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Acta Cryst. (2007). E63, m2233    [ doi:10.1107/S1600536807034277 ]

Poly[[[mu]2-trans-1,2-di-4-pyridylethylene]hexa-[mu]2-oxido-nickel(II)divanadate(V)]

C.-C. Wang

Abstract top

The structure of the title compound, [NiV2O6(C12H10N2)]n, is composed of corner-sharing [V2O6]2- chains along the c axis, with the [Ni(bpe)]2+ (bpe = trans-1,2-di-4-pyridylethylene) units covalently attached to every V site through O atoms. The Ni atom is octahedrally coordinated by two pyridyl N atoms from two different bpe ligands, and four O atoms from four different VO4 tetrahedra. All the C and H atoms are disordered over two positions each; the site occupancy factors are ca 0.55 and 0.45.

Comment top

Early transition metal oxide anion clusters (or POMs) are a rapidly growing class of compound. They have been of great interest because of their so-called 'Value-adding properties' and potential applications in such areas as catalysis, gas storage and chemical sensing (Khan, 2000; Khan, Yohannes & Doedens, 1999; Khan, Yohannes & Powell, 1999). Hydrothermal synthesis and structural characterization of vanadium oxide compounds containing Zn, Cu and Co -bipyridyl(or bipyridyl-like) complexes have been intensively studied because of their large structural diversity; for example, discrete zero-dimensional {Zn(2,2'-bpy)2}2V4O12 (Zhang et al., 1997); one dimensional [Cu(2,2'-bipy)V2O6] and [Cu(2,2'-bipy)2V2O6] (DeBord et al., 1996); two-dimensional [Zn(2,2'-bipy)2V6O17] (Zhang et al., 1996); and three-dimensional Co(bpy)V2O6 (Li et al., 2003), [Ni2(4,4'-bipy)3(H2O)2V4O12]. 2.5H2O (Yang et al., 2001), [{Co2(4,4'-tmdp)4}V4O12] (Khan et al., 2006) and [Ni(bpp)2]2(V4O12) (Zhang et al., 2007). The present work reports a new three-dimensional compound, Ni(bpe)V2O6, which is built from zigzag vanadium oxide chains [V2O6]2-, and complex nickel (II) cations, [Ni(bpe)]2+, as shown in Fig. 1. The N1 atom is coordinated to Ni1, while the N2 atom in the same bpe ligand is coordinated to Ni1vi [Symmetry codes: (vi) x, y + 1, z] in the next layer. Thus, the [Ni(bpe)]n2n+ chains are interpenetrated with each other. It is interesting that the bpe ligands assume two conformation modes, resulting in coexisting of the two conformations in the title compound, 50% probability respectively.

The crystal structure of the title compound can also be described as the neutral two-dimensional [NiV2O6] layers (Fig. 1) linked by neutral briding bpe ligand via Ni—O bonds to form 3-D framework. The Ni(II) center is octahedrally coordinated by two pyridyl N atoms from two different bpe ligands, and four O atoms from four VO4 units, as depicted in Fig. 1, in which the N1, O5, O5i and N2ii form the equatorial plane, while the axial position are occupied by O1 and O4i. The Ni-centered coordination octahedron is slightly distorted, with the bond lehgths, 2.0562 (19)- 2.0799 (17) Å for Ni—O bonds, 2.069 (2) Å and 2.081 (2) Å for Ni—N bonds, and the bond angles approximate to 90 ° or 180 °.

In the [V2O6] units, O2 and O3 bridge two adjacent vanadium atoms; O1 and O4 are coordinated to two nickel atoms respectively; O6 acts as terminal oxygen, while O5 is coordinated to two adjacent Ni atoms. The distance between the adjacent Ni atoms is short, 2.9862 (8) Å, so an eight-membered ring of Ni1—O1—V2—O4—Ni1i—O1i—V2i—O4i is built to form equatorial plane, while the O5 and O5i occupy the axial position.

Related literature top

For related literature, see: DeBord et al. (1996); Khan (2000); Khan et al. (2006); Khan, Yohannes & Doedens (1999); Khan, Yohannes & Powell (1999); Li et al. (2003); Yang et al. (2001); Zhang et al. (1996, 1997, 2007).

