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Acta Crystallogr Sect E Struct Rep Online. 2010 July 1; 66(Pt 7): m756–m757.
Published online 2010 June 5. doi:  10.1107/S1600536810020775
PMCID: PMC3006945

Tris(2,2′-bipyridine)­cobalt(II) μ6-oxido-dodeca-μ2-oxido-hexa­oxidohexa­molydate(VI)

Abstract

In the title compound, [Co(C10H8N2)3][Mo6O19], the Co2+ cation is surrounded in a distorted octa­hedral coordination by six N atoms from three 2,2′-bipyridine ligands. The distribution of Mo—O bond lengths in the Lindqvist isopolyanion is consistent with other structures containing the same unit. In the crystal, the cations and anions are linked by C—H(...)O inter­actions.

Related literature

For general background to polyoxometalates, see: Pope & Müller (1991 [triangle]). For polyoxometalates modified with amines, see: Zhang, Dou et al. (2009 [triangle]); Zhang, Wei et al. (2009 [triangle]). For another structure containing the μ6-oxido-dodeca­kis­-μ2-oxido-hexaoxidohexamolydate(VI) anion see: Dahlstrom et al. (1982 [triangle]). For Co—N bond lengths in a related structure, see: Li & Xu (2009 [triangle]).

An external file that holds a picture, illustration, etc.
Object name is e-66-0m756-scheme1.jpg

Experimental

Crystal data

  • [Co(C10H8N2)3][Mo6O19]
  • M r = 1407.12
  • Monoclinic, An external file that holds a picture, illustration, etc.
Object name is e-66-0m756-efi1.jpg
  • a = 12.310 (2) Å
  • b = 18.979 (4) Å
  • c = 17.150 (4) Å
  • β = 100.895 (3)°
  • V = 3934.4 (14) Å3
  • Z = 4
  • Mo Kα radiation
  • μ = 2.35 mm−1
  • T = 296 K
  • 0.12 × 0.10 × 0.08 mm

Data collection

  • Bruker APEXII CCD diffractometer
  • Absorption correction: multi-scan (SADABS; Bruker, 2001 [triangle]) T min = 0.766, T max = 0.834
  • 25652 measured reflections
  • 6500 independent reflections
  • 4649 reflections with I > 2σ(I)
  • R int = 0.041

Refinement

  • R[F 2 > 2σ(F 2)] = 0.032
  • wR(F 2) = 0.092
  • S = 1.00
  • 6500 reflections
  • 559 parameters
  • H-atom parameters constrained
  • Δρmax = 0.65 e Å−3
  • Δρmin = −0.54 e Å−3

Data collection: APEX2 (Bruker, 2004 [triangle]); cell refinement: SAINT-Plus (Bruker, 2001 [triangle]); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 [triangle]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 [triangle]); molecular graphics: SHELXTL (Sheldrick, 2008 [triangle]); software used to prepare material for publication: SHELXTL.

Table 1
Selected bond lengths (Å)
Table 2
Hydrogen-bond geometry (Å, °)

Supplementary Material

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536810020775/hb5476sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536810020775/hb5476Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Acknowledgments

Financial support from the 973 Key Program of the MOST (2006CB932905 and 2007CB81532), the National Natural Science Foundation of China (20501011), the Chinese Academy of Sciences (KJCX2-YW—M02), Shandong Provincial Education Department and Qilu Normal University is gratefully acknowledged.

supplementary crystallographic information

Comment

There has been extensive interest in heteropolyoxometalates, owing to their fascinating properties and great potential applications in many fields such as, catalysis, material science, medicine, and magnetochemistry (Pope et al., 1991). The organic amines, such as 3-(2-pyridyl)pyrazole and pyrazine, are used to effectively modify heteropolyoxomolybdates under hydrothermal condictions (Zhang, Dou et al., 2009; Zhang, Wei, Sun et al., 2009). Here, we describe the synthesis and structural characterization of the title compound.

As shown in Figure 1, the title compound consists of two subunits, viz. of a complex [Co(C10H8N2)3]2+ cation, one typical Lindqvist isopolyanion [Mo6O19]2- anion (Dahlstrom et al., 1982). The Co2+ cation is surrounded in a distorted octahedral coordination by six N atoms from three chelating 2,2'-bipyridine ligands. The Co—N bond lengths are in the range of 2.075 (5)—2.100 (5) Å, respectively, compared to reported one (Li & Xu, 2009).

