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

Journal logoCRYSTALLOGRAPHIC
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ISSN: 2056-9890
Volume 67| Part 7| July 2011| Pages m862-m863

Tri-μ-oxido-bis­­[(5,10,15,20-tetra­phenyl­porphyrinato-κ4N)niobium(V)]

aDépartement de Chimie, Faculté des Sciences de Monastir, Université de Monastir, Avenue de l'Environnement, 5019 Monastir, Tunisia, and bLaboratoire de Chimie de Coordination, CNRS UPR 8241, 205 Route de Norbonne, 31077 Toulouse, Cedex 04, France
*Correspondence e-mail: hnasri1@gmail.com

(Received 20 May 2011; accepted 29 May 2011; online 4 June 2011)

In the title dinuclear NbV compound, [Nb2(C44H28N4)2O3], each Nb atom is seven-coordinated with three bridging O atoms and four N atoms from a chelating tetra­phenyl­porphyrinate anion. The Nb—O bond lengths range from 1.757 (6) to 2.331 (6) Å, and the average (niobium–pyrrole N atom) distance is 2.239 Å. In the dinuclear mol­ecule, the Nb⋯Nb separation is 2.8200 (8) Å, and the dihedral angle between the two porphyrinate mean planes is 5.4 (1)°. Weak inter­molecular C—H⋯π inter­actions are present in the crystal structure.

Related literature

For a review of porphyrin complexes, see: Scheidt (2000[Scheidt, W. R. (2000). The Porphyrin Handbook, Vol. 3, edited by K. M. Kadish, R. M. Smith & R. Guilard, pp. 49-112. San Diego: Academic Press.]). For the synthesis of niobium(V) porphyrin derivatives, see: Johson & Scheidt (1978[Johson, F. J. & Scheidt, W. R. (1978). Inorg. Chem. 17, 1280-1287.]); Lecomte et al. (1979[Lecomte, C., Protas, J., Guilard, R., Fliniaux, B. & Fournari, P. (1979). J. Chem. Soc. Dalton Trans. pp. 1306-1312.]). For comparative bond lengths, see: Allen et al. (1987[Allen, F. H., Kennard, O., Watson, D. G., Brammer, L., Orpen, A. G. & Taylor, R. (1987). J. Chem. Soc. Perkin Trans. 2, pp. S1-19.]). For a description of the Cambridge Structural Database, see: Allen (2002[Allen, F. H. (2002). Acta Cryst. B58, 380-388.]).

[Scheme 1]

Experimental

Crystal data
  • [Nb2(C44H28N4)2O3]

  • Mr = 1459.28

  • Monoclinic, P n

  • a = 14.4823 (9) Å

  • b = 18.4007 (8) Å

  • c = 14.6257 (10) Å

  • β = 117.823 (7)°

  • V = 3446.9 (4) Å3

  • Z = 2

  • Mo Kα radiation

  • μ = 0.39 mm−1

  • T = 180 K

  • 0.5 × 0.3 × 0.1 mm

Data collection
  • Bruker APEXII CCD area-detector diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2007[Bruker (2007). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.72, Tmax = 1.00

  • 25553 measured reflections

  • 9945 independent reflections

  • 8244 reflections with I > 2σ(I)

  • Rint = 0.055

Refinement
  • R[F2 > 2σ(F2)] = 0.062

  • wR(F2) = 0.166

  • S = 1.06

  • 9945 reflections

  • 910 parameters

  • 32 restraints

  • H-atom parameters constrained

  • Δρmax = 1.20 e Å−3

  • Δρmin = −0.91 e Å−3

  • Absolute structure: Flack (1983[Flack, H. D. (1983). Acta Cryst. A39, 876-881.]), 2439 Friedel pairs

  • Flack parameter: −0.01 (6)

Table 1
Selected bond lengths (Å)

Nb1—O1 1.876 (6)
Nb1—O2 1.815 (6)
Nb1—O3 2.331 (6)
Nb1—N1 2.240 (7)
Nb1—N2 2.228 (7)
Nb1—N3 2.261 (7)
Nb1—N4 2.224 (7)
Nb2—O1 2.019 (6)
Nb2—O2 2.182 (6)
Nb2—O3 1.757 (6)
Nb2—N5 2.260 (7)
Nb2—N6 2.226 (7)
Nb2—N7 2.227 (7)
Nb2—N8 2.246 (7)

Table 2
Hydrogen-bond geometry (Å, °)

Cg1 and Cg2 are the centroids of the C27-benzene ring and N1-pyrrole ring, respectively.

D—H⋯A D—H H⋯A DA D—H⋯A
C22—H22⋯Cg1i 0.93 2.85 3.752 (14) 164
C40—H40⋯Cg2i 0.93 2.87 3.681 (14) 147
Symmetry code: (i) [x-{\script{1\over 2}}, -y, z-{\script{1\over 2}}].

Data collection: APEX2 (Bruker, 2007[Bruker (2007). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2007[Bruker (2007). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; program(s) used to solve structure: SIR2004 (Burla et al., 2005[Burla, M. C., Caliandro, R., Camalli, M., Carrozzini, B., Cascarano, G. L., De Caro, L., Giacovazzo, C., Polidori, G. & Spagna, R. (2005). J. Appl. Cryst. 38, 381-388.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: ORTEPIII (Burnett & Johnson, 1996[Burnett, M. N. & Johnson, C. K. (1996). ORTEPIII. Report ORNL-6895. Oak Ridge National Laboratory, Tennessee, USA.]); software used to prepare material for publication: publCIF (Westrip, 2010[Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.])..

Supporting information


Comment top

The search of the November 2010 release of the Cambridge Structural Database (Allen, 2002) reveals the presence of only one room temperature crystal structure of the [Nb2O3(C44H28N4)2] complex with four 1,2-dichloroethane solvate molecules (Lecomte et al., 1979) with R = 0.076 (space group Pccn). One year earlier, the room temperature crystal structure of this species was published (Johson & Scheidt, 1978) with R = 0.063 (space group Cc).

The current redetermination of this Nb(V) porphyrin species at 180 K provides a slightly lower R value (R = 0.062 based on 8239 independent observed reflections) than the two reported structures.

The asymmetric unit of the structure of (I) contains one complex [Nb2O3(C44H28N4)2]. The average equatorial niobium–pyrrole N atom (Nb—Np) distance in (I) is 2.239 (7) Å and each niobium is displaced by 1.01 Å from the 24 atome of the porphyrinato core.

