supplementary materials


xu5676 scheme

Acta Cryst. (2013). E69, m169    [ doi:10.1107/S1600536813004686 ]

Bis(azido-[kappa]N)bis[4-(dimethylamino)pyridine-[kappa]N]zinc

F. Guenifa, N. Hadjadj, O. Zeghouan, L. Bendjeddou and H. Merazig

Abstract top

In the title complex, [Zn(N3)2(C7H10N2)2], the ZnII atom is coordinated by two N atoms from two 4-(dimethylamino)pyridine (DMAP) ligands and by two N atoms from two azide anions in a distorted tetrahedral coordination geometry. In the crystal, weak C-H...N hydrogen bonds between the DMAP and azide ligands link these discrete complex molecules into a three-dimensional supramolecular network.

Comment top

Pyridine derivatives are an important class of ligand for constructing metal-organic frameworks. 4-Dimethylaminopyridine (DMAP) has good coordination ability, but there are few reports on its complexes (Tyrra et al., 2003) except a lot of reports on its nucleophilic properties (Fu et al., 2000). The DMAP complexes which exhibit luminescence properties were reported (Araki et al., 2005). In our systematic studies on transition metal complexes with the pyridine derivatives and other ligands, the title compound [Zn(C7H10N2)2(N3)2] was prepared and its X-ray structure is presented here.

The title complex (I), is a mononuclear Zn(II) complex, consisting of two 4-dimethylaminopyridine (DMAP) ligands and two azide anions (Figure 1), all ligands coordinating in a monodentate manner. The title compound exhibits a distorted tetrahedral coordination involving two N atoms from two 4-dimethylaminopyridine (DMAP) ligands at 2.031 (2), 2.018 (2) Å and two N atoms from two azide anions at 1.934 (3), 1.968 (2) Å, all coordinated in a monodentate fashion (Figure 1). The bond angles around Zn atom vary from 103.45 (13) to 127.06 (11)°.

The crystal structure can be described as double layers which stack along the b axis, at c = 1/4 and 3/4, where each layer is formed of pairs of monomers (Figure 2). In the structure of (I), mononuclear units are held together with weak intermolecular C—H···N hydrogen bonds between the 4-dimethylaminopyridine and the azide, forming an alternating centrosymmetric rings in two-dimensional network which can be described by the graph-set motif R22(12) and R66(44) (Bernstein et al., 1995) (Figure 3). The combination of the four intermolecular C—H···N hydrogen bonds generates a three-dimensional network.

Related literature top

For the property of complexes with dimethylaminopyridine ligand, see: Araki et al. (2005). For weak hydrogen-bonding modes, see: Bernstein et al. (1995). For related compounds, see: Fu (2000); Tyrra et al. (2003).

Experimental top

The title compound is prepared by reaction of methanolic solution containing Zn(CH3COO)2.2H2O, NaN3 and 4-dimethylaminopyridine in a 1:1:1 stoichiometric ratio. The solution was maintained in 293 K under agitation during one hour. Colorless crystals were appeared by evaporation of the solution at room temperature over the course of a few days.

Refinement top

The H atoms were placed at calculated positions with C—H = 0.93 and 0.96 Å, for aromatic and methyl H atoms, respectively, and refined in riding mode with Uiso(H) = 1.2Ueq(C) for aromatic H atoms and 1.5Ueq(C) for methyl H atoms.

Computing details top

Data collection: KappaCCD Reference Manual (Nonius, 1998); cell refinement: DENZO and SCALEPACK (Otwinowski & Minor, 1997); data reduction: DENZO and SCALEPACK (Otwinowski & Minor, 1997); program(s) used to solve structure: SIR2002 (Burla et al., 2003); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 for Windows (Farrugia, 2012); software used to prepare material for publication: WinGX (Farrugia, 2012), Mercury (Macrae et al., 2006) and POVRay (Persistence of Vision Team, 2004).

