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

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890
Volume 65| Part 9| September 2009| Pages m1031-m1032

4,4′-Diazenediyldipyridinium 4-(4-pyridyldiazen­yl)pyridinium octa­cyanidotungstate(V) dihydrate

aSchool of Material Science and Engineering, Jiangsu University of Science and Technology, Zhenjiang 212003, People's Republic of China
*Correspondence e-mail: aihuayuan@163.com

(Received 13 July 2009; accepted 29 July 2009; online 8 August 2009)

The asymmetric unit of the title complex, (C10H10N4)(C10H9N4)[W(CN)8]·2H2O, contains two 4,4′-diazenediyldipyridinium, [H2(4,4′-azpy)]2+, two 4-(4-pyridyldiazen­yl)pyridinium, [H(4,4′-azpy)]+, cations, two [WV(CN)8]3− anions, and four uncoordinated water mol­ecules. Each of the W centers is coordinated by eight CN groups in a slightly distorted square-anti­prismatic geometry. In the crystal structure, intra- and inter­molecular N—H⋯O, N—H⋯N and O—H⋯N hydrogen bonds link the cations and anions in an alternating fashion, forming a two-dimensional layered structure, in which they are further linked through the very weak ππ stacking inter­actions [shortest distance = 4.640 (2) Å] and van der Waals forces between adjacent layers, forming a three-dimensional supra­molecular network.

Related literature

For general background to heterometallic cyanido-bridged 4f–4d or 4f–5d assemblies, see: Chelebaeva et al. (2008[Chelebaeva, E., Larionova, J., Guari, Y., Ferreira, R. A. S., Carlos, L. D., Paz, F. A. A., Trifonov, A. & Gueŕin, C. (2008). Inorg. Chem. 47, 775-777.]); Ikeda et al. (2005[Ikeda, S., Hozumi, T., Hashimoto, K. & Ohkoshi, S. I. (2005). Dalton Trans. pp. 2120-2123.]); Kosaka et al. (2007[Kosaka, W., Hashimoto, K. & Ohkoshi, S. I. (2007). Bull. Chem. Soc. Jpn, 80, 2350-2356.]); Matoga et al. (2005[Matoga, D., Mikuriya, M., Handa, M. & Szklarzewicz, J. (2005). Chem. Lett. 34, 1550-1551.]); Przychodzeń et al. (2007[Przychodzeń, P., Pełka, R., Lewiński, K., Supel, J., Rams, M., Tomala, K. & Sieklucka, B. (2007). Inorg. Chem. 46, 8924-8938.]); Wang et al. (2006[Wang, Z. X., Shen, X. F., Wang, J., Zhang, P., Li, Y. Z., Nfor, E. N., Song, Y., Ohkoshi, S. I., Hashimoto, K. & You, X. Z. (2006). Angew. Chem. Int. Ed. 45, 3287-3291.]). For a related structure, see: Liu et al. (2008[Liu, W.-Y., Zhou, H. & Yuan, A.-H. (2008). Acta Cryst. E64, m1151.]).

[Scheme 1]

Experimental

Crystal data
  • (C10H10N4)(C10H9N4)[W(CN)8]·2H2O

  • Mr = 799.46

  • Orthorhombic, P 21 21 21

  • a = 12.7310 (16) Å

  • b = 16.499 (2) Å

  • c = 30.704 (4) Å

  • V = 6449.3 (14) Å3

  • Z = 8

  • Mo Kα radiation

  • μ = 3.64 mm−1

  • T = 291 K

  • 0.28 × 0.22 × 0.20 mm

Data collection
  • Bruker SMART APEX diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2004[Bruker (2004). SMART, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA. ]) Tmin = 0.391, Tmax = 0.483

  • 39717 measured reflections

  • 12501 independent reflections

  • 8553 reflections with I > 2σ(I)

  • Rint = 0.048

Refinement
  • R[F2 > 2σ(F2)] = 0.047

  • wR(F2) = 0.102

  • S = 1.03

  • 12501 reflections

  • 847 parameters

  • H-atom parameters constrained

  • Δρmax = 1.35 e Å−3

  • Δρmin = −1.71 e Å−3

  • Absolute structure: Flack (1983[Flack, H. D. (1983). Acta Cryst. A39, 876-881.]), 5514 Friedel pairs

  • Flack parameter: 0.045 (10)

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A DA D—H⋯A
N20—H20A⋯O2 0.86 1.83 2.671 (10) 166
N21—H21A⋯N17i 0.86 1.76 2.586 (10) 162
N24—H24⋯O3 0.86 1.73 2.560 (10) 162
N28—H28A⋯O4ii 0.86 1.84 2.670 (10) 161
N32—H32A⋯O1iii 0.86 1.88 2.719 (10) 166
O2—H2B⋯N3iv 0.85 2.47 2.914 (10) 113
O1—H1B⋯N7 0.85 2.58 3.076 (10) 119
O4—H4C⋯N4v 0.85 2.25 2.845 (9) 127
O3—H3C⋯N14v 0.85 2.50 2.960 (9) 115
O4—H4B⋯N10vi 0.85 2.47 2.913 (9) 114
Symmetry codes: (i) [x-{\script{1\over 2}}, -y+{\script{3\over 2}}, -z]; (ii) x, y+1, z; (iii) x, y+1, z+1; (iv) [-x+1, y-{\script{1\over 2}}, -z+{\script{1\over 2}}]; (v) [-x+{\script{3\over 2}}, -y+1, z+{\script{1\over 2}}]; (vi) [x-{\script{1\over 2}}, -y+{\script{3\over 2}}, -z+1].

Data collection: SMART (Bruker, 2004[Bruker (2004). SMART, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA. ]); cell refinement: SAINT (Bruker, 2004[Bruker (2004). SMART, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA. ]); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]) and DIAMOND (Brandenburg, 2006[Brandenburg, K. (2006). DIAMOND. Crystal Impact GbR, Bonn, Germany.]); software used to prepare material for publication: SHELXL97.