The [Mo6O19]2- polyoxoanion, possessing well known Lindquist structure, is formed by six MoO6 octahedra connected with each other through edge-sharing oxygen atoms and thus exhibits approximate Oh symmetry. Three kinds of oxygen atoms exist in the cluster, that is, terminal Oa, double-bridging oxygen Ob, and central oxygen Oc. Therefore, Mo—O band lengths can be grouped into three sets: Mo—Oa 1.669 (5)—1.682 (5) Å; Mo—Ob 1.888 (4)—1.951 (5) Å; and Mo—Oc 2.299 (4)—2.318 (4) Å; these bond distances have a rule of Mo—Oa<Mo—Ob<Mo—Oc. Comparing Mo=O bond distances with that of Lindqvist isopolyanion salt (Dahlstrom, 1982), Mo=O distances have no obvious change.

Experimental

A mixture of 2,2'-bipyridine (0.5 mmoL, 0.07 g), molybdenum(VI) oxide (1 mmol, 0.14 g), oxalic aicd (10 mmol, 0.09), p-carboxyphenylboronic acid (0.3 mmoL, 0.05 g), and cobalt(II) sulfate heptahydrate (0.2 mmol, 0.05 g) in 14 ml distilled water was sealed in a 25 ml Teflon-lined stainless steel autoclave and was kept at 433 K for three days. Upon cooling, red blocks of (I) were obtained. Anal. Calc. for C30H24CoMo6N6O19: C, 25.58; H, 1.71; N, 5.97. Found: C, 22.38; H, 1.52; N, 5.78%.

Refinement

All hydrogen atoms bound to carbon were refined using a riding model with distance C—H = 0.93 Å, Uiso = 1.2Ueq (C) for aromatic atoms.

Figures

Fig. 1.
The molecular structure of (I) shoiwng displacement ellipsoids drawn at the 30% probability level; H atoms are given as spheres of arbitrary radius.

Crystal data

[Co(C10H8N2)3][Mo6O19]F(000) = 2708
Mr = 1407.12Dx = 2.376 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 2413 reflections
a = 12.310 (2) Åθ = 2.4–24.3°
b = 18.979 (4) ŵ = 2.35 mm1
c = 17.150 (4) ÅT = 296 K
β = 100.895 (3)°Block, red
V = 3934.4 (14) Å30.12 × 0.10 × 0.08 mm
Z = 4

Data collection

Bruker APEXII CCD diffractometer6500 independent reflections
Radiation source: fine-focus sealed tube4649 reflections with I > 2σ(I)
graphiteRint = 0.041
[var phi] and ω scansθmax = 24.5°, θmin = 2.2°
Absorption correction: multi-scan (SADABS; Bruker, 2001)h = −14→13
Tmin = 0.766, Tmax = 0.834k = −22→22
25652 measured reflectionsl = −18→19

Refinement

Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.032Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.092H-atom parameters constrained
S = 1.00w = 1/[σ2(Fo2) + (0.041P)2 + 10.1791P] where P = (Fo2 + 2Fc2)/3
6500 reflections(Δ/σ)max = 0.003
559 parametersΔρmax = 0.65 e Å3
0 restraintsΔρmin = −0.54 e Å3

Special details

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)