Figures top
[Figure 1] Fig. 1. The asymmetric unit of the title structure with the atom numbering scheme. Displacement ellipsoids are drawn at the 50% probability level and H atoms are represented as small spheres of arbitrary radii.
[Figure 2] Fig. 2. view of the crystal structure of title compound, showing double layers along the b axis. Hydrogen atoms are omitted for clarity.
[Figure 3] Fig. 3. Part of the crystal structure, showing the aggregation of R22(12) and R66(44) hydrogen-bonding motifs. [Symmetry codes: (α) –x+1/2, y - 1/2, -z; (β) –x, -y, -z - 1; (@) –x+1/2, y - 1/2, -z; (#) x, y - 1, z; (°) x - 1/2, -y - 1/2, z - 1; (^) –x+1/2, y - 3/2, -z].
Bis(azido-κN)bis[4-(dimethylamino)pyridine-κN]zinc top
Crystal data top
[Zn(N3)2(C7H10N2)2]F(000) = 816
Mr = 393.79Dx = 1.431 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 4302 reflections
a = 14.819 (5) Åθ = 2.7–27.8°
b = 9.610 (5) ŵ = 1.36 mm1
c = 14.555 (5) ÅT = 293 K
β = 118.158 (5)°Prism, colourless
V = 1827.5 (13) Å30.3 × 0.2 × 0.2 mm
Z = 4
Data collection top
Nonius KappaCCD
diffractometer
3323 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.019
Graphite monochromatorθmax = 27.8°, θmin = 2.7°
φ scansh = 1819
15768 measured reflectionsk = 1212
4302 independent reflectionsl = 1917
Refinement top
Refinement on F20 restraints
Least-squares matrix: fullH-atom parameters constrained
R[F2 > 2σ(F2)] = 0.033 w = 1/[σ2(Fo2) + (0.0512P)2 + 0.563P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.098(Δ/σ)max = 0.006
S = 1.03Δρmax = 0.31 e Å3
4302 reflectionsΔρmin = 0.45 e Å3
230 parameters
Crystal data top
[Zn(N3)2(C7H10N2)2]V = 1827.5 (13) Å3
Mr = 393.79Z = 4
Monoclinic, P21/cMo Kα radiation
a = 14.819 (5) ŵ = 1.36 mm1
b = 9.610 (5) ÅT = 293 K
c = 14.555 (5) Å0.3 × 0.2 × 0.2 mm
β = 118.158 (5)°
Data collection top
Nonius KappaCCD
diffractometer
3323 reflections with I > 2σ(I)
15768 measured reflectionsRint = 0.019
4302 independent reflectionsθmax = 27.8°
Refinement top
R[F2 > 2σ(F2)] = 0.033H-atom parameters constrained
wR(F2) = 0.098Δρmax = 0.31 e Å3
S = 1.03Δρmin = 0.45 e Å3
4302 reflectionsAbsolute structure: ?
230 parametersFlack parameter: ?
0 restraintsRogers parameter: ?
Special details top

Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles

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
Zn0.71191 (2)0.27848 (3)0.61121 (2)0.0523 (1)
N1A0.77350 (13)0.40503 (19)0.73790 (13)0.0500 (5)
N1B0.69230 (13)0.40145 (19)0.49076 (13)0.0504 (5)
N2A0.89709 (15)0.6937 (2)0.98096 (15)0.0595 (6)
N2B0.64450 (14)0.6645 (2)0.24262 (14)0.0571 (6)
N30.57850 (19)0.2334 (3)0.5965 (2)0.0873 (10)
N40.52367 (14)0.1422 (2)0.59095 (14)0.0545 (6)
N50.4650 (2)0.0614 (3)0.5847 (2)0.0865 (10)
N60.81913 (18)0.1468 (2)0.62440 (17)0.0693 (8)
N70.87832 (14)0.0916 (2)0.70190 (16)0.0531 (6)
N80.93719 (16)0.0315 (3)0.77445 (17)0.0734 (8)
C1A0.9886 (2)0.7725 (3)0.9999 (2)0.0752 (10)
C1B0.7054 (2)0.6558 (3)0.1887 (2)0.0721 (9)
C2A0.8539 (2)0.7179 (3)1.05133 (19)0.0660 (9)
C2B0.5557 (2)0.7569 (3)0.1963 (2)0.0751 (9)
C3A0.85764 (15)0.5982 (2)0.90434 (15)0.0475 (6)
C3B0.66005 (15)0.5783 (2)0.32121 (15)0.0470 (6)
C4A0.90324 (17)0.5695 (3)0.84037 (18)0.0570 (7)
C4B0.73862 (17)0.4775 (2)0.36129 (17)0.0557 (7)
C5A0.85983 (17)0.4761 (3)0.76167 (18)0.0583 (8)
C5B0.75054 (17)0.3949 (3)0.44220 (17)0.0565 (7)
C6A0.73042 (16)0.4308 (2)0.80006 (16)0.0515 (7)
C6B0.61798 (16)0.4982 (2)0.45299 (18)0.0535 (7)
C7A0.76869 (16)0.5216 (2)0.88114 (16)0.0511 (7)
C7B0.59908 (16)0.5840 (2)0.37233 (18)0.0541 (7)
H1A20.978400.815740.936250.1128*
H1A11.001220.842741.051440.1128*
H1A31.046210.710701.024380.1128*
H1B10.683140.577740.142030.1081*
H4A0.963220.614890.852250.0684*
H4B0.782340.467480.332310.0668*
H1B20.697200.739740.149720.1081*
H5A0.892130.459920.721250.0699*
H5B0.802650.328980.465800.0677*
H1B30.776210.644260.238630.1081*
H6A0.670720.383240.786340.0618*
H6B0.576530.506710.484720.0642*
H2A10.869780.640531.098190.0990*
H7A0.735840.533120.921530.0613*
H7B0.545480.647500.350140.0650*
H2A20.882550.801391.090570.0990*
H2A30.780970.727651.011510.0990*
H2B10.554970.815350.249400.1128*
H2B20.559510.813630.143960.1128*
H2B30.494170.702230.165010.1128*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Zn0.0535 (2)0.0544 (2)0.0550 (2)0.0003 (1)0.0306 (1)0.0062 (1)
N1A0.0505 (9)0.0562 (10)0.0507 (9)0.0035 (8)0.0299 (8)0.0048 (8)
N1B0.0488 (9)0.0563 (10)0.0493 (9)0.0028 (8)0.0259 (8)0.0053 (8)
N2A0.0636 (11)0.0677 (12)0.0524 (10)0.0111 (9)0.0316 (9)0.0107 (9)
N2B0.0592 (11)0.0567 (10)0.0543 (10)0.0101 (9)0.0260 (9)0.0023 (9)
N30.0676 (14)0.0791 (15)0.133 (2)0.0182 (12)0.0619 (16)0.0337 (15)
N40.0539 (10)0.0610 (11)0.0555 (10)0.0035 (9)0.0315 (9)0.0063 (9)
N50.0932 (17)0.0744 (15)0.119 (2)0.0149 (14)0.0724 (16)0.0096 (14)