Supporting information


Comment top

Heterometallic cyanido-bridged 4f-4d or 4f-5d assemblies are of high interest in molecular magnetism over the recent years (Chelebaeva et al., 2008; Przychodzeń et al., 2007; Ikeda et al., 2005; Kosaka et al., 2007; Matoga et al., 2005; Wang et al., 2006). The combination of the octacyanometalate [M(CN)8]3-/4- (M = Mo, W, Nb) building blocks with the lanthanide ions are of interest not only in materials science but also in physics and theoretical chemistry, providing interesting cases of investigation. Herein, we employed 4,4'-azpy (4,4'-azobispyridine), [WV(CN)8]3-, and Ce3+ as building blocks in order to obtain a new lanthanide-containing octacyanotungstate(V)-based magnet. However, the unexpected supramolecular title complex without Ce3+ was obtained. We report herein its crystal structure.

The asymmetric unit of the title complex contains two 4,4'-diazenediyldi- pyridinium, [H2(4,4'-azpy)]2+, and two (4-pyridyldiazenyl)pyridinium, [H(4,4'-azpy)]+, cations, two [WV(CN)8]3- anions, and four uncoordinated water molecules (Fig. 1). Each of the W centers is coordinated by eight CN groups in a slightly distorted square antiprism. The average W-C bond distances are 2.153 (8) Å (for W1) and 2.178 (8) Å (for W2).

In the crystal structure, intra- and intermolecular N-H···O, N-H···N and O-H···N hydrogen bonds (Table 1) link the [H2(4,4'-azpy)]2+ and [H(4,4'-azpy)]+ cations and [W(CN)8]3- anions in an alternating fashion to form a two-dimensional layered structure (Fig. 2), in which they are further linked through the highly weak ππ stacking interactions [shortest distance = 4.640 (2) Å] and van der Waals forces between adjacent layers to form a three-dimensional supramolecular network (Fig. 3) as in the similiar complex (C10H10N4)(C10H9N4)[Mo(CN)8].4H2O (Liu et al., 2008).

Related literature top

For general background to heterometallic cyanido-bridged 4f–4d or 4f–5d assemblies, see: Chelebaeva et al. (2008); Ikeda et al. (2005); Kosaka et al. (2007); Matoga et al. (2005); Przychodzeń et al. (2007); Wang et al. (2006). For a related structure, see: Liu et al. (2008).

Experimental top

Single crystals of the title complex were prepared at room temperature in the dark by slow diffusion of an acetonitrile solution (2 ml) containing both Ce(NO3)3.6H2O (21.71 mg, 0.05 mmol) and 4,4'-azpy (9.21 mg, 0.05 mmol) in an acetonitrile solution (20 ml) of [HN(n-C4H9)3]3[W(CN)8].4H2O (46.60 mg, 0.05 mmol). After two weeks, pale yellow crystals were obtained.

Refinement top

H atoms were positioned geometrically with O-H = 0.85 Å (for H2O), N-H = 0.86 Å (for NH) and C-H = 0.93 Å, for aromatic H atoms, respectively, and constrained to ride on their parent atoms, with Uiso(H) = xUeq(C,N,O), where x = 1.5 for H2O H and x = 1.2 for all other H atoms.