Experimental top

A mixture of NiCl2.6H2O (0.239 g, 1 mmol), trans-1,2-bis(4-pyridyl)ethylene (0.182 g, 1 mmol), NH4VO3 (0.117 g, 1 mmol), and H2O (15 g, 833 mmol) was heated at 140 °C for 120 h. After cooling to room temperature, large green block-like crystals of Ni(bpe)(V2O6) were filtered and collected in 86% yield based on Co.

Refinement top

All H atoms were fixed geometrically and allowed to ride on their parent carbon atoms, with C—H distances of 0.93 Å and common isotropic displacement parameters (Uiso Å2).

All the C atoms within the (4-pyridyl)ethylene ligand are disordered over two positions with occupancy ratio of 0.55/0.45. This disorder was treated using a constrained refinement using PART and SAME commands available in SHELXL97 (Sheldrick, 1997). In the last stage of refinement, the C atomss of the disordered moieties were constrained to have the same anisotropic displacement parameters using the EADP instructions.

Computing details top

Data collection: RAPID-AUTO (Rigaku, 1998); cell refinement: RAPID-AUTO; data reduction: RAPID-AUTO; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPIII (Burnett & Johnson, 1996) and ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: SHELXL97.

Figures top
[Figure 1] Fig. 1. A partial packing view showing the octahedral envoironnment of the nickel atoms. Ellipsoids are drawn at the 50% probability level. H atom have been omitted for clarity and only one component of the disordered ligand is shown for clarity. [Symmetry code: (i) -x + 2, -y, -z + 1; (ii) x - 1/2, y - 1/2, -z + 1/2; (iii) -x + 3/2, -y + 1/2, z - 1/2)
Poly[[µ2-trans-1,2-di-4-pyridylethylene]hexa-µ2– oxidonickel(II)divanadate(V)] top
Crystal data top
[NiV2O6(C12H10N2)]F(000) = 1744
Mr = 438.81Dx = 1.905 Mg m−3
Orthorhombic, PbcnMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2n 2abCell parameters from 21006 reflections
a = 14.862 (3) Åθ = 3.0–27.5°
b = 7.6402 (15) ŵ = 2.44 mm−1
c = 26.947 (5) ÅT = 293 K
V = 3059.8 (11) Å3Block, green
Z = 80.23 × 0.19 × 0.10 mm
Data collection top
Rigaku R-AXIS RAPID IP area-detector
diffractometer		3500 independent reflections
Radiation source: rotating anode3062 reflections with I > 2σ(I)
graphiteRint = 0.044
oscillation scansθmax = 27.5°, θmin = 3.0°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)		h = −19→18
Tmin = 0.607, Tmax = 0.789k = −9→9
27995 measured reflectionsl = −34→33
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)] = 0.032Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.083H-atom parameters constrained
S = 1.03 w = 1/[σ2(Fo2) + (0.039P)2 + 5.844P]
where P = (Fo2 + 2Fc2)/3
3500 reflections(Δ/σ)max = 0.002
184 parametersΔρmax = 0.80 e Å−3
33 restraintsΔρmin = −0.71 e Å−3
Crystal data top
[NiV2O6(C12H10N2)]V = 3059.8 (11) Å3
Mr = 438.81Z = 8
Orthorhombic, PbcnMo Kα radiation
a = 14.862 (3) ŵ = 2.44 mm−1
b = 7.6402 (15) ÅT = 293 K
c = 26.947 (5) Å0.23 × 0.19 × 0.10 mm
Data collection top
Rigaku R-AXIS RAPID IP area-detector
diffractometer		3500 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)		3062 reflections with I > 2σ(I)
Tmin = 0.607, Tmax = 0.789Rint = 0.044
27995 measured reflectionsθmax = 27.5°
Refinement top
R[F2 > 2σ(F2)] = 0.032H-atom parameters constrained
wR(F2) = 0.083Δρmax = 0.80 e Å−3
S = 1.03Δρmin = −0.71 e Å−3
3500 reflectionsAbsolute structure: ?
184 parametersFlack parameter: ?
33 restraintsRogers parameter: ?
Special details top

