953.6 (3)
O17—Mo6—O2—Mo100.32 (7)O37—Mo9—O14—Mo3130.0 (3)
O11—Mo6—O2—Mo10−173.37 (8)O24—Mo9—O14—Mo327.0 (3)
O10—Mo6—O2—Mo10−90.89 (8)O27—Mo9—O14—Mo3−69.5 (3)
O32—Mo4—O2—P1151.3 (4)O21—Mo9—O14—Mo3−131.4 (3)
O5—Mo4—O2—P1−35.03 (14)O4—Mo9—O14—Mo3−58.6 (3)
O10—Mo4—O2—P1−134.58 (16)O35—Mo7—O15—Mo5168.30 (13)
O19—Mo4—O2—P1132.84 (15)O16—Mo7—O15—Mo5−86.70 (14)
O13—Mo4—O2—P150.22 (14)O24—Mo7—O15—Mo55.9 (3)
O32—Mo4—O2—Mo6−72.2 (5)O23—Mo7—O15—Mo569.77 (13)
O5—Mo4—O2—Mo6101.50 (8)O3—Mo7—O15—Mo5−2.73 (11)
O10—Mo4—O2—Mo61.94 (8)O33—Mo5—O15—Mo7−174.61 (13)
O19—Mo4—O2—Mo6−90.63 (8)O13—Mo5—O15—Mo731.8 (3)
O13—Mo4—O2—Mo6−173.26 (8)O22—Mo5—O15—Mo7−71.32 (14)
O32—Mo4—O2—Mo1017.1 (5)O7—Mo5—O15—Mo787.07 (13)
O5—Mo4—O2—Mo10−169.20 (8)O3—Mo5—O15—Mo72.76 (11)
O10—Mo4—O2—Mo1091.24 (8)O35—Mo7—O16—Mo3−128.1 (3)
O19—Mo4—O2—Mo10−1.33 (7)O15—Mo7—O16—Mo3126.8 (3)
O13—Mo4—O2—Mo10−83.96 (7)O24—Mo7—O16—Mo3−27.2 (2)
O38—Mo10—O2—P1153.2 (5)O23—Mo7—O16—Mo329.0 (4)
O20—Mo10—O2—P1−34.65 (14)O3—Mo7—O16—Mo353.3 (2)
O19—Mo10—O2—P1−134.12 (15)O31—Mo3—O16—Mo7132.5 (3)
O26—Mo10—O2—P150.90 (13)O14—Mo3—O16—Mo728.5 (3)
O17—Mo10—O2—P1134.53 (15)O9—Mo3—O16—Mo7−72.8 (4)
O38—Mo10—O2—Mo618.4 (5)O8—Mo3—O16—Mo7−130.9 (3)
O20—Mo10—O2—Mo6−169.48 (8)O1—Mo3—O16—Mo7−58.2 (2)
O19—Mo10—O2—Mo691.05 (8)O34—Mo6—O17—Mo10168.39 (13)
O26—Mo10—O2—Mo6−83.94 (8)O18—Mo6—O17—Mo10−83.98 (14)
O17—Mo10—O2—Mo6−0.30 (7)O11—Mo6—O17—Mo1013.8 (3)
O38—Mo10—O2—Mo4−71.2 (5)O10—Mo6—O17—Mo1071.72 (13)
O20—Mo10—O2—Mo4100.91 (8)O2—Mo6—O17—Mo10−0.49 (11)
O19—Mo10—O2—Mo41.44 (7)O38—Mo10—O17—Mo6−176.22 (13)
O26—Mo10—O2—Mo4−173.55 (8)O20—Mo10—O17—Mo626.3 (3)
O17—Mo10—O2—Mo4−89.91 (8)O19—Mo10—O17—Mo6−73.51 (14)
O1—P1—O3—Mo753.66 (16)O26—Mo10—O17—Mo683.69 (14)
O4—P1—O3—Mo7−66.51 (15)O2—Mo10—O17—Mo60.49 (11)
O2—P1—O3—Mo7173.36 (11)O34—Mo6—O18—Mo8−130.5 (3)
O1—P1—O3—Mo11172.90 (12)O17—Mo6—O18—Mo8123.8 (3)
O4—P1—O3—Mo1152.74 (16)O11—Mo6—O18—Mo8−30.3 (3)
O2—P1—O3—Mo11−67.39 (15)O10—Mo6—O18—Mo822.3 (4)
O1—P1—O3—Mo5−66.13 (15)O2—Mo6—O18—Mo850.9 (3)
O4—P1—O3—Mo5173.71 (12)O36—Mo8—O18—Mo6133.8 (3)
O2—P1—O3—Mo553.58 (16)O12—Mo8—O18—Mo630.4 (3)
O16—Mo7—O3—P1−34.99 (14)O21—Mo8—O18—Mo6−69.7 (4)