Computing details top

Data collection: SMART (Bruker, 2004); cell refinement: SAINT (Bruker, 2004); data reduction: SAINT (Bruker, 2004); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 2006); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. The molecular structure of the title molecule with the partial atom-numbering scheme. Displacement ellipsoids are drawn at the 30% probability level. The atoms of [H2(4,4'-azpy)]2+ and [H(4,4'-azpy)]+ cations are not labelled for clarity.
[Figure 2] Fig. 2. A partial packing digaram viewed down the a axis. Hydrogen bonds are shown as dashed lines.
[Figure 3] Fig. 3. The three-dimensional supramolecular network.
4,4'-Diazenediyldipyridinium 4-(4-pyridyldiazenyl)pyridinium octacyanidotungstate(V) dihydrate top
Crystal data top
(C10H10N4)(C10H9N4)[W(CN)8]·2H2OF(000) = 3144
Mr = 799.46Dx = 1.647 Mg m3
Orthorhombic, P212121Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2ac 2abCell parameters from 3042 reflections
a = 12.7310 (16) Åθ = 2.4–23.3°
b = 16.499 (2) ŵ = 3.64 mm1
c = 30.704 (4) ÅT = 291 K
V = 6449.3 (14) Å3Pale, yellow
Z = 80.28 × 0.22 × 0.20 mm
Data collection top
Bruker SMART APEX
diffractometer
12501 independent reflections
Radiation source: fine-focus sealed tube8553 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.048
ϕ and ω scansθmax = 26.0°, θmin = 1.3°
Absorption correction: multi-scan
(SADABS; Bruker, 2004)
h = 1515
Tmin = 0.391, Tmax = 0.483k = 2016
39717 measured reflectionsl = 2537
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)] = 0.047H-atom parameters constrained
wR(F2) = 0.102 w = 1/[σ2(Fo2) + (0.05P)2]
where P = (Fo2 + 2Fc2)/3
S = 1.03(Δ/σ)max < 0.001
12501 reflectionsΔρmax = 1.35 e Å3
847 parametersΔρmin = 1.71 e Å3
0 restraintsAbsolute structure: Flack (1983), 5514 Friedel pairs
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.045 (10)
Crystal data top
(C10H10N4)(C10H9N4)[W(CN)8]·2H2OV = 6449.3 (14) Å3
Mr = 799.46Z = 8
Orthorhombic, P212121Mo Kα radiation
a = 12.7310 (16) ŵ = 3.64 mm1
b = 16.499 (2) ÅT = 291 K
c = 30.704 (4) Å0.28 × 0.22 × 0.20 mm
Data collection top
Bruker SMART APEX
diffractometer
12501 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2004)
8553 reflections with I > 2σ(I)
Tmin = 0.391, Tmax = 0.483Rint = 0.048
39717 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.047H-atom parameters constrained
wR(F2) = 0.102Δρmax = 1.35 e Å3
S = 1.03Δρmin = 1.71 e Å3
12501 reflectionsAbsolute structure: Flack (1983), 5514 Friedel pairs
847 parametersAbsolute structure parameter: 0.045 (10)
0 restraints
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*/Ueq
C10.6378 (6)0.5473 (4)0.1970 (3)0.0297 (18)
C20.8138 (6)0.6063 (5)0.2335 (3)0.0313 (18)
C30.6200 (5)0.5979 (5)0.2747 (3)0.0336 (19)
C40.7952 (5)0.5479 (5)0.3113 (3)0.0342 (19)
C50.6367 (6)0.4511 (5)0.3072 (3)0.038 (2)
C60.8309 (6)0.4089 (5)0.2733 (3)0.0362 (19)
C70.6359 (7)0.4012 (5)0.2289 (3)0.038 (2)
C80.8104 (6)0.4661 (5)0.1968 (3)0.0324 (18)
C90.6935 (6)1.1035 (5)0.0145 (3)0.037 (2)
C100.8908 (6)1.0955 (5)0.0232 (3)0.040 (2)
C110.6993 (6)1.0445 (4)0.0620 (3)0.0301 (17)
C120.8724 (6)0.9562 (5)0.0597 (3)0.036 (2)
C130.6913 (6)0.8979 (5)0.0264 (3)0.0353 (19)
C140.8822 (6)0.9009 (5)0.0216 (3)0.0318 (18)
C150.6849 (6)0.9547 (5)0.0491 (3)0.0329 (19)
C160.8540 (6)1.0422 (5)0.0566 (3)0.035 (2)
C170.7019 (6)0.6236 (4)0.1048 (3)0.0340 (18)
H170.70530.60730.13370.041*
C180.6731 (6)0.5699 (5)0.0733 (3)0.0355 (19)
H180.65680.51680.08080.043*
C190.6678 (6)0.5951 (5)0.0291 (3)0.0339 (18)
C200.6898 (6)0.6746 (5)0.0179 (3)0.0360 (18)
H200.68520.69160.01090.043*
C210.7189 (6)0.7285 (5)0.0504 (3)0.0344 (18)
H210.73340.78210.04330.041*
C220.6516 (7)0.2790 (5)0.0626 (3)0.043 (2)
H220.65490.22360.05740.052*
C230.6590 (6)0.3321 (5)0.0289 (3)0.038 (2)
H230.66720.31350.00050.045*
C240.6540 (6)0.4142 (5)0.0375 (3)0.038 (2)
C250.6430 (7)0.4397 (6)0.0816 (3)0.047 (2)
H250.64260.49480.08800.056*
C260.6337 (6)0.3887 (5)0.1125 (3)0.040 (2)
H260.62290.40670.14090.048*
C270.3214 (7)0.6179 (5)0.1410 (3)0.043 (2)
H270.31260.60040.11240.051*
C280.3426 (6)0.5650 (5)0.1707 (3)0.039 (2)
