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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 68| Part 7| July 2012| Pages m926-m927
https://doi.org/10.1107/S1600536812026323

Bis(tetra­butyl­ammonium) [2-(eth­­oxy­carbony)phenyl­imido]-μ6-oxido-dodeca-μ2-oxido-penta­oxidohexa­molybdenum di­ethyl ether hemisolvate

Manxiang Wang,a Shikai Tao,b Jing Guo,c Jian Haod and Qiang Lia*

aDepartment of Chemistry, College of Science of Beijing Forestry University, Beijing 100083, People's Republic of China, bBeijing Petroleum Machinery Factory, Beijing 100083, People's Republic of China, cLiangxi Science Experimental Class of Beijing Forestry University, Beijing 100083, People's Republic of China, and dDepartment of Chemistry, College of Science of Beijing University of Chemical Technology, Beijing 100029, People's Republic of China
*Correspondence e-mail: liqiang@bjfu.edu.cn

(Received 5 April 2012; accepted 11 June 2012; online 16 June 2012)

In the title complex, [(C4H9)4N]2[Mo6O18(C9H9NO2)]·0.5C4H10O, the aryl­imido ligand is linked to an Mo atom of the Lindqvist-type polyoxidometalate anion by an Mo≡N bond of 1.726 (4) Å. The Mo≡N—C angles are 160.7 (5) and 167.6(5)° because of disorder affecting the aryl group, and is typical for the imido monodentate behaviour described in analogous hybrids. Light components of the structure are extensively disordered. The aryl ester group is disordered over two positions with occupancies refined to 0.559 (3) and 0.441 (3). Both independent tetra­butyl­ammonium cations have butyl chains partially split over two sites, with occupancies as in the aryl group of the anion. Finally, the ether solvent mol­ecule is disordered around an inversion centre. In the crystal, cations and anions inter­act via C—H⋯O contacts, involving O atoms of the polyoxidometalate anion and the ester group of the aryl­imido ligand as acceptor groups.

Related literature

For general background to polyoxidometalates and the synthesis of their organoimido derivatives, see: Hill (1998[Hill, C. L. (1998). Chem. Rev. 98, 1-2.]); Li et al. (2011[Li, Q., Xiao, Z., Chen, L. & Zhang, J. (2011). Acta Cryst. E67, m1404-m1405.]); Du et al. (1992[Du, Y., Rheingold, A. L. & Maatta, E. A. (1992). J. Am. Chem. Soc. 114, 345-346.]); Mohs et al. (1995[Mohs, T. R., Yap, G. P. A., Rheingold, A. L. & Maatta, E. A. (1995). Inorg. Chem. 34, 9-10.]); Clegg et al. (1995[Clegg, W., Errington, R. J., Fraser, K. A., Holmes, S. A. & Schäfer, A. (1995). J. Chem. Soc. Chem. Commun. pp. 455-456.]); Wu et al. (2004[Wu, P.-F., Li, Q., Ge, N., Wei, Y.-G., Wang, Y., Wang, P. & Guo, H.-Y. (2004). Eur. J. Inorg. Chem. pp. 2819-2822.]). For structural features characteristic of these complexes, see: Karlin & Wigley (2007[Karlin, K. D. & Wigley, D. E. (2007). Prog. Inorg. Chem. 42, 239-482.]); Li et al. (2008[Li, Q., Wei, Y.-G., Guo, H.-Y. & Zhan, C.-G. (2008). Inorg. Chim. Acta, 361, 2305-2313.]).

[Scheme 1]

Experimental

Crystal data

  • (C16H36N)2[Mo6O18(C9H9NO2)]·0.5C4H10O

  • Mr = 1548.79

  • Monoclinic, P 21 /n

  • a = 16.3974 (16) Å

  • b = 17.0854 (8) Å

  • c = 21.687 (3) Å

  • β = 106.709 (16)°

  • V = 5819.1 (10) Å3

  • Z = 4

  • Mo Kα radiation

  • μ = 1.33 mm−1

  • T = 101 K

  • 0.40 × 0.30 × 0.25 mm
Data collection

  • Agilent Xcalibur Eos Gemini diffractometer

  • Absorption correction: multi-scan (CrysAlis PRO; Agilent, 2011[Agilent (2011). CrysAlis PRO. Agilent Technologies, Yarnton, England.]) Tmin = 0.619, Tmax = 0.733

  • 31709 measured reflections

  • 11422 independent reflections

  • 8774 reflections with I > 2σ(I)

  • Rint = 0.038
Refinement

  • R[F2 > 2σ(F2)] = 0.039

  • wR(F2) = 0.088

  • S = 1.05

  • 11422 reflections

  • 854 parameters

  • 500 restraints

  • H-atom parameters constrained

  • Δρmax = 1.46 e Å−3

  • Δρmin = −0.81 e Å−3

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A D⋯A D—H⋯A
C3A—H3A⋯O19i 0.93 2.38 3.287 (9) 164
C5—H5⋯O7ii 0.93 2.58 3.449 (14) 155
C21—H21B⋯O15i 0.97 2.43 3.354 (5) 159
C25—H25A⋯O6iii 0.97 2.58 3.544 (5) 173
C41—H41B⋯O14 0.97 2.56 3.480 (6) 158
C44—H44B⋯O8i 0.96 2.57 3.495 (8) 162
C45—H45A⋯O1Aii 0.97 2.45 3.345 (8) 153
C45—H45A⋯O1ii 0.97 2.22 3.103 (9) 151
Symmetry codes: (i) [x-{\script{1\over 2}}, -y+{\script{3\over 2}}, z-{\script{1\over 2}}]; (ii) -x, -y+1, -z+1; (iii) -x, -y+2, -z+1.

Data collection: CrysAlis PRO (Agilent, 2011[Agilent (2011). CrysAlis PRO. Agilent Technologies, Yarnton, England.]); cell refinement: CrysAlis PRO; data reduction: CrysAlis PRO; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: DIAMOND (Brandenburg, 2010[Brandenburg, K. (2010). DIAMOND. Crystal Impact GbR, Bonn, Germany.]); software used to prepare material for publication: publCIF (Westrip, 2010[Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.]).

Supporting information

Crystal structure: contains datablocks I, global. DOI: https://doi.org/10.1107/S1600536812026323/bh2428sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536812026323/bh2428Isup2.hkl

checkCIF report


Comment top

Polyoxometalates and their organoimido derivatives have gained interest owing to their important optical, electronic, magnetic, catalytic, medical, remarkable self-assembly properties and chemical reactivity (Hill, 1998; Li et al., 2011). Up to date, a number of organoimido derivatives of hexamolybdate have been obtained via three types of reactions, which include reactions with phosphinimines (Du et al., 1992), isocyanates (Mohs et al., 1995), and aromatic amines (Clegg et al., 1995). Also, based on the DCC dehydrating protocol, we have developed a new approach to synthesize such hybrid materials (Wu et al., 2004).

Because the reaction of [α-Mo8O26]4- with aromatic amines hydrochlorides can easily take place under much more milder conditions to selectively yield mono-functionalized organoimido derivatives of hexamolybdate, such new hybrids can now be synthesized more easily and conveniently in a more controlled fashion. As well known, the ester group is an important reactive functional group which can be applied in ester exchange, hydrolyzation, and aminating reactions in organic syntheses, thus it is necessary to develop new aromatic ester derivatives of hexamolybdate. Based on our previous work, we expanded aromatic ester amines as raw materials, and obtained more stable building blocks to construct novel POM-based organic-inorganic hybrids. Here, we report the synthesis and structural characterization of a new aromatic ester derivative of hexamolybdate.

The asymmetric unit of the title compound includes one [Mo6O18N(C2H5OOCC6H4)]2- anion, two tetrabutylammonium cations, and a half ether molecule disordered by inversion (Fig. 1). Anions and cations are also disordered (see Refinement section). In the cluster anion one terminal oxo group is replaced by an alkylimido ligand (Fig. 2). The short Mo4≡N1 distance, 1.726 (4) Å, and approximately linear C1—N1≡Mo4 and C1A—N1≡Mo4 bond angles, 160.7 (5) and 167.6 (5)°, are typical of organoimido groups bonded at an octahedral d0 metal center, and are consistent with a significant degree of Mo≡N triple bond character (Karlin & Wigley, 2007; Li et al., 2008). Another notable structural feature is that the Mo4—O3 distances between the Mo atom carrying the imido group and the central O atom within the cluster anion cage, 2.196 (3) Å, which is significantly shorter than the other Mo—O3 bond lengths (ca. 2.34 Å). This is consistent with the weak trans-influence of the imido group compared to the oxo group.

In the crystal, cations and anions form hydrogen bonds (Fig. 3), the donor groups being methylene groups in the cations and aromatic CH groups of the aryl ring, while acceptors groups are O atoms from the polyoxometalate cluster and the ester moieties.

Related literature top

For general background to polyoxometalates and the synthesis of their organoimido derivatives, see: Hill (1998); Li et al. (2011); Du et al. (1992); Mohs et al. (1995); Clegg et al. (1995); Wu et al. (2004). For structural features characteristic of these complexes, see: Karlin & Wigley (2007); Li et al. (2008).

Experimental top

A mixture of (Bu4N)4[α-Mo8O26] (1.0 mmol), DCC (2.7 mmol) and ethyl o-aminobenzoate hydrochloride (1.4 mmol) was refluxed in anhydrous acetonitrile (10 ml) for about 6 h. After dissolution, the mixture turned red, and a large amount of white precipitate formed, which was identified as dicyclohexyl urea. After cooling the suspension to room temperature, the white precipitate was removed by filtration, and acetonitrile was allowed to slowly evaporate. The product deposited from the filtrate as a red colloid-like solid. This red solid was washed with ethanol and Et2O several times, and the residue was dissolved in acetone. Single crystals used for X-ray diffraction were obtained by diffusion of ether into this solution. The product was obtained as orange crystals in moderate yield (50-60 %).

Refinement top

The structure is strongly disordered. All the arylester groups is disordered over two positions, for which occupancies were refined, converging to 0.559 (3) and 0.441 (3). In the N2-cation, C36 is disordered with C37. The N3-cation has three disordered butyl chains: C47—C48 is disordered with C49—C50; C54 is disordered with C55; and C57—C58—C59 is disordered with C60—C61—C62. Occupancies were restrained to be identical to those refined for the anion disorder. Finally, the occupancy for the ether molecule, which is placed on an inversion center, was fixed to 1/2. Bond lengths for C—C groups involving disordered parts of the cations were restrained with DFIX to suitable target values, as well as bond lengths in the ether molecule. A set of SIMU and SAME restraints were applied to the arylester, while SIMU and DELU restraints were used in the disordered parts of the cations. Finally, SIMU restraints were applied for the ether solvent (Sheldrick, 2008). All H atoms were placed in idealized positions, and refined as riding on their parent atoms, with C—H fixed to 0.93 (aromatic CH), 0.96 (methyl CH3) and 0.97 Å (methylene CH2). Isotropic displacement parameters for H atoms were calculated as Uiso(H) = 1.2 Ueq(parent C) for aromatic and methylene groups, and Uiso(H) = 1. Ueq(parent C) for methyl groups.