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

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Ni11.000877 (19)0.03138 (4)0.445312 (11)0.01140 (9)
O11.08060 (12)−0.1892 (2)0.44057 (6)0.0187 (4)
O21.24362 (13)−0.2685 (3)0.48670 (8)0.0310 (5)
O31.10701 (13)−0.5327 (2)0.47517 (7)0.0230 (4)
O41.08061 (12)−0.2425 (2)0.53989 (6)0.0194 (4)
O51.07726 (11)0.1096 (2)0.50603 (6)0.0138 (3)
O61.15705 (16)0.3446 (3)0.56686 (8)0.0360 (5)
V11.14782 (3)0.28571 (5)0.510151 (15)0.01393 (11)
V21.12514 (3)−0.30379 (5)0.486666 (15)0.01319 (11)
N11.08372 (17)0.1648 (4)0.39593 (8)0.0304 (6)
C11.0407 (4)0.2985 (8)0.3690 (2)0.0322 (4)0.55
H10.98730.34720.38060.039*0.55
C21.0790 (5)0.3575 (8)0.32457 (19)0.0322 (4)0.55
H21.04850.43860.30510.039*0.55
C31.1633 (5)0.2942 (8)0.3095 (2)0.0322 (4)0.55
C41.2067 (4)0.1802 (8)0.3419 (2)0.0322 (4)0.55
H41.26480.14260.33490.039*0.55
C51.1639 (5)0.1224 (10)0.3842 (2)0.0322 (4)0.55
H51.19540.04840.40540.039*0.55
C61.2037 (4)0.3516 (8)0.2623 (2)0.0322 (4)0.55
H61.16750.41430.24050.039*0.55
C71.2868 (4)0.3206 (8)0.2489 (2)0.0322 (4)0.55
H71.32220.26150.27180.039*0.55
C81.3312 (4)0.3678 (9)0.2018 (2)0.0322 (4)0.55
C91.4152 (4)0.3013 (8)0.1912 (2)0.0322 (4)0.55
H91.44260.22440.21330.039*0.55
C101.4589 (5)0.3481 (9)0.1482 (2)0.0322 (4)0.55
H101.51530.30040.14160.039*0.55
N21.42232 (15)0.4621 (3)0.11494 (8)0.0228 (5)
C111.3373 (5)0.5090 (15)0.1216 (3)0.0322 (4)0.55
H111.30800.57020.09650.039*0.55
C121.2906 (4)0.4698 (9)0.1648 (2)0.0322 (4)0.55
H121.23230.51120.16920.039*0.55
C1A1.0590 (6)0.2575 (13)0.3583 (3)0.0416 (7)0.45
H1A0.99900.29170.35640.050*0.45
C2A1.1169 (6)0.3095 (13)0.3203 (3)0.0416 (7)0.45
H2A1.09620.38240.29510.050*0.45
C3A1.2059 (6)0.2521 (13)0.3201 (3)0.0416 (7)0.45
C4A1.2356 (5)0.1556 (12)0.3599 (3)0.0416 (7)0.45
H4A1.29620.12780.36350.050*0.45
C5A1.1726 (6)0.1008 (16)0.3948 (3)0.0416 (7)0.45
H5A1.18990.01840.41830.050*0.45
C6A1.2666 (5)0.3011 (11)0.2792 (2)0.0416 (7)0.45
H6A1.32790.29050.28550.050*0.45
C7A1.2445 (6)0.3571 (12)0.2358 (2)0.0416 (7)0.45
H7A1.18340.37230.22970.050*0.45
C8A1.3068 (5)0.3995 (14)0.1947 (3)0.0416 (7)0.45
C9A1.3985 (5)0.3595 (13)0.1970 (3)0.0416 (7)0.45
H9A1.42300.31180.22570.050*0.45
C10A1.4533 (6)0.3920 (13)0.1556 (3)0.0416 (7)0.45