H280.35080.51090.16280.047*
C290.3538 (6)0.5877 (5)0.2162 (3)0.037 (2)
C300.3463 (6)0.6675 (5)0.2279 (3)0.0355 (19)
H300.35440.68350.25680.043*
C310.3253 (6)0.7263 (6)0.1939 (3)0.039 (2)
H310.32100.78110.20090.047*
C320.3825 (6)0.2770 (5)0.3084 (3)0.037 (2)
H320.39480.22240.30280.045*
C330.3711 (7)0.3313 (5)0.2739 (3)0.046 (2)
H330.37690.31350.24530.055*
C340.3510 (6)0.4119 (5)0.2828 (3)0.035 (2)
C350.3408 (6)0.4365 (5)0.3262 (3)0.040 (2)
H350.32460.49020.33260.047*
C360.3540 (7)0.3845 (5)0.3579 (4)0.045 (2)
H360.34860.40270.38650.054*
C370.6111 (6)0.7734 (5)0.6976 (3)0.0336 (19)
H370.61480.71790.70290.040*
C380.6055 (6)0.8260 (5)0.7325 (3)0.038 (2)
H380.60450.80640.76080.046*
C390.6013 (6)0.9083 (5)0.7244 (3)0.037 (2)
C400.6034 (6)0.9347 (6)0.6811 (3)0.039 (2)
H400.60160.99010.67570.047*
C410.6078 (6)0.8834 (5)0.6467 (3)0.0330 (18)
H410.60860.90300.61830.040*
C420.6139 (6)1.1089 (5)0.8685 (3)0.037 (2)
H420.61081.09140.89730.045*
C430.6087 (6)1.0550 (5)0.8382 (3)0.038 (2)
H430.60271.00020.84510.046*
C440.6124 (6)1.0821 (5)0.7922 (3)0.035 (2)
C450.6253 (6)1.1616 (5)0.7834 (3)0.036 (2)
H450.63121.17880.75470.043*
C460.6301 (6)1.2177 (5)0.8166 (3)0.036 (2)
H460.63721.27270.81070.043*
C470.4424 (8)0.7636 (6)0.9344 (3)0.048 (2)
H470.45950.70950.93900.058*
C480.4385 (6)0.8192 (5)0.9690 (3)0.043 (2)
H480.45360.80270.99730.052*
C490.4116 (5)0.8998 (5)0.9601 (3)0.035 (2)
C500.3877 (6)0.9236 (6)0.9184 (3)0.043 (2)
H500.36820.97710.91340.052*
C510.3917 (5)0.8720 (5)0.8846 (3)0.036 (2)
H510.37620.88910.85650.043*
C520.3989 (7)1.2149 (6)1.0509 (3)0.040 (2)
H520.39701.27021.04510.048*
C530.4044 (5)1.1586 (4)1.0177 (3)0.0294 (18)
H530.40411.17700.98910.035*
C540.4104 (6)1.0752 (5)1.0252 (3)0.038 (2)
C550.4061 (7)1.0507 (5)1.0724 (3)0.042 (2)
H550.40910.99621.07990.050*
C560.3982 (6)1.1049 (5)1.1021 (3)0.040 (2)
H560.39361.08791.13090.047*
N10.5960 (5)0.5701 (4)0.1664 (2)0.0311 (15)
N20.8569 (6)0.6651 (4)0.2237 (3)0.0438 (18)
N30.5657 (5)0.6483 (5)0.2883 (3)0.0446 (19)
N40.8368 (5)0.5730 (4)0.3427 (2)0.0308 (15)
N50.5944 (5)0.4196 (4)0.3371 (2)0.0376 (17)
N60.8863 (5)0.3586 (4)0.2865 (2)0.0353 (16)
N70.5832 (5)0.3496 (4)0.2153 (2)0.0365 (17)
N80.8538 (5)0.4451 (4)0.1666 (3)0.0368 (17)
N90.6442 (5)1.1600 (4)0.0255 (2)0.0358 (16)
N100.9452 (5)1.1469 (4)0.0326 (3)0.0400 (18)
N110.6588 (5)1.0669 (4)0.0903 (3)0.0444 (19)
N120.9160 (5)0.9315 (4)0.0883 (2)0.0348 (16)
N130.6466 (6)0.8433 (4)0.0388 (2)0.0411 (18)
N140.9354 (5)0.8508 (4)0.0345 (2)0.0328 (16)
N150.6319 (5)0.9307 (4)0.0754 (3)0.0392 (18)
N160.8838 (6)1.0715 (4)0.0877 (3)0.046 (2)
N170.7265 (5)0.7036 (4)0.0933 (2)0.0335 (15)
N180.6520 (6)0.5431 (5)0.0041 (3)0.0310 (19)
N190.6672 (7)0.4666 (5)0.0023 (4)0.046 (2)
N200.6395 (6)0.3066 (4)0.1039 (3)0.039 (2)
H20A0.63550.27260.12500.047*
N210.3112 (6)0.7012 (4)0.1502 (3)0.0408 (17)
H21A0.29690.73550.13000.049*
N220.3621 (6)0.5397 (5)0.2529 (3)0.036 (2)
N230.3483 (7)0.4622 (5)0.2472 (4)0.045 (2)
N240.3757 (6)0.3036 (4)0.3505 (3)0.042 (2)
H240.38470.27070.37190.051*
N250.6113 (5)0.8007 (4)0.6551 (3)0.0384 (18)
H25A0.61350.76660.63390.046*
N260.6018 (6)0.9564 (5)0.7602 (3)0.032 (2)
N270.5977 (7)1.0325 (5)0.7605 (3)0.042 (3)
N280.6237 (5)1.1889 (4)0.8611 (3)0.0406 (18)
H28A0.62611.22240.88250.049*
N290.4199 (5)0.7923 (4)0.8931 (2)0.0364 (17)
N300.4065 (5)0.9466 (4)0.9941 (3)0.0328 (18)
N310.4201 (5)1.0249 (4)0.9923 (3)0.0333 (19)
N320.3964 (5)1.1847 (4)1.0941 (2)0.0324 (16)
H32A0.39351.21821.11550.039*
H2B0.56580.15480.15250.049*
H2C0.67390.15180.15810.049*
O10.4023 (4)0.3080 (3)0.15273 (19)0.0362 (14)
H1B0.45890.33470.14950.054*
H1C0.35000.33930.14890.054*
O20.6195 (5)0.1824 (4)0.1591 (2)0.0351 (16)
O30.3947 (4)0.1827 (3)0.4021 (2)0.0330 (15)
H3B0.34700.14810.39690.050*
H3C0.45460.16100.39840.050*
O40.6277 (4)0.3185 (4)0.9132 (2)0.0415 (15)
H4B0.56870.33850.90590.062*
H4C0.67670.34450.90070.062*
W10.721961 (19)0.50218 (3)0.253569 (10)0.03326 (9)
W20.783580 (19)1.00055 (3)0.003054 (9)0.03288 (8)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.035 (4)0.024 (4)0.030 (5)0.000 (3)0.011 (4)0.009 (4)