Structure description top

Polyoxometalates and their organoimido derivatives have gained interest owing to their important optical, electronic, magnetic, catalytic, medical, remarkable self-assembly properties and chemical reactivity (Hill, 1998; Li et al., 2011). Up to date, a number of organoimido derivatives of hexamolybdate have been obtained via three types of reactions, which include reactions with phosphinimines (Du et al., 1992), isocyanates (Mohs et al., 1995), and aromatic amines (Clegg et al., 1995). Also, based on the DCC dehydrating protocol, we have developed a new approach to synthesize such hybrid materials (Wu et al., 2004).

Because the reaction of [α-Mo8O26]4- with aromatic amines hydrochlorides can easily take place under much more milder conditions to selectively yield mono-functionalized organoimido derivatives of hexamolybdate, such new hybrids can now be synthesized more easily and conveniently in a more controlled fashion. As well known, the ester group is an important reactive functional group which can be applied in ester exchange, hydrolyzation, and aminating reactions in organic syntheses, thus it is necessary to develop new aromatic ester derivatives of hexamolybdate. Based on our previous work, we expanded aromatic ester amines as raw materials, and obtained more stable building blocks to construct novel POM-based organic-inorganic hybrids. Here, we report the synthesis and structural characterization of a new aromatic ester derivative of hexamolybdate.

The asymmetric unit of the title compound includes one [Mo6O18N(C2H5OOCC6H4)]2- anion, two tetrabutylammonium cations, and a half ether molecule disordered by inversion (Fig. 1). Anions and cations are also disordered (see Refinement section). In the cluster anion one terminal oxo group is replaced by an alkylimido ligand (Fig. 2). The short Mo4≡N1 distance, 1.726 (4) Å, and approximately linear C1—N1≡Mo4 and C1A—N1≡Mo4 bond angles, 160.7 (5) and 167.6 (5)°, are typical of organoimido groups bonded at an octahedral d0 metal center, and are consistent with a significant degree of Mo≡N triple bond character (Karlin & Wigley, 2007; Li et al., 2008). Another notable structural feature is that the Mo4—O3 distances between the Mo atom carrying the imido group and the central O atom within the cluster anion cage, 2.196 (3) Å, which is significantly shorter than the other Mo—O3 bond lengths (ca. 2.34 Å). This is consistent with the weak trans-influence of the imido group compared to the oxo group.

In the crystal, cations and anions form hydrogen bonds (Fig. 3), the donor groups being methylene groups in the cations and aromatic CH groups of the aryl ring, while acceptors groups are O atoms from the polyoxometalate cluster and the ester moieties.

For general background to polyoxometalates and the synthesis of their organoimido derivatives, see: Hill (1998); Li et al. (2011); Du et al. (1992); Mohs et al. (1995); Clegg et al. (1995); Wu et al. (2004). For structural features characteristic of these complexes, see: Karlin & Wigley (2007); Li et al. (2008).

Computing details top

Data collection: CrysAlis PRO (Agilent, 2011); cell refinement: CrysAlis PRO (Agilent, 2011); data reduction: CrysAlis PRO (Agilent, 2011); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg, 2010); software used to prepare material for publication: publCIF (Westrip, 2010).