O15—Mo7—O3—P1−133.13 (15)O25—Mo8—O18—Mo6−129.3 (3)
O24—Mo7—O3—P150.70 (14)O4—Mo8—O18—Mo6−56.8 (3)
O23—Mo7—O3—P1134.99 (15)O38—Mo10—O19—Mo4167.91 (13)
O16—Mo7—O3—Mo11−169.97 (8)O20—Mo10—O19—Mo4−85.94 (14)
O15—Mo7—O3—Mo1191.90 (8)O26—Mo10—O19—Mo49.1 (3)
O24—Mo7—O3—Mo11−84.28 (8)O17—Mo10—O19—Mo468.68 (13)
O23—Mo7—O3—Mo110.02 (7)O2—Mo10—O19—Mo4−2.14 (11)
O16—Mo7—O3—Mo5100.00 (8)O32—Mo4—O19—Mo10−174.21 (14)
O15—Mo7—O3—Mo51.87 (8)O5—Mo4—O19—Mo1031.7 (3)
O24—Mo7—O3—Mo5−174.31 (8)O10—Mo4—O19—Mo10−72.42 (14)
O23—Mo7—O3—Mo5−90.01 (8)O13—Mo4—O19—Mo1085.72 (13)
O39—Mo11—O3—P1152.1 (4)O2—Mo4—O19—Mo102.19 (11)
O28—Mo11—O3—P1−33.96 (14)O38—Mo10—O20—Mo11−128.0 (2)
O23—Mo11—O3—P1−134.54 (15)O19—Mo10—O20—Mo11126.2 (2)
O20—Mo11—O3—P152.26 (14)O26—Mo10—O20—Mo11−27.5 (2)
O22—Mo11—O3—P1134.82 (15)O17—Mo10—O20—Mo1129.2 (4)
O39—Mo11—O3—Mo7−73.4 (5)O2—Mo10—O20—Mo1153.4 (2)
O28—Mo11—O3—Mo7100.56 (8)O39—Mo11—O20—Mo10132.5 (2)
O23—Mo11—O3—Mo7−0.02 (7)O28—Mo11—O20—Mo1027.9 (2)
O20—Mo11—O3—Mo7−173.21 (8)O23—Mo11—O20—Mo10−73.8 (3)
O22—Mo11—O3—Mo7−90.66 (8)O22—Mo11—O20—Mo10−130.8 (3)
O39—Mo11—O3—Mo516.4 (5)O3—Mo11—O20—Mo10−58.6 (2)
O28—Mo11—O3—Mo5−169.65 (8)O36—Mo8—O21—Mo9168.30 (13)
O23—Mo11—O3—Mo589.77 (8)O12—Mo8—O21—Mo9−85.09 (14)
O20—Mo11—O3—Mo5−83.42 (8)O18—Mo8—O21—Mo911.8 (3)
O22—Mo11—O3—Mo5−0.87 (7)O25—Mo8—O21—Mo970.12 (13)
O33—Mo5—O3—P1147.5 (4)O4—Mo8—O21—Mo9−1.33 (11)
O13—Mo5—O3—P1−35.04 (14)O37—Mo9—O21—Mo8−176.25 (14)
O22—Mo5—O3—P1−135.02 (15)O24—Mo9—O21—Mo828.9 (3)
O7—Mo5—O3—P150.58 (14)O27—Mo9—O21—Mo8−72.92 (14)
O15—Mo5—O3—P1133.10 (15)O14—Mo9—O21—Mo883.60 (14)
O33—Mo5—O3—Mo712.7 (5)O4—Mo9—O21—Mo81.34 (11)
O13—Mo5—O3—Mo7−169.88 (8)O33—Mo5—O22—Mo11168.07 (13)
O22—Mo5—O3—Mo790.14 (8)O13—Mo5—O22—Mo11−85.14 (14)
O7—Mo5—O3—Mo7−84.26 (8)O7—Mo5—O22—Mo1111.7 (3)
O15—Mo5—O3—Mo7−1.74 (7)O15—Mo5—O22—Mo1170.25 (13)
O33—Mo5—O3—Mo11−76.5 (5)O3—Mo5—O22—Mo11−1.37 (11)
O13—Mo5—O3—Mo11100.92 (8)O39—Mo11—O22—Mo5−175.29 (14)
O22—Mo5—O3—Mo110.94 (8)O28—Mo11—O22—Mo528.1 (3)
O7—Mo5—O3—Mo11−173.46 (8)O23—Mo11—O22—Mo5−73.81 (14)
O15—Mo5—O3—Mo11−90.94 (8)O20—Mo11—O22—Mo584.73 (13)