xyzUiso*/Ueq
C10.8841 (6)0.1849 (4)0.0079 (4)0.0458 (17)
H10.89620.13710.00080.055*
C20.9125 (6)0.2314 (4)−0.0452 (4)0.0523 (19)
H20.94380.2154−0.08730.063*
C30.8947 (7)0.3012 (4)−0.0362 (4)0.061 (2)
H30.91300.3336−0.07230.073*
C40.8498 (6)0.3235 (4)0.0264 (4)0.0526 (19)
H40.83780.37120.03380.063*
C50.8221 (5)0.2735 (3)0.0793 (4)0.0395 (15)
C60.7754 (5)0.2926 (3)0.1498 (4)0.0355 (14)
C70.7683 (6)0.3610 (3)0.1751 (4)0.0478 (17)
H70.78960.39820.14610.057*
C80.7294 (6)0.3736 (4)0.2435 (4)0.0554 (19)
H80.72500.41960.26150.066*
C90.6975 (5)0.3189 (4)0.2848 (4)0.0472 (17)
H90.67110.32650.33150.057*
C100.7051 (5)0.2527 (4)0.2561 (4)0.0425 (16)
H100.68300.21520.28430.051*
C110.5497 (5)0.1943 (4)0.0374 (4)0.0478 (17)
H110.54920.22820.07650.057*
C120.4747 (6)0.1997 (5)−0.0318 (5)0.063 (2)
H120.42480.2369−0.03980.076*
C130.4737 (7)0.1496 (5)−0.0891 (5)0.078 (3)
H130.42250.1521−0.13640.094*
C140.5478 (6)0.0964 (5)−0.0764 (4)0.065 (2)
H140.54840.0622−0.11510.078*
C150.6226 (5)0.0931 (4)−0.0056 (4)0.0427 (16)
C160.7059 (6)0.0373 (3)0.0130 (4)0.0447 (16)
C170.7080 (7)−0.0232 (4)−0.0324 (5)0.067 (2)
H170.6542−0.0295−0.07790.080*
C180.7867 (8)−0.0727 (4)−0.0117 (6)0.079 (3)
H180.7881−0.1130−0.04230.095*
C190.8636 (7)−0.0623 (4)0.0551 (5)0.063 (2)
H190.9189−0.09550.07090.076*
C200.8592 (6)−0.0022 (4)0.0993 (4)0.0542 (19)
H200.91240.00430.14500.065*
C211.0059 (5)0.1421 (3)0.2316 (4)0.0452 (17)
H211.02360.15870.18450.054*
C221.0883 (6)0.1384 (4)0.2973 (4)0.0529 (19)
H221.16040.15150.29490.063*
C230.9551 (5)0.0950 (4)0.3682 (4)0.0472 (17)
H230.93600.07910.41510.057*
C240.8764 (5)0.0987 (3)0.2994 (3)0.0329 (14)
C250.7600 (5)0.0778 (3)0.2945 (4)0.0330 (14)
C260.7195 (6)0.0507 (3)0.3593 (4)0.0454 (17)
H260.76570.04430.40830.054*
C270.6079 (6)0.0339 (4)0.3479 (4)0.0519 (18)
H270.57840.01590.38980.062*
C280.5422 (6)0.0433 (4)0.2765 (4)0.0511 (18)
H280.46750.03160.26860.061*
C290.5867 (5)0.0701 (4)0.2165 (4)0.0451 (17)
H290.54100.07710.16730.054*
C301.0613 (6)0.1148 (4)0.3668 (5)0.0531 (19)
H301.11510.11240.41280.064*
Co10.76522 (6)0.13938 (4)0.14146 (4)0.02958 (19)
Mo10.62552 (4)0.16746 (3)0.70535 (3)0.03880 (16)
Mo20.68058 (5)0.03933 (3)0.59227 (3)0.03863 (15)
Mo30.93267 (4)0.09804 (3)0.60537 (3)0.04001 (16)
Mo40.72000 (5)0.20190 (3)0.54351 (3)0.04164 (16)
Mo50.87672 (5)0.22739 (3)0.71735 (4)0.04679 (17)
Mo60.83628 (5)0.06397 (3)0.76648 (3)0.04393 (17)
N10.8397 (4)0.2045 (3)0.0694 (3)0.0371 (12)
N20.7428 (4)0.2385 (3)0.1891 (3)0.0355 (12)
N30.6238 (4)0.1425 (3)0.0512 (3)0.0421 (13)
N40.7816 (4)0.0472 (3)0.0790 (3)0.0401 (13)
N50.6935 (4)0.0870 (3)0.2251 (3)0.0395 (13)
N60.9018 (4)0.1232 (3)0.2313 (3)0.0373 (12)
O10.6778 (4)0.2537 (3)0.4646 (3)0.0632 (14)
O20.8518 (4)0.1606 (2)0.5229 (3)0.0467 (11)
O30.6467 (3)0.1147 (2)0.5161 (2)0.0424 (11)
O40.9808 (3)0.1811 (2)0.6620 (3)0.0492 (12)
O50.8119 (4)0.2659 (2)0.6171 (3)0.0518 (12)
O60.9511 (4)0.2935 (3)0.7643 (3)0.0744 (17)
O70.6093 (3)0.2189 (2)0.6099 (3)0.0447 (11)
O80.7392 (4)0.2354 (2)0.7496 (3)0.0494 (12)
O90.5168 (4)0.1929 (3)0.7438 (3)0.0539 (12)
O100.7046 (3)0.1044 (2)0.7871 (3)0.0484 (12)
O110.9111 (4)0.1509 (3)0.7929 (3)0.0518 (12)
O120.7786 (3)0.13302 (19)0.6550 (2)0.0329 (9)
O130.5755 (3)0.0853 (2)0.6474 (3)0.0419 (11)
O140.8815 (4)0.0131 (3)0.8463 (3)0.0705 (16)
O150.7458 (4)0.0007 (2)0.6930 (3)0.0485 (12)
O160.9500 (3)0.0484 (2)0.7010 (3)0.0475 (12)
O170.6077 (4)−0.0283 (2)0.5469 (3)0.0600 (14)
O180.8188 (3)0.0303 (2)0.5606 (2)0.0438 (11)
O191.0407 (4)0.0735 (3)0.5655 (3)0.0565 (13)

