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

Journal logoIUCrDATA
ISSN: 2414-3146
Volume 9| Part 5| May 2024| x240463
https://doi.org/10.1107/S2414314624004632

Octa­kis(di­butyl­ammonium) deca­molybdate(VI)

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Papa Aly Gueye,a* Lamine Yaffa,a Dame Seye,b Daouda Ndoye,a Bocar Traoré,a Mamadou Sidibé,a Cheikh Abdoul Khadir Diopa and Sergiu Shovac

aLaboratoire de Chimie Minérale et Analytique (LACHIMIA), Département de Chimie, Faculté des Sciences et Techniques, Université Cheikh Anta Diop de Dakar, Senegal, bDépartement Physique Chimie, UFR Sciences et Technologies, Université Ibra Der Thiam de Thiès, Senegal, and cInorganic Polymers Department, "Petru Poni" Institute of Macramolecular Chemistry, Alea Gr. Ghica Voda 41 A, Iasi 700487, Romania
*Correspondence e-mail: papaaly1.gueye@ucad.edu.sn

Edited by M. Weil, Vienna University of Technology, Austria (Received 6 March 2024; accepted 18 May 2024; online 31 May 2024)

This article is part of a collection of articles to commemorate the founding of the African Crystallographic Association and the 75th anniversary of the IUCr.

In the title salt, (C8H20N)8[Mo10O34], the [Mo10O34]8− polyanion is located about an inversion centre and can be considered as a β-type octa­molybdate anion to which two additional MoO4 tetra­hedra are linked via common corners. The [Mo10O34]8− polyanions are packed in rows extending parallel to [001] and are connected to the di­butyl­ammonium counter-cations through N—H⋯O hydrogen-bonding inter­actions.

CCDC reference: 2332866

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[Scheme 3D1]
Chemical scheme
[Scheme 1]

Structure description

Polyoxometalates (POMs) are obtained by self-assembly of transition-metal oxide units [MOn]p− in acidic media (M = metal; n = 3, 4, 6, ⋯; p = 0, 1, 2, 3, ⋯). POMs and their derivatives are an important group of materials that have attracted considerable inter­est in areas such as electrochemistry (Zhang et al., 2021[Zhang, J. Y., Chang, Z. H., Wang, X. L., Wang, X. & Lin, H. Y. (2021). New J. Chem. 45, 3328-3334.]), materials science (Hao et al., 2007[Hao, J., Ruhlmann, L., Zhu, Y., Li, Q. & Wei, Y. (2007). Inorg. Chem. 46, 4960-4967.]; Li et al., 2007[Li, T., Lü, J., Gao, S., Li, F. & Cao, R. (2007). Chem. Lett. 36, 356-357.]), and medicine (Cronin et al., 2002[Cronin, L., Beugholt, C., Krickemeyer, E., Schmidtmann, M., Bögge, H., Kögerler, P., Luong, T. K. K. & Müller, A. (2002). Angew. Chem. Int. Ed. 41, 2805-2808.]; Müller et al., 1999[Müller, A., Shah, S. Q. N., Bögge, H. & Schmidtmann, M. (1999). Nature, 397, 48-50.]). In recent years, research on organic–inorganic hybrid POMs has experienced significant growth, supported by possible modifications and/or functional­izations of the oxide surface of the POM with preselected organic moieties (Xu et al., 2003[Xu, L., Qin, C., Wang, X., Wei, Y. & Wang, E. (2003). Inorg. Chem. 42, 7342-7344.]). The structural diversity of the corresponding isopolyoxomolybdates is due to characteristic large polyanionic units and organic ammonium cations, which consolidate the crystal structures through non-covalent supra­molecular inter­actions. In this regard, several octa­molybdate polyanions [Mo8O26]4–, charge-balanced by organic counter-ions, have been synthesized and structurally characterized (Allis et al., 2004[Allis, D. G., Burkholder, E. & Zubieta, J. A. (2004). Polyhedron, 23, 1145-1152.]; Harchani & Haddad, 2015[Harchani, A. & Haddad, A. (2015). J. Clust Sci. 26, 1773-1785.]). For the current study, we used diiso­butyl­ammonium as a counter-cation and obtained the hybrid organic–inorganic deca­molybdate (C8H20N)8[Mo10O34].

The asymmetric unit of (C8H20N)8[Mo10O34] is shown in Fig. 1[link]. The [Mo10O34]8– anion is located about an inversion centre and is displayed in Fig. 2[link]. Such kind of deca­molybdate anion is known from other ammonium salts and has been reported for the first time for (NH4)8[Mo10O34] (Fuchs et al., 1975[Fuchs, J., Hartl, H., Hunnius, W.-D. & Mahjour, S. (1975). Angew. Chem. 87, 634-635.]). The [Mo10O34]8– anion can be considered as a β-type octa­molydate to which two additional MoO4 tetra­hedra are added via vertex-sharing. Two types of β-octa­molybdate anions can be distinguished, type A with the general formula [Mo8O26]4– and type B with the general formula [HxMo8O28](8–x) (Pavani et al., 2007[Pavani, K., Lofland, S. E., Ramanujachary, K. V. & Ramanan, A. (2007). Eur. J. Inorg. Chem. pp. 568-578.]). Thus, the [Mo10O34]8– anion of the title compound can be considered as of the β-octa­molybdate B type (Du et al. 2011[Du, J., Yu, J., Tang, J., Wang, J., Zhang, W., Thiel, W. R. & Jia, M. (2011). Eur. J. Inorg. Chem. pp. 2361-2365.]; Isobe et al. 1978[Isobe, M., Marumo, F., Yamase, T. & Ikawa, T. (1978). Acta Cryst. B34, 2728-2731.]).

[Figure 1]
Figure 1
The asymmetric unit of the title compound. Displacement ellipsoids are drawn at the 50% probability level. Dotted lines indicate N—H⋯O hydrogen-bonding inter­actions. The C-bound H atoms are omitted for clarity.
[Figure 2]
Figure 2
The centrosymmetric [Mo10O34]8– polyanion in the title compound. Displacement ellipsoids are drawn at the 50% probability level.