O1—P1—O4—Mo12174.12 (12)O3—Mo11—O22—Mo51.40 (11)
O2—P1—O4—Mo1254.44 (16)O39—Mo11—O23—Mo7169.15 (13)
O3—P1—O4—Mo12−65.66 (16)O28—Mo11—O23—Mo7−83.13 (13)
O1—P1—O4—Mo853.07 (16)O20—Mo11—O23—Mo715.6 (3)
O2—P1—O4—Mo8−66.61 (16)O22—Mo11—O23—Mo771.52 (13)
O3—P1—O4—Mo8173.30 (12)O3—Mo11—O23—Mo70.03 (11)
O1—P1—O4—Mo9−66.12 (16)O35—Mo7—O23—Mo11−177.09 (13)
O2—P1—O4—Mo9174.20 (12)O16—Mo7—O23—Mo1125.5 (3)
O3—P1—O4—Mo954.11 (16)O15—Mo7—O23—Mo11−74.39 (13)
O26—Mo12—O4—P1−33.80 (15)O24—Mo7—O23—Mo1182.29 (13)
O25—Mo12—O4—P1−133.70 (16)O3—Mo7—O23—Mo11−0.03 (11)
O27—Mo12—O4—P1133.73 (16)O37—Mo9—O24—Mo7−126.3 (3)
O28—Mo12—O4—P150.69 (14)O27—Mo9—O24—Mo7127.3 (3)
O26—Mo12—O4—Mo8102.14 (8)O21—Mo9—O24—Mo728.1 (4)
O25—Mo12—O4—Mo82.24 (8)O14—Mo9—O24—Mo7−25.8 (3)
O27—Mo12—O4—Mo8−90.32 (8)O4—Mo9—O24—Mo754.3 (3)
O28—Mo12—O4—Mo8−173.36 (8)O35—Mo7—O24—Mo9129.2 (3)
O26—Mo12—O4—Mo9−168.99 (8)O16—Mo7—O24—Mo926.9 (3)
O25—Mo12—O4—Mo991.12 (8)O15—Mo7—O24—Mo9−68.4 (4)
O27—Mo12—O4—Mo9−1.45 (7)O23—Mo7—O24—Mo9−133.3 (3)
O28—Mo12—O4—Mo9−84.49 (8)O3—Mo7—O24—Mo9−59.9 (3)
O36—Mo8—O4—P1154.5 (4)O40—Mo12—O25—Mo8168.20 (13)
O12—Mo8—O4—P1−33.75 (14)O26—Mo12—O25—Mo8−86.65 (14)
O21—Mo8—O4—P1−133.97 (16)O27—Mo12—O25—Mo868.83 (13)
O18—Mo8—O4—P151.82 (14)O28—Mo12—O25—Mo86.8 (3)
O25—Mo8—O4—P1134.36 (16)O4—Mo12—O25—Mo8−3.29 (11)
O36—Mo8—O4—Mo1218.1 (5)O36—Mo8—O25—Mo12−172.97 (13)
O12—Mo8—O4—Mo12−170.17 (8)O12—Mo8—O25—Mo1232.2 (3)
O21—Mo8—O4—Mo1289.60 (8)O21—Mo8—O25—Mo12−71.42 (14)
O18—Mo8—O4—Mo12−84.61 (8)O18—Mo8—O25—Mo1286.42 (13)
O25—Mo8—O4—Mo12−2.07 (7)O4—Mo8—O25—Mo123.33 (11)
O36—Mo8—O4—Mo9−70.7 (5)O40—Mo12—O26—Mo10−131.5 (3)
O12—Mo8—O4—Mo9101.11 (8)O25—Mo12—O26—Mo10124.5 (3)
O21—Mo8—O4—Mo90.89 (8)O27—Mo12—O26—Mo1021.9 (4)
O18—Mo8—O4—Mo9−173.32 (8)O28—Mo12—O26—Mo10−29.9 (3)
O25—Mo8—O4—Mo9−90.78 (8)O4—Mo12—O26—Mo1050.8 (3)
O24—Mo9—O4—P1−33.86 (14)O38—Mo10—O26—Mo12133.6 (3)
O27—Mo9—O4—P1−134.13 (16)O20—Mo10—O26—Mo1230.7 (3)
O21—Mo9—O4—P1134.05 (15)O19—Mo10—O26—Mo12−67.4 (4)
O14—Mo9—O4—P150.97 (14)O17—Mo10—O26—Mo12−128.0 (3)
O24—Mo9—O4—Mo12101.83 (8)O2—Mo10—O26—Mo12−56.5 (3)
O27—Mo9—O4—Mo121.56 (8)O37—Mo9—O27—Mo12169.17 (13)