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
C10.057 (4)0.042 (4)0.041 (4)−0.006 (3)0.017 (3)−0.004 (3)
C20.064 (5)0.061 (5)0.034 (4)−0.010 (4)0.015 (4)−0.004 (4)
C30.086 (6)0.055 (5)0.043 (4)−0.018 (4)0.015 (4)0.010 (4)
C40.079 (5)0.036 (4)0.041 (4)−0.006 (4)0.006 (4)0.006 (3)
C50.036 (4)0.048 (4)0.032 (4)−0.004 (3)0.001 (3)0.002 (3)
C60.036 (4)0.033 (4)0.034 (4)−0.003 (3)−0.002 (3)−0.001 (3)
C70.061 (5)0.030 (4)0.050 (4)−0.001 (3)0.006 (4)−0.002 (3)
C80.064 (5)0.042 (4)0.057 (5)0.009 (4)0.003 (4)−0.016 (4)
C90.049 (4)0.049 (4)0.043 (4)0.009 (3)0.008 (3)−0.011 (4)
C100.043 (4)0.055 (4)0.029 (4)0.011 (3)0.005 (3)0.005 (3)
C110.048 (4)0.055 (4)0.040 (4)0.011 (4)0.009 (3)−0.003 (3)
C120.043 (4)0.089 (6)0.056 (5)0.028 (4)0.007 (4)0.004 (5)
C130.045 (5)0.128 (8)0.056 (5)0.025 (5)−0.001 (4)−0.008 (6)
C140.053 (5)0.091 (6)0.048 (5)0.005 (5)0.002 (4)−0.022 (4)
C150.036 (4)0.054 (4)0.038 (4)−0.008 (3)0.006 (3)−0.006 (3)
C160.055 (4)0.035 (4)0.048 (4)−0.009 (3)0.017 (4)−0.003 (3)
C170.083 (6)0.051 (5)0.060 (5)−0.005 (4)0.000 (4)−0.018 (4)
C180.115 (8)0.039 (5)0.087 (7)0.003 (5)0.029 (6)−0.021 (5)
C190.076 (6)0.040 (4)0.080 (6)0.011 (4)0.030 (5)0.004 (4)
C200.055 (5)0.050 (5)0.057 (5)0.012 (4)0.011 (4)0.006 (4)
C210.046 (4)0.041 (4)0.050 (4)−0.004 (3)0.013 (3)0.005 (3)
C220.038 (4)0.048 (4)0.068 (5)−0.006 (3)0.000 (4)0.006 (4)
C230.047 (4)0.051 (4)0.040 (4)0.007 (3)0.000 (3)0.004 (3)
C240.045 (4)0.025 (3)0.029 (3)0.005 (3)0.008 (3)−0.001 (3)
C250.039 (4)0.026 (3)0.034 (4)−0.001 (3)0.008 (3)−0.005 (3)
C260.056 (5)0.045 (4)0.036 (4)−0.001 (3)0.011 (3)0.003 (3)
C270.058 (5)0.054 (4)0.049 (4)−0.008 (4)0.022 (4)0.004 (4)
C280.043 (4)0.057 (5)0.055 (5)−0.011 (3)0.013 (4)0.003 (4)
C290.039 (4)0.057 (4)0.037 (4)−0.010 (3)0.003 (3)0.004 (3)
C300.042 (4)0.046 (4)0.065 (5)0.002 (3)−0.006 (4)0.005 (4)
Co10.0301 (4)0.0305 (4)0.0280 (4)−0.0009 (3)0.0050 (3)0.0012 (3)