The [Mo10O34]8– polyanion is made up of eight MoO6 octa­hedra linked to each other by edge and/or vertex sharing, building up an octa­molybdate anion. Similar POMs with an Mo8 core linked to the ends by MoxOy groups are found in the crystal structures of [NH3(CH2)2NH2(CH2)2NH3]2[Mo9O30] and [NH3(CH2)2NH2(CH2)3NH3]2[Mo10O33] (Chakrabarti & Natarajan, 2002[Chakrabarti, S. & Natarajan, S. (2002). Cryst. Growth Des. 2, 333-335.]). In (C8H20N)8[Mo10O34], the β-octa­molybdate polyanion is linked with two additional MoO4 tetra­hedra, which can be expressed by the formula [(MoO3)2β-Mo8O28]8–. Bond-valence calculations show that the five crystallographically unique Mo atoms are in the +VI oxidation state. According to the role of the oxygen ligands (terminal or bridging) in the β-octa­molybdate moiety, the corresponding Mo—O bond lengths for Mo1–Mo4 range from 1.703 (3) to 2.451 (3) Å and the O—Mo—O bond angles from 71.01 (12) to 179.57 (14)°. These values are in the range expected for octa­hedrally coordinated MoVI atoms and in agreement with those in the previously reported octa­molybdate structure. (Pavani & Ramanan, 2005[Pavani, K. & Ramanan, A. (2005). Eur. J. Inorg. Chem. pp. 3080-3087.]; Wu et al., 2002[Wu, C.-D., Lu, C.-Z., Zhuang, H.-H. & Huang, J.-S. (2002). Inorg. Chem. 41, 5636-5637.]). The Mo5 site is tetra­hedrally surrounded by three terminal oxygen atoms (O15, O16, O17) with bond lengths between 1.738 (4) and 1.767 (4) Å and a bridging oxygen atom O14 to the β-octa­molybdate anion with 1.804 (4) Ā. The angles of the tetra­hedron range from 107.5 (2) to 112.0 (2)°.

In the crystal, the [Mo10O34]8– polyanions are stacked into rows parallel to [001] and surrounded by di­butyl­ammonium counter-cations. Next to Coulombic inter­actions, cations and anions are linked through rather strong N—H⋯O hydrogen bonds between the ammonium cations and the terminal oxygen atoms of the MoO4 tetra­hedra (O15⋯H3A—N3 and O17⋯H3B—N3; Table 1[link], Fig. 3[link]). The other ammonium groups are involved in hydrogen-bonding inter­actions with the terminal O atoms of the β-octa­molybdate moiety (Table 1[link]).

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A D⋯A D—H⋯A
N1—H1A⋯O2i 0.91 1.72 2.627 (6) 172
N1—H1B⋯O10i 0.91 1.97 2.755 (6) 143
N2—H2C⋯O15 0.91 1.91 2.778 (6) 160
N2—H2D⋯O7ii 0.91 1.90 2.812 (5) 176
N3—H3A⋯O15iii 0.91 1.87 2.770 (6) 172
N3—H3B⋯O17 0.91 1.88 2.786 (6) 176
N4—H4A⋯O11 0.91 1.80 2.695 (6) 166
N4—H4B⋯O16 0.91 1.86 2.762 (7) 172
Symmetry codes: (i) [-x+2, -y+1, -z+1]; (ii) [-x+1, y+{\script{1\over 2}}, -z+{\script{3\over 2}}]; (iii) [-x+1, -y+1, -z+2].
[Figure 3]
Figure 3
The unit-cell packing viewed down [001] with hydrogen bonds indicated by blue dashed lines.

The UV-vis absorption spectrum of the title compound was recorded in the range 250–700 nm in aqueous solution (0.1 N) and is shown in Fig. 4[link]. It shows two absorption bands at 297 nm and 353 nm. The strongest band at 297 nm is attributed to a charge-transfer transition of the type Ot —Mo and the shoulder peak at 353 nm to a charge-transfer transition of the type Mo—O—Mo (Gong et al., 2006[Gong, Y., Hu, C., Li, H., Tang, W., Huang, K. & Hou, W. (2006). J. Mol. Struct. 784, 228-238.]; Zhang et al., 1997[Zhang, X.-M., Shan, B.-Z., You, X.-Z. & Fun, H.-K. (1997). Polyhedron, 16, 95-102.])

[Figure 4]
Figure 4
UV/Vis spectrum of the title compound.

Synthesis and crystallization

Ammonium hepta­molybdate, (NH4)6[Mo7O24]·4H2O (4.943 g), and di­butyl­amine, C8H19N (1.559 g), were dissolved in 40 ml of hot water. The mixture was heated for 2 h at 473 K under reflux and then filtered. The filtrate was kept for three months at ambient conditions, affording colourless crystals in about 8% yield (based on Mo).

Refinement

Crystal data, data collection and structure refinement details are summarized in Table 2[link].

Table 2
Experimental details

Crystal data
Chemical formula (C8H20N)8[Mo10O34]
Mr 2545.39
Crystal system, space group Monoclinic, P21/c
Temperature (K) 130
a, b, c (Å) 14.21628 (18), 20.7477 (2), 18.2210 (2)
β (°) 110.0785 (15)
V (Å3) 5047.74 (12)
Z 2
Radiation type Cu Kα
μ (mm−1) 10.44
Crystal size (mm) 0.15 × 0.03 × 0.02
 
Data collection
Diffractometer XtaLAB Synergy, Dualflex, HyPix
Absorption correction Multi-scan (CrysAlis PRO; Rigaku OD, 2023[Rigaju OD (2021). CrysAlis PRO. Rigaku Oxford Diffraction, Yarnton, England.])
Tmin, Tmax 0.500, 1.000
No. of measured, independent and observed [I > 2σ(I)] reflections 42024, 9853, 8753
Rint 0.043
(sin θ/λ)max (Å−1) 0.625
 
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.045, 0.119, 1.02
No. of reflections 9853
No. of parameters 541
No. of restraints 18
H-atom treatment H-atom parameters constrained
Δρmax, Δρmin (e Å−3) 1.65, −1.09
Computer programs: CrysAlis PRO (Rigaku OD, 2023[Rigaju OD (2021). CrysAlis PRO. Rigaku Oxford Diffraction, Yarnton, England.]), SHELXT (Sheldrick, 2015a[Sheldrick, G. M. (2015a). Acta Cryst. A71, 3-8.]), SHELXL (Sheldrick, 2015b[Sheldrick, G. M. (2015b). Acta Cryst. C71, 3-8.]) and OLEX2 (Dolomanov et al., 2009[Dolomanov, O. V., Bourhis, L. J., Gildea, R. J., Howard, J. A. K. & Puschmann, H. (2009). J. Appl. Cryst. 42, 339-341.]).