O21—Mo9—O4—Mo12−90.26 (8)O24—Mo9—O27—Mo12−84.17 (14)
O14—Mo9—O4—Mo12−173.33 (8)O21—Mo9—O27—Mo1269.40 (13)
O24—Mo9—O4—Mo8−168.74 (8)O14—Mo9—O27—Mo128.9 (3)
O27—Mo9—O4—Mo890.99 (8)O4—Mo9—O27—Mo12−2.31 (11)
O21—Mo9—O4—Mo8−0.83 (7)O40—Mo12—O27—Mo9−173.45 (14)
O14—Mo9—O4—Mo8−83.91 (8)O26—Mo12—O27—Mo932.8 (3)
O32—Mo4—O5—Mo1−130.9 (2)O25—Mo12—O27—Mo9−72.06 (14)
O10—Mo4—O5—Mo1124.2 (2)O28—Mo12—O27—Mo985.21 (14)
O19—Mo4—O5—Mo122.4 (4)O4—Mo12—O27—Mo92.36 (11)
O13—Mo4—O5—Mo1−30.8 (2)O39—Mo11—O28—Mo12−128.7 (3)
O2—Mo4—O5—Mo150.4 (2)O23—Mo11—O28—Mo12126.2 (3)
O29—Mo1—O5—Mo4135.0 (2)O20—Mo11—O28—Mo12−28.3 (3)
O7—Mo1—O5—Mo431.8 (2)O22—Mo11—O28—Mo1227.3 (4)
O8—Mo1—O5—Mo4−63.6 (4)O3—Mo11—O28—Mo1252.5 (3)
O6—Mo1—O5—Mo4−126.9 (3)O40—Mo12—O28—Mo11131.1 (3)
O1—Mo1—O5—Mo4−55.1 (2)O26—Mo12—O28—Mo1129.2 (3)
O30—Mo2—O6—Mo1167.74 (13)O25—Mo12—O28—Mo11−67.5 (4)
O11—Mo2—O6—Mo1−85.03 (14)O27—Mo12—O28—Mo11−131.0 (3)
O12—Mo2—O6—Mo111.7 (3)O4—Mo12—O28—Mo11−57.7 (3)
O9—Mo2—O6—Mo170.50 (14)C1S—O1S—C2S—C3S177.2 (3)
O1—Mo2—O6—Mo1−0.93 (12)O1S—C2S—C3S—N1S50.8 (3)
O29—Mo1—O6—Mo2−173.21 (14)C4S—O2S—C5S—C6S−168.4 (3)
O7—Mo1—O6—Mo227.0 (3)O2S—C5S—C6S—N2S62.7 (4)
O8—Mo1—O6—Mo2−72.34 (14)C7S—O3S—C8S—C9S86.4 (4)
O5—Mo1—O6—Mo284.91 (14)O3S—C8S—C9S—N3S66.0 (4)
O1—Mo1—O6—Mo20.94 (12)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H1WA···O2W0.752.002.726 (5)161
O1W—H1WB···O31i0.852.142.936 (4)157
O2W—H2WB···O150.831.992.807 (3)167
O2W—H2WA···O22ii0.902.032.780 (3)140
O3W—H3WA···O40iii0.882.052.904 (3)162
O3W—H3WB···O10iv0.841.972.772 (3)159
N1S—H1NA···O3W0.911.932.812 (4)164
N1S—H1NB···O2Sv0.912.593.182 (4)123
N1S—H1NB···O9v0.912.242.949 (4)134
N1S—H1NC···O1S0.912.312.731 (4)108
N1S—H1NC···O31v0.912.483.110 (4)127
N1S—H1NC···O35ii0.912.282.887 (3)124
N2S—H2NA···O2S0.912.422.814 (5)106
N2S—H2NA···O80.911.942.811 (3)159
N2S—H2NB···O1W0.911.832.629 (5)145
N2S—H2NC···O3S0.911.932.798 (5)158
N3S—H3NA···O23ii0.912.313.110 (4)146
N3S—H3NB···O34iv0.912.082.955 (4)161
N3S—H3NC···O2W0.911.962.822 (4)158
Symmetry codes: (i) −x, −y+1, −z+1; (ii) −x+1, −y+1, −z+1; (iii) x+1, y, z+1; (iv) x+1/2, −y+3/2, z+1/2; (v) x+1, y, z.