As is clearly seen in Fig. 1 and Fig. 2, the two niobium(V) porphyrin moieties are joined together by three bridging oxo ligand. Thus, each NbV ion is seven-coordinated. Only one of the bridging oxo ligands forms a nearly symmetric bridge; the other two bridges are quite asymmetric. Unique Nb—O bond lenghts are listed in Table 1. The distance between the two niobium(V) atoms is 2.8200 (8) Å. The two porphyrinato planes are not quite parallel; the dihedral angle between them is 5.4 (1)°. The two porphyrinato rings have a "slipped" configuration with respect to each other; the angles between the normals to the ring passing through the closest niobium atom and the Nb—Nb vector are 16° and 20°.

Related literature top

For a review of porphyrin complexes, see: Scheidt (2000). For the synthesis of niobium(V) porphyrin derivatives, see: Johson & Scheidt (1978); Lecomte et al. (1979). For comparative bond lengths, see: Allen et al. (1987). For a description of the Cambridge Structural Database, see: Allen (2002).

Experimental top

A solution of NbCl5 (1.50 g, 5.55 mmol) in benzonitrile (21 ml) was introduced under argon in a reactor. A solution of the tetraphenylporphyrin (TPP) (1.00 g, 1.62 mmol) in the same solvent (30 ml) was then added. The mixture was heated under reflux for four hours and then hydrolysed (2 ml of water). The resulting solid was chromatographed and recrystallized.

Refinement top

H atoms were placed using assumed geometry with C—H = 0.93 Å. Displacement parameters of the H atoms were set to 1.2 times the isotropic equivalent for the bonded carbon atoms.

Computing details top

Data collection: APEX2 (Bruker, 2007); cell refinement: SAINT (Bruker, 2007); data reduction: SAINT (Bruker, 2007); program(s) used to solve structure: SIR2004 (Burla et al., 2005); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEPIII (Burnett & Johnson, 1996); software used to prepare material for publication: publCIF (Westrip, 2010)..

Figures top
[Figure 1] Fig. 1. A view of the structure of complex [Nb2O3(C44H28N4)2] showing the atom numbering scheme. Displacement ellipsoids are drawn at 30%. The H atoms have been omitted for clarity.
[Figure 2] Fig. 2. A drawing showing the coordination polyhedrons of the the two niobium atoms Nb1 and Nb2. Displacement ellipsoids are drawn at 50%.
Tri-µ-oxido-bis[(5,10,15,20-tetraphenylporphyrinato-κ4N)niobium(V)] top
Crystal data top
[Nb2(C44H28N4)2O3]F(000) = 1492
Mr = 1459.28Dx = 1.406 Mg m3
Monoclinic, PnMo Kα radiation, λ = 0.71073 Å
Hall symbol: P -2yacCell parameters from 12579 reflections
a = 14.4823 (9) Åθ = 3.0–32.1°
b = 18.4007 (8) ŵ = 0.39 mm1
c = 14.6257 (10) ÅT = 180 K
β = 117.823 (7)°Plate, dark purple
V = 3446.9 (4) Å30.5 × 0.3 × 0.1 mm
Z = 2
Data collection top
Bruker APEXII CCD area-detector
diffractometer
9945 independent reflections
Radiation source: fine-focus sealed tube8244 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.055
Detector resolution: 8.2632 pixels mm-1θmax = 26.0°, θmin = 3.0°
ω scansh = 1617
Absorption correction: multi-scan
(SADABS; Bruker, 2007)
k = 2222
Tmin = 0.72, Tmax = 1.00l = 1815
25553 measured reflections
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.062H-atom parameters constrained
wR(F2) = 0.166 w = 1/[σ2(Fo2) + (0.0709P)2 + 14.5546P]
whereP = (Fo2 + 2Fc2)/3
S = 1.06(Δ/σ)max < 0.001
9945 reflectionsΔρmax = 1.20 e Å3
910 parametersΔρmin = 0.91 e Å3
32 restraintsAbsolute structure: Flack (1983), 2439 Friedel pairs
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.01 (6)
Crystal data top
[Nb2(C44H28N4)2O3]V = 3446.9 (4) Å3
Mr = 1459.28Z = 2
Monoclinic, PnMo Kα radiation
a = 14.4823 (9) ŵ = 0.39 mm1
b = 18.4007 (8) ÅT = 180 K
c = 14.6257 (10) Å0.5 × 0.3 × 0.1 mm
β = 117.823 (7)°
Data collection top
Bruker APEXII CCD area-detector
diffractometer
9945 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2007)
8244 reflections with I > 2σ(I)
Tmin = 0.72, Tmax = 1.00Rint = 0.055
25553 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.062H-atom parameters constrained
wR(F2) = 0.166 w = 1/[σ2(Fo2) + (0.0709P)2 + 14.5546P]
whereP = (Fo2 + 2Fc2)/3
S = 1.06Δρmax = 1.20 e Å3
9945 reflectionsΔρmin = 0.91 e Å3
910 parametersAbsolute structure: Flack (1983), 2439 Friedel pairs
32 restraintsAbsolute structure parameter: 0.01 (6)
Special details top