H10A1.51390.36240.15730.050*0.45
C11A1.3369 (7)0.514 (2)0.1146 (4)0.0416 (7)0.45
H11A1.31760.58160.08790.050*0.45
C12A1.2752 (6)0.4754 (14)0.1509 (3)0.0416 (7)0.45
H12A1.21430.49890.14650.050*0.45
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni10.01027 (15)0.01366 (17)0.01028 (16)−0.00039 (11)0.00018 (10)0.00108 (11)
O10.0176 (9)0.0193 (10)0.0193 (8)0.0044 (7)0.0003 (7)−0.0010 (7)
O20.0108 (9)0.0283 (11)0.0540 (13)−0.0018 (8)−0.0035 (9)0.0026 (10)
O30.0249 (10)0.0123 (9)0.0317 (10)−0.0005 (7)−0.0049 (8)−0.0013 (7)
O40.0206 (9)0.0167 (9)0.0210 (9)0.0048 (7)−0.0020 (7)0.0011 (7)
O50.0104 (8)0.0149 (9)0.0162 (8)−0.0033 (7)−0.0002 (6)0.0000 (6)
O60.0485 (14)0.0337 (13)0.0260 (10)−0.0179 (11)−0.0051 (10)−0.0060 (9)
V10.0098 (2)0.0119 (2)0.0201 (2)−0.00288 (15)−0.00073 (15)−0.00112 (15)
V20.00889 (19)0.0101 (2)0.0206 (2)0.00108 (14)−0.00144 (15)−0.00086 (15)
N10.0322 (14)0.0399 (15)0.0189 (11)−0.0144 (12)0.0053 (10)0.0043 (10)
C10.0380 (10)0.0327 (10)0.0257 (9)0.0049 (8)0.0186 (8)0.0072 (7)
C20.0380 (10)0.0327 (10)0.0257 (9)0.0049 (8)0.0186 (8)0.0072 (7)
C30.0380 (10)0.0327 (10)0.0257 (9)0.0049 (8)0.0186 (8)0.0072 (7)
C40.0380 (10)0.0327 (10)0.0257 (9)0.0049 (8)0.0186 (8)0.0072 (7)
C50.0380 (10)0.0327 (10)0.0257 (9)0.0049 (8)0.0186 (8)0.0072 (7)
C60.0380 (10)0.0327 (10)0.0257 (9)0.0049 (8)0.0186 (8)0.0072 (7)
C70.0380 (10)0.0327 (10)0.0257 (9)0.0049 (8)0.0186 (8)0.0072 (7)
C80.0380 (10)0.0327 (10)0.0257 (9)0.0049 (8)0.0186 (8)0.0072 (7)
C90.0380 (10)0.0327 (10)0.0257 (9)0.0049 (8)0.0186 (8)0.0072 (7)
C100.0380 (10)0.0327 (10)0.0257 (9)0.0049 (8)0.0186 (8)0.0072 (7)
N20.0208 (11)0.0324 (14)0.0152 (10)−0.0036 (10)0.0025 (9)0.0019 (9)
C110.0380 (10)0.0327 (10)0.0257 (9)0.0049 (8)0.0186 (8)0.0072 (7)
C120.0380 (10)0.0327 (10)0.0257 (9)0.0049 (8)0.0186 (8)0.0072 (7)
C1A0.0366 (13)0.0581 (18)0.0303 (12)−0.0040 (12)0.0104 (10)0.0100 (12)
C2A0.0366 (13)0.0581 (18)0.0303 (12)−0.0040 (12)0.0104 (10)0.0100 (12)
C3A0.0366 (13)0.0581 (18)0.0303 (12)−0.0040 (12)0.0104 (10)0.0100 (12)
C4A0.0366 (13)0.0581 (18)0.0303 (12)−0.0040 (12)0.0104 (10)0.0100 (12)
C5A0.0366 (13)0.0581 (18)0.0303 (12)−0.0040 (12)0.0104 (10)0.0100 (12)
C6A0.0366 (13)0.0581 (18)0.0303 (12)−0.0040 (12)0.0104 (10)0.0100 (12)