N60.0831 (14)0.0720 (14)0.0663 (13)0.0223 (12)0.0464 (12)0.0047 (11)
N70.0517 (10)0.0619 (11)0.0593 (11)0.0050 (9)0.0374 (10)0.0141 (9)
N80.0582 (12)0.1026 (17)0.0617 (12)0.0082 (12)0.0301 (10)0.0011 (12)
C1A0.0760 (17)0.0805 (17)0.0680 (16)0.0282 (14)0.0331 (14)0.0180 (13)
C1B0.0857 (17)0.0749 (17)0.0660 (15)0.0100 (14)0.0442 (14)0.0078 (13)
C2A0.0845 (17)0.0680 (15)0.0526 (13)0.0008 (13)0.0382 (13)0.0065 (11)
C2B0.0756 (17)0.0686 (15)0.0731 (17)0.0221 (13)0.0284 (14)0.0147 (13)
C3A0.0468 (10)0.0538 (11)0.0436 (10)0.0001 (9)0.0227 (9)0.0029 (9)
C3B0.0429 (10)0.0474 (11)0.0465 (10)0.0017 (8)0.0176 (9)0.0104 (8)
C4A0.0506 (11)0.0679 (14)0.0637 (13)0.0142 (10)0.0362 (10)0.0113 (11)
C4B0.0547 (12)0.0661 (13)0.0554 (12)0.0146 (11)0.0335 (10)0.0008 (10)
C5A0.0559 (12)0.0734 (14)0.0602 (13)0.0069 (11)0.0395 (11)0.0087 (11)
C5B0.0521 (11)0.0654 (13)0.0575 (12)0.0201 (10)0.0305 (10)0.0037 (10)
C6A0.0484 (11)0.0582 (12)0.0559 (12)0.0064 (9)0.0313 (10)0.0020 (10)
C6B0.0462 (10)0.0581 (12)0.0643 (13)0.0008 (9)0.0327 (10)0.0113 (10)
C7A0.0530 (11)0.0616 (13)0.0503 (11)0.0022 (10)0.0340 (10)0.0006 (9)
C7B0.0435 (10)0.0530 (12)0.0670 (13)0.0089 (9)0.0270 (10)0.0053 (10)
Geometric parameters (Å, º) top
Zn—N1A2.031 (2)C4B—C5B1.361 (3)
Zn—N1B2.018 (2)C6A—C7A1.358 (3)
Zn—N31.935 (3)C6B—C7B1.351 (3)
Zn—N61.969 (3)C1A—H1A20.9600
N1A—C5A1.344 (4)C1A—H1A10.9600
N1A—C6A1.354 (3)C1A—H1A30.9600
N1B—C5B1.351 (3)C1B—H1B10.9600
N1B—C6B1.345 (3)C1B—H1B20.9600
N2A—C1A1.461 (4)C1B—H1B30.9600
N2A—C2A1.460 (4)C2A—H2A10.9600
N2A—C3A1.346 (3)C2A—H2A20.9600
N2B—C1B1.451 (4)C2A—H2A30.9600
N2B—C2B1.462 (4)C2B—H2B10.9600
N2B—C3B1.341 (3)C2B—H2B20.9600
N3—N41.172 (4)C2B—H2B30.9600
N4—N51.137 (4)C4A—H4A0.9300
N6—N71.179 (3)C4B—H4B0.9300
N7—N81.158 (3)C5A—H5A0.9300
C3A—C4A1.412 (4)C5B—H5B0.9300
C3A—C7A1.405 (3)C6A—H6A0.9300
C3B—C4B1.412 (3)C6B—H6B0.9300
C3B—C7B1.417 (4)C7A—H7A0.9300
C4A—C5A1.355 (4)C7B—H7B0.9300
Zn···H1B1i3.5000C7B···H2B32.9000
N1A···N1B3.210 (3)C7B···H2B12.7300
N1A···N33.113 (4)C7B···H2A3xi3.0800
N1A···N63.225 (3)H1A2···C4A2.7100
N1B···N1A3.210 (3)H1A2···H4A2.2400
N1B···N33.205 (4)H1A1···H2A22.1300
N1B···N63.139 (3)H1A1···N8vii2.5600
N3···N1A3.113 (4)H1A3···C4A2.8500
N3···N1B3.205 (4)H1A3···H4A2.3900
N3···C6A3.339 (4)H1A3···H5Bix2.4500
N3···C7Bii3.367 (4)H1B1···C4B3.0500
N4···N5iii3.286 (4)H1B1···Znvi3.5000
N4···C7Bii3.382 (4)H4A···C1A2.5100
N5···C2Bi3.427 (4)H4A···H1A22.2400
N5···N4iii3.286 (4)H4A···H1A32.3900
N6···N1B3.139 (3)H4A···N7ix2.8200
N6···C5B3.348 (4)H4B···C1B2.5900
N6···N1A3.225 (3)H4B···H1B32.1500