Mo10.0331 (3)0.0401 (3)0.0451 (3)0.0020 (2)0.0123 (3)−0.0020 (3)
Mo20.0368 (3)0.0331 (3)0.0451 (4)−0.0059 (2)0.0056 (3)−0.0064 (3)
Mo30.0320 (3)0.0490 (4)0.0402 (3)0.0000 (3)0.0099 (3)−0.0069 (3)
Mo40.0430 (3)0.0396 (3)0.0428 (3)0.0011 (3)0.0094 (3)0.0095 (3)
Mo50.0413 (3)0.0481 (4)0.0522 (4)−0.0139 (3)0.0117 (3)−0.0186 (3)
Mo60.0384 (3)0.0556 (4)0.0369 (3)0.0076 (3)0.0049 (3)0.0077 (3)
N10.042 (3)0.039 (3)0.030 (3)−0.003 (2)0.007 (2)−0.002 (2)
N20.036 (3)0.041 (3)0.028 (3)0.001 (2)0.001 (2)0.001 (2)
N30.037 (3)0.045 (3)0.045 (3)0.001 (3)0.008 (3)0.003 (3)
N40.040 (3)0.038 (3)0.042 (3)−0.001 (2)0.007 (3)0.000 (3)
N50.042 (3)0.037 (3)0.039 (3)−0.004 (2)0.006 (3)0.004 (2)
N60.035 (3)0.036 (3)0.040 (3)−0.005 (2)0.005 (2)0.003 (2)
O10.063 (3)0.067 (3)0.060 (3)0.004 (3)0.014 (3)0.027 (3)
O20.046 (3)0.053 (3)0.044 (3)−0.002 (2)0.015 (2)0.002 (2)
O30.035 (2)0.049 (3)0.039 (3)−0.003 (2)−0.004 (2)0.001 (2)
O40.036 (3)0.062 (3)0.049 (3)−0.012 (2)0.007 (2)−0.014 (2)
O50.054 (3)0.032 (2)0.073 (3)−0.008 (2)0.019 (3)0.003 (2)
O60.063 (3)0.069 (4)0.090 (4)−0.023 (3)0.012 (3)−0.036 (3)
O70.041 (3)0.040 (3)0.054 (3)0.005 (2)0.011 (2)0.004 (2)
O80.044 (3)0.051 (3)0.056 (3)−0.001 (2)0.015 (2)−0.021 (2)
O90.039 (3)0.066 (3)0.061 (3)0.006 (2)0.018 (2)0.000 (3)
O100.043 (3)0.064 (3)0.042 (3)0.007 (2)0.016 (2)0.009 (2)
O110.040 (3)0.070 (3)0.043 (3)−0.004 (2)0.003 (2)−0.012 (2)
O120.032 (2)0.031 (2)0.038 (2)−0.0016 (18)0.0104 (18)−0.0038 (19)
O130.034 (2)0.038 (2)0.054 (3)−0.0053 (19)0.008 (2)0.001 (2)
O140.056 (3)0.096 (4)0.057 (3)0.017 (3)0.006 (3)0.026 (3)
O150.050 (3)0.036 (2)0.059 (3)−0.001 (2)0.008 (2)0.010 (2)
O160.039 (3)0.059 (3)0.043 (3)0.007 (2)0.005 (2)−0.001 (2)
O170.057 (3)0.043 (3)0.079 (4)−0.010 (2)0.008 (3)−0.018 (3)
O180.044 (3)0.044 (3)0.043 (3)0.004 (2)0.008 (2)−0.010 (2)
O190.041 (3)0.080 (4)0.050 (3)0.006 (2)0.014 (2)−0.009 (3)