C7A0.0366 (13)0.0581 (18)0.0303 (12)−0.0040 (12)0.0104 (10)0.0100 (12)
C8A0.0366 (13)0.0581 (18)0.0303 (12)−0.0040 (12)0.0104 (10)0.0100 (12)
C9A0.0366 (13)0.0581 (18)0.0303 (12)−0.0040 (12)0.0104 (10)0.0100 (12)
C10A0.0366 (13)0.0581 (18)0.0303 (12)−0.0040 (12)0.0104 (10)0.0100 (12)
C11A0.0366 (13)0.0581 (18)0.0303 (12)−0.0040 (12)0.0104 (10)0.0100 (12)
C12A0.0366 (13)0.0581 (18)0.0303 (12)−0.0040 (12)0.0104 (10)0.0100 (12)
Geometric parameters (Å, °) top
Ni1—O4i2.0558 (19)C7—H70.9300
Ni1—O5i2.0561 (17)C8—C91.378 (8)
Ni1—O12.0641 (19)C8—C121.402 (8)
Ni1—N2ii2.069 (2)C9—C101.377 (7)
Ni1—O52.0790 (16)C9—H90.9300
Ni1—N12.080 (2)C10—N21.362 (7)
Ni1—Ni1i2.9862 (8)C10—H100.9300
O1—V21.6575 (18)N2—C10A1.304 (9)
O2—V21.781 (2)N2—C111.326 (7)
O2—V1iii1.782 (2)N2—C11A1.331 (10)
O3—V1iv1.783 (2)N2—Ni1vii2.069 (2)
O3—V21.7966 (19)C11—C121.388 (7)
O4—V21.6476 (18)C11—H110.9300
O4—Ni1i2.0558 (19)C12—H120.9300
O5—V11.7098 (17)C1A—C2A1.397 (9)
O5—Ni1i2.0561 (17)C1A—H1A0.9300
O6—V11.599 (2)C2A—C3A1.393 (11)
V1—O2v1.782 (2)C2A—H2A0.9300
V1—O3vi1.783 (2)C3A—C4A1.376 (10)
N1—C51.275 (7)C3A—C6A1.472 (9)
N1—C1A1.290 (8)C4A—C5A1.391 (9)
N1—C11.407 (6)C4A—H4A0.9300
N1—C5A1.409 (9)C5A—H5A0.9300
C1—C21.401 (7)C6A—C7A1.288 (9)
C1—H10.9300C6A—H6A0.9300
C2—C31.403 (8)C7A—C8A1.480 (9)
C2—H20.9300C7A—H7A0.9300
C3—C41.391 (8)C8A—C12A1.395 (9)
C3—C61.472 (6)C8A—C9A1.398 (10)
C4—C51.379 (7)C9A—C10A1.402 (9)
C4—H40.9300C9A—H9A0.9300
C5—H50.9300C10A—H10A0.9300
C6—C71.309 (7)C11A—C12A1.374 (9)
C6—H60.9300C11A—H11A0.9300
C7—C81.474 (6)C12A—H12A0.9300
O4i—Ni1—O5i87.39 (7)C7—C6—H6117.6
O4i—Ni1—O1172.16 (7)C3—C6—H6117.6
O5i—Ni1—O186.33 (7)C6—C7—C8128.1 (6)
O4i—Ni1—N2ii91.18 (9)C6—C7—H7115.9
O5i—Ni1—N2ii92.73 (8)C8—C7—H7115.9
O1—Ni1—N2ii93.80 (9)C9—C8—C12116.6 (5)
O4i—Ni1—O586.77 (7)C9—C8—C7119.6 (5)
O5i—Ni1—O587.53 (7)C12—C8—C7123.7 (5)
O1—Ni1—O588.27 (7)C10—C9—C8120.4 (6)
N2ii—Ni1—O5177.92 (9)C10—C9—H9119.8
O4i—Ni1—N195.08 (10)C8—C9—H9119.8
O5i—Ni1—N1177.51 (10)N2—C10—C9122.1 (5)
O1—Ni1—N191.19 (10)N2—C10—H10118.9
N2ii—Ni1—N187.56 (10)C9—C10—H10118.9
O5—Ni1—N192.27 (8)C10A—N2—C11109.5 (5)
O4i—Ni1—Ni1i85.95 (5)C10A—N2—C11A117.8 (5)
O5i—Ni1—Ni1i44.07 (5)C11—N2—C11A8.4 (6)
O1—Ni1—Ni1i86.27 (5)C10A—N2—C1017.0 (5)
N2ii—Ni1—Ni1i136.77 (7)C11—N2—C10117.7 (4)