N7···C1Bi3.434 (4)H4B···N7vi2.9100
N8···C5Aiv3.332 (4)H4B···N8vi2.7900
N3···H6A2.8300H1B2···H2B22.1200
N3···H7Bii2.5800H5A···N8ix2.5900
N4···H7Bii2.5900H5B···N62.8100
N5···H2B1ii2.8300H5B···C1Aiv2.9400
N5···H7Av2.9500H5B···H1A3iv2.4500
N5···H2B3i2.7400H1B3···C4B2.6500
N6···H2A1vi2.9300H1B3···H4B2.1500
N6···H5B2.8100H1B3···N7vi2.9100
N7···H4Aiv2.8200H1B3···N8vi2.7600
N7···H1B3i2.9100H6A···N32.8300
N7···H2A1vi2.6600H6B···H6Bii2.5100
N7···H4Bi2.9100H2A1···C7A3.0100
N8···H5Aiv2.5900H2A1···N6i2.9300
N8···H1A1vii2.5600H2A1···N7i2.6600
N8···H2A2vii2.9400H2A1···N8i2.8100
N8···H4Bi2.7900H7A···C2A2.5800
N8···H1B3i2.7600H7A···H2A32.2000
N8···H2A1vi2.8100H7A···N5xii2.9500
C1B···N7vi3.434 (4)H7B···C2B2.5400
C2B···N5vi3.427 (4)H7B···H2B12.2300
C2B···C6Bviii3.383 (4)H7B···H2B32.4900
C5A···N8ix3.332 (4)H7B···N3ii2.5800
C6B···C2Bx3.383 (4)H7B···N4ii2.5900
C7B···N3ii3.367 (4)H2A2···H1A12.1300
C7B···N4ii3.382 (4)H2A2···N8vii2.9400
C1A···H5Bix2.9400H2A3···C7A2.6900
C1A···H4A2.5100H2A3···H7A2.2000
C1B···H4B2.5900H2A3···C7Bxiii3.0800
C2A···H7A2.5800H2B1···C7B2.7300
C2B···H7B2.5400H2B1···H7B2.2300
C4A···H1A22.7100H2B1···N5ii2.8300
C4A···H1A32.8500H2B2···H1B22.1200
C4B···H1B32.6500H2B2···C6Bviii2.9200
C4B···H1B13.0500H2B3···C7B2.9000
C6B···H2B2x2.9200H2B3···H7B2.4900
C7A···H2A13.0100H2B3···N5vi2.7400
C7A···H2A32.6900
N1A—Zn—N1B104.89 (7)N2A—C1A—H1A3109.00
N1A—Zn—N3103.45 (10)H1A2—C1A—H1A1109.00
N1A—Zn—N6107.47 (9)H1A2—C1A—H1A3109.00
N1B—Zn—N3108.32 (10)H1A1—C1A—H1A3110.00
N1B—Zn—N6103.88 (9)N2B—C1B—H1B1110.00
N3—Zn—N6127.05 (11)N2B—C1B—H1B2109.00
Zn—N1A—C5A120.24 (16)N2B—C1B—H1B3109.00
Zn—N1A—C6A124.39 (16)H1B1—C1B—H1B2109.00
C5A—N1A—C6A115.28 (19)H1B1—C1B—H1B3109.00
Zn—N1B—C5B124.17 (16)H1B2—C1B—H1B3109.00
Zn—N1B—C6B120.96 (16)N2A—C2A—H2A1109.00
C5B—N1B—C6B114.9 (2)N2A—C2A—H2A2109.00
C1A—N2A—C2A117.4 (2)N2A—C2A—H2A3109.00
C1A—N2A—C3A120.7 (2)H2A1—C2A—H2A2109.00
C2A—N2A—C3A121.8 (2)H2A1—C2A—H2A3109.00
C1B—N2B—C2B116.1 (2)H2A2—C2A—H2A3109.00
C1B—N2B—C3B121.7 (2)N2B—C2B—H2B1110.00
C2B—N2B—C3B121.6 (2)N2B—C2B—H2B2109.00
Zn—N3—N4144.5 (2)N2B—C2B—H2B3109.00
N3—N4—N5174.7 (3)H2B1—C2B—H2B2110.00
Zn—N6—N7125.8 (2)H2B1—C2B—H2B3109.00
N6—N7—N8176.0 (3)H2B2—C2B—H2B3109.00
N2A—C3A—C4A121.6 (2)C3A—C4A—H4A120.00
N2A—C3A—C7A123.2 (2)C5A—C4A—H4A120.00
C4A—C3A—C7A115.21 (19)C3B—C4B—H4B120.00
N2B—C3B—C4B123.5 (2)C5B—C4B—H4B120.00
N2B—C3B—C7B121.9 (2)N1A—C5A—H5A118.00
C4B—C3B—C7B114.55 (19)C4A—C5A—H5A118.00
C3A—C4A—C5A120.2 (2)N1B—C5B—H5B118.00
C3B—C4B—C5B120.2 (2)C4B—C5B—H5B118.00
N1A—C5A—C4A124.7 (2)N1A—C6A—H6A118.00