Structural data

CCDC reference: 2332866

Crystal structure: contains datablock I. DOI: https://doi.org/10.1107/S2414314624004632/wm4210sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S2414314624004632/wm4210Isup4.hkl

checkCIF report


Computing details top

Octakis(dibutylammonium) decamolybdate(VI) top
Crystal data top
(C8H20N)8[Mo10O34]F(000) = 2584
Mr = 2545.39Dx = 1.675 Mg m−3
Monoclinic, P21/cCu Kα radiation, λ = 1.54184 Å
a = 14.21628 (18) ÅCell parameters from 25536 reflections
b = 20.7477 (2) Åθ = 3.3–76.7°
c = 18.2210 (2) ŵ = 10.44 mm−1
β = 110.0785 (15)°T = 130 K
V = 5047.74 (12) Å3Needle, clear colourless
Z = 20.15 × 0.03 × 0.02 mm
Data collection top
XtaLAB Synergy, Dualflex, HyPix
diffractometer		9853 independent reflections
Radiation source: micro-focus sealed X-ray tube, PhotonJet (Cu) X-ray Source8753 reflections with I > 2σ(I)
Mirror monochromatorRint = 0.043
Detector resolution: 10.0000 pixels mm-1θmax = 74.5°, θmin = 3.3°
ω scansh = −17→14
Absorption correction: multi-scan
(CrysAlisPro; Rigaku OD, 2023)		k = −24→24
Tmin = 0.500, Tmax = 1.000l = −22→22
42024 measured reflections
Refinement top
Refinement on F2Primary atom site location: dual
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.045H-atom parameters constrained
wR(F2) = 0.119 w = 1/[σ2(Fo2) + (0.0685P)2 + 16.9839P]
where P = (Fo2 + 2Fc2)/3
S = 1.02(Δ/σ)max = 0.001
9853 reflectionsΔρmax = 1.65 e Å−3
541 parametersΔρmin = −1.09 e Å−3
18 restraints
Special details top