Geometric parameters (Å, °)

C1—N11.330 (8)C25—C261.398 (8)
C1—C21.361 (9)C26—C271.387 (9)
C1—H10.9300C26—H260.9300
C2—C31.358 (10)C27—C281.346 (9)
C2—H20.9300C27—H270.9300
C3—C41.364 (10)C28—C291.354 (9)
C3—H30.9300C28—H280.9300
C4—C51.400 (9)C29—N51.334 (8)
C4—H40.9300C29—H290.9300
C5—N11.343 (8)C30—H300.9300
C5—C61.479 (8)Co1—N52.075 (5)
C6—N21.331 (7)Co1—N62.078 (5)
C6—C71.376 (8)Co1—N12.079 (5)
C7—C81.367 (9)Co1—N42.081 (5)
C7—H70.9300Co1—N22.091 (5)
C8—C91.358 (10)Co1—N32.100 (5)
C8—H80.9300Mo1—O91.671 (4)
C9—C101.359 (9)Mo1—O71.884 (4)
C9—H90.9300Mo1—O131.888 (4)
C10—N21.345 (7)Mo1—O81.948 (4)
C10—H100.9300Mo1—O101.957 (4)
C11—N31.331 (8)Mo1—O122.310 (4)
C11—C121.362 (9)Mo2—O171.671 (4)
C11—H110.9300Mo2—O181.888 (4)
C12—C131.366 (11)Mo2—O151.909 (4)
C12—H120.9300Mo2—O31.929 (4)
C13—C141.350 (11)Mo2—O131.948 (4)
C13—H130.9300Mo2—O122.299 (4)
C14—C151.379 (9)Mo3—O191.673 (4)
C14—H140.9300Mo3—O161.868 (4)
C15—N31.350 (8)Mo3—O41.888 (4)
C15—C161.467 (9)Mo3—O181.950 (4)
C16—N41.336 (8)Mo3—O21.968 (4)
C16—C171.390 (9)Mo3—O122.318 (4)
C17—C181.349 (11)Mo4—O11.673 (5)
C17—H170.9300Mo4—O21.894 (4)
C18—C191.354 (11)Mo4—O31.900 (4)
C18—H180.9300Mo4—O51.951 (5)
C19—C201.377 (10)Mo4—O71.961 (4)
C19—H190.9300Mo4—O122.316 (4)
C20—N41.336 (8)Mo5—O61.669 (5)
C20—H200.9300Mo5—O81.884 (4)
C21—N61.330 (8)Mo5—O51.900 (5)
C21—C221.368 (9)Mo5—O111.939 (5)
C21—H210.9300Mo5—O41.943 (4)
C22—C301.373 (10)Mo5—O122.307 (4)
C22—H220.9300Mo6—O141.682 (5)
C23—C301.365 (9)Mo6—O101.887 (4)
C23—C241.379 (8)Mo6—O111.902 (5)
C23—H230.9300Mo6—O151.934 (4)
C24—N61.347 (7)Mo6—O161.976 (4)
C24—C251.474 (8)Mo6—O122.316 (4)
C25—N51.323 (7)
N1—C1—C2123.1 (7)O17—Mo2—O18103.3 (2)
N1—C1—H1118.5O17—Mo2—O15102.9 (2)
C2—C1—H1118.5O18—Mo2—O1588.73 (19)
C3—C2—C1119.3 (7)O17—Mo2—O3103.1 (2)
C3—C2—H2120.3O18—Mo2—O387.96 (18)
C1—C2—H2120.3O15—Mo2—O3153.89 (18)
C2—C3—C4119.4 (7)O17—Mo2—O13102.9 (2)
C2—C3—H3120.3O18—Mo2—O13153.82 (17)
C4—C3—H3120.3O15—Mo2—O1386.36 (19)
C3—C4—C5119.0 (7)O3—Mo2—O1385.28 (18)
C3—C4—H4120.5O17—Mo2—O12179.2 (2)
C5—C4—H4120.5O18—Mo2—O1277.50 (15)
N1—C5—C4120.9 (6)O15—Mo2—O1277.28 (16)
N1—C5—C6116.1 (5)O3—Mo2—O1276.72 (16)
C4—C5—C6123.0 (6)O13—Mo2—O1276.34 (15)
N2—C6—C7121.6 (6)O19—Mo3—O16104.5 (2)
N2—C6—C5115.2 (5)O19—Mo3—O4104.3 (2)