Figures top
[Figure 1] Fig. 1. The asymmetric unit of the title compound. A single site for disordered groups has been retained. See the archived CIF for a complete view.
[Figure 2] Fig. 2. A view of the anion of the title compound, with displacement ellipsoids shown at the 50% probability level. One position of the disordered aryl group is shown.
[Figure 3] Fig. 3. A view showing hydrogen bonds in the crystal.
Bis(tetrabutylammonium) [2-(ethoxycarbony)phenylimido]-µ6-oxido-dodeca-µ2-oxido- pentaoxidohexamolybdenum diethyl ether hemisolvate top
Crystal data top
(C16H36N)2[Mo6O18(C9H9NO2)]·0.5C4H10OF(000) = 3124
Mr = 1548.79Dx = 1.768 Mg m−3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 9126 reflections
a = 16.3974 (16) Åθ = 3.0–29.3°
b = 17.0854 (8) ŵ = 1.33 mm−1
c = 21.687 (3) ÅT = 101 K
β = 106.709 (16)°Prism, orange
V = 5819.1 (10) Å30.40 × 0.30 × 0.25 mm
Z = 4
Data collection top
Agilent Xcalibur Eos Gemini
diffractometer		11422 independent reflections
Radiation source: fine-focus sealed tube8774 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.038
Detector resolution: 16.0971 pixels mm-1θmax = 26.0°, θmin = 3.0°
ω scansh = −18→20
Absorption correction: multi-scan
(CrysAlis PRO; Agilent, 2011)		k = −21→20
Tmin = 0.619, Tmax = 0.733l = −23→26
31709 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)] = 0.039Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.088H-atom parameters constrained
S = 1.05 w = 1/[σ2(Fo2) + (0.0243P)2 + 15.7229P]
where P = (Fo2 + 2Fc2)/3
11422 reflections(Δ/σ)max = 0.003
854 parametersΔρmax = 1.46 e Å−3
500 restraintsΔρmin = −0.81 e Å−3
0 constraints
Crystal data top
(C16H36N)2[Mo6O18(C9H9NO2)]·0.5C4H10OV = 5819.1 (10) Å3
Mr = 1548.79Z = 4
Monoclinic, P21/nMo Kα radiation
a = 16.3974 (16) ŵ = 1.33 mm−1
b = 17.0854 (8) ÅT = 101 K
c = 21.687 (3) Å0.40 × 0.30 × 0.25 mm
β = 106.709 (16)°
Data collection top
Agilent Xcalibur Eos Gemini
diffractometer		11422 independent reflections
Absorption correction: multi-scan
(CrysAlis PRO; Agilent, 2011)		8774 reflections with I > 2σ(I)
Tmin = 0.619, Tmax = 0.733Rint = 0.038
31709 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.039500 restraints
wR(F2) = 0.088H-atom parameters constrained
S = 1.05 w = 1/[σ2(Fo2) + (0.0243P)2 + 15.7229P]
where P = (Fo2 + 2Fc2)/3
11422 reflectionsΔρmax = 1.46 e Å−3
854 parametersΔρmin = −0.81 e Å−3
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Mo10.13934 (2)0.73051 (2)0.69604 (2)0.02405 (10)
Mo20.02537 (3)0.77620 (2)0.79380 (2)0.02889 (11)
Mo3−0.14888 (2)0.71677 (2)0.68630 (2)0.02216 (10)
Mo4−0.03375 (2)0.67183 (2)0.592661 (19)0.02048 (9)
Mo50.01623 (2)0.59741 (2)0.73540 (2)0.02414 (10)
Mo6−0.02612 (2)0.84988 (2)0.64686 (2)0.02159 (10)
O3−0.00579 (17)0.72276 (16)0.68949 (15)0.0201 (6)
O40.24275 (19)0.7419 (2)0.69912 (18)0.0357 (8)
O5−0.25062 (19)0.70524 (18)0.68807 (17)0.0313 (8)
O6−0.04756 (19)0.94123 (17)0.61622 (17)0.0315 (8)
O70.0367 (2)0.50668 (18)0.76667 (17)0.0331 (8)
O80.0486 (2)0.8132 (2)0.86895 (18)0.0442 (9)
O9−0.14729 (17)0.67117 (16)0.60821 (15)0.0212 (7)
O10−0.00610 (18)0.58029 (16)0.64367 (15)0.0222 (7)
O110.08570 (18)0.69854 (17)0.60962 (15)0.0241 (7)
O12−0.05685 (17)0.78646 (16)0.57403 (14)0.0204 (6)
O13−0.14205 (18)0.81707 (17)0.65775 (17)0.0287 (8)
O14−0.09814 (18)0.61154 (17)0.72434 (15)0.0244 (7)
O150.13247 (18)0.63098 (18)0.72674 (16)0.0292 (8)
O160.08876 (18)0.83694 (17)0.65953 (16)0.0264 (7)
O17−0.0922 (2)0.74992 (18)0.77413 (16)0.0309 (8)
O180.04689 (19)0.66369 (19)0.80821 (15)0.0306 (8)
O190.13364 (19)0.77597 (19)0.77511 (16)0.0322 (8)
O20−0.0036 (2)0.86502 (17)0.73992 (16)0.0303 (8)
N1−0.0593 (2)0.6384 (2)0.51431 (19)0.0244 (8)
C1−0.1064 (7)0.6223 (9)0.4506 (5)0.024 (2)0.441 (3)
C2−0.1956 (6)0.6319 (6)0.4341 (5)0.027 (2)0.441 (3)
H2−0.22120.64470.46590.032*0.441 (3)
C3−0.2451 (7)0.6225 (6)0.3711 (5)0.032 (2)0.441 (3)
H3−0.30390.62800.36070.039*0.441 (3)
C4−0.2070 (7)0.6049 (7)0.3239 (6)0.036 (2)0.441 (3)
H4−0.24050.59950.28150.043*0.441 (3)
C5−0.1199 (8)0.5952 (8)0.3386 (6)0.036 (2)0.441 (3)
H5−0.09520.58410.30600.043*0.441 (3)
C6−0.0689 (7)0.6019 (6)0.4019 (5)0.0275 (19)0.441 (3)
C70.0246 (8)0.5889 (7)0.4151 (6)0.0270 (19)0.441 (3)
O10.0601 (5)0.5984 (5)0.3730 (4)0.041 (2)0.441 (3)
O20.0641 (6)0.5669 (7)0.4742 (5)0.031 (2)0.441 (3)
C80.1557 (6)0.5532 (7)0.4879 (5)0.031 (2)0.441 (3)
H8B0.17980.58840.46260.038*0.441 (3)
H8A0.16630.49980.47720.038*0.441 (3)
C90.1959 (11)0.5681 (11)0.5596 (8)0.038 (4)0.441 (3)
H9C0.19290.62290.56840.057*0.441 (3)
H9A0.25430.55180.57160.057*0.441 (3)
H9B0.16560.53890.58390.057*0.441 (3)
C1A−0.0762 (6)0.6282 (7)0.4486 (4)0.0255 (19)0.559 (3)
C2A−0.1593 (5)0.6491 (5)0.4117 (4)0.0297 (17)0.559 (3)
H2A−0.19900.66630.43180.036*0.559 (3)
C3A−0.1807 (6)0.6437 (5)0.3455 (5)0.0362 (19)0.559 (3)
H3A−0.23540.65720.32100.043*0.559 (3)
C4A−0.1225 (7)0.6189 (6)0.3155 (5)0.039 (2)0.559 (3)
H4A−0.13750.61660.27080.046*0.559 (3)
C5A−0.0418 (5)0.5972 (5)0.3512 (4)0.0327 (17)0.559 (3)
H5A−0.00320.57950.33020.039*0.559 (3)
C6A−0.0174 (7)0.6012 (5)0.4175 (4)0.0268 (17)0.559 (3)
C7A0.0725 (8)0.5762 (8)0.4522 (6)0.029 (2)0.559 (3)
O1A0.1254 (4)0.5633 (4)0.4235 (3)0.0364 (15)0.559 (3)
O2A0.0876 (4)0.5706 (4)0.5147 (4)0.0350 (15)0.559 (3)
C8A0.1737 (7)0.5492 (9)0.5516 (8)0.036 (3)0.559 (3)
H8AA0.19340.50620.53050.043*0.559 (3)
H8AB0.17340.53180.59420.043*0.559 (3)
C9A0.2347 (6)0.6189 (7)0.5580 (5)0.045 (3)0.559 (3)
H9AA0.23600.63530.51600.067*0.559 (3)
H9AB0.29080.60360.58290.067*0.559 (3)
H9AC0.21530.66140.57920.067*0.559 (3)
N2−0.1640 (2)0.9199 (2)0.39232 (18)0.0223 (8)
C21−0.1699 (3)0.8997 (3)0.3232 (2)0.0245 (10)
H21A−0.15480.84500.32160.029*
H21B−0.22880.90530.29770.029*
C22−0.1147 (3)0.9479 (3)0.2916 (2)0.0333 (12)
H22A−0.05540.94370.31670.040*
H22B−0.13111.00250.29040.040*
C23−0.1248 (3)0.9191 (3)0.2237 (3)0.0404 (13)
H23A−0.10820.86450.22550.048*
H23B−0.18450.92220.19950.048*
C24−0.0734 (4)0.9641 (4)0.1880 (3)0.065 (2)
H24A−0.08140.94130.14620.097*
H24B−0.01420.96200.21170.097*
H24C−0.09191.01760.18330.097*
C25−0.0725 (3)0.9137 (2)0.4357 (2)0.0228 (10)
H25A−0.03980.95620.42500.027*
H25B−0.07310.92150.47990.027*
C26−0.0259 (3)0.8377 (3)0.4326 (2)0.0270 (10)
H26A−0.02720.82690.38840.032*
H26B−0.05360.79480.44790.032*
C270.0666 (3)0.8454 (3)0.4747 (2)0.0331 (12)
H27A0.09330.88890.45930.040*
H27B0.06700.85690.51860.040*
C280.1178 (3)0.7720 (3)0.4743 (3)0.0416 (13)
H28A0.11480.75850.43070.062*
H28B0.09510.72990.49360.062*
H28C0.17610.78090.49830.062*
C29−0.2222 (3)0.8623 (3)0.4138 (2)0.0267 (10)
H29A−0.19590.81100.41800.032*
H29B−0.27550.85890.37980.032*
C30−0.2422 (3)0.8808 (3)0.4759 (2)0.0262 (10)
H30A−0.18960.88640.51030.031*
H30B−0.27280.93000.47150.031*
C31−0.2960 (3)0.8160 (3)0.4928 (3)0.0429 (14)
H31A−0.26090.76970.50530.052*
H31B−0.34180.80300.45460.052*
C32−0.3340 (3)0.8376 (3)0.5467 (3)0.0417 (14)
H32A−0.36550.79390.55580.063*
H32B−0.28910.85100.58460.063*
H32C−0.37150.88160.53370.063*
C33−0.1902 (3)1.0039 (2)0.3993 (2)0.0290 (11)
H33A−0.15111.03830.38630.035*
H33B−0.18391.01380.44450.035*
C34−0.2801 (3)1.0255 (3)0.3611 (3)0.0368 (12)
H34A−0.28531.02570.31540.044*
H34B−0.32020.98770.36890.044*
C35−0.2989 (5)1.1074 (4)0.3830 (3)0.067 (2)
H35A−0.34121.13280.34810.080*0.559 (3)
H35B−0.24731.13860.39280.080*0.559 (3)
H35C−0.24911.13910.38500.080*0.441 (3)
H35D−0.30141.10180.42690.080*0.441 (3)
C36−0.3310 (6)1.1041 (6)0.4418 (5)0.043 (3)0.559 (3)
H36A−0.37341.06390.43620.065*0.559 (3)
H36B−0.28451.09280.47920.065*0.559 (3)
H36C−0.35571.15370.44740.065*0.559 (3)
C37−0.3721 (7)1.1540 (7)0.3496 (7)0.050 (4)0.441 (3)
H37A−0.36791.16790.30780.075*0.441 (3)