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

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Mo10.46738 (3)0.39489 (2)0.35188 (2)0.02715 (10)
Mo20.39496 (3)0.38023 (2)0.50285 (2)0.02920 (10)
Mo30.60253 (3)0.46487 (2)0.57062 (2)0.02504 (10)
Mo40.50325 (3)0.45478 (2)0.70777 (2)0.02984 (10)
Mo50.60971 (3)0.54579 (2)0.89668 (2)0.03279 (11)
O10.3980 (3)0.37372 (16)0.25734 (19)0.0367 (8)
O20.5564 (3)0.45633 (15)0.33548 (19)0.0323 (7)
O30.5479 (3)0.33261 (16)0.3883 (2)0.0358 (7)
O40.5043 (2)0.43977 (14)0.47119 (17)0.0248 (6)
O50.3602 (3)0.37118 (15)0.39495 (18)0.0298 (7)
O60.2865 (3)0.37049 (17)0.5231 (2)0.0386 (8)
O70.4603 (3)0.30910 (16)0.53384 (19)0.0343 (7)
O80.4764 (2)0.43107 (15)0.59639 (18)0.0284 (6)
O90.6765 (3)0.39936 (16)0.60011 (19)0.0345 (7)
O100.6746 (2)0.51676 (16)0.53399 (19)0.0305 (7)
O110.6152 (2)0.50842 (14)0.66534 (18)0.0284 (6)
O120.3977 (3)0.41825 (18)0.7121 (2)0.0425 (9)
O130.5989 (3)0.39987 (17)0.7488 (2)0.0419 (8)
O140.5422 (4)0.50320 (18)0.8079 (2)0.0483 (10)
O150.5518 (3)0.61967 (17)0.9041 (2)0.0406 (8)
O160.7336 (3)0.5584 (2)0.9045 (2)0.0486 (9)
O170.6081 (3)0.49797 (18)0.9747 (2)0.0473 (9)
N11.2542 (4)0.5261 (3)0.5803 (3)0.0528 (13)
H1A1.3178380.5331970.6133100.063*
H1B1.2579810.4981540.5428520.063*
C11.0075 (8)0.6326 (6)0.3483 (6)0.103 (4)
H1C1.0034110.6708080.3156170.155*
H1D0.9449010.6278890.3589980.155*
H1E1.0184270.5942900.3208360.155*
C21.0942 (7)0.6403 (5)0.4248 (5)0.087 (3)
H2A1.1520690.6592910.4141060.104*
H2B1.0744030.6706270.4589300.104*
C31.1249 (5)0.5784 (4)0.4665 (4)0.068 (2)
H3C1.1438490.5476960.4323360.081*
H3D1.0678470.5597940.4786130.081*
C41.2132 (5)0.5878 (4)0.5420 (4)0.0581 (16)
H4C1.2667560.6116910.5303940.070*
H4D1.1914450.6142350.5784670.070*
C51.1975 (5)0.4946 (4)0.6249 (4)0.0613 (17)
H5A1.2171670.4486460.6335710.074*
H5B1.1249200.4965060.5945920.074*
C61.2188 (7)0.5285 (5)0.7041 (5)0.078 (2)
H6A1.2920660.5335440.7298560.093*
H6B1.1885950.5720410.6952170.093*
C71.1781 (8)0.4919 (6)0.7566 (6)0.097 (3)
H7A1.2048900.4474270.7633020.116*
H7B1.1042020.4894540.7330080.116*
C81.2075 (11)0.5256 (7)0.8371 (6)0.132 (5)
H8A1.1641480.5630350.8333960.197*
H8B1.2774550.5396970.8530900.197*
H8C1.1996230.4952910.8758800.197*
N20.5610 (4)0.7400 (2)0.8400 (3)0.0435 (11)
H2C0.5587260.6971060.8498750.052*
H2D0.5511620.7617700.8801370.052*
C90.9281 (8)0.7162 (6)0.9733 (10)0.136 (5)
H9A0.9255360.7308301.0237150.204*
H9B0.9937390.7266320.9699190.204*
H9C0.9177040.6694410.9687510.204*
C100.8498 (7)0.7484 (4)0.9101 (6)0.083 (3)
H10A0.8569780.7366030.8596270.099*
H10B0.8587360.7955910.9166400.099*
C110.7436 (5)0.7304 (3)0.9077 (4)0.0569 (16)
H11A0.7379170.6828720.9081170.068*
H11B0.7338970.7470210.9555390.068*
C120.6631 (5)0.7559 (3)0.8388 (4)0.0496 (14)
H12A0.6705110.7377800.7908570.059*
H12B0.6699320.8033130.8370230.059*
C130.4791 (5)0.7553 (3)0.7679 (3)0.0521 (15)
H13A0.4875010.7300370.7244890.063*
H13B0.4827720.8015850.7557590.063*
C140.3794 (6)0.7416 (4)0.7727 (5)0.071 (2)
H14A0.3692980.7684210.8142440.085*
H14B0.3763300.6957720.7868850.085*
C150.2959 (6)0.7553 (4)0.6953 (6)0.085 (3)
H15A0.3014430.8005690.6801120.102*
H15B0.3050730.7271830.6543780.102*
C160.1939 (9)0.7446 (7)0.6986 (9)0.138 (5)
H16A0.1873670.7676910.7435060.207*
H16B0.1833560.6984270.7038950.207*
H16C0.1437020.7607230.6504030.207*
N30.5165 (4)0.3786 (2)0.9706 (3)0.0484 (12)
H3A0.4981440.3764341.0137610.058*
H3B0.5489260.4167750.9727300.058*
C180.2616 (9)0.3213 (6)0.8363 (6)0.105 (3)
H18A0.2613410.3527060.7952950.126*0.333 (15)
H18B0.2440140.2785600.8110630.126*0.333 (15)
H18C0.2270940.3595990.8472260.126*0.667 (15)
H18D0.2672730.3273100.7840330.126*0.667 (15)
C190.3625 (8)0.3181 (4)0.8945 (6)0.091 (3)
H19A0.3985490.2815990.8813100.110*
H19B0.3568310.3090390.9461310.110*
C200.4248 (7)0.3793 (4)0.9009 (4)0.0668 (19)
H20A0.4435530.3834910.8536030.080*
H20B0.3837930.4172320.9033520.080*
C210.5880 (6)0.3257 (4)0.9748 (6)0.080 (2)
H21A0.5585980.2842380.9830430.096*
H21B0.6006950.3229880.9247520.096*
C220.6830 (8)0.3368 (6)1.0391 (7)0.102 (3)
H22A0.6687670.3397391.0885250.123*
H22B0.7103070.3789251.0306550.123*
C230.7605 (11)0.2871 (8)1.0484 (10)0.156 (6)