Geometry. All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'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 > 2σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Nb10.30292 (4)0.17400 (4)0.75581 (4)0.0230 (2)
Nb20.25738 (4)0.32308 (4)0.71453 (4)0.02206 (19)
O10.3090 (5)0.2549 (3)0.8366 (5)0.0382 (16)
O20.3490 (4)0.2377 (3)0.6913 (5)0.0333 (14)
O30.1663 (5)0.2527 (3)0.6570 (5)0.0438 (17)
N10.4324 (5)0.1081 (4)0.7547 (6)0.0287 (16)
N20.3852 (6)0.1297 (4)0.9160 (6)0.0338 (18)
N30.1636 (6)0.1342 (3)0.7721 (6)0.0288 (16)
N40.2133 (5)0.1139 (4)0.6083 (6)0.0284 (16)
N50.4245 (6)0.3621 (4)0.7989 (6)0.0318 (17)
N60.2825 (5)0.3623 (3)0.5839 (5)0.0268 (15)
N70.1144 (6)0.3904 (4)0.6303 (6)0.0298 (16)
N80.2545 (5)0.3907 (3)0.8410 (5)0.0256 (15)
C10.4400 (8)0.0919 (5)0.6671 (8)0.033 (2)
C20.5435 (8)0.0736 (5)0.6927 (8)0.036 (2)
H20.56770.06020.64640.043*
C30.6003 (7)0.0789 (5)0.7943 (8)0.038 (2)
H30.67130.06900.83180.046*
C40.5332 (8)0.1024 (6)0.8368 (8)0.037 (2)
C50.5645 (8)0.1139 (4)0.9402 (8)0.032 (2)
C60.4935 (7)0.1256 (5)0.9758 (8)0.034 (2)
C70.5203 (9)0.1409 (5)1.0831 (8)0.041 (2)
H70.58710.14501.13840.049*
C80.4293 (7)0.1479 (5)1.0865 (7)0.039 (2)
H80.42350.15451.14660.047*
C90.3446 (9)0.1438 (5)0.9868 (8)0.035 (2)
C100.2392 (8)0.1516 (5)0.9573 (8)0.037 (2)
C110.1580 (8)0.1455 (5)0.8607 (8)0.030 (2)
C120.0482 (8)0.1504 (5)0.8352 (8)0.039 (2)
H120.02250.15980.88160.046*
C130.0082 (8)0.1394 (5)0.7355 (8)0.042 (2)
H130.08070.13870.69860.051*
C140.0649 (8)0.1284 (5)0.6939 (8)0.031 (2)
C150.0350 (7)0.1188 (4)0.5892 (7)0.0287 (19)
C160.1052 (7)0.1089 (5)0.5503 (7)0.0298 (19)
C170.0775 (7)0.0961 (5)0.4450 (8)0.040 (2)
H170.01040.09110.39070.048*
C180.1665 (7)0.0926 (5)0.4390 (7)0.035 (2)
H180.17150.08500.37850.042*
C190.2527 (8)0.1023 (6)0.5388 (8)0.033 (2)
C200.3556 (8)0.0931 (5)0.5668 (8)0.033 (2)
C210.3834 (7)0.0793 (5)0.4818 (8)0.035 (2)
C220.3753 (9)0.0110 (6)0.4399 (9)0.050 (3)
H220.35150.02720.46500.060*
C230.4010 (9)0.0024 (6)0.3624 (9)0.053 (3)
H230.39470.04890.33530.063*
C240.4372 (10)0.0554 (7)0.3244 (10)0.066 (3)
H240.45450.04730.27150.079*
C250.4468 (12)0.1241 (7)0.3661 (12)0.075 (4)
H250.47250.16200.34240.090*
C260.4191 (10)0.1369 (7)0.4416 (9)0.059 (3)
H260.42350.18370.46710.070*
C270.7459 (9)0.1612 (5)0.9975 (9)0.046 (3)
H270.72060.19200.94050.056*
C280.8498 (9)0.1609 (6)1.0673 (9)0.052 (3)
H280.89390.19301.05730.062*
C290.8929 (11)0.1146 (8)1.1530 (10)0.056 (4)
H290.96430.11331.19740.067*
C300.8228 (9)0.0705 (6)1.1684 (9)0.049 (3)
H300.84750.04091.22670.059*
C310.7198 (8)0.0698 (5)1.1004 (7)0.042 (2)
H310.67610.03871.11250.051*
C320.6773 (7)0.1135 (5)1.0136 (7)0.034 (2)
C330.2005 (12)0.2385 (8)1.0674 (11)0.078 (4)
H330.21070.27671.03150.094*
C340.1731 (12)0.2528 (8)1.1436 (12)0.075 (4)
H340.16430.30091.15770.090*
C350.1584 (12)0.1991 (8)1.1994 (11)0.076 (4)
H350.14410.20951.25370.092*
C360.1656 (12)0.1274 (8)1.1715 (11)0.073 (4)
H360.15270.08941.20590.088*
C370.1910 (10)0.1122 (7)1.0953 (10)0.060 (3)
H370.19400.06411.07710.072*
C380.2128 (8)0.1685 (6)1.0439 (8)0.040 (2)
C390.0765 (7)0.1179 (5)0.5115 (7)0.032 (2)
C400.1353 (9)0.0562 (7)0.4896 (11)0.070 (4)
H400.10460.01360.52480.084*
C410.2426 (11)0.0554 (8)0.4144 (12)0.080 (5)
H410.28010.01220.39810.096*
C420.2883 (9)0.1160 (8)0.3683 (10)0.056 (3)
H420.35980.11660.32410.067*
C430.2294 (10)0.1801 (7)0.3856 (12)0.076 (4)
H430.25800.22160.34590.091*
C440.1285 (10)0.1794 (6)0.4627 (11)0.065 (4)
H440.09340.22350.48320.078*
C450.4836 (7)0.3637 (4)0.9034 (7)0.030 (2)
C460.5922 (7)0.3488 (5)0.9348 (8)0.040 (2)
H460.64610.34391.00190.048*
C470.5990 (8)0.3433 (5)0.8460 (8)0.043 (2)
H470.66010.33650.84100.052*
C480.4984 (8)0.3497 (5)0.7625 (8)0.034 (2)
C490.4725 (7)0.3466 (5)0.6575 (8)0.0304 (19)
C500.3732 (8)0.3522 (6)0.5766 (8)0.037 (2)
C510.3462 (8)0.3518 (5)0.4704 (8)0.037 (2)
H510.39330.34640.44430.045*
C520.2435 (7)0.3604 (5)0.4133 (8)0.038 (2)
H520.20630.36070.34150.045*
C530.2009 (8)0.3690 (6)0.4855 (8)0.034 (2)
C540.0953 (8)0.3809 (5)0.4539 (7)0.032 (2)
C550.0559 (8)0.3913 (5)0.5241 (7)0.035 (2)
C560.0514 (7)0.4098 (5)0.4921 (8)0.040 (2)
H560.10460.41620.42500.047*
C570.0576 (7)0.4156 (5)0.5804 (7)0.034 (2)
H570.11850.42490.58490.041*
C580.0421 (7)0.4054 (5)0.6655 (8)0.030 (2)
C590.0659 (7)0.4104 (4)0.7676 (7)0.0293 (19)
C600.1670 (7)0.4084 (5)0.8505 (8)0.0294 (19)
C610.1965 (7)0.4265 (5)0.9552 (8)0.037 (2)