C7—C6—C5123.2 (6)O16—Mo3—O489.9 (2)
C8—C7—C6119.3 (7)O19—Mo3—O18102.9 (2)
C8—C7—H7120.4O16—Mo3—O1888.10 (19)
C6—C7—H7120.4O4—Mo3—O18152.37 (18)
C9—C8—C7119.8 (6)O19—Mo3—O2102.0 (2)
C9—C8—H8120.1O16—Mo3—O2153.38 (18)
C7—C8—H8120.1O4—Mo3—O286.13 (19)
C8—C9—C10118.1 (6)O18—Mo3—O283.50 (18)
C8—C9—H9120.9O19—Mo3—O12177.44 (19)
C10—C9—H9120.9O16—Mo3—O1277.75 (16)
N2—C10—C9123.6 (6)O4—Mo3—O1276.77 (16)
N2—C10—H10118.2O18—Mo3—O1275.87 (15)
C9—C10—H10118.2O2—Mo3—O1275.71 (16)
N3—C11—C12122.6 (7)O1—Mo4—O2103.8 (2)
N3—C11—H11118.7O1—Mo4—O3104.5 (2)
C12—C11—H11118.7O2—Mo4—O388.71 (19)
C13—C12—C11119.1 (7)O1—Mo4—O5102.2 (2)
C13—C12—H12120.5O2—Mo4—O588.06 (19)
C11—C12—H12120.5O3—Mo4—O5153.15 (18)
C14—C13—C12119.4 (7)O1—Mo4—O7103.3 (2)
C14—C13—H13120.3O2—Mo4—O7152.92 (18)
C12—C13—H13120.3O3—Mo4—O786.39 (18)
C13—C14—C15119.6 (7)O5—Mo4—O784.46 (19)
C13—C14—H14120.2O1—Mo4—O12178.4 (2)
C15—C14—H14120.2O2—Mo4—O1277.12 (16)
N3—C15—C14121.2 (7)O3—Mo4—O1276.83 (15)
N3—C15—C16115.6 (6)O5—Mo4—O1276.46 (16)
C14—C15—C16123.2 (6)O7—Mo4—O1275.83 (15)
N4—C16—C17120.5 (7)O6—Mo5—O8103.8 (2)
N4—C16—C15115.5 (6)O6—Mo5—O5104.2 (2)
C17—C16—C15124.0 (7)O8—Mo5—O589.3 (2)
C18—C17—C16121.0 (8)O6—Mo5—O11102.1 (3)
C18—C17—H17119.5O8—Mo5—O1187.6 (2)
C16—C17—H17119.5O5—Mo5—O11153.44 (19)
C17—C18—C19118.2 (8)O6—Mo5—O4102.9 (2)
C17—C18—H18120.9O8—Mo5—O4153.17 (18)
C19—C18—H18120.9O5—Mo5—O486.3 (2)
C18—C19—C20119.6 (8)O11—Mo5—O484.69 (19)
C18—C19—H19120.2O6—Mo5—O12177.9 (2)
C20—C19—H19120.2O8—Mo5—O1277.15 (16)
N4—C20—C19122.6 (7)O5—Mo5—O1277.63 (16)
N4—C20—H20118.7O11—Mo5—O1275.97 (16)
C19—C20—H20118.7O4—Mo5—O1276.05 (15)
N6—C21—C22123.6 (6)O14—Mo6—O10104.1 (2)
N6—C21—H21118.2O14—Mo6—O11103.5 (2)
C22—C21—H21118.2O10—Mo6—O1189.9 (2)
C21—C22—C30117.9 (7)O14—Mo6—O15103.6 (2)
C21—C22—H22121.0O10—Mo6—O1588.0 (2)
C30—C22—H22121.0O11—Mo6—O15152.55 (19)
C30—C23—C24119.4 (7)O14—Mo6—O16102.5 (2)
C30—C23—H23120.3O10—Mo6—O16153.36 (18)
C24—C23—H23120.3O11—Mo6—O1684.39 (19)
N6—C24—C23121.2 (6)O15—Mo6—O1685.39 (19)
N6—C24—C25115.2 (5)O14—Mo6—O12178.3 (2)
C23—C24—C25123.6 (6)O10—Mo6—O1277.53 (16)
N5—C25—C26120.7 (6)O11—Mo6—O1276.43 (17)
N5—C25—C24116.5 (5)O15—Mo6—O1276.39 (15)
C26—C25—C24122.9 (6)O16—Mo6—O1275.83 (16)
C27—C26—C25117.7 (6)C1—N1—C5118.3 (5)
C27—C26—H26121.2C1—N1—Co1126.7 (4)