O5—Ni1—Ni1i43.46 (5)C11A—N2—C10125.3 (5)
N1—Ni1—Ni1i135.68 (7)C10A—N2—Ni1vii124.5 (4)
V2—O1—Ni1127.89 (10)C11—N2—Ni1vii125.1 (3)
V2—O2—V1iii158.52 (14)C11A—N2—Ni1vii117.1 (4)
V1iv—O3—V2127.96 (11)C10—N2—Ni1vii117.0 (3)
V2—O4—Ni1i128.95 (10)N2—C11—C12122.1 (6)
V1—O5—Ni1i135.83 (9)N2—C11—H11118.9
V1—O5—Ni1127.75 (9)C12—C11—H11118.9
Ni1i—O5—Ni192.47 (7)C11—C12—C8120.1 (6)
O6—V1—O5109.64 (10)C11—C12—H12120.0
O6—V1—O2v109.07 (12)C8—C12—H12120.0
O5—V1—O2v110.44 (9)N1—C1A—C2A123.8 (7)
O6—V1—O3vi108.39 (11)N1—C1A—H1A118.1
O5—V1—O3vi111.67 (9)C2A—C1A—H1A118.1
O2v—V1—O3vi107.54 (10)C3A—C2A—C1A119.9 (7)
O4—V2—O1109.98 (9)C3A—C2A—H2A120.0
O4—V2—O2110.70 (10)C1A—C2A—H2A120.0
O1—V2—O2108.38 (10)C4A—C3A—C2A118.1 (6)
O4—V2—O3111.52 (10)C4A—C3A—C6A121.5 (8)
O1—V2—O3108.97 (9)C2A—C3A—C6A120.3 (8)
O2—V2—O3107.19 (10)C3A—C4A—C5A118.2 (7)
C5—N1—C1A102.2 (5)C3A—C4A—H4A120.9
C5—N1—C1118.8 (4)C5A—C4A—H4A120.9
C1A—N1—C121.0 (4)C4A—C5A—N1122.8 (7)
C5—N1—C5A14.0 (4)C4A—C5A—H5A118.6
C1A—N1—C5A116.1 (5)N1—C5A—H5A118.6
C1—N1—C5A131.9 (5)C7A—C6A—C3A127.4 (8)
C5—N1—Ni1126.0 (3)C7A—C6A—H6A116.3
C1A—N1—Ni1127.1 (4)C3A—C6A—H6A116.3
C1—N1—Ni1114.6 (3)C6A—C7A—C8A126.4 (8)
C5A—N1—Ni1113.5 (4)C6A—C7A—H7A116.8
C2—C1—N1119.3 (5)C8A—C7A—H7A116.8
C2—C1—H1120.3C12A—C8A—C9A117.2 (7)
N1—C1—H1120.3C12A—C8A—C7A120.9 (7)
C1—C2—C3120.0 (6)C9A—C8A—C7A121.9 (7)
C1—C2—H2120.0C8A—C9A—C10A119.5 (7)
C3—C2—H2120.0C8A—C9A—H9A120.3
C4—C3—C2116.7 (5)C10A—C9A—H9A120.3
C4—C3—C6122.6 (6)N2—C10A—C9A122.4 (8)
C2—C3—C6120.7 (6)N2—C10A—H10A118.8
C5—C4—C3120.4 (6)C9A—C10A—H10A118.8
C5—C4—H4119.8N2—C11A—C12A124.5 (8)
C3—C4—H4119.8N2—C11A—H11A117.8
N1—C5—C4123.7 (5)C12A—C11A—H11A117.8
N1—C5—H5118.2C11A—C12A—C8A117.9 (8)
C4—C5—H5118.2C11A—C12A—H12A121.1
C7—C6—C3124.8 (6)C8A—C12A—H12A121.1
Symmetry codes: (i) −x+2, −y, −z+1; (ii) x−1/2, y−1/2, −z+1/2; (iii) −x+5/2, y−1/2, z; (iv) x, y−1, z; (v) −x+5/2, y+1/2, z; (vi) x, y+1, z; (vii) x+1/2, y+1/2, −z+1/2.
Acknowledgements top

The authors gratefully acknowledge financial support from the Beijing Academic Innovation Group in Sustainable Water/Waste Recycle Technologies (BJE10016200611) and the Research Fund of Beijing University of Civil Engineering and Architecture.

references
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