Poly[bis-(μ(2)-5-n-butyl-tetra-zolato-κN:N)zinc(II)].

In the title complex, [Zn(C(5)H(9)N(4))(2)](n), the Zn(II) center is coordinated by four N atoms of different tetra-zolate ligands with a slightly distorted tetra-hedral geometry [Zn-N distances and N-Zn-N angles are in the ranges 1.991 (2)-2.007 (2) Å and 104.22 (8)-116.13 (8)°, respectively]. Each ligand links two Zn(II) atoms through its 1- and 4-position tetra-zole N atoms, forming a single, fully connected three-dimensional framework with a diamond-like topology. In the crystal structure, the Zn⋯Zn separations across each tetra-zole unit are 6.115 (2) and 6.134 (2) Å and the Zn⋯Zn⋯Zn angles are in the range 107.77 (8)-116.83 (8)°.

Related literature

For related literature, see: Li et al. (2007 ▶) and references therein; Wang et al. (2005 ▶); Ye et al. (2005 ▶).

Experimental

Crystal data

[Zn(C5H9N4)2]

M = 315.69

Orthorhombic,

a = 9.6534 (19) Å

b = 10.096 (2) Å

c = 14.359 (3) Å

V = 1399.4 (5) Å3

Z = 4

Mo Kα radiation

μ = 1.76 mm−1

T = 113 (2) K

0.24 × 0.22 × 0.22 mm

Data collection

Bruker SMART 1000 CCD area-detector diffractometer

Absorption correction: multi-scan (SADABS; Bruker, 1998 ▶) T min = 0.978, T max = 1.000 (expected range = 0.665–0.680)

17371 measured reflections

3325 independent reflections

3068 reflections with I > 2σ(I)

R int = 0.032

Refinement

R[F 2 > 2σ(F 2)] = 0.022

wR(F 2) = 0.050

S = 1.02

3325 reflections

172 parameters

H-atom parameters constrained

Δρmax = 0.50 e Å−3

Δρmin = −0.35 e Å−3

Absolute structure: Flack (1983 ▶), 1405 Friedel pairs

Flack parameter: −0.012 (9)

Data collection: SMART (Bruker, 1998 ▶); cell refinement: SAINT (Bruker, 1998 ▶); data reduction: SHELXTL (Bruker, 1998 ▶); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997 ▶); molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Crystal structure: contains datablocks global, I. DOI: 10.1107/S160053680706518X/sf2013sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S160053680706518X/sf2013Isup2.hkl

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

[Zn(C5H9N4)2]	F000 = 656
Mr = 315.69	Dx = 1.498 Mg m−3
Orthorhombic, P212121	Mo Kα radiation λ = 0.71073 Å
Hall symbol: P 2ac 2ab	Cell parameters from 5045 reflections
a = 9.6534 (19) Å	θ = 2.8–27.9º
b = 10.096 (2) Å	µ = 1.76 mm−1
c = 14.359 (3) Å	T = 113 (2) K
V = 1399.4 (5) Å3	Block, colorless
Z = 4	0.24 × 0.22 × 0.22 mm

Bruker Smart 1000 CCD area-detector diffractometer	3325 independent reflections
Radiation source: fine-focus sealed tube	3068 reflections with I > 2σ(I)
Monochromator: graphite	Rint = 0.032
T = 113(2) K	θmax = 27.9º
φ and ω scan	θmin = 2.8º
Absorption correction: multi-scan(SADABS; Bruker, 1998)	h = −11→12
Tmin = 0.978, Tmax = 1.000	k = −13→13
17371 measured reflections	l = −18→18

Refinement on F2	Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: full	H-atom parameters constrained
R[F2 > 2σ(F2)] = 0.022	w = 1/[σ2(Fo2) + (0.0274P)2] where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.050	(Δ/σ)max = 0.001
S = 1.02	Δρmax = 0.50 e Å−3
3325 reflections	Δρmin = −0.35 e Å−3
172 parameters	Extinction correction: none
Primary atom site location: structure-invariant direct methods	Absolute structure: Flack (1983), 1405 Friedel pairs
Secondary atom site location: difference Fourier map	Flack parameter: −0.012 (9)

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.