H610.15130.44150.98040.044*
C620.2997 (7)0.4184 (5)1.0113 (7)0.036 (2)
H620.33920.42661.08180.044*
C630.3394 (7)0.3935 (5)0.9391 (7)0.026 (2)
C640.4404 (7)0.3792 (4)0.9720 (7)0.032 (2)
C650.5182 (7)0.3802 (5)1.0863 (7)0.035 (2)
C660.6035 (7)0.4271 (5)1.1273 (8)0.039 (2)
H660.61480.45921.08430.047*
C670.6702 (8)0.4258 (6)1.2302 (8)0.045 (2)
H670.72650.45761.25670.054*
C680.6574 (9)0.3788 (7)1.2968 (9)0.044 (3)
H680.70500.37791.36680.053*
C690.5731 (9)0.3337 (6)1.2573 (9)0.048 (3)
H690.56140.30331.30160.057*
C700.5047 (9)0.3323 (6)1.1529 (8)0.047 (3)
H700.44970.29931.12700.056*
C710.5589 (7)0.3314 (5)0.6317 (8)0.037 (2)
C720.5948 (9)0.3860 (7)0.5932 (10)0.057 (3)
H720.56580.43220.58390.068*
C730.6738 (10)0.3726 (8)0.5680 (10)0.064 (3)
H730.69620.40980.54010.076*
C740.7191 (10)0.3070 (8)0.5828 (11)0.071 (4)
H740.77400.29950.56770.085*
C750.6841 (11)0.2509 (7)0.6205 (12)0.069 (4)
H750.71280.20470.62810.083*
C760.6055 (10)0.2640 (6)0.6471 (11)0.060 (3)
H760.58390.22680.67580.071*
C770.0062 (10)0.4507 (6)0.2897 (9)0.063 (4)
H770.04670.49100.32310.075*
C780.0669 (10)0.4561 (6)0.1884 (9)0.064 (4)
H780.07710.50070.15500.077*
C790.1257 (11)0.3975 (8)0.1344 (9)0.064 (4)
H790.17420.40100.06490.077*
C800.1097 (12)0.3328 (6)0.1883 (10)0.078 (5)
H800.14850.29190.15470.094*
C810.0390 (10)0.3284 (6)0.2880 (9)0.057 (3)
H810.03020.28400.32160.068*
C820.0212 (7)0.3863 (5)0.3433 (7)0.0291 (19)
C830.0641 (8)0.4936 (6)0.7802 (8)0.044 (2)
H830.04160.53100.75260.052*
C840.1427 (9)0.5056 (7)0.8061 (9)0.059 (3)
H840.17330.55130.79500.071*
C850.1773 (10)0.4514 (8)0.8482 (10)0.066 (3)
H850.23050.46020.86530.079*
C860.1322 (10)0.3859 (8)0.8636 (13)0.072 (4)
H860.15450.34890.89200.086*
C870.0532 (9)0.3720 (6)0.8380 (10)0.054 (3)
H870.02300.32610.84950.064*
C880.0189 (7)0.4263 (6)0.7953 (8)0.039 (2)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Nb10.0245 (4)0.0207 (4)0.0247 (4)0.0001 (3)0.0123 (3)0.0003 (3)
Nb20.0212 (4)0.0230 (4)0.0270 (4)0.0004 (3)0.0155 (3)0.0011 (3)
O10.055 (4)0.028 (3)0.022 (3)0.006 (3)0.011 (3)0.003 (2)
O20.029 (3)0.032 (3)0.047 (4)0.002 (2)0.025 (3)0.003 (3)
O30.041 (4)0.033 (3)0.041 (4)0.003 (3)0.005 (3)0.001 (3)
N10.030 (4)0.031 (4)0.031 (4)0.001 (3)0.019 (3)0.008 (3)
N20.029 (4)0.034 (4)0.033 (4)0.005 (3)0.010 (3)0.014 (3)
N30.042 (4)0.019 (3)0.034 (4)0.003 (3)0.024 (3)0.006 (3)
N40.024 (4)0.032 (4)0.033 (4)0.007 (3)0.016 (3)0.007 (3)
N50.027 (4)0.032 (4)0.032 (4)0.007 (3)0.010 (3)0.001 (3)
N60.033 (4)0.021 (3)0.031 (4)0.004 (3)0.019 (3)0.003 (3)
N70.032 (4)0.028 (3)0.034 (4)0.007 (3)0.019 (3)0.002 (3)
N80.027 (4)0.021 (3)0.032 (4)0.003 (3)0.016 (3)0.005 (3)
C10.037 (5)0.032 (4)0.033 (5)0.000 (4)0.018 (4)0.001 (4)
C20.047 (6)0.030 (4)0.041 (6)0.004 (4)0.028 (5)0.002 (4)
C30.033 (5)0.038 (5)0.045 (6)0.002 (4)0.018 (4)0.004 (4)
C40.027 (5)0.046 (6)0.037 (6)0.004 (4)0.014 (4)0.008 (4)
C50.032 (5)0.023 (4)0.041 (5)0.008 (4)0.018 (4)0.005 (4)
C60.031 (5)0.029 (5)0.036 (6)0.001 (4)0.012 (4)0.011 (4)
C70.048 (6)0.043 (5)0.032 (5)0.003 (4)0.018 (5)0.006 (4)
C80.040 (5)0.041 (5)0.033 (5)0.002 (4)0.014 (4)0.000 (4)
C90.044 (6)0.026 (4)0.039 (6)0.003 (4)0.024 (5)0.009 (4)
C100.054 (6)0.031 (4)0.039 (6)0.001 (4)0.032 (5)0.007 (4)
C110.041 (6)0.021 (4)0.042 (6)0.006 (4)0.030 (5)0.001 (4)
C120.041 (6)0.048 (5)0.043 (6)0.006 (5)0.034 (5)0.010 (4)
C130.036 (5)0.049 (6)0.042 (6)0.005 (4)0.019 (4)0.006 (5)
C140.038 (5)0.031 (5)0.031 (5)0.008 (4)0.021 (4)0.002 (4)
C150.030 (5)0.025 (4)0.035 (5)0.003 (3)0.018 (4)0.001 (3)
C160.034 (5)0.023 (4)0.031 (5)0.001 (3)0.014 (4)0.006 (4)
C170.027 (5)0.051 (6)0.036 (5)0.004 (4)0.010 (4)0.001 (5)
C180.043 (5)0.032 (4)0.026 (4)0.002 (4)0.013 (4)0.002 (4)
C190.031 (5)0.036 (5)0.040 (6)0.006 (4)0.024 (4)0.002 (4)
C200.039 (5)0.029 (4)0.035 (5)0.006 (4)0.019 (4)0.001 (4)
C210.032 (5)0.039 (5)0.039 (5)0.001 (4)0.021 (4)0.002 (4)
C220.060 (7)0.048 (6)0.050 (6)0.004 (5)0.032 (5)0.004 (5)
C230.066 (7)0.052 (6)0.055 (7)0.006 (5)0.040 (6)0.007 (5)
C240.076 (9)0.084 (9)0.068 (8)0.004 (7)0.060 (7)0.010 (7)
C250.107 (11)0.065 (8)0.088 (10)0.012 (7)0.075 (9)0.002 (7)
C260.081 (8)0.057 (7)0.058 (7)0.020 (6)0.048 (6)0.003 (6)
C270.052 (6)0.041 (5)0.047 (6)0.002 (4)0.023 (5)0.001 (4)
C280.054 (7)0.042 (6)0.059 (7)0.010 (5)0.027 (5)0.008 (5)
C290.043 (7)0.068 (8)0.047 (7)0.014 (6)0.012 (6)0.016 (6)
C300.051 (6)0.045 (6)0.044 (6)0.017 (5)0.015 (5)0.003 (5)