H23A0.7758270.2840820.9994110.187*
H23B0.7341820.2448001.0574160.187*
C240.8592 (12)0.3022 (9)1.1178 (9)0.163 (7)
H24A0.8915810.3401871.1051140.245*
H24B0.9045910.2651681.1266570.245*
H24C0.8432570.3106131.1651480.245*
C17X0.189 (2)0.3390 (16)0.868 (2)0.106 (5)0.333 (15)
H17A0.1249530.3445330.8256050.159*0.333 (15)
H17B0.2089920.3797470.8962160.159*0.333 (15)
H17C0.1835070.3054270.9036590.159*0.333 (15)
C170.2031 (13)0.2674 (8)0.8340 (12)0.106 (5)0.667 (15)
H17D0.2341060.2295590.8195330.159*0.667 (15)
H17E0.1361770.2739970.7952890.159*0.667 (15)
H17F0.1975920.2605610.8855940.159*0.667 (15)
N40.7926 (4)0.5318 (3)0.7782 (3)0.0639 (17)
H4A0.7330730.5307220.7379740.077*
H4B0.7791780.5421450.8220930.077*
C250.9612 (7)0.6165 (5)0.5961 (6)0.088 (3)
H25A0.8977920.6154230.5520360.132*
H25B0.9972530.5759330.5981680.132*
H25C1.0021220.6524880.5893470.132*
C260.9400 (8)0.6254 (5)0.6717 (7)0.097 (3)
H26A1.0045350.6289660.7153950.116*
H26B0.9033080.6663670.6688370.116*
C270.8807 (5)0.5722 (4)0.6890 (4)0.0587 (17)
H27A0.9195940.5316750.6959640.070*
H27B0.8183040.5663490.6436710.070*
C280.8530 (6)0.5842 (5)0.7627 (5)0.076 (2)
H28A0.9153320.5889590.8083610.091*
H28B0.8151980.6250500.7563180.091*
C290.8358 (6)0.4650 (5)0.7886 (5)0.084 (3)
H29C0.8512430.4510590.7420690.100*0.354 (12)
H29D0.7894720.4335820.7989990.100*0.354 (12)
H29A0.7873410.4372310.8019320.100*0.646 (12)
H29B0.8348840.4509590.7364750.100*0.646 (12)
C300.9371 (9)0.4479 (14)0.8450 (7)0.116 (9)0.646 (12)
H30A0.9513450.4020230.8380080.140*0.646 (12)
H30B0.9885240.4743330.8336780.140*0.646 (12)
C310.9435 (14)0.4588 (10)0.9272 (9)0.118 (4)0.646 (12)
H31A0.9288630.5047270.9333060.142*0.646 (12)
H31B1.0131400.4503510.9618470.142*0.646 (12)
C320.8742 (14)0.4181 (10)0.9538 (11)0.118 (4)0.646 (12)
H32A0.8111530.4117780.9102580.178*0.646 (12)
H32B0.8605890.4397400.9969010.178*0.646 (12)
H32C0.9053800.3761520.9715610.178*0.646 (12)
C30X0.930 (2)0.4727 (16)0.8584 (18)0.116 (9)0.354 (12)
H30C0.9140770.4963080.9000960.140*0.354 (12)
H30D0.9792750.4980750.8437030.140*0.354 (12)
C31X0.973 (2)0.4078 (16)0.888 (2)0.118 (4)0.354 (12)
H31C1.0408510.4136030.9269960.142*0.354 (12)
H31D0.9785450.3820110.8444730.142*0.354 (12)
C32X0.910 (2)0.3715 (18)0.926 (2)0.118 (4)0.354 (12)
H32D0.8468120.3584460.8860390.178*0.354 (12)
H32E0.8955630.3992590.9645030.178*0.354 (12)
H32F0.9462410.3331170.9523370.178*0.354 (12)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mo10.0428 (2)0.01922 (17)0.02010 (17)0.00043 (13)0.01172 (15)−0.00267 (12)
Mo20.0424 (2)0.02309 (19)0.02335 (18)−0.00671 (14)0.01292 (15)−0.00140 (13)
Mo30.03428 (19)0.01990 (17)0.02015 (17)0.00191 (13)0.00831 (14)−0.00127 (12)
Mo40.0462 (2)0.02416 (19)0.01977 (18)−0.00317 (14)0.01209 (15)−0.00028 (13)
Mo50.0532 (2)0.02420 (19)0.02242 (19)−0.00053 (15)0.01481 (17)−0.00126 (13)
O10.056 (2)0.0296 (17)0.0240 (16)−0.0013 (15)0.0126 (15)−0.0059 (13)
O20.0432 (19)0.0299 (17)0.0275 (16)0.0011 (13)0.0169 (14)−0.0018 (13)
O30.052 (2)0.0268 (17)0.0303 (17)0.0063 (14)0.0166 (15)−0.0031 (13)
O40.0383 (16)0.0193 (14)0.0198 (14)−0.0021 (12)0.0137 (12)0.0006 (11)
O50.0451 (18)0.0216 (15)0.0237 (15)−0.0047 (13)0.0130 (14)−0.0026 (12)
O60.047 (2)0.0343 (19)0.0380 (19)−0.0090 (15)0.0195 (16)−0.0030 (15)
O70.052 (2)0.0274 (17)0.0259 (16)−0.0035 (14)0.0164 (15)0.0004 (13)
O80.0424 (18)0.0222 (15)0.0220 (15)−0.0007 (13)0.0130 (13)0.0001 (12)
O90.0438 (19)0.0296 (17)0.0290 (17)0.0063 (14)0.0110 (14)−0.0011 (13)
O100.0340 (17)0.0302 (17)0.0277 (16)0.0014 (13)0.0111 (13)−0.0039 (13)
O110.0402 (17)0.0216 (15)0.0224 (15)−0.0015 (12)0.0097 (13)−0.0010 (12)
O120.065 (2)0.037 (2)0.0317 (18)−0.0111 (17)0.0241 (17)−0.0015 (15)
O130.061 (2)0.0318 (18)0.0295 (18)−0.0034 (16)0.0103 (16)0.0049 (14)
O140.086 (3)0.0331 (19)0.0272 (18)−0.0084 (19)0.0214 (19)−0.0041 (15)
O150.062 (2)0.0308 (18)0.0322 (18)0.0013 (16)0.0202 (17)−0.0009 (14)
O160.057 (2)0.044 (2)0.045 (2)0.0032 (18)0.0185 (19)−0.0007 (18)
O170.076 (3)0.0330 (19)0.0311 (19)−0.0027 (18)0.0162 (18)0.0021 (15)
N10.042 (3)0.078 (4)0.041 (3)0.005 (2)0.017 (2)−0.016 (3)
C10.089 (7)0.137 (9)0.067 (6)0.042 (6)0.005 (5)−0.010 (6)
C20.082 (6)0.102 (7)0.070 (5)0.033 (5)0.018 (4)−0.002 (5)