C20.029 (3)0.034 (4)0.031 (5)0.006 (3)0.008 (3)0.013 (4)
C30.025 (4)0.039 (5)0.036 (5)0.010 (3)0.003 (3)0.011 (4)
C40.025 (4)0.053 (5)0.024 (5)0.006 (3)0.001 (3)0.012 (4)
C50.038 (4)0.049 (5)0.026 (5)0.001 (4)0.005 (4)0.000 (4)
C60.038 (4)0.041 (5)0.030 (5)0.003 (4)0.004 (4)0.004 (4)
C70.042 (4)0.047 (5)0.025 (5)0.011 (4)0.001 (4)0.001 (4)
C80.043 (4)0.023 (4)0.032 (5)0.002 (3)0.005 (4)0.005 (3)
C90.040 (4)0.033 (4)0.038 (6)0.010 (3)0.010 (4)0.014 (4)
C100.035 (4)0.045 (5)0.039 (6)0.010 (4)0.003 (4)0.004 (4)
C110.036 (4)0.025 (4)0.029 (5)0.001 (3)0.005 (4)0.005 (3)
C120.033 (4)0.039 (5)0.037 (5)0.007 (3)0.015 (4)0.008 (4)
C130.040 (4)0.038 (5)0.028 (5)0.004 (3)0.001 (3)0.003 (4)
C140.028 (4)0.034 (4)0.033 (5)0.002 (3)0.001 (3)0.000 (4)
C150.026 (3)0.047 (5)0.026 (5)0.001 (3)0.012 (3)0.001 (4)
C160.029 (4)0.030 (4)0.045 (6)0.004 (3)0.002 (4)0.008 (4)
C170.035 (4)0.032 (4)0.035 (5)0.010 (3)0.001 (3)0.001 (4)
C180.048 (5)0.030 (4)0.029 (5)0.007 (3)0.018 (4)0.010 (4)
C190.034 (4)0.034 (4)0.033 (5)0.003 (3)0.005 (3)0.005 (4)
C200.042 (4)0.037 (4)0.029 (5)0.005 (3)0.005 (3)0.000 (4)
C210.035 (4)0.030 (4)0.038 (5)0.011 (4)0.004 (4)0.002 (4)
C220.047 (5)0.034 (5)0.049 (6)0.004 (4)0.027 (4)0.003 (4)
C230.043 (4)0.027 (4)0.044 (6)0.012 (3)0.023 (4)0.008 (4)
C240.029 (4)0.032 (4)0.051 (6)0.008 (3)0.004 (4)0.010 (4)
C250.058 (5)0.040 (5)0.041 (6)0.001 (4)0.002 (5)0.001 (5)
C260.025 (4)0.034 (5)0.060 (7)0.017 (3)0.016 (4)0.002 (4)
C270.046 (4)0.031 (4)0.052 (6)0.022 (4)0.023 (4)0.018 (4)
C280.044 (4)0.038 (5)0.036 (5)0.006 (4)0.013 (4)0.009 (4)
C290.039 (4)0.040 (5)0.032 (5)0.007 (4)0.014 (4)0.000 (4)
C300.037 (4)0.041 (5)0.029 (5)0.004 (3)0.021 (4)0.005 (4)
C310.030 (4)0.051 (5)0.036 (5)0.004 (4)0.001 (3)0.007 (4)
C320.034 (4)0.033 (5)0.045 (6)0.010 (3)0.002 (4)0.001 (4)
C330.055 (5)0.029 (5)0.054 (7)0.027 (4)0.007 (4)0.013 (4)
C340.034 (4)0.027 (4)0.045 (6)0.011 (3)0.018 (4)0.001 (4)
C350.037 (4)0.031 (4)0.050 (6)0.014 (3)0.012 (4)0.010 (4)
C360.044 (5)0.030 (5)0.061 (7)0.007 (4)0.027 (5)0.000 (4)
C370.036 (4)0.025 (4)0.040 (6)0.006 (3)0.011 (4)0.002 (4)
C380.033 (4)0.039 (5)0.044 (6)0.005 (3)0.000 (4)0.011 (4)
C390.042 (4)0.038 (5)0.032 (5)0.015 (4)0.012 (4)0.008 (4)
C400.038 (4)0.051 (5)0.029 (5)0.021 (4)0.001 (3)0.004 (4)
C410.041 (4)0.031 (4)0.027 (5)0.009 (3)0.003 (3)0.011 (4)
C420.038 (4)0.034 (5)0.039 (6)0.001 (3)0.010 (4)0.010 (4)
C430.033 (4)0.031 (5)0.051 (6)0.011 (3)0.002 (4)0.006 (4)
C440.030 (4)0.029 (4)0.047 (6)0.010 (3)0.016 (4)0.005 (4)
C450.030 (4)0.034 (4)0.044 (6)0.017 (3)0.004 (3)0.009 (4)
C460.039 (4)0.035 (5)0.034 (5)0.021 (3)0.015 (4)0.004 (4)
C470.068 (6)0.048 (5)0.028 (5)0.010 (5)0.008 (4)0.004 (4)
C480.042 (4)0.040 (5)0.048 (6)0.003 (4)0.017 (4)0.001 (4)
C490.021 (3)0.038 (5)0.046 (6)0.014 (3)0.002 (3)0.004 (4)
C500.042 (4)0.048 (5)0.038 (6)0.017 (4)0.027 (4)0.003 (4)
C510.019 (3)0.048 (5)0.040 (6)0.015 (3)0.003 (3)0.002 (4)
C520.048 (5)0.050 (5)0.023 (5)0.014 (4)0.001 (4)0.004 (4)
C530.031 (4)0.025 (4)0.033 (5)0.001 (3)0.005 (3)0.002 (3)
C540.026 (4)0.043 (5)0.044 (6)0.020 (3)0.006 (4)0.008 (4)
C550.052 (5)0.028 (5)0.045 (6)0.004 (4)0.001 (4)0.006 (4)
C560.041 (4)0.040 (5)0.038 (6)0.013 (4)0.017 (4)0.005 (4)
N10.035 (3)0.026 (3)0.032 (4)0.003 (3)0.003 (3)0.009 (3)
N20.048 (4)0.044 (4)0.040 (5)0.009 (3)0.002 (3)0.008 (4)
N30.040 (4)0.048 (5)0.046 (5)0.012 (3)0.001 (3)0.009 (4)
N40.045 (4)0.028 (3)0.019 (4)0.013 (3)0.011 (3)0.000 (3)
N50.035 (3)0.039 (4)0.039 (5)0.009 (3)0.013 (3)0.002 (3)
N60.047 (4)0.036 (4)0.022 (4)0.012 (3)0.006 (3)0.018 (3)
N70.038 (3)0.028 (4)0.043 (5)0.001 (3)0.021 (3)0.001 (3)
N80.044 (4)0.036 (4)0.030 (4)0.002 (3)0.004 (3)0.011 (3)
N90.035 (3)0.047 (4)0.025 (4)0.012 (3)0.010 (3)0.009 (3)
N100.037 (3)0.041 (4)0.042 (5)0.018 (3)0.001 (3)0.010 (3)
N110.040 (4)0.037 (4)0.057 (6)0.006 (3)0.021 (4)0.003 (4)
N120.026 (3)0.049 (4)0.030 (4)0.009 (3)0.002 (3)0.003 (3)
N130.064 (4)0.039 (4)0.020 (4)0.015 (4)0.017 (3)0.004 (3)
N140.028 (3)0.033 (4)0.038 (4)0.010 (3)0.012 (3)0.013 (3)
N150.035 (3)0.039 (4)0.044 (5)0.009 (3)0.004 (3)0.012 (4)
N160.044 (4)0.034 (4)0.060 (6)0.011 (3)0.005 (4)0.020 (4)