H37B−0.42321.12430.34520.075*0.441 (3)
H37C−0.37381.20070.37390.075*0.441 (3)
N3−0.2747 (3)0.4430 (2)0.6884 (2)0.0345 (10)
C41−0.2807 (3)0.5100 (3)0.6413 (2)0.0328 (12)
H41A−0.26240.49100.60530.039*
H41B−0.24080.55040.66250.039*
C42−0.3682 (3)0.5476 (4)0.6148 (3)0.0584 (18)
H42A−0.41080.50690.60110.070*
H42B−0.38170.57750.64860.070*
C43−0.3713 (3)0.6013 (3)0.5582 (3)0.0485 (15)
H43A−0.32240.63590.57000.058*
H43B−0.42210.63340.54980.058*
C44−0.3717 (6)0.5593 (5)0.4983 (4)0.086 (3)
H44A−0.31840.53280.50450.129*
H44B−0.37980.59620.46370.129*
H44C−0.41720.52180.48810.129*
C45−0.1809 (4)0.4211 (3)0.7129 (3)0.0507 (17)
H45A−0.16120.40710.67620.061*
H45B−0.14920.46690.73270.061*
C46−0.1597 (5)0.3539 (4)0.7613 (4)0.082 (3)
H46A−0.19160.30770.74230.099*0.559 (3)
H46B−0.17680.36790.79910.099*0.559 (3)
H46C−0.20450.31480.75020.099*0.441 (3)
H46D−0.15530.37330.80420.099*0.441 (3)
C47−0.0640 (9)0.3350 (8)0.7814 (7)0.053 (3)0.559 (3)
H47A−0.05020.31570.74350.064*0.559 (3)
H47B−0.03370.38400.79330.064*0.559 (3)
C48−0.0274 (8)0.2766 (6)0.8361 (6)0.051 (3)0.559 (3)
H48A0.02670.25790.83350.077*0.559 (3)
H48B−0.06580.23330.83230.077*0.559 (3)
H48C−0.02020.30210.87680.077*0.559 (3)
C49−0.0756 (12)0.3176 (11)0.7597 (11)0.068 (5)0.441 (3)
H49A−0.07730.30480.71580.082*0.441 (3)
H49B−0.02940.35420.77660.082*0.441 (3)
C50−0.0621 (9)0.2445 (8)0.8004 (8)0.050 (4)0.441 (3)
H50A−0.09700.20310.77680.075*0.441 (3)
H50B−0.00330.22940.81120.075*0.441 (3)
H50C−0.07750.25460.83920.075*0.441 (3)
C51−0.3090 (3)0.4661 (3)0.7443 (2)0.0324 (12)
H51A−0.30490.42110.77240.039*
H51B−0.36890.47910.72730.039*
C52−0.2644 (4)0.5333 (4)0.7835 (3)0.0555 (17)
H52A−0.20480.52000.80200.067*
H52B−0.26710.57820.75550.067*
C53−0.3021 (4)0.5557 (4)0.8372 (3)0.0491 (15)
H53A−0.32970.51110.85040.059*0.559 (3)
H53B−0.25850.57530.87430.059*0.559 (3)
H53C−0.36370.55520.82000.059*0.441 (3)
H53D−0.28680.51550.87010.059*0.441 (3)
C54−0.3657 (9)0.6184 (8)0.8085 (7)0.083 (5)0.559 (3)
H54A−0.41480.59520.77870.125*0.559 (3)
H54B−0.34050.65550.78620.125*0.559 (3)
H54C−0.38250.64450.84210.125*0.559 (3)
C55−0.2766 (8)0.6321 (7)0.8683 (7)0.047 (3)0.441 (3)
H55A−0.29690.67320.83750.071*0.441 (3)
H55B−0.21570.63460.88420.071*0.441 (3)
H55C−0.30070.63830.90350.071*0.441 (3)
C56−0.3273 (4)0.3745 (3)0.6559 (3)0.0604 (16)
H56A−0.38030.39320.62680.072*0.559 (3)
H56B−0.34070.34140.68800.072*0.559 (3)
H56C−0.30630.32860.68190.072*0.441 (3)
H56D−0.38510.38330.65750.072*0.441 (3)
C57−0.3322 (8)0.3535 (7)0.5855 (6)0.040 (2)0.441 (3)
H57A−0.27860.33010.58480.048*0.441 (3)
H57B−0.33940.40140.56050.048*0.441 (3)
C58−0.4051 (16)0.2968 (14)0.5529 (9)0.040 (3)0.441 (3)
H58A−0.40440.25240.58090.048*0.441 (3)
H58B−0.45940.32330.54560.048*0.441 (3)
C59−0.3947 (9)0.2684 (9)0.4888 (7)0.052 (3)0.441 (3)
H59A−0.34140.24140.49620.078*0.441 (3)
H59B−0.39560.31250.46110.078*0.441 (3)
H59C−0.44050.23360.46860.078*0.441 (3)
C60−0.2759 (6)0.3243 (6)0.6160 (5)0.0432 (19)0.559 (3)
H60A−0.25940.35740.58530.052*0.559 (3)
H60B−0.22490.30170.64500.052*0.559 (3)
C61−0.3362 (6)0.2602 (6)0.5814 (5)0.041 (2)0.559 (3)
H61A−0.30510.22430.56180.050*0.559 (3)
H61B−0.35580.23100.61270.050*0.559 (3)
C62−0.4127 (12)0.2906 (12)0.5299 (7)0.053 (4)0.559 (3)
H62A−0.39390.32340.50060.079*0.559 (3)
H62B−0.44450.24730.50670.079*0.559 (3)
H62C−0.44810.32040.54950.079*0.559 (3)
C1010.0391 (19)0.4428 (14)1.1046 (8)0.072 (6)0.50
H10H−0.01660.42321.10230.107*0.50
H10I0.08140.40931.13180.107*0.50
H10J0.04520.49481.12220.107*0.50
C1020.0505 (8)0.4445 (8)1.0375 (6)0.059 (3)0.50
H10F0.03730.39381.01710.071*0.50
H10G0.10870.45791.03970.071*0.50
O103−0.008 (2)0.503 (2)1.0017 (11)0.043 (3)0.50
C1040.0004 (8)0.5075 (7)0.9368 (6)0.051 (3)0.50
H10D−0.02490.46200.91170.061*0.50
H10E0.05950.51160.93720.061*0.50
C105−0.0486 (16)0.5817 (10)0.9103 (10)0.064 (5)0.50
H10A−0.04790.58950.86660.096*0.50
H10B−0.10640.57670.91150.096*0.50
H10C−0.02240.62570.93600.096*0.50
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mo10.01366 (18)0.0267 (2)0.0309 (2)−0.00060 (15)0.00505 (16)−0.00190 (18)
Mo20.0269 (2)0.0363 (2)0.0227 (2)−0.00515 (18)0.00589 (17)−0.00936 (19)
Mo30.01683 (19)0.02216 (18)0.0299 (2)−0.00188 (15)0.01057 (16)−0.00479 (17)
Mo40.01943 (19)0.02174 (18)0.0208 (2)−0.00087 (15)0.00670 (15)−0.00375 (16)
Mo50.0206 (2)0.02525 (19)0.0251 (2)0.00071 (16)0.00420 (16)0.00308 (17)
Mo60.01640 (18)0.01828 (18)0.0296 (2)−0.00127 (14)0.00589 (16)−0.00219 (16)
O30.0121 (13)0.0237 (14)0.0246 (17)−0.0008 (11)0.0055 (12)−0.0037 (13)
O40.0163 (16)0.0409 (19)0.048 (2)−0.0009 (14)0.0070 (15)0.0014 (17)
O50.0228 (16)0.0302 (17)0.045 (2)−0.0034 (14)0.0166 (15)−0.0086 (16)
O60.0235 (16)0.0216 (15)0.049 (2)−0.0024 (13)0.0092 (15)−0.0015 (15)
O70.0320 (18)0.0315 (17)0.034 (2)0.0018 (15)0.0055 (15)0.0074 (16)
O80.046 (2)0.056 (2)0.030 (2)−0.0121 (19)0.0106 (17)−0.0178 (19)
O90.0157 (14)0.0222 (15)0.0247 (18)−0.0019 (12)0.0045 (12)−0.0026 (13)
O100.0241 (16)0.0201 (14)0.0230 (18)0.0013 (12)0.0078 (13)−0.0022 (13)
O110.0233 (16)0.0266 (15)0.0260 (19)0.0026 (13)0.0129 (14)−0.0007 (14)
O120.0209 (15)0.0211 (14)0.0189 (17)0.0007 (12)0.0052 (13)0.0009 (13)
O130.0201 (16)0.0210 (15)0.047 (2)0.0021 (13)0.0123 (15)−0.0031 (15)
O140.0246 (16)0.0273 (16)0.0240 (18)−0.0028 (13)0.0111 (14)−0.0010 (14)
O150.0180 (15)0.0307 (17)0.036 (2)0.0041 (13)0.0030 (14)0.0093 (15)
O160.0200 (16)0.0252 (16)0.035 (2)−0.0034 (13)0.0095 (14)−0.0021 (14)
O170.0344 (18)0.0331 (17)0.031 (2)−0.0032 (15)0.0185 (15)−0.0110 (15)
O180.0316 (18)0.0392 (18)0.0192 (19)−0.0083 (15)0.0047 (14)0.0013 (15)
O190.0249 (17)0.0387 (18)0.029 (2)−0.0030 (14)0.0016 (14)−0.0070 (16)
O200.0321 (18)0.0244 (16)0.036 (2)−0.0074 (14)0.0124 (15)−0.0127 (15)
N10.0263 (19)0.0233 (18)0.025 (2)0.0017 (15)0.0090 (16)−0.0007 (16)
C10.028 (4)0.023 (4)0.024 (4)0.002 (4)0.012 (4)−0.001 (3)
C20.029 (4)0.028 (4)0.025 (5)0.006 (4)0.011 (4)0.002 (4)
C30.029 (4)0.032 (4)0.030 (4)0.013 (4)0.001 (4)0.001 (4)
C40.039 (4)0.040 (5)0.026 (5)0.007 (4)0.004 (4)0.007 (4)
C50.039 (4)0.038 (4)0.029 (5)0.005 (4)0.006 (4)0.003 (4)
C60.029 (4)0.028 (3)0.028 (4)0.002 (4)0.012 (3)−0.001 (3)
C70.027 (4)0.028 (4)0.030 (4)−0.002 (4)0.015 (4)−0.005 (3)
O10.039 (4)0.053 (5)0.037 (5)−0.007 (4)0.021 (4)−0.002 (4)
O20.028 (3)0.037 (3)0.030 (4)0.001 (3)0.010 (4)−0.004 (4)
C80.022 (4)0.040 (4)0.036 (4)0.004 (3)0.013 (3)−0.001 (4)
C90.016 (7)0.046 (8)0.043 (7)0.001 (6)−0.006 (6)−0.008 (7)
C1A0.029 (4)0.021 (3)0.026 (4)0.004 (4)0.007 (3)0.001 (3)
C2A0.027 (4)0.028 (3)0.032 (4)0.008 (3)0.005 (3)−0.004 (3)
C3A0.033 (4)0.034 (4)0.032 (4)0.005 (3)−0.006 (3)0.004 (3)
C4A0.039 (4)0.043 (4)0.028 (5)0.003 (4)0.000 (4)0.001 (4)
C5A0.035 (3)0.033 (3)0.031 (4)0.002 (3)0.009 (3)−0.002 (3)
C6A0.028 (4)0.025 (3)0.028 (3)0.001 (3)0.009 (3)0.000 (3)
C7A0.027 (4)0.028 (3)0.033 (5)0.002 (3)0.010 (4)−0.005 (4)
O1A0.031 (3)0.048 (3)0.034 (4)−0.005 (3)0.015 (3)−0.010 (3)
O2A0.026 (3)0.044 (3)0.034 (4)0.008 (3)0.006 (3)0.003 (3)
C8A0.019 (5)0.045 (5)0.043 (5)0.009 (4)0.006 (4)0.004 (5)
C9A0.027 (5)0.068 (7)0.036 (6)0.015 (5)0.003 (4)−0.007 (5)
N20.0163 (18)0.0225 (18)0.026 (2)−0.0048 (14)0.0020 (16)0.0008 (16)
C210.022 (2)0.026 (2)0.022 (3)−0.0051 (19)0.0007 (19)0.000 (2)
C220.032 (3)0.040 (3)0.025 (3)−0.013 (2)0.004 (2)0.001 (2)
C230.040 (3)0.049 (3)0.031 (3)−0.019 (3)0.008 (2)−0.009 (3)
C240.086 (5)0.080 (5)0.030 (4)−0.051 (4)0.019 (3)−0.013 (3)
C250.019 (2)0.029 (2)0.018 (2)−0.0077 (18)0.0014 (18)−0.0025 (19)
C260.021 (2)0.037 (3)0.021 (3)−0.003 (2)0.0034 (19)−0.001 (2)
C270.023 (2)0.048 (3)0.029 (3)−0.005 (2)0.008 (2)0.000 (2)
C280.028 (3)0.058 (3)0.038 (3)0.003 (2)0.008 (2)0.009 (3)
C290.020 (2)0.026 (2)0.031 (3)−0.0051 (18)0.003 (2)0.002 (2)