C30.054 (4)0.088 (6)0.060 (4)0.018 (4)0.017 (3)−0.008 (4)
C40.046 (3)0.082 (5)0.048 (3)0.009 (3)0.018 (3)−0.009 (3)
C50.052 (4)0.080 (5)0.054 (4)0.003 (3)0.021 (3)−0.007 (3)
C60.091 (6)0.087 (6)0.068 (5)0.018 (5)0.043 (5)−0.006 (4)
C70.088 (6)0.138 (9)0.069 (6)0.022 (6)0.034 (5)0.010 (6)
C80.148 (11)0.186 (13)0.058 (6)0.072 (10)0.031 (6)−0.005 (7)
N20.075 (3)0.024 (2)0.035 (2)0.003 (2)0.022 (2)−0.0035 (17)
C90.067 (6)0.115 (10)0.221 (17)−0.008 (6)0.044 (8)0.018 (10)
C100.080 (5)0.057 (5)0.125 (8)−0.010 (4)0.051 (6)0.006 (5)
C110.071 (4)0.034 (3)0.075 (5)−0.003 (3)0.037 (4)0.000 (3)
C120.082 (4)0.028 (3)0.051 (3)−0.007 (3)0.039 (3)−0.008 (2)
C130.082 (4)0.033 (3)0.039 (3)0.007 (3)0.018 (3)−0.007 (2)
C140.089 (5)0.044 (4)0.064 (5)−0.003 (3)0.005 (4)−0.002 (3)
C150.070 (5)0.064 (5)0.095 (7)0.000 (4)−0.005 (4)−0.012 (4)
C160.086 (8)0.120 (10)0.179 (15)−0.008 (7)0.010 (8)0.010 (10)
N30.076 (3)0.040 (3)0.042 (3)−0.004 (2)0.035 (3)−0.001 (2)
C180.103 (8)0.138 (10)0.080 (7)0.005 (7)0.038 (6)0.004 (6)
C190.108 (7)0.066 (5)0.074 (6)−0.014 (5)−0.002 (5)0.000 (4)
C200.103 (6)0.054 (4)0.042 (4)0.008 (4)0.023 (4)0.000 (3)
C210.071 (5)0.064 (5)0.109 (7)0.000 (4)0.035 (5)−0.018 (5)
C220.090 (7)0.112 (8)0.100 (8)0.013 (6)0.026 (6)0.019 (6)
C230.120 (10)0.151 (13)0.176 (15)0.045 (9)0.025 (10)−0.044 (11)
C240.143 (13)0.201 (18)0.128 (12)0.051 (12)0.023 (10)−0.022 (12)
C17X0.094 (10)0.100 (10)0.135 (14)−0.002 (8)0.053 (9)0.015 (9)
C170.094 (10)0.100 (10)0.135 (14)−0.002 (8)0.053 (9)0.015 (9)
N40.040 (3)0.114 (5)0.038 (3)−0.007 (3)0.013 (2)−0.019 (3)
C250.063 (5)0.129 (8)0.076 (6)−0.003 (5)0.029 (4)0.022 (5)
C260.090 (6)0.107 (8)0.106 (8)−0.035 (6)0.051 (6)−0.028 (6)
C270.039 (3)0.085 (5)0.047 (3)0.001 (3)0.009 (3)−0.007 (3)
C280.055 (4)0.116 (7)0.057 (4)−0.021 (4)0.019 (3)−0.034 (4)
C290.058 (4)0.131 (8)0.065 (5)0.012 (5)0.025 (4)0.019 (5)
C300.058 (6)0.20 (2)0.088 (10)0.030 (9)0.021 (6)0.058 (12)
C310.110 (9)0.138 (12)0.098 (9)0.018 (7)0.023 (6)0.028 (8)
C320.110 (9)0.138 (12)0.098 (9)0.018 (7)0.023 (6)0.028 (8)
C30X0.058 (6)0.20 (2)0.088 (10)0.030 (9)0.021 (6)0.058 (12)
C31X0.110 (9)0.138 (12)0.098 (9)0.018 (7)0.023 (6)0.028 (8)
C32X0.110 (9)0.138 (12)0.098 (9)0.018 (7)0.023 (6)0.028 (8)
Geometric parameters (Å, º) top
Mo1—O11.723 (3)C15—H15B0.9900
Mo1—O21.891 (3)C15—C161.489 (16)
Mo1—O31.703 (3)C16—H16A0.9800
Mo1—O42.255 (3)C16—H16B0.9800
Mo1—O52.001 (3)C16—H16C0.9800
Mo1—O11i2.291 (3)N3—H3A0.9100
Mo2—O42.211 (3)N3—H3B0.9100
Mo2—O51.865 (3)N3—C201.475 (10)
Mo2—O61.717 (4)N3—C211.481 (9)
Mo2—O71.732 (3)C18—H18A0.9900
Mo2—O82.001 (3)C18—H18B0.9900
Mo2—O10i2.354 (3)C18—H18C0.9900
Mo3—O41.941 (3)C18—H18D0.9900
Mo3—O4i2.451 (3)C18—C191.463 (14)
Mo3—O82.122 (3)C18—C17X1.386 (18)
Mo3—O91.690 (3)C18—C171.386 (16)
Mo3—O101.767 (3)C19—H19A0.9900
Mo3—O111.901 (3)C19—H19B0.9900
Mo4—O2i2.070 (3)C19—C201.529 (12)
Mo4—O81.994 (3)C20—H20A0.9900
Mo4—O112.284 (3)C20—H20B0.9900
Mo4—O121.706 (4)C21—H21A0.9900
Mo4—O131.734 (4)C21—H21B0.9900
Mo4—O141.987 (4)C21—C221.471 (14)
Mo5—O141.804 (4)C22—H22A0.9900
Mo5—O151.767 (4)C22—H22B0.9900
Mo5—O161.738 (4)C22—C231.476 (16)
Mo5—O171.741 (4)C23—H23A0.9900
N1—H1A0.9100C23—H23B0.9900
N1—H1B0.9100C23—C241.56 (2)
N1—C41.479 (9)C24—H24A0.9800
N1—C51.480 (9)C24—H24B0.9800
C1—H1C0.9800C24—H24C0.9800
C1—H1D0.9800C17X—H17A0.9800
C1—H1E0.9800C17X—H17B0.9800
C1—C21.520 (12)C17X—H17C0.9800
C2—H2A0.9900C17—H17D0.9800
C2—H2B0.9900C17—H17E0.9800
C2—C31.480 (13)C17—H17F0.9800
C3—H3C0.9900N4—H4A0.9100
C3—H3D0.9900N4—H4B0.9100
C3—C41.523 (10)N4—C281.471 (11)
C4—H4C0.9900N4—C291.500 (12)
C4—H4D0.9900C25—H25A0.9800
C5—H5A0.9900C25—H25B0.9800
C5—H5B0.9900C25—H25C0.9800
C5—C61.540 (10)C25—C261.518 (13)
C6—H6A0.9900C26—H26A0.9900
C6—H6B0.9900C26—H26B0.9900
C6—C71.485 (13)C26—C271.488 (12)
C7—H7A0.9900C27—H27A0.9900
C7—H7B0.9900C27—H27B0.9900
C7—C81.547 (14)C27—C281.543 (10)
C8—H8A0.9800C28—H28A0.9900
C8—H8B0.9800C28—H28B0.9900
C8—H8C0.9800C29—H29C0.9900
N2—H2C0.9100C29—H29D0.9900
N2—H2D0.9100C29—H29A0.9900
N2—C121.496 (8)C29—H29B0.9900
N2—C131.461 (8)C29—C301.497 (11)
C9—H9A0.9800C29—C30X1.502 (12)
C9—H9B0.9800C30—H30A0.9900
C9—H9C0.9800C30—H30B0.9900