C310.046 (6)0.037 (5)0.033 (5)0.008 (4)0.010 (4)0.004 (4)
C320.032 (5)0.035 (5)0.037 (5)0.001 (4)0.018 (4)0.015 (4)
C330.100 (7)0.087 (7)0.075 (7)0.001 (6)0.064 (6)0.009 (5)
C340.095 (7)0.066 (6)0.080 (7)0.010 (5)0.054 (5)0.005 (5)
C350.088 (7)0.090 (7)0.062 (6)0.007 (6)0.044 (5)0.002 (5)
C360.092 (7)0.084 (7)0.065 (6)0.004 (5)0.054 (5)0.006 (5)
C370.077 (6)0.058 (6)0.063 (6)0.003 (5)0.047 (5)0.001 (5)
C380.039 (5)0.056 (6)0.033 (5)0.006 (4)0.023 (4)0.000 (5)
C390.034 (5)0.026 (4)0.036 (5)0.007 (3)0.016 (4)0.003 (4)
C400.050 (7)0.053 (6)0.077 (9)0.020 (5)0.004 (6)0.013 (6)
C410.054 (8)0.073 (9)0.082 (10)0.007 (7)0.005 (7)0.006 (8)
C420.031 (6)0.086 (9)0.047 (7)0.002 (6)0.015 (5)0.001 (7)
C430.055 (8)0.064 (8)0.081 (10)0.013 (6)0.007 (7)0.010 (7)
C440.053 (7)0.039 (6)0.078 (9)0.003 (5)0.010 (6)0.002 (6)
C450.032 (5)0.020 (4)0.030 (5)0.007 (4)0.009 (4)0.004 (4)
C460.028 (5)0.045 (5)0.043 (6)0.002 (4)0.013 (4)0.007 (4)
C470.043 (6)0.045 (5)0.043 (6)0.007 (4)0.022 (5)0.004 (4)
C480.049 (6)0.023 (4)0.035 (5)0.000 (4)0.023 (4)0.003 (4)
C490.029 (5)0.031 (4)0.045 (5)0.002 (4)0.028 (4)0.001 (4)
C500.036 (6)0.037 (5)0.035 (6)0.005 (4)0.015 (4)0.004 (4)
C510.043 (6)0.042 (5)0.040 (6)0.001 (4)0.030 (5)0.006 (4)
C520.038 (5)0.046 (5)0.041 (5)0.002 (4)0.029 (4)0.003 (4)
C530.035 (5)0.046 (6)0.024 (5)0.002 (4)0.017 (4)0.004 (4)
C540.039 (5)0.026 (4)0.031 (5)0.007 (4)0.016 (4)0.003 (4)
C550.033 (5)0.032 (5)0.033 (5)0.010 (4)0.009 (4)0.006 (4)
C560.027 (5)0.044 (5)0.043 (6)0.002 (4)0.012 (4)0.008 (4)
C570.026 (4)0.035 (4)0.043 (5)0.003 (3)0.018 (4)0.001 (4)
C580.024 (4)0.031 (5)0.039 (5)0.001 (4)0.017 (4)0.004 (4)
C590.026 (5)0.022 (4)0.044 (5)0.005 (3)0.020 (4)0.000 (4)
C600.029 (5)0.025 (4)0.039 (5)0.000 (4)0.020 (4)0.004 (4)
C610.034 (5)0.044 (5)0.041 (6)0.002 (4)0.024 (4)0.006 (4)
C620.039 (5)0.038 (5)0.029 (5)0.001 (4)0.013 (4)0.001 (4)
C630.024 (5)0.023 (4)0.032 (5)0.002 (3)0.014 (4)0.001 (4)
C640.035 (5)0.024 (4)0.031 (5)0.011 (3)0.009 (4)0.005 (4)
C650.032 (5)0.031 (4)0.034 (5)0.007 (4)0.010 (4)0.001 (4)
C660.038 (5)0.036 (5)0.041 (5)0.001 (4)0.016 (4)0.000 (4)
C670.031 (5)0.053 (6)0.043 (6)0.002 (4)0.012 (4)0.010 (5)
C680.041 (6)0.061 (7)0.029 (6)0.004 (5)0.016 (5)0.002 (5)
C690.053 (6)0.047 (6)0.050 (6)0.012 (5)0.030 (5)0.010 (5)
C700.050 (6)0.047 (6)0.037 (5)0.005 (5)0.014 (5)0.005 (4)
C710.030 (5)0.051 (6)0.040 (5)0.002 (4)0.024 (4)0.004 (4)
C720.049 (6)0.071 (7)0.069 (8)0.007 (6)0.043 (6)0.009 (6)
C730.058 (7)0.081 (9)0.074 (9)0.003 (6)0.050 (7)0.011 (7)
C740.058 (8)0.102 (11)0.080 (9)0.010 (7)0.055 (7)0.015 (8)
C750.067 (8)0.062 (7)0.097 (10)0.005 (6)0.054 (7)0.014 (7)
C760.075 (8)0.044 (6)0.097 (10)0.003 (5)0.072 (7)0.002 (6)
C770.068 (8)0.042 (6)0.052 (7)0.013 (5)0.006 (6)0.005 (5)
C780.080 (9)0.048 (6)0.047 (7)0.010 (6)0.015 (6)0.018 (5)
C790.063 (8)0.091 (10)0.025 (6)0.006 (7)0.009 (5)0.000 (6)
C800.096 (11)0.043 (6)0.053 (8)0.005 (6)0.000 (7)0.020 (6)
C810.072 (8)0.047 (6)0.043 (6)0.010 (5)0.021 (6)0.000 (5)
C820.031 (5)0.028 (4)0.034 (5)0.002 (3)0.020 (4)0.000 (4)
C830.049 (6)0.048 (5)0.042 (6)0.007 (4)0.028 (5)0.003 (4)
C840.054 (7)0.075 (8)0.061 (7)0.024 (6)0.038 (6)0.001 (6)
C850.060 (7)0.097 (10)0.063 (8)0.007 (7)0.047 (6)0.007 (7)
C860.059 (8)0.078 (9)0.110 (12)0.003 (7)0.066 (8)0.010 (8)
C870.062 (7)0.054 (6)0.067 (8)0.002 (5)0.047 (6)0.000 (6)
C880.030 (5)0.054 (6)0.038 (5)0.006 (4)0.020 (4)0.001 (4)
Geometric parameters (Å, º) top
Nb1—O11.876 (6)C36—C371.356 (18)
Nb1—O21.815 (6)C36—H360.9300
Nb1—O32.331 (6)C37—C381.400 (16)
Nb1—N12.240 (7)C37—H370.9300
Nb1—N22.228 (7)C39—C441.362 (14)
Nb1—N32.261 (7)C39—C401.365 (13)
Nb1—N42.224 (7)C40—C411.425 (17)
Nb1—Nb22.8200 (8)C40—H400.9300
Nb2—O12.019 (6)C41—C421.311 (19)
Nb2—O22.182 (6)C41—H410.9300
Nb2—O31.757 (6)C42—C431.409 (19)
Nb2—N52.260 (7)C42—H420.9300
Nb2—N62.226 (7)C43—C441.367 (16)
Nb2—N72.227 (7)C43—H430.9300
Nb2—N82.246 (7)C44—H440.9300
N1—C11.369 (12)C45—C641.438 (15)
N1—C41.395 (12)C45—C461.445 (14)
N2—C61.396 (12)C46—C471.352 (15)
N2—C91.433 (14)C46—H460.9300
N3—C111.352 (12)C47—C481.402 (15)
N3—C141.355 (12)C47—H470.9300
N4—C161.393 (11)C48—C491.401 (14)
N4—C191.395 (12)C49—C501.375 (14)
N5—C451.359 (11)C49—C711.492 (13)
N5—C481.419 (13)C50—C511.413 (15)
N6—C531.377 (12)C51—C521.332 (13)
N6—C501.378 (13)C51—H510.9300
N7—C551.379 (12)C52—C531.460 (14)
N7—C581.392 (12)C52—H520.9300