N170.036 (3)0.036 (4)0.029 (4)0.002 (3)0.013 (3)0.002 (3)
N180.021 (3)0.037 (4)0.035 (5)0.002 (3)0.007 (3)0.008 (4)
N190.044 (5)0.038 (4)0.057 (7)0.009 (3)0.001 (5)0.001 (4)
N200.041 (4)0.032 (4)0.044 (5)0.002 (3)0.007 (4)0.007 (4)
N210.049 (4)0.034 (4)0.039 (5)0.009 (3)0.004 (3)0.004 (3)
N220.033 (4)0.041 (4)0.035 (5)0.004 (3)0.012 (4)0.001 (4)
N230.049 (5)0.030 (4)0.056 (6)0.006 (3)0.028 (5)0.008 (4)
N240.045 (4)0.026 (4)0.055 (6)0.010 (3)0.023 (4)0.006 (4)
N250.039 (4)0.029 (4)0.047 (5)0.008 (3)0.011 (3)0.003 (3)
N260.039 (4)0.032 (4)0.026 (5)0.009 (3)0.001 (4)0.005 (3)
N270.048 (5)0.035 (4)0.044 (6)0.016 (3)0.015 (4)0.016 (4)
N280.041 (4)0.043 (4)0.038 (5)0.000 (3)0.010 (3)0.001 (4)
N290.042 (4)0.032 (4)0.034 (4)0.012 (3)0.013 (3)0.003 (3)
N300.032 (3)0.033 (4)0.033 (5)0.013 (3)0.003 (3)0.002 (4)
N310.028 (3)0.024 (4)0.049 (5)0.004 (2)0.003 (3)0.012 (3)
N320.038 (3)0.039 (4)0.021 (4)0.012 (3)0.002 (3)0.002 (3)
O10.025 (3)0.042 (3)0.042 (4)0.007 (2)0.002 (2)0.011 (3)
O20.042 (3)0.028 (3)0.036 (4)0.001 (3)0.013 (3)0.004 (3)
O30.033 (3)0.035 (3)0.032 (3)0.012 (3)0.017 (3)0.008 (3)
O40.038 (3)0.037 (3)0.050 (4)0.017 (3)0.004 (3)0.003 (3)
W10.03339 (12)0.03505 (16)0.03134 (19)0.0016 (3)0.00019 (12)0.0005 (3)
W20.03320 (13)0.03300 (16)0.03245 (19)0.0027 (3)0.00128 (11)0.0007 (2)
Geometric parameters (Å, º) top
C1—N11.143 (10)C33—H330.9300
C1—W12.173 (8)C34—N231.373 (13)
C2—N21.154 (10)C34—C351.400 (12)
C2—W12.167 (8)C35—C361.308 (13)
C3—N31.159 (10)C35—H350.9300
C3—W12.145 (7)C36—N241.382 (11)
C4—N41.175 (10)C36—H360.9300
C4—W12.140 (8)C37—N251.379 (11)
C5—N51.183 (10)C37—C381.380 (12)
C5—W12.146 (9)C37—H370.9300
C6—N61.162 (10)C38—C391.381 (12)
C6—W12.159 (8)C38—H380.9300
C7—N71.162 (10)C39—N261.355 (11)
C7—W12.133 (8)C39—C401.399 (12)
C8—N81.134 (11)C40—C411.354 (11)
C8—W12.159 (9)C40—H400.9300
C9—N91.174 (10)C41—N251.390 (10)
C9—W22.119 (7)C41—H410.9300
C10—N101.132 (10)C42—C431.289 (12)
C10—W22.168 (8)C42—N281.344 (10)
C11—N111.076 (11)C42—H420.9300
C11—W22.225 (9)C43—C441.483 (13)
C12—N121.115 (10)C43—H430.9300
C12—W22.200 (8)C44—N271.285 (12)
C13—N131.131 (10)C44—C451.349 (11)
C13—W22.183 (8)C45—C461.379 (11)
C14—N141.141 (10)C45—H450.9300
C14—W22.202 (8)C46—N281.449 (11)
C15—N151.125 (10)C46—H460.9300
C15—W22.172 (8)C47—N291.384 (12)
C16—N161.134 (11)C47—C481.404 (13)
C16—W22.152 (9)C47—H470.9300
C17—C181.360 (11)C48—C491.400 (11)
C17—N171.402 (10)C48—H480.9300
C17—H170.9300C49—N301.300 (12)
C18—C191.421 (11)C49—C501.375 (12)
C18—H180.9300C50—C511.343 (12)
C19—N181.349 (12)C50—H500.9300
C19—C201.385 (11)C51—N291.387 (10)
C20—C211.387 (11)C51—H510.9300
C20—H200.9300C52—C531.379 (12)
C21—N171.382 (11)C52—N321.417 (11)
C21—H210.9300C52—H520.9300
C22—N201.355 (12)C53—C541.397 (11)
C22—C231.361 (12)C53—H530.9300
C22—H220.9300C54—N311.316 (12)
C23—C241.381 (11)C54—C551.503 (13)
C23—H230.9300C55—C561.282 (12)
C24—N191.394 (13)C55—H550.9300
C24—C251.426 (13)C56—N321.339 (10)
C25—C261.273 (12)C56—H560.9300
C25—H250.9300N18—N191.278 (9)
C26—N201.382 (10)N20—H20A0.8600
C26—H260.9300N21—H21A0.8600
C27—C281.290 (11)N22—N231.303 (9)
C27—N211.409 (10)N24—H240.8600
C27—H270.9300N25—H25A0.8600
C28—C291.454 (12)N26—N271.257 (8)
C28—H280.9300N28—H28A0.8600
C29—C301.369 (11)N30—N311.303 (10)
C29—N221.383 (12)N32—H32A0.8600
C30—C311.450 (12)O1—H1B0.8499
C30—H300.9300O1—H1C0.8501
C31—N211.416 (11)O2—H2B0.8456
C31—H310.9300O2—H2C0.8576
C32—N241.367 (12)O3—H3B0.8499
C32—C331.396 (12)O3—H3C0.8499
C32—H320.9300O4—H4B0.8501
C33—C341.382 (11)O4—H4C0.8500
N1—C1—W1177.8 (7)N30—C49—C50124.5 (8)
N2—C2—W1175.2 (7)N30—C49—C48114.9 (8)
N3—C3—W1176.5 (8)C50—C49—C48120.5 (9)
N4—C4—W1179.0 (7)C51—C50—C49122.0 (8)
N5—C5—W1176.1 (7)C51—C50—H50119.0
N6—C6—W1175.5 (7)C49—C50—H50119.0
N7—C7—W1175.5 (8)C50—C51—N29117.8 (8)
N8—C8—W1177.3 (7)C50—C51—H51121.1
N9—C9—W2178.0 (8)N29—C51—H51121.1
N10—C10—W2177.6 (8)C53—C52—N32117.1 (8)
N11—C11—W2179.0 (7)C53—C52—H52121.5
N12—C12—W2177.9 (7)N32—C52—H52121.5
N13—C13—W2177.6 (8)C52—C53—C54122.9 (9)
N14—C14—W2178.2 (7)C52—C53—H53118.5
N15—C15—W2178.3 (8)C54—C53—H53118.5