C9—C101.460 (16)C30—C311.486 (12)
C10—H10A0.9900C31—H31A0.9900
C10—H10B0.9900C31—H31B0.9900
C10—C111.541 (10)C31—C321.500 (12)
C11—H11A0.9900C32—H32A0.9800
C11—H11B0.9900C32—H32B0.9800
C11—C121.476 (10)C32—H32C0.9800
C12—H12A0.9900C30X—H30C0.9900
C12—H12B0.9900C30X—H30D0.9900
C13—H13A0.9900C30X—C31X1.502 (13)
C13—H13B0.9900C31X—H31C0.9900
C13—C141.477 (11)C31X—H31D0.9900
C14—H14A0.9900C31X—C32X1.502 (12)
C14—H14B0.9900C32X—H32D0.9800
C14—C151.526 (11)C32X—H32E0.9800
C15—H15A0.9900C32X—H32F0.9800
O1—Mo1—O2101.45 (16)N2—C13—H13B109.0
O1—Mo1—O4158.94 (15)N2—C13—C14112.9 (6)
O1—Mo1—O594.45 (16)H13A—C13—H13B107.8
O1—Mo1—O11i89.75 (14)C14—C13—H13A109.0
O2—Mo1—O485.83 (12)C14—C13—H13B109.0
O2—Mo1—O5150.37 (13)C13—C14—H14A109.3
O2—Mo1—O11i74.19 (13)C13—C14—H14B109.3
O3—Mo1—O1105.88 (17)C13—C14—C15111.6 (7)
O3—Mo1—O2100.13 (16)H14A—C14—H14B108.0
O3—Mo1—O492.02 (14)C15—C14—H14A109.3
O3—Mo1—O599.31 (15)C15—C14—H14B109.3
O3—Mo1—O11i164.24 (14)C14—C15—H15A108.9
O4—Mo1—O11i73.09 (11)C14—C15—H15B108.9
O5—Mo1—O471.33 (12)H15A—C15—H15B107.7
O5—Mo1—O11i81.10 (12)C16—C15—C14113.3 (10)
O4—Mo2—O10i71.49 (11)C16—C15—H15A108.9
O5—Mo2—O474.75 (12)C16—C15—H15B108.9
O5—Mo2—O8144.85 (13)C15—C16—H16A109.5
O5—Mo2—O10i81.80 (12)C15—C16—H16B109.5
O6—Mo2—O4152.33 (15)C15—C16—H16C109.5
O6—Mo2—O5106.39 (17)H16A—C16—H16B109.5
O6—Mo2—O7104.51 (17)H16A—C16—H16C109.5
O6—Mo2—O8100.31 (15)H16B—C16—H16C109.5
O6—Mo2—O10i81.24 (15)H3A—N3—H3B107.4
O7—Mo2—O4102.40 (14)C20—N3—H3A108.3
O7—Mo2—O5100.16 (15)C20—N3—H3B108.3
O7—Mo2—O894.73 (15)C20—N3—C21116.0 (6)
O7—Mo2—O10i172.96 (14)C21—N3—H3A108.3
O8—Mo2—O471.01 (12)C21—N3—H3B108.3
O8—Mo2—O10i80.09 (12)H18A—C18—H18B107.8
O4—Mo3—O4i75.88 (12)H18C—C18—H18D107.6
O4—Mo3—O874.10 (12)C19—C18—H18A109.0
O8—Mo3—O4i81.68 (11)C19—C18—H18B109.0
O9—Mo3—O4i179.57 (15)C19—C18—H18C108.6
O9—Mo3—O4104.54 (15)C19—C18—H18D108.6
O9—Mo3—O898.32 (15)C17X—C18—H18A109.0
O9—Mo3—O10103.39 (16)C17X—C18—H18B109.0
O9—Mo3—O11103.82 (15)C17X—C18—C19113.1 (19)
O10—Mo3—O497.80 (14)C17—C18—H18C108.6
O10—Mo3—O4i76.62 (12)C17—C18—H18D108.6
O10—Mo3—O8158.14 (14)C17—C18—C19114.5 (12)
O10—Mo3—O1199.60 (14)C18—C19—H19A108.6
O11—Mo3—O4i75.77 (12)C18—C19—H19B108.6
O11—Mo3—O4142.06 (14)C18—C19—C20114.7 (9)
O11—Mo3—O877.31 (13)H19A—C19—H19B107.6
O2i—Mo4—O1171.28 (12)C20—C19—H19A108.6
O8—Mo4—O2i85.53 (13)C20—C19—H19B108.6
O8—Mo4—O1171.79 (12)N3—C20—C19112.1 (6)
O12—Mo4—O2i99.29 (17)N3—C20—H20A109.2
O12—Mo4—O894.19 (15)N3—C20—H20B109.2
O12—Mo4—O11163.32 (15)C19—C20—H20A109.2
O12—Mo4—O13105.07 (19)C19—C20—H20B109.2
O12—Mo4—O1498.93 (17)H20A—C20—H20B107.9
O13—Mo4—O2i155.20 (16)N3—C21—H21A109.5
O13—Mo4—O897.15 (15)N3—C21—H21B109.5
O13—Mo4—O1186.08 (15)H21A—C21—H21B108.1
O13—Mo4—O1490.34 (18)C22—C21—N3110.5 (8)
O14—Mo4—O2i81.24 (15)C22—C21—H21A109.5
O14—Mo4—O8162.67 (14)C22—C21—H21B109.5
O14—Mo4—O1193.27 (14)C21—C22—H22A108.5
O15—Mo5—O14112.07 (19)C21—C22—H22B108.5
O16—Mo5—O14111.0 (2)C21—C22—C23115.3 (11)
O16—Mo5—O15110.43 (19)H22A—C22—H22B107.5
O16—Mo5—O17108.5 (2)C23—C22—H22A108.5
O17—Mo5—O14107.55 (18)C23—C22—H22B108.5
O17—Mo5—O15107.13 (18)C22—C23—H23A109.1
Mo1—O2—Mo4i116.86 (17)C22—C23—H23B109.1
Mo1—O4—Mo3i96.86 (11)C22—C23—C24112.3 (12)
Mo2—O4—Mo193.97 (11)H23A—C23—H23B107.9
Mo2—O4—Mo3i96.67 (11)C24—C23—H23A109.1
Mo3—O4—Mo1149.92 (16)C24—C23—H23B109.1
Mo3—O4—Mo2104.56 (12)C23—C24—H24A109.5
Mo3—O4—Mo3i104.12 (12)C23—C24—H24B109.5
Mo2—O5—Mo1115.25 (16)C23—C24—H24C109.5
Mo2—O8—Mo3105.76 (13)H24A—C24—H24B109.5
Mo4—O8—Mo2148.17 (17)H24A—C24—H24C109.5
Mo4—O8—Mo3105.24 (14)H24B—C24—H24C109.5
Mo3—O10—Mo2i114.80 (15)C18—C17X—H17A109.5
Mo3—O11—Mo1i114.04 (14)C18—C17X—H17B109.5
Mo3—O11—Mo4102.46 (13)C18—C17X—H17C109.5
Mo4—O11—Mo1i95.11 (12)H17A—C17X—H17B109.5
Mo5—O14—Mo4165.0 (3)H17A—C17X—H17C109.5
H1A—N1—H1B107.4H17B—C17X—H17C109.5
C4—N1—H1A108.2C18—C17—H17D109.5
C4—N1—H1B108.2C18—C17—H17E109.5
C4—N1—C5116.2 (5)C18—C17—H17F109.5
C5—N1—H1A108.2H17D—C17—H17E109.5
C5—N1—H1B108.2H17D—C17—H17F109.5
H1C—C1—H1D109.5H17E—C17—H17F109.5
H1C—C1—H1E109.5H4A—N4—H4B107.2
H1D—C1—H1E109.5C28—N4—H4A107.9
C2—C1—H1C109.5C28—N4—H4B107.9
C2—C1—H1D109.5C28—N4—C29117.8 (6)
C2—C1—H1E109.5C29—N4—H4A107.9
C1—C2—H2A109.1C29—N4—H4B107.9
C1—C2—H2B109.1H25A—C25—H25B109.5