N8—C601.376 (11)C53—C541.393 (14)
N8—C631.389 (11)C54—C551.401 (14)
C1—C201.404 (14)C54—C821.469 (13)
C1—C21.406 (14)C55—C561.439 (13)
C2—C31.323 (14)C56—C571.340 (14)
C2—H20.9300C56—H560.9300
C3—C41.444 (15)C57—C581.412 (13)
C3—H30.9300C57—H570.9300
C4—C51.377 (14)C58—C591.370 (14)
C5—C61.369 (15)C59—C601.400 (13)
C5—C321.478 (13)C59—C881.489 (13)
C6—C71.458 (15)C60—C611.424 (14)
C7—C81.348 (15)C61—C621.336 (13)
C7—H70.9300C61—H610.9300
C8—C91.402 (14)C62—C631.490 (14)
C8—H80.9300C62—H620.9300
C9—C101.386 (15)C63—C641.334 (13)
C10—C111.357 (14)C64—C651.519 (13)
C10—C381.516 (14)C65—C661.393 (13)
C11—C121.457 (14)C65—C701.394 (15)
C12—C131.312 (14)C66—C671.357 (14)
C12—H120.9300C66—H660.9300
C13—C141.461 (15)C67—C681.379 (16)
C13—H130.9300C67—H670.9300
C14—C151.395 (13)C68—C691.361 (16)
C15—C161.389 (13)C68—H680.9300
C15—C391.478 (12)C69—C701.379 (15)
C16—C171.418 (14)C69—H690.9300
C17—C181.334 (14)C70—H700.9300
C17—H170.9300C71—C721.368 (16)
C18—C191.421 (13)C71—C761.378 (14)
C18—H180.9300C72—C731.379 (16)
C19—C201.359 (14)C72—H720.9300
C20—C211.496 (14)C73—C741.342 (18)
C21—C221.380 (14)C73—H730.9300
C21—C261.420 (14)C74—C751.374 (19)
C22—C231.370 (15)C74—H740.9300
C22—H220.9300C75—C761.385 (17)
C23—C241.410 (17)C75—H750.9300
C23—H230.9300C76—H760.9300
C24—C251.383 (18)C77—C781.364 (16)
C24—H240.9300C77—C821.381 (14)
C25—C261.360 (18)C77—H770.9300
C25—H250.9300C78—C791.374 (17)
C26—H260.9300C78—H780.9300
C27—C281.368 (16)C79—C801.386 (19)
C27—C321.426 (15)C79—H790.9300
C27—H270.9300C80—C811.336 (17)
C28—C291.398 (18)C80—H800.9300
C28—H280.9300C81—C821.376 (13)
C29—C301.398 (19)C81—H810.9300
C29—H290.9300C83—C881.370 (14)
C30—C311.352 (14)C83—C841.375 (15)
C30—H300.9300C83—H830.9300
C31—C321.381 (13)C84—C851.383 (18)
C31—H310.9300C84—H840.9300
C33—C381.366 (17)C85—C861.339 (18)
C33—C341.37 (2)C85—H850.9300
C33—H330.9300C86—C871.384 (17)
C34—C351.36 (2)C86—H860.9300
C34—H340.9300C87—C881.387 (15)
C35—C361.40 (2)C87—H870.9300
C35—H350.9300
O2—Nb1—O183.9 (3)C30—C31—H31118.8
O2—Nb1—N490.4 (3)C32—C31—H31118.8
O1—Nb1—N4147.1 (3)C31—C32—C27117.6 (9)
O2—Nb1—N2129.5 (3)C31—C32—C5122.6 (9)
O1—Nb1—N277.5 (3)C27—C32—C5119.8 (9)
N4—Nb1—N2128.4 (3)C38—C33—C34120.4 (14)
O2—Nb1—N180.5 (3)C38—C33—H33119.8
O1—Nb1—N1129.8 (3)C34—C33—H33119.8
N4—Nb1—N180.5 (3)C35—C34—C33122.2 (14)
N2—Nb1—N176.7 (3)C35—C34—H34118.9
O2—Nb1—N3145.7 (3)C33—C34—H34118.9
O1—Nb1—N388.4 (3)C34—C35—C36117.2 (14)
N4—Nb1—N378.2 (3)C34—C35—H35121.4
N2—Nb1—N380.6 (3)C36—C35—H35121.4
N1—Nb1—N3128.1 (3)C37—C36—C35121.4 (13)
O2—Nb1—O371.8 (3)C37—C36—H36119.3
O1—Nb1—O371.0 (2)C35—C36—H36119.3
N4—Nb1—O376.4 (2)C36—C37—C38120.2 (12)
N2—Nb1—O3139.6 (3)C36—C37—H37119.9
N1—Nb1—O3143.5 (3)C38—C37—H37119.9
N3—Nb1—O374.1 (3)C33—C38—C37118.4 (11)
O2—Nb1—Nb250.68 (19)C33—C38—C10121.1 (10)
O1—Nb1—Nb245.65 (18)C37—C38—C10120.2 (10)
N4—Nb1—Nb2107.68 (18)C44—C39—C40115.8 (10)
N2—Nb1—Nb2122.5 (2)C44—C39—C15122.2 (8)
N1—Nb1—Nb2129.65 (18)C40—C39—C15121.9 (9)
N3—Nb1—Nb2101.91 (17)C39—C40—C41121.8 (11)
O3—Nb1—Nb238.44 (15)C39—C40—H40119.1
O3—Nb2—O181.4 (3)C41—C40—H40119.1
O3—Nb2—O276.7 (3)C42—C41—C40119.7 (13)
O1—Nb2—O271.9 (3)C42—C41—H41120.2
O3—Nb2—N6102.4 (3)C40—C41—H41120.2
O1—Nb2—N6145.0 (3)C41—C42—C43120.1 (11)
O2—Nb2—N675.3 (2)C41—C42—H42119.9
O3—Nb2—N781.3 (3)C43—C42—H42119.9
O1—Nb2—N7134.4 (3)C44—C43—C42117.6 (12)
O2—Nb2—N7142.2 (3)C44—C43—H43121.2
N6—Nb2—N780.0 (3)C42—C43—H43121.2
O3—Nb2—N8120.3 (3)C39—C44—C43123.9 (11)
O1—Nb2—N876.0 (3)C39—C44—H44118.0
O2—Nb2—N8140.6 (2)C43—C44—H44118.0
N6—Nb2—N8126.9 (3)N5—C45—C64122.6 (9)
N7—Nb2—N877.1 (3)N5—C45—C46112.0 (9)
O3—Nb2—N5150.3 (3)C64—C45—C46125.4 (8)
O1—Nb2—N581.6 (3)C47—C46—C45105.4 (9)
O2—Nb2—N574.9 (2)C47—C46—H46127.3
N6—Nb2—N578.6 (3)C45—C46—H46127.3
N7—Nb2—N5127.4 (3)C46—C47—C48108.6 (10)
N8—Nb2—N578.5 (3)C46—C47—H47125.7
O3—Nb2—Nb155.5 (2)C48—C47—H47125.7
O1—Nb2—Nb141.65 (18)C49—C48—C47126.1 (10)
O2—Nb2—Nb140.07 (16)C49—C48—N5123.7 (9)
N6—Nb2—Nb1112.57 (18)C47—C48—N5110.2 (9)
N7—Nb2—Nb1136.36 (19)C50—C49—C48125.3 (10)
N8—Nb2—Nb1117.08 (18)C50—C49—C71117.4 (10)
N5—Nb2—Nb196.21 (19)C48—C49—C71117.2 (9)
Nb1—O1—Nb292.7 (3)C49—C50—N6126.5 (10)
Nb1—O2—Nb289.3 (3)C49—C50—C51125.9 (10)
Nb2—O3—Nb186.0 (2)N6—C50—C51107.5 (8)
C1—N1—C4106.3 (8)C52—C51—C50110.1 (10)
C1—N1—Nb1123.9 (6)C52—C51—H51124.9
C4—N1—Nb1125.2 (6)C50—C51—H51124.9
C6—N2—C9106.0 (8)C51—C52—C53106.5 (9)
C6—N2—Nb1124.9 (7)C51—C52—H52126.7