N16—C16—W2172.3 (7)N31—C54—C53120.0 (8)
C18—C17—N17119.7 (8)N31—C54—C55125.0 (8)
C18—C17—H17120.2C53—C54—C55115.0 (8)
N17—C17—H17120.2C56—C55—C54120.0 (8)
C17—C18—C19120.0 (8)C56—C55—H55120.0
C17—C18—H18120.0C54—C55—H55120.0
C19—C18—H18120.0C55—C56—N32123.8 (9)
N18—C19—C20116.4 (8)C55—C56—H56118.1
N18—C19—C18122.9 (8)N32—C56—H56118.1
C20—C19—C18120.4 (8)C21—N17—C17120.2 (7)
C19—C20—C21118.8 (8)N19—N18—C19125.0 (11)
C19—C20—H20120.6N18—N19—C24124.1 (12)
C21—C20—H20120.6C22—N20—C26121.0 (8)
N17—C21—C20121.0 (7)C22—N20—H20A119.5
N17—C21—H21119.5C26—N20—H20A119.5
C20—C21—H21119.5C27—N21—C31117.7 (7)
N20—C22—C23120.2 (8)C27—N21—H21A121.1
N20—C22—H22119.9C31—N21—H21A121.1
C23—C22—H22119.9N23—N22—C29116.2 (11)
C22—C23—C24118.8 (9)N22—N23—C34118.8 (11)
C22—C23—H23120.6C32—N24—C36118.6 (9)
C24—C23—H23120.6C32—N24—H24120.7
C23—C24—N19117.0 (9)C36—N24—H24120.7
C23—C24—C25118.5 (9)C37—N25—C41119.7 (8)
N19—C24—C25124.4 (8)C37—N25—H25A120.1
C26—C25—C24121.4 (9)C41—N25—H25A120.1
C26—C25—H25119.3N27—N26—C39126.3 (10)
C24—C25—H25119.3N26—N27—C44129.6 (11)
C25—C26—N20120.0 (10)C42—N28—C46119.1 (8)
C25—C26—H26120.0C42—N28—H28A120.4
N20—C26—H26120.0C46—N28—H28A120.4
C28—C27—N21122.4 (9)C47—N29—C51123.4 (8)
C28—C27—H27118.8C49—N30—N31123.2 (9)
N21—C27—H27118.8N30—N31—C54125.5 (9)
C27—C28—C29121.7 (9)C56—N32—C52121.1 (8)
C27—C28—H28119.1C56—N32—H32A119.4
C29—C28—H28119.1C52—N32—H32A119.4
C30—C29—N22109.9 (8)H1B—O1—H1C109.5
C30—C29—C28119.6 (8)H2B—O2—H2C109.2
N22—C29—C28130.1 (8)H3B—O3—H3C109.5
C29—C30—C31117.8 (8)H4B—O4—H4C109.5
C29—C30—H30121.1C7—W1—C4142.5 (3)
C31—C30—H30121.1C7—W1—C3111.8 (3)
N21—C31—C30120.6 (8)C4—W1—C375.8 (3)
N21—C31—H31119.7C7—W1—C572.9 (3)
C30—C31—H31119.7C4—W1—C573.9 (3)
N24—C32—C33120.3 (8)C3—W1—C575.6 (3)
N24—C32—H32119.8C7—W1—C682.7 (3)
C33—C32—H32119.8C4—W1—C674.9 (3)
C34—C33—C32119.1 (9)C3—W1—C6146.0 (3)
C34—C33—H33120.4C5—W1—C680.2 (3)
C32—C33—H33120.4C7—W1—C876.5 (3)
N23—C34—C33115.4 (9)C4—W1—C8122.6 (3)
N23—C34—C35125.5 (8)C3—W1—C8139.7 (3)
C33—C34—C35119.0 (8)C5—W1—C8140.8 (3)
C36—C35—C34120.4 (8)C6—W1—C872.2 (3)
C36—C35—H35119.8C7—W1—C2142.7 (3)
C34—C35—H35119.8C4—W1—C273.8 (3)
C35—C36—N24122.4 (10)C3—W1—C280.1 (3)
C35—C36—H36118.8C5—W1—C2143.4 (3)
N24—C36—H36118.8C6—W1—C2107.3 (3)
N25—C37—C38121.8 (8)C8—W1—C273.0 (3)
N25—C37—H37119.1C7—W1—C174.4 (3)
C38—C37—H37119.1C4—W1—C1139.2 (3)
C37—C38—C39118.8 (9)C3—W1—C172.0 (3)
C37—C38—H38120.6C5—W1—C1120.0 (3)
C39—C38—H38120.6C6—W1—C1141.8 (3)
N26—C39—C38115.5 (8)C8—W1—C172.9 (3)
N26—C39—C40126.0 (8)C2—W1—C176.6 (3)
C38—C39—C40118.4 (8)C9—W2—C1675.7 (3)
C41—C40—C39123.2 (9)C9—W2—C1080.4 (3)
C41—C40—H40118.4C16—W2—C1075.5 (3)
C39—C40—H40118.4C9—W2—C1577.2 (3)
C40—C41—N25118.1 (9)C16—W2—C1574.0 (3)
C40—C41—H41121.0C10—W2—C15145.7 (3)
N25—C41—H41121.0C9—W2—C13114.5 (3)
C43—C42—N28124.1 (9)C16—W2—C13138.7 (3)
C43—C42—H42117.9C10—W2—C13143.7 (3)
N28—C42—H42117.9C15—W2—C1370.2 (3)
C42—C43—C44118.5 (8)C9—W2—C12138.2 (3)
C42—C43—H43120.8C16—W2—C12124.4 (3)
C44—C43—H43120.8C10—W2—C1272.0 (3)
N27—C44—C45119.0 (9)C15—W2—C12139.9 (3)
N27—C44—C43121.6 (8)C13—W2—C1276.0 (3)
C45—C44—C43119.3 (8)C9—W2—C14145.0 (3)
C44—C45—C46120.6 (9)C16—W2—C1473.0 (3)
C44—C45—H45119.7C10—W2—C14106.2 (3)
C46—C45—H45119.7C15—W2—C1479.4 (3)
C45—C46—N28118.3 (8)C13—W2—C1480.8 (3)
C45—C46—H46120.8C12—W2—C1474.4 (3)
N28—C46—H46120.8C9—W2—C1171.6 (3)
N29—C47—C48117.5 (9)C16—W2—C11142.1 (3)
N29—C47—H47121.2C10—W2—C1180.6 (3)
C48—C47—H47121.2C15—W2—C11115.7 (3)
C49—C48—C47118.8 (9)C13—W2—C1174.1 (3)
C49—C48—H48120.6C12—W2—C1173.4 (3)
C47—C48—H48120.6C14—W2—C11142.9 (3)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N20—H20A···O20.861.832.671 (10)166
N21—H21A···N17i0.861.762.586 (10)162
N24—H24···O30.861.732.560 (10)162
N28—H28A···O4ii0.861.842.670 (10)161
N32—H32A···O1iii0.861.882.719 (10)166
O2—H2B···N3iv0.852.472.914 (10)113
O1—H1B···N70.852.583.076 (10)119
O4—H4C···N4v0.852.252.845 (9)127
O3—H3C···N14v0.852.502.960 (9)115
O4—H4B···N10vi0.852.472.913 (9)114
Symmetry codes: (i) x1/2, y+3/2, z; (ii) x, y+1, z; (iii) x, y+1, z+1; (iv) x+1, y1/2, z+1/2; (v) x+3/2, y+1, z+1/2; (vi) x1/2, y+3/2, z+1.