H2A—C2—H2B107.8H25A—C25—H25C109.5
C3—C2—C1112.5 (9)H25B—C25—H25C109.5
C3—C2—H2A109.1C26—C25—H25A109.5
C3—C2—H2B109.1C26—C25—H25B109.5
C2—C3—H3C109.4C26—C25—H25C109.5
C2—C3—H3D109.4C25—C26—H26A108.8
C2—C3—C4111.0 (7)C25—C26—H26B108.8
H3C—C3—H3D108.0H26A—C26—H26B107.7
C4—C3—H3C109.4C27—C26—C25114.0 (8)
C4—C3—H3D109.4C27—C26—H26A108.8
N1—C4—C3112.6 (6)C27—C26—H26B108.8
N1—C4—H4C109.1C26—C27—H27A108.9
N1—C4—H4D109.1C26—C27—H27B108.9
C3—C4—H4C109.1C26—C27—C28113.4 (7)
C3—C4—H4D109.1H27A—C27—H27B107.7
H4C—C4—H4D107.8C28—C27—H27A108.9
N1—C5—H5A109.6C28—C27—H27B108.9
N1—C5—H5B109.6N4—C28—C27112.8 (6)
N1—C5—C6110.1 (6)N4—C28—H28A109.0
H5A—C5—H5B108.1N4—C28—H28B109.0
C6—C5—H5A109.6C27—C28—H28A109.0
C6—C5—H5B109.6C27—C28—H28B109.0
C5—C6—H6A109.2H28A—C28—H28B107.8
C5—C6—H6B109.2N4—C29—H29C111.3
H6A—C6—H6B107.9N4—C29—H29D111.3
C7—C6—C5112.1 (8)N4—C29—H29A106.3
C7—C6—H6A109.2N4—C29—H29B106.3
C7—C6—H6B109.2N4—C29—C30X102.4 (16)
C6—C7—H7A109.7H29C—C29—H29D109.2
C6—C7—H7B109.7H29A—C29—H29B106.4
C6—C7—C8110.0 (11)C30—C29—N4124.2 (13)
H7A—C7—H7B108.2C30—C29—H29A106.3
C8—C7—H7A109.7C30—C29—H29B106.3
C8—C7—H7B109.7C30X—C29—H29C111.3
C7—C8—H8A109.5C30X—C29—H29D111.3
C7—C8—H8B109.5C29—C30—H30A109.3
C7—C8—H8C109.5C29—C30—H30B109.3
H8A—C8—H8B109.5H30A—C30—H30B108.0
H8A—C8—H8C109.5C31—C30—C29111.5 (13)
H8B—C8—H8C109.5C31—C30—H30A109.3
H2C—N2—H2D107.6C31—C30—H30B109.3
C12—N2—H2C108.6C30—C31—H31A108.5
C12—N2—H2D108.6C30—C31—H31B108.5
C13—N2—H2C108.6C30—C31—C32114.9 (13)
C13—N2—H2D108.6H31A—C31—H31B107.5
C13—N2—C12114.6 (5)C32—C31—H31A108.5
H9A—C9—H9B109.5C32—C31—H31B108.5
H9A—C9—H9C109.5C31—C32—H32A109.5
H9B—C9—H9C109.5C31—C32—H32B109.5
C10—C9—H9A109.5C31—C32—H32C109.5
C10—C9—H9B109.5H32A—C32—H32B109.5
C10—C9—H9C109.5H32A—C32—H32C109.5
C9—C10—H10A109.0H32B—C32—H32C109.5
C9—C10—H10B109.0C29—C30X—H30C109.6
C9—C10—C11112.7 (8)C29—C30X—H30D109.6
H10A—C10—H10B107.8C29—C30X—C31X110 (2)
C11—C10—H10A109.0H30C—C30X—H30D108.1
C11—C10—H10B109.0C31X—C30X—H30C109.6
C10—C11—H11A108.8C31X—C30X—H30D109.6
C10—C11—H11B108.8C30X—C31X—H31C109.1
H11A—C11—H11B107.7C30X—C31X—H31D109.1
C12—C11—C10113.8 (6)C30X—C31X—C32X112.5 (14)
C12—C11—H11A108.8H31C—C31X—H31D107.8
C12—C11—H11B108.8C32X—C31X—H31C109.1
N2—C12—H12A109.1C32X—C31X—H31D109.1
N2—C12—H12B109.1C31X—C32X—H32D109.5
C11—C12—N2112.4 (5)C31X—C32X—H32E109.5
C11—C12—H12A109.1C31X—C32X—H32F109.5
C11—C12—H12B109.1H32D—C32X—H32E109.5
H12A—C12—H12B107.9H32D—C32X—H32F109.5
N2—C13—H13A109.0H32E—C32X—H32F109.5
O1—Mo1—O2—Mo4i72.5 (2)C5—C6—C7—C8176.2 (8)
O3—Mo1—O2—Mo4i−178.82 (17)N2—C13—C14—C15−177.5 (6)
O4—Mo1—O2—Mo4i−87.51 (17)C9—C10—C11—C12−172.9 (9)
O4—Mo2—O5—Mo118.83 (15)C10—C11—C12—N2−177.6 (6)
O4—Mo3—O10—Mo2i78.67 (16)C12—N2—C13—C14−177.5 (5)
O4i—Mo3—O10—Mo2i5.27 (13)C13—N2—C12—C11−171.1 (5)
O5—Mo1—O2—Mo4i−48.5 (4)C13—C14—C15—C16−177.6 (8)
O6—Mo2—O5—Mo1170.08 (17)N3—C21—C22—C23−179.5 (12)
O7—Mo2—O5—Mo1−81.38 (19)C18—C19—C20—N3168.1 (8)
O8—Mo2—O5—Mo132.2 (3)C20—N3—C21—C22170.1 (8)
O8—Mo3—O10—Mo2i12.3 (4)C21—N3—C20—C1960.7 (9)
O9—Mo3—O10—Mo2i−174.29 (16)C21—C22—C23—C24180.0 (14)
O10i—Mo2—O5—Mo191.78 (17)C17X—C18—C19—C20−95.2 (19)
O11i—Mo1—O2—Mo4i−13.91 (15)C17—C18—C19—C20−176.1 (12)
O11—Mo3—O10—Mo2i−67.48 (17)N4—C29—C30—C3164 (2)
O15—Mo5—O14—Mo4130.5 (8)N4—C29—C30X—C31X168 (2)
O16—Mo5—O14—Mo46.5 (9)C25—C26—C27—C28−175.7 (8)
O17—Mo5—O14—Mo4−112.0 (9)C26—C27—C28—N4178.8 (8)
N1—C5—C6—C7−170.0 (7)C28—N4—C29—C3052.8 (12)
C1—C2—C3—C4178.8 (7)C28—N4—C29—C30X60.7 (19)
C2—C3—C4—N1−172.8 (6)C29—N4—C28—C2757.9 (9)
C4—N1—C5—C6−77.2 (8)C29—C30—C31—C3263 (3)
C5—N1—C4—C3−78.5 (7)C29—C30X—C31X—C32X−70 (4)
Symmetry code: (i) −x+1, −y+1, −z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1A···O2ii0.911.722.627 (6)172
N1—H1B···O10ii0.911.972.755 (6)143
N2—H2C···O150.911.912.778 (6)160
N2—H2D···O7iii0.911.902.812 (5)176
N3—H3A···O15iv0.911.872.770 (6)172
N3—H3B···O170.911.882.786 (6)176
N4—H4A···O110.911.802.695 (6)166
N4—H4B···O160.911.862.762 (7)172
Symmetry codes: (ii) −x+2, −y+1, −z+1; (iii) −x+1, y+1/2, −z+3/2; (iv) −x+1, −y+1, −z+2.
 

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Volume 9| Part 5| May 2024| x240463
https://doi.org/10.1107/S2414314624004632