C9—N2—Nb1119.7 (6)C53—C52—H52126.7
C11—N3—C14108.0 (8)N6—C53—C54129.4 (9)
C11—N3—Nb1120.5 (6)N6—C53—C52107.4 (9)
C14—N3—Nb1125.4 (6)C54—C53—C52123.1 (9)
C16—N4—C19105.7 (8)C53—C54—C55122.5 (9)
C16—N4—Nb1127.2 (6)C53—C54—C82120.1 (9)
C19—N4—Nb1122.1 (6)C55—C54—C82117.4 (9)
C45—N5—C48103.7 (8)N7—C55—C54125.3 (9)
C45—N5—Nb2125.0 (6)N7—C55—C56111.8 (9)
C48—N5—Nb2123.2 (6)C54—C55—C56122.8 (9)
C53—N6—C50108.4 (8)C57—C56—C55104.7 (9)
C53—N6—Nb2121.4 (6)C57—C56—H56127.7
C50—N6—Nb2124.5 (6)C55—C56—H56127.7
C55—N7—C58104.0 (8)C56—C57—C58109.8 (9)
C55—N7—Nb2123.6 (6)C56—C57—H57125.1
C58—N7—Nb2124.8 (6)C58—C57—H57125.1
C60—N8—C63107.4 (8)C59—C58—N7124.6 (8)
C60—N8—Nb2125.9 (6)C59—C58—C57125.8 (9)
C63—N8—Nb2121.6 (5)N7—C58—C57109.6 (9)
N1—C1—C20124.3 (9)C58—C59—C60124.8 (9)
N1—C1—C2110.1 (8)C58—C59—C88119.3 (8)
C20—C1—C2125.6 (10)C60—C59—C88115.6 (9)
C3—C2—C1108.0 (9)N8—C60—C59124.0 (9)
C3—C2—H2126.0N8—C60—C61109.7 (8)
C1—C2—H2126.0C59—C60—C61126.3 (9)
C2—C3—C4108.3 (9)C62—C61—C60108.7 (9)
C2—C3—H3125.8C62—C61—H61125.6
C4—C3—H3125.8C60—C61—H61125.6
C5—C4—N1127.6 (9)C61—C62—C63106.9 (8)
C5—C4—C3125.2 (9)C61—C62—H62126.5
N1—C4—C3107.2 (9)C63—C62—H62126.5
C6—C5—C4121.4 (9)C64—C63—N8131.1 (9)
C6—C5—C32119.8 (9)C64—C63—C62121.7 (9)
C4—C5—C32118.8 (9)N8—C63—C62107.1 (7)
C5—C6—N2126.4 (10)C63—C64—C45123.2 (9)
C5—C6—C7124.7 (9)C63—C64—C65121.3 (10)
N2—C6—C7108.7 (9)C45—C64—C65115.4 (8)
C8—C7—C6106.5 (9)C66—C65—C70118.5 (9)
C8—C7—H7126.8C66—C65—C64122.3 (9)
C6—C7—H7126.8C70—C65—C64119.2 (8)
C7—C8—C9110.6 (10)C67—C66—C65119.6 (10)
C7—C8—H8124.7C67—C66—H66120.2
C9—C8—H8124.7C65—C66—H66120.2
C10—C9—C8128.2 (10)C66—C67—C68122.4 (10)
C10—C9—N2123.9 (9)C66—C67—H67118.8
C8—C9—N2107.9 (9)C68—C67—H67118.8
C11—C10—C9127.5 (10)C69—C68—C67118.1 (10)
C11—C10—C38116.9 (9)C69—C68—H68120.9
C9—C10—C38115.6 (9)C67—C68—H68120.9
N3—C11—C10126.9 (10)C68—C69—C70121.4 (11)
N3—C11—C12108.1 (8)C68—C69—H69119.3
C10—C11—C12125.0 (9)C70—C69—H69119.3
C13—C12—C11108.3 (9)C69—C70—C65119.9 (10)
C13—C12—H12125.9C69—C70—H70120.0
C11—C12—H12125.9C65—C70—H70120.0
C12—C13—C14106.7 (9)C72—C71—C76118.4 (10)
C12—C13—H13126.6C72—C71—C49119.4 (9)
C14—C13—H13126.6C76—C71—C49122.2 (9)
N3—C14—C15126.9 (9)C71—C72—C73120.1 (12)
N3—C14—C13108.8 (8)C71—C72—H72119.9
C15—C14—C13124.2 (9)C73—C72—H72119.9
C16—C15—C14123.7 (8)C74—C73—C72121.5 (12)
C16—C15—C39115.4 (8)C74—C73—H73119.3
C14—C15—C39120.9 (9)C72—C73—H73119.3
C15—C16—N4124.9 (8)C73—C74—C75119.7 (12)
C15—C16—C17125.2 (8)C73—C74—H74120.1
N4—C16—C17109.9 (8)C75—C74—H74120.1
C18—C17—C16106.7 (8)C74—C75—C76119.2 (12)
C18—C17—H17126.6C74—C75—H75120.4
C16—C17—H17126.6C76—C75—H75120.4
C17—C18—C19109.7 (9)C71—C76—C75121.0 (11)
C17—C18—H18125.1C71—C76—H76119.5
C19—C18—H18125.1C75—C76—H76119.5
C20—C19—N4124.2 (9)C78—C77—C82121.0 (10)
C20—C19—C18127.4 (10)C78—C77—H77119.5
N4—C19—C18107.9 (8)C82—C77—H77119.5
C19—C20—C1127.9 (10)C77—C78—C79121.7 (11)
C19—C20—C21116.9 (9)C77—C78—H78119.1
C1—C20—C21115.1 (9)C79—C78—H78119.1
C22—C21—C26117.8 (10)C78—C79—C80117.0 (10)
C22—C21—C20121.6 (9)C78—C79—H79121.5
C26—C21—C20120.6 (9)C80—C79—H79121.5
C23—C22—C21122.1 (11)C81—C80—C79120.8 (11)
C23—C22—H22118.9C81—C80—H80119.6
C21—C22—H22118.9C79—C80—H80119.6
C22—C23—C24119.0 (11)C80—C81—C82123.1 (11)
C22—C23—H23120.5C80—C81—H81118.4
C24—C23—H23120.5C82—C81—H81118.4
C25—C24—C23119.7 (11)C81—C82—C77116.3 (9)
C25—C24—H24120.1C81—C82—C54122.1 (8)
C23—C24—H24120.1C77—C82—C54121.6 (8)
C26—C25—C24120.6 (12)C88—C83—C84119.7 (10)
C26—C25—H25119.7C88—C83—H83120.1
C24—C25—H25119.7C84—C83—H83120.1
C25—C26—C21120.7 (12)C83—C84—C85121.7 (11)
C25—C26—H26119.6C83—C84—H84119.2
C21—C26—H26119.6C85—C84—H84119.2
C28—C27—C32118.9 (10)C86—C85—C84118.4 (11)
C28—C27—H27120.6C86—C85—H85120.8
C32—C27—H27120.6C84—C85—H85120.8
C27—C28—C29123.2 (12)C85—C86—C87121.3 (13)
C27—C28—H28118.4C85—C86—H86119.3
C29—C28—H28118.4C87—C86—H86119.3
C28—C29—C30116.4 (11)C86—C87—C88120.3 (11)
C28—C29—H29121.8C86—C87—H87119.8
C30—C29—H29121.8C88—C87—H87119.8
C31—C30—C29121.4 (11)C83—C88—C87118.6 (10)
C31—C30—H30119.3C83—C88—C59121.7 (9)
C29—C30—H30119.3C87—C88—C59119.7 (9)
C30—C31—C32122.5 (11)
Hydrogen-bond geometry (Å, º) top
Cg1 and Cg2 are the centroids of the C27-benzene ring and N1-pyrrole ring, respectively.
D—H···AD—HH···AD···AD—H···A
C22—H22···Cg1i0.932.853.752 (14)164
C40—H40···Cg2i0.932.873.681 (14)147
Symmetry code: (i) x1/2, y, z1/2.