C25—C26—H26121.2C5—N1—Co1113.9 (4)
C28—C27—C26120.5 (6)C6—N2—C10117.6 (6)
C28—C27—H27119.8C6—N2—Co1114.9 (4)
C26—C27—H27119.8C10—N2—Co1127.3 (4)
C27—C28—C29118.8 (7)C11—N3—C15118.0 (6)
C27—C28—H28120.6C11—N3—Co1126.6 (5)
C29—C28—H28120.6C15—N3—Co1114.0 (4)
N5—C29—C28122.6 (6)C20—N4—C16118.1 (6)
N5—C29—H29118.7C20—N4—Co1126.1 (5)
C28—C29—H29118.7C16—N4—Co1115.7 (4)
C23—C30—C22119.7 (7)C25—N5—C29119.8 (5)
C23—C30—H30120.2C25—N5—Co1114.4 (4)
C22—C30—H30120.2C29—N5—Co1125.3 (4)
N5—Co1—N678.9 (2)C21—N6—C24118.1 (6)
N5—Co1—N1171.4 (2)C21—N6—Co1127.3 (4)
N6—Co1—N198.20 (19)C24—N6—Co1114.0 (4)
N5—Co1—N492.8 (2)Mo4—O2—Mo3116.7 (2)
N6—Co1—N496.5 (2)Mo4—O3—Mo2116.5 (2)
N1—Co1—N495.6 (2)Mo3—O4—Mo5117.2 (2)
N5—Co1—N293.2 (2)Mo5—O5—Mo4116.0 (2)
N6—Co1—N289.51 (19)Mo1—O7—Mo4116.6 (2)
N1—Co1—N278.62 (19)Mo5—O8—Mo1116.8 (2)
N4—Co1—N2172.2 (2)Mo6—O10—Mo1116.3 (2)
N5—Co1—N397.0 (2)Mo6—O11—Mo5117.1 (2)
N6—Co1—N3173.0 (2)Mo2—O12—Mo5179.7 (2)
N1—Co1—N386.7 (2)Mo2—O12—Mo190.06 (13)
N4—Co1—N378.0 (2)Mo5—O12—Mo189.99 (13)
N2—Co1—N396.3 (2)Mo2—O12—Mo489.78 (14)
O9—Mo1—O7103.4 (2)Mo5—O12—Mo489.91 (13)
O9—Mo1—O13103.9 (2)Mo1—O12—Mo490.02 (13)
O7—Mo1—O1390.01 (18)Mo2—O12—Mo690.04 (13)
O9—Mo1—O8103.0 (2)Mo5—O12—Mo690.27 (14)
O7—Mo1—O886.9 (2)Mo1—O12—Mo689.78 (13)
O13—Mo1—O8152.92 (17)Mo4—O12—Mo6179.7 (2)
O9—Mo1—O10102.8 (2)Mo2—O12—Mo390.00 (13)
O7—Mo1—O10153.66 (18)Mo5—O12—Mo389.96 (13)
O13—Mo1—O1086.59 (19)Mo1—O12—Mo3179.6 (2)
O8—Mo1—O1084.4 (2)Mo4—O12—Mo390.40 (13)
O9—Mo1—O12178.6 (2)Mo6—O12—Mo389.79 (13)
O7—Mo1—O1277.40 (16)Mo1—O13—Mo2116.4 (2)
O13—Mo1—O1277.16 (15)Mo2—O15—Mo6116.3 (2)
O8—Mo1—O1275.91 (15)Mo3—O16—Mo6116.6 (2)
O10—Mo1—O1276.38 (15)Mo2—O18—Mo3116.5 (2)

Hydrogen-bond geometry (Å, °)

D—H···AD—HH···AD···AD—H···A
C2—H2···O11i0.932.363.166 (9)145
C4—H4···O17ii0.932.523.165 (9)127
C11—H11···O4iii0.932.513.400 (8)161
C12—H12···O2iii0.932.473.277 (10)145
C20—H20···O14iv0.932.533.159 (9)125
C22—H22···O8v0.932.543.230 (9)132
C26—H26···O180.932.583.459 (8)157

Symmetry codes: (i) x, y, z−1; (ii) −x+3/2, y+1/2, −z+1/2; (iii) x−1/2, −y+1/2, z−1/2; (iv) −x+2, −y, −z+1; (v) x+1/2, −y+1/2, z−1/2.

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: HB5476).

References

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