C300.017 (2)0.031 (2)0.027 (3)0.0011 (19)0.0009 (19)0.004 (2)
C310.043 (3)0.038 (3)0.054 (4)−0.005 (2)0.024 (3)0.008 (3)
C320.031 (3)0.051 (3)0.048 (4)0.006 (2)0.018 (3)0.015 (3)
C330.035 (3)0.019 (2)0.033 (3)−0.005 (2)0.010 (2)0.000 (2)
C340.042 (3)0.035 (3)0.034 (3)0.013 (2)0.013 (2)0.011 (2)
C350.101 (6)0.046 (4)0.066 (5)0.033 (4)0.045 (4)0.024 (3)
C360.036 (5)0.041 (5)0.051 (7)0.002 (4)0.010 (5)−0.005 (5)
C370.037 (7)0.048 (7)0.064 (10)0.002 (6)0.013 (7)−0.004 (7)
N30.045 (3)0.024 (2)0.044 (3)−0.0119 (18)0.027 (2)−0.0028 (19)
C410.035 (3)0.037 (3)0.029 (3)−0.010 (2)0.014 (2)0.002 (2)
C420.033 (3)0.091 (5)0.052 (4)−0.005 (3)0.015 (3)0.009 (4)
C430.032 (3)0.056 (4)0.052 (4)−0.001 (3)0.002 (3)0.006 (3)
C440.123 (7)0.082 (5)0.055 (5)0.025 (5)0.031 (5)0.016 (4)
C450.068 (4)0.033 (3)0.071 (5)0.018 (3)0.053 (4)0.020 (3)
C460.098 (4)0.062 (4)0.120 (6)0.051 (4)0.084 (5)0.059 (4)
C470.084 (4)0.023 (5)0.074 (9)0.016 (5)0.056 (6)0.014 (5)
C480.057 (6)0.041 (6)0.056 (8)−0.017 (4)0.020 (5)0.009 (5)
C490.084 (8)0.050 (9)0.097 (12)0.033 (7)0.068 (8)0.034 (8)
C500.038 (7)0.039 (7)0.073 (11)0.010 (5)0.018 (7)0.017 (6)
C510.034 (3)0.035 (3)0.036 (3)−0.002 (2)0.023 (2)0.002 (2)
C520.060 (4)0.058 (4)0.062 (5)−0.020 (3)0.039 (3)−0.018 (3)
C530.052 (4)0.059 (4)0.045 (4)−0.012 (3)0.026 (3)−0.007 (3)
C540.086 (10)0.090 (10)0.097 (12)0.017 (8)0.064 (9)−0.012 (9)
C550.051 (8)0.050 (7)0.046 (9)0.007 (6)0.022 (7)−0.011 (7)
C560.090 (4)0.048 (3)0.063 (4)−0.035 (3)0.053 (3)−0.021 (3)
C570.048 (5)0.030 (4)0.048 (4)−0.012 (4)0.026 (4)−0.007 (4)
C580.044 (6)0.038 (5)0.045 (7)−0.006 (5)0.024 (6)−0.013 (6)
C590.052 (7)0.055 (7)0.049 (8)−0.010 (6)0.017 (6)−0.018 (7)
C600.044 (4)0.038 (4)0.053 (5)−0.017 (3)0.023 (4)−0.006 (4)
C610.041 (4)0.039 (4)0.050 (5)−0.006 (4)0.022 (4)−0.009 (4)
C620.047 (6)0.061 (7)0.055 (9)−0.007 (5)0.023 (8)−0.021 (8)
C1010.077 (10)0.080 (12)0.062 (12)0.017 (10)0.028 (9)0.020 (10)
C1020.050 (6)0.061 (6)0.058 (7)0.006 (5)0.004 (5)0.008 (6)
O1030.044 (8)0.046 (5)0.044 (4)0.007 (5)0.021 (4)0.002 (4)
C1040.051 (6)0.065 (6)0.039 (6)−0.004 (5)0.016 (5)0.010 (5)
C1050.069 (11)0.077 (12)0.043 (10)−0.002 (9)0.011 (8)0.011 (9)
Geometric parameters (Å, º) top
Mo1—O32.347 (3)C32—H32A0.9600
Mo1—O41.689 (3)C32—H32B0.9600
Mo1—O111.907 (3)C32—H32C0.9600
Mo1—O151.841 (3)C33—C341.514 (7)
Mo1—O162.060 (3)C33—H33A0.9700
Mo1—O191.909 (3)C33—H33B0.9700
Mo2—O32.355 (3)C34—C351.538 (7)
Mo2—O81.686 (4)C34—H34A0.9700
Mo2—O171.904 (3)C34—H34B0.9700
Mo2—O181.963 (3)C35—C361.515 (12)
Mo2—O191.931 (3)C35—C371.449 (8)
Mo2—O201.891 (3)C35—H35A0.9700
Mo3—O32.330 (3)C35—H35B0.9700
Mo3—O51.691 (3)C35—H35C0.9700
Mo3—O91.871 (3)C35—H35D0.9700
Mo3—O131.836 (3)C36—H36A0.9600
Mo3—O142.052 (3)C36—H36B0.9600
Mo3—O171.948 (3)C36—H36C0.9600
Mo4—N11.726 (4)C37—H37A0.9600
Mo4—O32.196 (3)C37—H37B0.9600
Mo4—O91.985 (3)C37—H37C0.9600
Mo4—O101.894 (3)N3—C411.519 (6)
Mo4—O111.941 (3)N3—C451.523 (7)
Mo4—O122.013 (3)N3—C511.529 (6)
Mo5—O32.346 (3)N3—C561.502 (6)
Mo5—O71.687 (3)C41—C421.525 (7)
Mo5—O101.939 (3)C41—H41A0.9700
Mo5—O141.837 (3)C41—H41B0.9700
Mo5—O152.050 (3)C42—H42A0.9700
Mo5—O181.890 (3)C42—H42B0.9700
Mo6—O32.346 (3)C43—C421.520 (8)
Mo6—O61.693 (3)C43—C441.481 (9)
Mo6—O121.862 (3)C43—H43A0.9700
Mo6—O132.059 (3)C43—H43B0.9700
Mo6—O161.837 (3)C44—H44A0.9600
Mo6—O201.961 (3)C44—H44B0.9600
N1—C11.403 (10)C44—H44C0.9600
C1—C21.411 (12)C45—C461.527 (7)
C1—C61.409 (13)C45—H45A0.9700
C2—C31.383 (12)C45—H45B0.9700
C2—H20.9300C46—C491.521 (16)
C3—C41.378 (14)C46—H46A0.9700
C3—H30.9300C46—H46B0.9700
C4—C51.381 (16)C46—H46C0.9700
C4—H40.9300C46—H46D0.9700
C5—C61.392 (14)C47—C461.537 (14)
C5—H50.9300C47—C481.535 (13)
C6—C71.494 (13)C47—H47A0.9700
C7—O11.227 (11)C47—H47B0.9700
C7—O21.312 (15)C48—H48A0.9600
O2—C81.464 (12)C48—H48B0.9600
C8—C91.526 (16)C48—H48C0.9600
C8—H8A0.9700C49—H49A0.9700
C8—H8B0.9700C49—H49B0.9700
C9—H9C0.9600C50—C491.509 (16)
C9—H9A0.9600C50—H50A0.9600
C9—H9B0.9600C50—H50B0.9600
N1—C1A1.383 (9)C50—H50C0.9600
C1A—C2A1.412 (11)C51—C521.490 (7)
C1A—C6A1.404 (12)C51—H51A0.9700
C2A—C3A1.379 (11)C51—H51B0.9700
C2A—H2A0.9300C52—H52A0.9700
C3A—C4A1.368 (13)C52—H52B0.9700
C3A—H3A0.9300C53—C521.517 (8)
C4A—C5A1.377 (13)C53—C541.500 (14)
C4A—H4A0.9300C53—C551.474 (13)
C5A—C6A1.380 (11)C53—H53A0.9700
C5A—H5A0.9300C53—H53B0.9700
C6A—C7A1.512 (13)C53—H53C0.9700
C7A—O1A1.224 (11)C53—H53D0.9700
C7A—O2A1.308 (13)C54—H54A0.9600
O2A—C8A1.455 (13)C54—H54B0.9600
C8A—C9A1.535 (13)C54—H54C0.9600
C8A—H8AA0.9700C55—H55A0.9600
C8A—H8AB0.9700C55—H55B0.9600
C9A—H9AA0.9600C55—H55C0.9600
C9A—H9AB0.9600C56—C571.547 (14)
C9A—H9AC0.9600C56—C601.616 (11)
N2—C211.514 (6)C56—H56A0.9700
N2—C251.530 (5)C56—H56B0.9700
N2—C291.533 (5)C56—H56C0.9700
N2—C331.517 (5)C56—H56D0.9700
C21—C221.525 (6)C57—C581.54 (3)
C21—H21A0.9700C57—H57A0.9700
C21—H21B0.9700C57—H57B0.9700
C22—C231.516 (7)C58—H58A0.9700
C22—H22A0.9700C58—H58B0.9700
C22—H22B0.9700C59—C581.53 (2)
C23—C241.509 (7)C59—H59A0.9600
C23—H23A0.9700C59—H59B0.9600
C23—H23B0.9700C59—H59C0.9600
C24—H24A0.9600C60—C611.522 (13)
C24—H24B0.9600C60—H60A0.9700
C24—H24C0.9600C60—H60B0.9700
C25—C261.517 (6)C61—H61A0.9700
C25—H25A0.9700C61—H61B0.9700
C25—H25B0.9700C62—C611.51 (2)
C26—C271.535 (6)C62—H62A0.9600
C26—H26A0.9700C62—H62B0.9600
C26—H26B0.9700C62—H62C0.9600
C27—H27A0.9700C101—H10H0.9600
C27—H27B0.9700C101—H10I0.9600
C28—C271.510 (7)C101—H10J0.9600
C28—H28A0.9600C102—C1011.520 (10)
C28—H28B0.9600C102—H10F0.9700
C28—H28C0.9600C102—H10G0.9700
C29—C301.509 (6)O103—C1021.447 (18)
C29—H29A0.9700O103—C1041.452 (19)
C29—H29B0.9700C104—H10D0.9700
C30—C311.524 (6)C104—H10E0.9700
C30—H30A0.9700C105—C1041.522 (9)
C30—H30B0.9700C105—H10A0.9600
C31—H31A0.9700C105—H10B0.9600
C31—H31B0.9700C105—H10C0.9600
C32—C311.520 (7)
O4—Mo1—O3176.42 (14)C28—C27—H27A109.1
O4—Mo1—O11104.24 (15)C28—C27—H27B109.1
O4—Mo1—O15104.91 (15)H27A—C27—H27B107.8
O4—Mo1—O16101.65 (14)C27—C28—H28A109.5
O4—Mo1—O19103.03 (16)C27—C28—H28B109.5
O11—Mo1—O375.59 (11)C27—C28—H28C109.5
O11—Mo1—O1681.61 (12)H28A—C28—H28B109.5
O11—Mo1—O19150.63 (13)H28B—C28—H28C109.5
O15—Mo1—O378.66 (11)H28A—C28—H28C109.5
O15—Mo1—O1191.83 (14)C30—C29—N2116.8 (4)
O15—Mo1—O16153.44 (12)C30—C29—H29B108.1
O15—Mo1—O1991.55 (15)N2—C29—H29A108.1
O16—Mo1—O374.77 (11)N2—C29—H29B108.1
O19—Mo1—O376.51 (12)C30—C29—H29A108.1
O19—Mo1—O1682.41 (13)H29B—C29—H29A107.3
O8—Mo2—O3179.10 (16)C29—C30—C31110.6 (4)
O8—Mo2—O17103.75 (16)C29—C30—H30A109.5
O8—Mo2—O18103.47 (17)C29—C30—H30B109.5
O8—Mo2—O19103.76 (16)C31—C30—H30A109.5
O8—Mo2—O20104.08 (17)C31—C30—H30B109.5
O17—Mo2—O376.54 (12)H30B—C30—H30A108.1
O17—Mo2—O1885.92 (13)C32—C31—C30113.7 (4)
O17—Mo2—O19152.23 (14)C30—C31—H31A108.8
O18—Mo2—O375.68 (12)C30—C31—H31B108.8
O19—Mo2—O375.89 (12)C32—C31—H31A108.8
O19—Mo2—O1884.11 (13)C32—C31—H31B108.8
O20—Mo2—O376.76 (12)H31B—C31—H31A107.7
O20—Mo2—O1789.59 (14)C31—C32—H32A109.5
O20—Mo2—O18152.37 (14)C31—C32—H32B109.5
O20—Mo2—O1987.39 (14)C31—C32—H32C109.5
O5—Mo3—O3174.93 (14)H32B—C32—H32A109.5
O5—Mo3—O9104.04 (14)H32C—C32—H32A109.5
O5—Mo3—O13105.81 (14)H32C—C32—H32B109.5
O5—Mo3—O14100.22 (14)C34—C33—N2115.8 (4)
O5—Mo3—O17102.03 (15)C34—C33—H33B108.3
O9—Mo3—O376.66 (11)N2—C33—H33A108.3
O9—Mo3—O1483.66 (12)N2—C33—H33B108.3
O9—Mo3—O17151.53 (12)C34—C33—H33A108.3
O13—Mo3—O379.08 (11)H33B—C33—H33A107.4
O13—Mo3—O993.74 (14)C33—C34—C35107.6 (5)
O13—Mo3—O14153.66 (12)C33—C34—H34A110.2
O13—Mo3—O1790.00 (14)C33—C34—H34B110.2
O14—Mo3—O374.81 (11)C35—C34—H34A110.2
O17—Mo3—O376.38 (12)C35—C34—H34B110.2
O17—Mo3—O1480.64 (13)H34B—C34—H34A108.5
N1—Mo4—O3175.66 (14)C34—C35—H35A109.2
N1—Mo4—O9101.01 (15)C34—C35—H35B109.2
N1—Mo4—O10104.57 (15)C34—C35—H35C106.4