Experimental details

Crystal data
Chemical formula(C10H10N4)(C10H9N4)[W(CN)8]·2H2O
Mr799.46
Crystal system, space groupOrthorhombic, P212121
Temperature (K)291
a, b, c (Å)12.7310 (16), 16.499 (2), 30.704 (4)
V3)6449.3 (14)
Z8
Radiation typeMo Kα
µ (mm1)3.64
Crystal size (mm)0.28 × 0.22 × 0.20
Data collection
DiffractometerBruker SMART APEX
diffractometer
Absorption correctionMulti-scan
(SADABS; Bruker, 2004)
Tmin, Tmax0.391, 0.483
No. of measured, independent and
observed [I > 2σ(I)] reflections
39717, 12501, 8553
Rint0.048
(sin θ/λ)max1)0.617
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.047, 0.102, 1.03
No. of reflections12501
No. of parameters847
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)1.35, 1.71
Absolute structureFlack (1983), 5514 Friedel pairs
Absolute structure parameter0.045 (10)

Computer programs: SMART (Bruker, 2004), SAINT (Bruker, 2004), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 2006).

Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N20—H20A···O20.861.832.671 (10)166
N21—H21A···N17i0.861.762.586 (10)162
N24—H24···O30.861.732.560 (10)162.0
N28—H28A···O4ii0.861.842.670 (10)161
N32—H32A···O1iii0.861.882.719 (10)166
O2—H2B···N3iv0.852.472.914 (10)113
O1—H1B···N70.852.583.076 (10)119
O4—H4C···N4v0.852.252.845 (9)127
O3—H3C···N14v0.852.502.960 (9)115
O4—H4B···N10vi0.852.472.913 (9)114
Symmetry codes: (i) x1/2, y+3/2, z; (ii) x, y+1, z; (iii) x, y+1, z+1; (iv) x+1, y1/2, z+1/2; (v) x+3/2, y+1, z+1/2; (vi) x1/2, y+3/2, z+1.
 

Acknowledgements

The work was supported by the University Natural Science Foundation of Jiangsu Province (grant No. 07KJB150030).

References

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Volume 65| Part 9| September 2009| Pages m1031-m1032
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