Experimental details

Crystal data
Chemical formula[Nb2(C44H28N4)2O3]
Mr1459.28
Crystal system, space groupMonoclinic, Pn
Temperature (K)180
a, b, c (Å)14.4823 (9), 18.4007 (8), 14.6257 (10)
β (°) 117.823 (7)
V3)3446.9 (4)
Z2
Radiation typeMo Kα
µ (mm1)0.39
Crystal size (mm)0.5 × 0.3 × 0.1
Data collection
DiffractometerBruker APEXII CCD area-detector
diffractometer
Absorption correctionMulti-scan
(SADABS; Bruker, 2007)
Tmin, Tmax0.72, 1.00
No. of measured, independent and
observed [I > 2σ(I)] reflections
25553, 9945, 8244
Rint0.055
(sin θ/λ)max1)0.617
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.062, 0.166, 1.06
No. of reflections9945
No. of parameters910
No. of restraints32
H-atom treatmentH-atom parameters constrained
w = 1/[σ2(Fo2) + (0.0709P)2 + 14.5546P]
whereP = (Fo2 + 2Fc2)/3
Δρmax, Δρmin (e Å3)1.20, 0.91
Absolute structureFlack (1983), 2439 Friedel pairs
Absolute structure parameter0.01 (6)

Computer programs: APEX2 (Bruker, 2007), SAINT (Bruker, 2007), SIR2004 (Burla et al., 2005), SHELXL97 (Sheldrick, 2008), ORTEPIII (Burnett & Johnson, 1996), publCIF (Westrip, 2010)..

Selected bond lengths (Å) top
Nb1—O11.876 (6)Nb2—O12.019 (6)
Nb1—O21.815 (6)Nb2—O22.182 (6)
Nb1—O32.331 (6)Nb2—O31.757 (6)
Nb1—N12.240 (7)Nb2—N52.260 (7)
Nb1—N22.228 (7)Nb2—N62.226 (7)
Nb1—N32.261 (7)Nb2—N72.227 (7)
Nb1—N42.224 (7)Nb2—N82.246 (7)
Hydrogen-bond geometry (Å, º) top
Cg1 and Cg2 are the centroids of the C27-benzene ring and N1-pyrrole ring, respectively.
D—H···AD—HH···AD···AD—H···A
C22—H22···Cg1i0.932.853.752 (14)164
C40—H40···Cg2i0.932.873.681 (14)147
Symmetry code: (i) x1/2, y, z1/2.
 

Acknowledgements

The authors gratefully acknowledge financial support from the Ministry of Higher Education and Scientific Research of Tunisia.

References

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First citationScheidt, W. R. (2000). The Porphyrin Handbook, Vol. 3, edited by K. M. Kadish, R. M. Smith & R. Guilard, pp. 49–112. San Diego: Academic Press.  Google Scholar
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Volume 67| Part 7| July 2011| Pages m862-m863
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