N1—Mo4—O11102.16 (15)C34—C35—H35D106.4
N1—Mo4—O1298.37 (15)C36—C35—C34112.0 (6)
O9—Mo4—O377.76 (11)C36—C35—H35A109.2
O9—Mo4—O1284.73 (11)C36—C35—H35B109.2
O10—Mo4—O379.61 (12)C37—C35—C34123.8 (8)
O10—Mo4—O988.56 (12)C37—C35—H35B110.6
O10—Mo4—O1191.39 (12)C37—C35—H35C106.4
O10—Mo4—O12156.94 (12)C37—C35—H35D106.4
O11—Mo4—O378.68 (11)H35B—C35—H35A107.9
O11—Mo4—O9156.06 (12)H35D—C35—H35C106.4
O11—Mo4—O1286.02 (12)C35—C36—H36A109.5
O12—Mo4—O377.41 (11)C35—C36—H36B109.5
O7—Mo5—O3176.81 (13)C35—C36—H36C109.5
O7—Mo5—O10103.36 (15)C35—C37—H37A109.5
O7—Mo5—O14104.52 (14)C35—C37—H37B109.5
O7—Mo5—O15102.21 (14)C35—C37—H37C109.5
O7—Mo5—O18103.90 (16)H37A—C37—H37B109.5
O10—Mo5—O375.03 (11)H37A—C37—H37C109.5
O10—Mo5—O1581.63 (13)H37C—C37—H37B109.5
O14—Mo5—O378.33 (11)C56—N3—C41110.8 (4)
O14—Mo5—O1090.08 (13)C56—N3—C45111.0 (4)
O14—Mo5—O15153.18 (13)C41—N3—C45106.5 (3)
O14—Mo5—O1892.67 (14)C56—N3—C51106.3 (4)
O15—Mo5—O374.89 (10)C41—N3—C51111.8 (4)
O18—Mo5—O377.23 (12)C45—N3—C51110.6 (4)
O18—Mo5—O10150.94 (13)N3—C41—C42116.3 (4)
O18—Mo5—O1582.99 (14)N3—C41—H41A108.2
O6—Mo6—O3176.21 (12)C42—C41—H41A108.2
O6—Mo6—O12103.21 (15)N3—C41—H41B108.2
O6—Mo6—O13101.63 (13)C42—C41—H41B108.2
O6—Mo6—O16104.94 (14)H41A—C41—H41B107.4
O6—Mo6—O20103.81 (15)C43—C42—C41111.6 (4)
O12—Mo6—O376.62 (11)C43—C42—H42A109.3
O12—Mo6—O1384.56 (13)C41—C42—H42A109.3
O12—Mo6—O20151.02 (12)C43—C42—H42B109.3
O13—Mo6—O374.58 (11)C41—C42—H42B109.3
O16—Mo6—O378.83 (11)H42A—C42—H42B108.0
O16—Mo6—O1294.16 (13)C44—C43—C42114.0 (6)
O16—Mo6—O13152.95 (13)C44—C43—H43B108.8
O16—Mo6—O2088.86 (14)C42—C43—H43B108.8
O20—Mo6—O375.72 (11)C44—C43—H43A108.8
O20—Mo6—O1379.93 (13)C42—C43—H43A108.8
Mo1—O3—Mo289.07 (10)H43B—C43—H43A107.7
Mo3—O3—Mo1178.16 (15)C43—C44—H44B109.5
Mo3—O3—Mo289.09 (10)C43—C44—H44C109.5
Mo3—O3—Mo590.19 (10)H44B—C44—H44C109.5
Mo3—O3—Mo690.07 (9)C43—C44—H44A109.5
Mo4—O3—Mo190.55 (10)H44B—C44—H44A109.5
Mo4—O3—Mo2179.33 (15)H44C—C44—H44A109.5
Mo4—O3—Mo391.29 (10)N3—C45—C46115.6 (4)
Mo4—O3—Mo590.48 (10)N3—C45—H45B108.4
Mo4—O3—Mo691.32 (11)C46—C45—H45B108.4
Mo5—O3—Mo189.78 (9)N3—C45—H45A108.4
Mo5—O3—Mo288.97 (10)C46—C45—H45A108.4
Mo5—O3—Mo6178.17 (15)H45B—C45—H45A107.4
Mo6—O3—Mo189.91 (10)C49—C46—C45108.6 (8)
Mo6—O3—Mo289.23 (10)C45—C46—C47111.4 (7)
Mo3—O9—Mo4114.15 (14)C49—C46—H46D110.0
Mo4—O10—Mo5114.69 (14)C45—C46—H46D110.0
Mo1—O11—Mo4114.13 (15)C49—C46—H46C110.0
Mo6—O12—Mo4113.99 (14)C45—C46—H46C110.0
Mo3—O13—Mo6116.13 (14)H46D—C46—H46C108.4
Mo5—O14—Mo3116.64 (14)C45—C46—H46A109.4
Mo1—O15—Mo5116.52 (14)C47—C46—H46A109.4
Mo6—O16—Mo1116.47 (14)C45—C46—H46B109.4
Mo2—O17—Mo3117.11 (16)C47—C46—H46B109.4
Mo5—O18—Mo2117.47 (16)H46A—C46—H46B108.0
Mo1—O19—Mo2118.34 (16)C48—C47—C46119.8 (11)
Mo2—O20—Mo6118.01 (15)C46—C47—H47A107.4
C1—N1—Mo4160.7 (5)C46—C47—H47B107.4
C1A—N1—Mo4167.6 (5)C48—C47—H47A107.4
N1—C1—C2117.6 (9)C48—C47—H47B107.4
N1—C1—C6123.4 (9)H47A—C47—H47B106.9
C6—C1—C2118.8 (9)C50—C49—C46107.7 (13)
C3—C2—C1120.5 (10)C46—C49—H49A110.2
C3—C2—H2119.7C46—C49—H49B110.2
C1—C2—H2119.7C50—C49—H49A110.2
C4—C3—C2119.8 (10)C50—C49—H49B110.2
C4—C3—H3120.1H49A—C49—H49B108.5
C2—C3—H3120.1C49—C50—H50A109.5
C3—C4—C5120.9 (11)C49—C50—H50B109.5
C3—C4—H4119.6C49—C50—H50C109.5
C5—C4—H4119.6H50B—C50—H50C109.5
C4—C5—C6120.4 (12)H50B—C50—H50A109.5
C4—C5—H5119.8H50A—C50—H50C109.5
C6—C5—H5119.8C52—C51—N3114.8 (4)
C5—C6—C1119.5 (11)N3—C51—H51A108.6
C5—C6—C7118.0 (10)N3—C51—H51B108.6
C1—C6—C7122.5 (10)C52—C51—H51A108.6
O1—C7—O2123.9 (12)C52—C51—H51B108.6
O1—C7—C6121.2 (11)H51B—C51—H51A107.5
O2—C7—C6115.0 (9)C51—C52—C53112.9 (5)
C7—O2—C8115.7 (10)C51—C52—H52A109.0
O2—C8—C9107.3 (11)C51—C52—H52B109.0
O2—C8—H8A110.3C53—C52—H52A109.0
O2—C8—H8B110.3C53—C52—H52B109.0
C9—C8—H8A110.3H52B—C52—H52A107.8
C9—C8—H8B110.3C52—C53—H53A110.9
H8B—C8—H8A108.5C52—C53—H53B110.9
C8—C9—H9A109.5C52—C53—H53C108.1
C8—C9—H9C109.5C52—C53—H53D108.1
H9C—C9—H9A109.5C54—C53—C52104.4 (7)
C8—C9—H9B109.5C54—C53—H53A110.9
H9A—C9—H9B109.5C54—C53—H53B110.9
H9C—C9—H9B109.5C55—C53—C52116.7 (7)
N1—C1A—C6A125.0 (8)C55—C53—H53A131.0
N1—C1A—C2A115.3 (8)C55—C53—H53C108.1
C6A—C1A—C2A119.7 (8)C55—C53—H53D108.1
C3A—C2A—C1A119.3 (8)H53A—C53—H53B108.9
C3A—C2A—H2A120.4H53C—C53—H53D107.3
C1A—C2A—H2A120.4C53—C54—H54A109.5
C4A—C3A—C2A120.8 (9)C53—C54—H54B109.5
C4A—C3A—H3A119.6C53—C54—H54C109.5
C2A—C3A—H3A119.6H54B—C54—H54A109.5
C3A—C4A—C5A120.3 (10)H54C—C54—H54A109.5
C3A—C4A—H4A119.8H54B—C54—H54C109.5
C5A—C4A—H4A119.8C53—C55—H55A109.5
C4A—C5A—C6A121.1 (9)C53—C55—H55B109.5
C4A—C5A—H5A119.4C53—C55—H55C109.5
C6A—C5A—H5A119.4H55A—C55—H55B109.5
C5A—C6A—C1A118.8 (9)H55A—C55—H55C109.5
C5A—C6A—C7A117.0 (9)H55B—C55—H55C109.5
C1A—C6A—C7A124.1 (8)N3—C56—C57120.2 (6)
O1A—C7A—O2A124.3 (11)N3—C56—C60110.3 (5)
O1A—C7A—C6A122.0 (10)N3—C56—H56A109.6
O2A—C7A—C6A113.7 (8)N3—C56—H56B109.6
C7A—O2A—C8A116.9 (9)N3—C56—H56C107.3
O2A—C8A—C9A111.0 (10)N3—C56—H56D107.3
H8AA—C8A—H8AB108.0C57—C56—H56C107.3
O2A—C8A—H8AA109.4C57—C56—H56D107.3
O2A—C8A—H8AB109.4C60—C56—H56A109.6
C9A—C8A—H8AA109.4C60—C56—H56B109.6
C9A—C8A—H8AB109.4C60—C56—H56D140.1
C21—N2—C25111.4 (3)H56A—C56—H56B108.1
C21—N2—C29106.6 (3)H56D—C56—H56C106.9
C21—N2—C33112.0 (3)C58—C57—C56114.3 (11)
C25—N2—C29110.8 (3)C56—C57—H57A108.7
C33—N2—C25105.1 (3)C56—C57—H57B108.7
C33—N2—C29111.0 (3)C58—C57—H57A108.7
N2—C21—C22116.4 (3)C58—C57—H57B108.7
N2—C21—H21B108.2H57B—C57—H57A107.6
N2—C21—H21A108.2C59—C58—C57110.0 (17)
C22—C21—H21B108.2C59—C58—H58A109.7
C22—C21—H21A108.2C59—C58—H58B109.7
H21B—C21—H21A107.3C57—C58—H58A109.7
C23—C22—C21110.4 (4)C57—C58—H58B109.7
C21—C22—H22A109.6H58A—C58—H58B108.2
C21—C22—H22B109.6C58—C59—H59A109.5
C23—C22—H22A109.6C58—C59—H59B109.5
C23—C22—H22B109.6C58—C59—H59C109.5
H22B—C22—H22A108.1H59B—C59—H59A109.5
C24—C23—C22114.4 (4)H59C—C59—H59A109.5
C22—C23—H23A108.7H59B—C59—H59C109.5
C22—C23—H23B108.7C56—C60—H60A110.5
C24—C23—H23A108.7C56—C60—H60B110.5
C24—C23—H23B108.7C61—C60—C56106.4 (7)
H23A—C23—H23B107.6C61—C60—H60A110.5
C23—C24—H24A109.5C61—C60—H60B110.5
C23—C24—H24B109.5H60A—C60—H60B108.6
C23—C24—H24C109.5C62—C61—C60113.7 (11)
H24A—C24—H24B109.5C60—C61—H61A108.8
H24A—C24—H24C109.5C60—C61—H61B108.8
H24B—C24—H24C109.5C62—C61—H61A108.8
C26—C25—N2116.7 (3)C62—C61—H61B108.8
C26—C25—H25A108.1H61A—C61—H61B107.7
N2—C25—H25A108.1O103—C102—C101106.6 (15)
N2—C25—H25B108.1O103—C102—H10G110.4
C26—C25—H25B108.1C101—C102—H10G110.4
H25A—C25—H25B107.3O103—C102—H10F110.4
C25—C26—C27108.9 (4)C101—C102—H10F110.4
C25—C26—H26A109.9H10G—C102—H10F108.6
C25—C26—H26B109.9C102—O103—C104109.1 (16)
C27—C26—H26A109.9O103—C104—C105102.8 (15)
C27—C26—H26B109.9O103—C104—H10D111.2
H26A—C26—H26B108.3C105—C104—H10D111.2
C28—C27—C26112.5 (4)O103—C104—H10E111.2
C26—C27—H27A109.1C105—C104—H10E111.2
C26—C27—H27B109.1H10D—C104—H10E109.1
O4—Mo1—O19—Mo2−179.71 (18)O20—Mo2—O3—Mo193.44 (12)
O15—Mo1—O19—Mo2−74.02 (19)O17—Mo2—O3—Mo1−173.77 (13)
O11—Mo1—O19—Mo222.5 (4)O19—Mo2—O3—Mo12.81 (11)
O16—Mo1—O19—Mo280.02 (18)O18—Mo2—O3—Mo1−84.60 (11)
O3—Mo1—O19—Mo23.94 (16)O6—Mo6—O16—Mo1−179.33 (17)
O8—Mo2—O19—Mo1175.2 (2)O12—Mo6—O16—Mo1−74.46 (18)
O20—Mo2—O19—Mo1−80.93 (19)O20—Mo6—O16—Mo176.68 (17)
O17—Mo2—O19—Mo13.2 (4)O13—Mo6—O16—Mo111.7 (4)
O18—Mo2—O19—Mo172.75 (19)O3—Mo6—O16—Mo11.01 (15)
O3—Mo2—O19—Mo1−3.93 (16)O4—Mo1—O16—Mo6179.14 (19)
O4—Mo1—O11—Mo4175.01 (16)O15—Mo1—O16—Mo6−0.9 (4)
O15—Mo1—O11—Mo469.13 (16)O11—Mo1—O16—Mo676.23 (18)
O19—Mo1—O11—Mo4−27.3 (4)O19—Mo1—O16—Mo6−79.04 (18)
O16—Mo1—O11—Mo4−85.01 (15)O3—Mo1—O16—Mo6−1.03 (15)
O3—Mo1—O11—Mo4−8.68 (13)O4—Mo1—O15—Mo5176.53 (18)
N1—Mo4—O11—Mo1−175.19 (17)O11—Mo1—O15—Mo5−78.21 (18)
O10—Mo4—O11—Mo1−69.95 (16)O19—Mo1—O15—Mo572.61 (19)
O9—Mo4—O11—Mo119.6 (4)O16—Mo1—O15—Mo5−3.4 (4)