Experimental details

Crystal data
Chemical formula(C3H10NO)3[PMo12O40]·3H2O
Mr2104.66
Crystal system, space groupMonoclinic, P21/n
Temperature (K)100
a, b, c (Å)12.7806 (2), 27.0489 (4), 14.6360 (2)
β (°) 114.876 (1)
V (Å3)4590.24 (12)
Z4
Radiation typeMo Kα
µ (mm−1)3.32
Crystal size (mm)0.10 × 0.05 × 0.03
Data collection
DiffractometerBruker SMART APEXII CCD area-detector
Absorption correctionMulti-scan
(SADABS; Bruker, 2005)
Tmin, Tmax0.820, 0.907
No. of measured, independent and
observed [I > 2/s(I)] reflections		100492, 12174, 10404
Rint0.042
(sin θ/λ)max (Å−1)0.682
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.022, 0.052, 1.00
No. of reflections12174
No. of parameters646
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å−3)0.66, −0.69

Computer programs: APEX2 (Bruker, 2005), SAINT (Bruker, 2005), SHELXTL (Sheldrick, 2008).

Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H1WA···O2W0.752.002.726 (5)161
O1W—H1WB···O31i0.852.142.936 (4)157
O2W—H2WB···O150.831.992.807 (3)167
O2W—H2WA···O22ii0.902.032.780 (3)140
O3W—H3WA···O40iii0.882.052.904 (3)162
O3W—H3WB···O10iv0.841.972.772 (3)159
N1S—H1NA···O3W0.911.932.812 (4)164
N1S—H1NB···O2Sv0.912.593.182 (4)123
N1S—H1NB···O9v0.912.242.949 (4)134
N1S—H1NC···O1S0.912.312.731 (4)108
N1S—H1NC···O31v0.912.483.110 (4)127
N1S—H1NC···O35ii0.912.282.887 (3)124
N2S—H2NA···O2S0.912.422.814 (5)106
N2S—H2NA···O80.911.942.811 (3)159
N2S—H2NB···O1W0.911.832.629 (5)145
N2S—H2NC···O3S0.911.932.798 (5)158
N3S—H3NA···O23ii0.912.313.110 (4)146
N3S—H3NB···O34iv0.912.082.955 (4)161
N3S—H3NC···O2W0.911.962.822 (4)158
Symmetry codes: (i) −x, −y+1, −z+1; (ii) −x+1, −y+1, −z+1; (iii) x+1, y, z+1; (iv) x+1/2, −y+3/2, z+1/2; (v) x+1, y, z.
 

Acknowledgements

Support of this investigation by the Islamic Azad University-North Tehran Branch is gratefully acknowledged.

References

First citationBruker (2005). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.  Google Scholar
 First citationGong, Y., Hu, C., Li, H., Tang, W., Huang, K. & Hou, W. (2006). J. Mol. Struct. 784, 228–238.  Web of Science CSD CrossRef CAS Google Scholar
 First citationHan, Z., Zhao, Y., Peng, J., Tian, A., Feng, Y. & Liu, Q. (2005). J. Solid State Chem. 178, 1386–1394.  Web of Science CSD CrossRef CAS Google Scholar
 First citationPourayoubi, M. & Mahjoub, A. R. (2007). Acta Cryst. E63, m2622–m2623.  Web of Science CSD CrossRef IUCr Journals Google Scholar
 First citationPourayoubi, M. & Mahjoub, A. R. (2010). J. Iran. Chem. Soc. Accepted.  Google Scholar
 First citationRaissi Shabari, A., Pourayoubi, M. & Ghamari, D. (2009). Acta Cryst. E65, m1586.  Web of Science CSD CrossRef IUCr Journals Google Scholar
 First citationSheldrick, G. M. (2008). Acta Cryst. A64, 112–122.  Web of Science CrossRef CAS IUCr Journals Google Scholar

This is an open-access article distributed under the terms of the Creative Commons Attribution (CC-BY) Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.

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ISSN: 2056-9890
Volume 66| Part 8| August 2010| Page m1000
https://doi.org/10.1107/S1600536810028801
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