N1B—C5B—C4B124.9 (2)C7A—C6A—H6A118.00
N1A—C6A—C7A124.3 (2)N1B—C6B—H6B118.00
N1B—C6B—C7B124.8 (2)C7B—C6B—H6B118.00
C3A—C7A—C6A120.4 (2)C3A—C7A—H7A120.00
C3B—C7B—C6B120.7 (2)C6A—C7A—H7A120.00
N2A—C1A—H1A2109.00C3B—C7B—H7B120.00
N2A—C1A—H1A1109.00C6B—C7B—H7B120.00
N1B—Zn—N1A—C5A55.4 (2)C6B—N1B—C5B—C4B0.3 (3)
N1B—Zn—N1A—C6A120.80 (17)Zn—N1B—C6B—C7B179.51 (18)
N3—Zn—N1A—C5A168.85 (19)C5B—N1B—C6B—C7B0.6 (3)
N3—Zn—N1A—C6A7.35 (19)C1A—N2A—C3A—C4A0.6 (3)
N6—Zn—N1A—C5A54.7 (2)C1A—N2A—C3A—C7A178.6 (2)
N6—Zn—N1A—C6A129.09 (17)C2A—N2A—C3A—C4A176.3 (2)
N1A—Zn—N1B—C5B107.05 (19)C2A—N2A—C3A—C7A4.5 (3)
N1A—Zn—N1B—C6B72.84 (18)C1B—N2B—C3B—C4B3.1 (3)
N3—Zn—N1B—C5B143.0 (2)C1B—N2B—C3B—C7B178.3 (2)
N3—Zn—N1B—C6B37.13 (19)C2B—N2B—C3B—C4B173.3 (2)
N6—Zn—N1B—C5B5.6 (2)C2B—N2B—C3B—C7B8.1 (3)
N6—Zn—N1B—C6B174.48 (17)N2A—C3A—C4A—C5A177.8 (2)
N1A—Zn—N3—N4124.7 (4)C7A—C3A—C4A—C5A1.5 (3)
N1B—Zn—N3—N4124.4 (3)N2A—C3A—C7A—C6A177.3 (2)
N6—Zn—N3—N40.1 (4)C4A—C3A—C7A—C6A2.0 (3)
N1A—Zn—N6—N740.6 (3)N2B—C3B—C4B—C5B179.1 (2)
N1B—Zn—N6—N7151.4 (2)C7B—C3B—C4B—C5B0.4 (3)
N3—Zn—N6—N782.3 (3)N2B—C3B—C7B—C6B178.4 (2)
Zn—N1A—C5A—C4A175.6 (2)C4B—C3B—C7B—C6B0.4 (3)
C6A—N1A—C5A—C4A0.9 (4)C3A—C4A—C5A—N1A0.0 (4)
Zn—N1A—C6A—C7A176.03 (16)C3B—C4B—C5B—N1B0.8 (4)
C5A—N1A—C6A—C7A0.3 (3)N1A—C6A—C7A—C3A1.1 (3)
Zn—N1B—C5B—C4B179.65 (19)N1B—C6B—C7B—C3B0.9 (4)
Symmetry codes: (i) x, y1/2, z+1/2; (ii) x+1, y1, z+1; (iii) x+1, y, z+1; (iv) x+2, y+1/2, z+3/2; (v) x+1, y+1/2, z+3/2; (vi) x, y1/2, z1/2; (vii) x+2, y1, z+2; (viii) x+1, y1/2, z+1/2; (ix) x+2, y1/2, z+3/2; (x) x+1, y+1/2, z+1/2; (xi) x, y3/2, z1/2; (xii) x+1, y1/2, z+3/2; (xiii) x, y3/2, z+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C1A—H1A1···N8vii0.96002.56003.484 (4)163.00
C5A—H5A···N8ix0.93002.59003.332 (4)137.00
C7B—H7B···N3ii0.93002.58003.367 (4)143.00
C7B—H7B···N4ii0.93002.59003.382 (4)143.00
Symmetry codes: (ii) x+1, y1, z+1; (vii) x+2, y1, z+2; (ix) x+2, y1/2, z+3/2.
Selected bond lengths (Å) top
Zn—N1A2.031 (2)Zn—N31.935 (3)
Zn—N1B2.018 (2)Zn—N61.969 (3)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C1A—H1A1···N8i0.96002.56003.484 (4)163.00
C5A—H5A···N8ii0.93002.59003.332 (4)137.00
C7B—H7B···N3iii0.93002.58003.367 (4)143.00
C7B—H7B···N4iii0.93002.59003.382 (4)143.00
Symmetry codes: (i) x+2, y1, z+2; (ii) x+2, y1/2, z+3/2; (iii) x+1, y1, z+1.
Acknowledgements top

Technical support (X-ray measurements at SCDRX) by Université Henry Poincaré, Nancy 1, is gratefully acknowledged.

references
References top

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