O12—Mo4—O11—Mo187.10 (16)O3—Mo1—O15—Mo5−3.30 (16)
O3—Mo4—O11—Mo19.16 (14)O7—Mo5—O15—Mo1−178.03 (19)
O5—Mo3—O9—Mo4−177.97 (16)O14—Mo5—O15—Mo16.7 (4)
O13—Mo3—O9—Mo474.70 (16)O18—Mo5—O15—Mo1−75.26 (19)
O17—Mo3—O9—Mo4−22.2 (4)O10—Mo5—O15—Mo180.01 (18)
O14—Mo3—O9—Mo4−78.99 (15)O3—Mo5—O15—Mo13.35 (16)
O3—Mo3—O9—Mo4−3.14 (13)N1—Mo4—O10—Mo5−174.82 (16)
N1—Mo4—O9—Mo3−172.43 (17)O11—Mo4—O10—Mo582.24 (16)
O10—Mo4—O9—Mo383.00 (16)O9—Mo4—O10—Mo5−73.81 (15)
O11—Mo4—O9—Mo3−7.2 (4)O12—Mo4—O10—Mo5−0.9 (4)
O12—Mo4—O9—Mo3−74.91 (15)O3—Mo4—O10—Mo54.01 (13)
O3—Mo4—O9—Mo33.32 (14)O7—Mo5—O10—Mo4179.02 (16)
O6—Mo6—O12—Mo4177.05 (15)O14—Mo5—O10—Mo474.07 (16)
O16—Mo6—O12—Mo470.64 (16)O18—Mo5—O10—Mo4−21.6 (3)
O20—Mo6—O12—Mo4−24.5 (3)O15—Mo5—O10—Mo4−80.33 (16)
O13—Mo6—O12—Mo4−82.25 (15)O3—Mo5—O10—Mo4−3.83 (13)
O3—Mo6—O12—Mo4−6.83 (13)O8—Mo2—O20—Mo6174.89 (18)
N1—Mo4—O12—Mo6−173.72 (17)O17—Mo2—O20—Mo6−81.03 (18)
O10—Mo4—O12—Mo612.2 (4)O19—Mo2—O20—Mo671.35 (18)
O11—Mo4—O12—Mo6−72.00 (16)O18—Mo2—O20—Mo6−0.7 (4)
O9—Mo4—O12—Mo685.89 (16)O3—Mo2—O20—Mo6−4.77 (15)
O3—Mo4—O12—Mo67.28 (13)O6—Mo6—O20—Mo2−179.06 (17)
O7—Mo5—O14—Mo3−179.84 (17)O16—Mo6—O20—Mo2−73.96 (18)
O18—Mo5—O14—Mo375.05 (17)O12—Mo6—O20—Mo222.6 (4)
O10—Mo5—O14—Mo3−76.01 (17)O13—Mo6—O20—Mo281.31 (17)
O15—Mo5—O14—Mo3−4.7 (4)O3—Mo6—O20—Mo24.81 (15)
O3—Mo5—O14—Mo3−1.32 (14)O7—Mo5—O18—Mo2−175.81 (17)
O5—Mo3—O14—Mo5−177.62 (18)O14—Mo5—O18—Mo2−70.14 (18)
O13—Mo3—O14—Mo5−6.4 (4)O10—Mo5—O18—Mo224.8 (4)
O9—Mo3—O14—Mo579.21 (17)O15—Mo5—O18—Mo283.29 (17)
O17—Mo3—O14—Mo5−76.96 (17)O3—Mo5—O18—Mo27.26 (15)
O3—Mo3—O14—Mo51.35 (15)O8—Mo2—O18—Mo5173.04 (18)
O5—Mo3—O13—Mo6−178.02 (18)O20—Mo2—O18—Mo5−11.4 (4)
O9—Mo3—O13—Mo6−72.28 (18)O17—Mo2—O18—Mo569.86 (18)
O17—Mo3—O13—Mo679.47 (18)O19—Mo2—O18—Mo5−84.18 (18)
O14—Mo3—O13—Mo611.0 (4)O3—Mo2—O18—Mo5−7.27 (15)
O3—Mo3—O13—Mo63.35 (16)C21—N2—C29—C30−167.3 (4)
O6—Mo6—O13—Mo3176.61 (19)C33—N2—C29—C30−45.0 (5)
O16—Mo6—O13—Mo3−14.3 (4)C25—N2—C29—C3071.3 (5)
O12—Mo6—O13—Mo374.21 (18)C21—N2—C25—C26−51.8 (5)
O20—Mo6—O13—Mo3−81.21 (19)C33—N2—C25—C26−173.3 (4)
O3—Mo6—O13—Mo3−3.39 (16)C29—N2—C25—C2666.7 (5)
O8—Mo2—O17—Mo3172.49 (19)C21—N2—C33—C3459.5 (5)
O20—Mo2—O17—Mo368.09 (18)C25—N2—C33—C34−179.3 (4)
O19—Mo2—O17—Mo3−15.5 (4)C29—N2—C33—C34−59.6 (5)
O18—Mo2—O17—Mo3−84.62 (18)N2—C25—C26—C27175.1 (4)
O3—Mo2—O17—Mo3−8.38 (15)N2—C29—C30—C31−176.6 (4)
O5—Mo3—O17—Mo2−176.45 (18)N2—C33—C34—C35170.9 (4)
O13—Mo3—O17—Mo2−70.27 (18)C29—C30—C31—C32−168.1 (4)
O9—Mo3—O17—Mo227.6 (4)C25—C26—C27—C28−180.0 (4)
O14—Mo3—O17—Mo284.99 (18)C56—N3—C41—C4264.8 (6)
O3—Mo3—O17—Mo28.48 (15)C45—N3—C41—C42−174.4 (5)
O10—Mo4—O3—Mo3−93.22 (11)C51—N3—C41—C42−53.6 (6)
O11—Mo4—O3—Mo3173.23 (12)C56—N3—C45—C46−59.2 (7)
O9—Mo4—O3—Mo3−2.43 (10)C41—N3—C45—C46−179.8 (6)
O12—Mo4—O3—Mo384.82 (11)C51—N3—C45—C4658.5 (7)
O10—Mo4—O3—Mo5−3.01 (10)C44—C43—C42—C4172.5 (7)
O11—Mo4—O3—Mo5−96.56 (11)N3—C41—C42—C43−167.8 (5)
O9—Mo4—O3—Mo587.77 (11)C33—C34—C35—C37168.2 (8)
O12—Mo4—O3—Mo5175.02 (11)C33—C34—C35—C36−85.9 (7)
O10—Mo4—O3—Mo6176.69 (12)C33—N2—C21—C2260.4 (5)
O11—Mo4—O3—Mo683.14 (11)C25—N2—C21—C22−57.1 (5)
O9—Mo4—O3—Mo6−92.53 (11)C29—N2—C21—C22−178.1 (4)
O12—Mo4—O3—Mo6−5.27 (10)N2—C21—C22—C23177.9 (4)
O10—Mo4—O3—Mo186.77 (11)C56—N3—C51—C52179.5 (5)
O11—Mo4—O3—Mo1−6.78 (10)C41—N3—C51—C52−59.5 (6)
O9—Mo4—O3—Mo1177.55 (12)C45—N3—C51—C5259.0 (6)
O12—Mo4—O3—Mo1−95.19 (11)C21—C22—C23—C24179.1 (5)
O13—Mo3—O3—Mo4−93.96 (14)N3—C51—C52—C53178.3 (5)
O9—Mo3—O3—Mo42.59 (11)C55—C53—C52—C51−165.7 (8)
O17—Mo3—O3—Mo4173.35 (13)C54—C53—C52—C51−93.1 (8)
O14—Mo3—O3—Mo489.54 (12)C41—N3—C56—C5737.4 (9)
O13—Mo3—O3—Mo5175.55 (14)C45—N3—C56—C57−80.6 (9)
O9—Mo3—O3—Mo5−87.89 (12)C51—N3—C56—C57159.1 (8)
O17—Mo3—O3—Mo582.87 (12)C41—N3—C56—C6080.9 (7)
O14—Mo3—O3—Mo5−0.95 (10)C45—N3—C56—C60−37.2 (7)
O13—Mo3—O3—Mo6−2.64 (12)C51—N3—C56—C60−157.4 (6)
O9—Mo3—O3—Mo693.91 (12)N3—C56—C60—C61−176.1 (7)
O17—Mo3—O3—Mo6−95.32 (12)C57—C56—C60—C61−62.9 (9)
O14—Mo3—O3—Mo6−179.14 (13)N3—C45—C46—C49156.9 (12)
O13—Mo3—O3—Mo286.59 (13)N3—C45—C46—C47178.4 (8)
O9—Mo3—O3—Mo2−176.86 (12)C48—C47—C46—C49−102 (3)
O17—Mo3—O3—Mo2−6.09 (11)C48—C47—C46—C45172.1 (10)
O14—Mo3—O3—Mo2−89.91 (12)C56—C60—C61—C6266.5 (12)
O14—Mo5—O3—Mo4−90.25 (12)O10—Mo4—N1—C1A−160 (2)
O18—Mo5—O3—Mo4174.26 (13)O11—Mo4—N1—C1A−65 (2)
O10—Mo5—O3—Mo43.00 (10)O9—Mo4—N1—C1A109 (2)
O15—Mo5—O3—Mo488.19 (12)O12—Mo4—N1—C1A23 (2)
O14—Mo5—O3—Mo31.04 (11)O10—Mo4—N1—C1117 (2)
O18—Mo5—O3—Mo3−94.45 (12)O11—Mo4—N1—C1−148 (2)
O10—Mo5—O3—Mo394.29 (12)O9—Mo4—N1—C126 (2)
O15—Mo5—O3—Mo3179.48 (14)O12—Mo4—N1—C1−60 (2)
O14—Mo5—O3—Mo1179.20 (13)C1—N1—C1A—C6A−149 (3)
O18—Mo5—O3—Mo183.72 (12)Mo4—N1—C1A—C6A95 (2)
O10—Mo5—O3—Mo1−87.55 (11)C1—N1—C1A—C2A33 (2)
O15—Mo5—O3—Mo1−2.35 (11)Mo4—N1—C1A—C2A−84 (2)
O14—Mo5—O3—Mo290.13 (12)N1—C1A—C2A—C3A177.4 (8)
O18—Mo5—O3—Mo2−5.36 (11)C6A—C1A—C2A—C3A−1.0 (15)
O10—Mo5—O3—Mo2−176.62 (12)C1A—C2A—C3A—C4A−0.3 (14)
O15—Mo5—O3—Mo2−91.43 (12)C2A—C3A—C4A—C5A1.4 (16)
O16—Mo6—O3—Mo4−91.34 (13)C3A—C4A—C5A—C6A−1.2 (15)
O12—Mo6—O3—Mo45.72 (10)C4A—C5A—C6A—C1A−0.1 (14)
O20—Mo6—O3—Mo4176.98 (13)C4A—C5A—C6A—C7A−179.9 (10)
O13—Mo6—O3—Mo493.69 (12)N1—C1A—C6A—C5A−177.1 (9)
O16—Mo6—O3—Mo3177.37 (14)C2A—C1A—C6A—C5A1.2 (14)
O12—Mo6—O3—Mo3−85.57 (11)N1—C1A—C6A—C7A2.7 (17)
O20—Mo6—O3—Mo385.68 (12)C2A—C1A—C6A—C7A−179.0 (10)
O13—Mo6—O3—Mo32.40 (11)C5A—C6A—C7A—O1A10.0 (16)
O16—Mo6—O3—Mo1−0.80 (12)C1A—C6A—C7A—O1A−169.8 (11)
O12—Mo6—O3—Mo196.27 (12)C5A—C6A—C7A—O2A−170.7 (9)
O20—Mo6—O3—Mo1−92.48 (12)C1A—C6A—C7A—O2A9.5 (16)
O13—Mo6—O3—Mo1−175.76 (14)O1A—C7A—O2A—C8A1.3 (18)
O16—Mo6—O3—Mo288.28 (12)C6A—C7A—O2A—C8A−178.1 (9)
O12—Mo6—O3—Mo2−174.66 (12)C7A—O2A—C8A—C9A76.1 (15)
O20—Mo6—O3—Mo2−3.41 (10)C1A—N1—C1—C618.7 (17)
O13—Mo6—O3—Mo2−86.69 (12)Mo4—N1—C1—C6163.2 (11)
O15—Mo1—O3—Mo4−87.90 (13)C1A—N1—C1—C2−157 (4)
O11—Mo1—O3—Mo46.99 (11)Mo4—N1—C1—C2−13 (3)
O19—Mo1—O3—Mo4177.71 (14)N1—C1—C2—C3175.3 (10)
O16—Mo1—O3—Mo492.04 (12)C6—C1—C2—C3−0.8 (19)
O15—Mo1—O3—Mo52.58 (12)C1—C2—C3—C4−1.1 (17)
O11—Mo1—O3—Mo597.46 (12)C2—C3—C4—C51.1 (18)
O19—Mo1—O3—Mo5−91.81 (13)C3—C4—C5—C61.0 (19)
O16—Mo1—O3—Mo5−177.48 (13)C4—C5—C6—C1−2.9 (19)
O15—Mo1—O3—Mo6−179.22 (14)C4—C5—C6—C7178.5 (11)
O11—Mo1—O3—Mo6−84.33 (12)N1—C1—C6—C5−173.1 (12)
O19—Mo1—O3—Mo686.39 (13)C2—C1—C6—C52.8 (19)
O16—Mo1—O3—Mo60.72 (11)N1—C1—C6—C75 (2)
O15—Mo1—O3—Mo291.55 (13)C2—C1—C6—C7−178.7 (11)
O11—Mo1—O3—Mo2−173.57 (12)C5—C6—C7—O124.4 (17)
O19—Mo1—O3—Mo2−2.84 (12)C1—C6—C7—O1−154.1 (12)
O16—Mo1—O3—Mo2−88.51 (12)C5—C6—C7—O2−155.5 (12)
O20—Mo2—O3—Mo3−86.56 (12)C1—C6—C7—O225.9 (17)
O17—Mo2—O3—Mo36.23 (12)O1—C7—O2—C8−0.5 (18)
O19—Mo2—O3—Mo3−177.18 (13)C6—C7—O2—C8179.5 (10)
O18—Mo2—O3—Mo395.40 (12)C7—O2—C8—C9152.8 (12)
O20—Mo2—O3—Mo5−176.77 (12)C102—O103—C104—C105−168 (2)
O17—Mo2—O3—Mo5−83.98 (12)C104—O103—C102—C101−180 (2)
O19—Mo2—O3—Mo592.61 (12)N3—C56—C57—C58−165.0 (12)
O18—Mo2—O3—Mo55.19 (10)C60—C56—C57—C58108.8 (16)
O20—Mo2—O3—Mo63.52 (11)C56—C57—C58—C59−169.8 (13)
O17—Mo2—O3—Mo696.31 (12)C45—C46—C49—C50−172.0 (13)
O19—Mo2—O3—Mo6−87.10 (12)C47—C46—C49—C5087 (3)
O18—Mo2—O3—Mo6−174.52 (12)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C3A—H3A···O19i0.932.383.287 (9)164
C5—H5···O7ii0.932.583.449 (14)155
C21—H21B···O15i0.972.433.354 (5)159
C25—H25A···O6iii0.972.583.544 (5)173
C41—H41B···O140.972.563.480 (6)158
C44—H44B···O8i0.962.573.495 (8)162
C45—H45A···O1Aii0.972.453.345 (8)153
C45—H45A···O1ii0.972.223.103 (9)151
C32—H32B···O130.962.543.387 (6)147
C3—H3···O19i0.932.472.986 (10)115
C37—H37A···O4iii0.962.603.173 (14)118
C5A—H5A···O7ii0.932.493.133 (9)126
C9—H9C···O110.962.543.25 (2)130
C9A—H9AC···O110.962.483.262 (10)138
Symmetry codes: (i) x−1/2, −y+3/2, z−1/2; (ii) −x, −y+1, −z+1; (iii) −x, −y+2, −z+1.

Experimental details

Crystal data
Chemical formula(C16H36N)2[Mo6O18(C9H9NO2)]·0.5C4H10O
Mr1548.79
Crystal system, space groupMonoclinic, P21/n
Temperature (K)101
a, b, c (Å)16.3974 (16), 17.0854 (8), 21.687 (3)
β (°) 106.709 (16)
V (Å3)5819.1 (10)
Z4
Radiation typeMo Kα
µ (mm−1)1.33
Crystal size (mm)0.40 × 0.30 × 0.25
Data collection
DiffractometerAgilent Xcalibur Eos Gemini
Absorption correctionMulti-scan
(CrysAlis PRO; Agilent, 2011)
Tmin, Tmax0.619, 0.733
No. of measured, independent and
observed [I > 2σ(I)] reflections		31709, 11422, 8774
Rint0.038
(sin θ/λ)max (Å−1)0.617
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.039, 0.088, 1.05
No. of reflections11422
No. of parameters854
No. of restraints500
H-atom treatmentH-atom parameters constrained
w = 1/[σ2(Fo2) + (0.0243P)2 + 15.7229P]
where P = (Fo2 + 2Fc2)/3
Δρmax, Δρmin (e Å−3)1.46, −0.81

Computer programs: CrysAlis PRO (Agilent, 2011), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), DIAMOND (Brandenburg, 2010), publCIF (Westrip, 2010).

Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C3A—H3A···O19i0.932.383.287 (9)164.1
C5—H5···O7ii0.932.583.449 (14)154.9
C21—H21B···O15i0.972.433.354 (5)158.8
C25—H25A···O6iii0.972.583.544 (5)172.7
C41—H41B···O140.972.563.480 (6)158.1
C44—H44B···O8i0.962.573.495 (8)161.6
C45—H45A···O1Aii0.972.453.345 (8)153.3
C45—H45A···O1ii0.972.223.103 (9)151.2
Symmetry codes: (i) x−1/2, −y+3/2, z−1/2; (ii) −x, −y+1, −z+1; (iii) −x, −y+2, −z+1.
 

Acknowledgements

This work was supported by the Beijing Forestry University Young Scientist Fund (2008XJS16). We also sincerely thank Jin Zhang of Tsinghua University for her help with the figures.

References

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Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890
Volume 68| Part 7| July 2012| Pages m926-m927
https://doi.org/10.1107/S1600536812026323
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