	x	y	z	Uiso*/Ueq
Zn1	−0.029407 (19)	−0.736890 (17)	−0.131493 (12)	0.01072 (6)
C1	−0.26406 (18)	−0.79890 (17)	0.00726 (12)	0.0128 (4)
C2	−0.2305 (2)	−0.94018 (19)	0.02652 (15)	0.0211 (4)
H2A	−0.2072	−0.9498	0.0919	0.025*
H2B	−0.1497	−0.9653	−0.0096	0.025*
C3	−0.3495 (2)	−1.03381 (19)	0.00312 (17)	0.0294 (5)
H3A	−0.3606	−1.0382	−0.0639	0.035*
H3B	−0.4347	−0.9993	0.0294	0.035*
C4	−0.3233 (3)	−1.1747 (2)	0.0416 (2)	0.0495 (7)
H4A	−0.2441	−1.2133	0.0101	0.059*
H4B	−0.3018	−1.1693	0.1075	0.059*
C5	−0.4459 (3)	−1.2612 (2)	0.0281 (2)	0.0636 (8)
H5A	−0.4274	−1.3472	0.0538	0.085*
H5B	−0.4652	−1.2695	−0.0373	0.085*
H5C	−0.5245	−1.2230	0.0590	0.085*
C6	0.04569 (18)	−0.97174 (16)	−0.25457 (11)	0.0131 (4)
C7	0.19069 (19)	−0.92793 (18)	−0.27100 (14)	0.0168 (4)
H7A	0.2021	−0.8392	−0.2463	0.020*
H7B	0.2073	−0.9240	−0.3376	0.020*
C8	0.29893 (19)	−1.01919 (19)	−0.22630 (15)	0.0226 (4)
H8A	0.2883	−1.1079	−0.2512	0.027*
H8B	0.2828	−1.0232	−0.1597	0.027*
C9	0.4475 (2)	−0.9711 (2)	−0.24428 (16)	0.0313 (5)
H9A	0.5121	−1.0369	−0.2210	0.038*
H9B	0.4619	−0.9629	−0.3109	0.038*
C10	0.4783 (2)	−0.8388 (2)	−0.1982 (2)	0.0468 (7)
H10A	0.5718	−0.8128	−0.2120	0.070*
H10B	0.4673	−0.8470	−0.1320	0.070*
H10C	0.4154	−0.7729	−0.2214	0.070*
N1	−0.19539 (15)	−0.71806 (14)	−0.05010 (10)	0.0135 (3)
N2	−0.25827 (17)	−0.59748 (15)	−0.04447 (12)	0.0188 (4)
N3	−0.36058 (17)	−0.60558 (15)	0.01261 (11)	0.0177 (3)
N4	−0.36690 (14)	−0.73163 (15)	0.04700 (10)	0.0137 (3)
N5	−0.04611 (16)	−0.90468 (13)	−0.20430 (10)	0.0131 (3)
N6	−0.16579 (16)	−0.97651 (15)	−0.20460 (11)	0.0162 (3)
N7	−0.14673 (16)	−1.08254 (16)	−0.25271 (11)	0.0162 (3)
N8	−0.01317 (16)	−1.08258 (14)	−0.28558 (10)	0.0136 (3)

	U11	U22	U33	U12	U13	U23
Zn1	0.01061 (9)	0.01059 (9)	0.01096 (9)	−0.00005 (7)	0.00044 (8)	0.00010 (7)
C1	0.0115 (8)	0.0141 (9)	0.0126 (8)	0.0008 (6)	−0.0007 (7)	−0.0011 (7)
C2	0.0235 (11)	0.0146 (10)	0.0250 (10)	0.0049 (8)	0.0080 (9)	0.0031 (8)
C3	0.0306 (12)	0.0158 (11)	0.0418 (14)	−0.0035 (9)	0.0143 (10)	−0.0064 (9)
C4	0.0491 (16)	0.0252 (13)	0.074 (2)	0.0053 (12)	0.0047 (16)	−0.0033 (13)
C5	0.066 (2)	0.0236 (13)	0.071 (2)	−0.0005 (14)	0.0079 (17)	0.0005 (14)
C6	0.0151 (9)	0.0116 (8)	0.0126 (8)	0.0030 (7)	−0.0003 (8)	0.0003 (6)
C7	0.0139 (9)	0.0140 (9)	0.0223 (10)	−0.0017 (7)	0.0028 (8)	−0.0055 (8)
C8	0.0185 (10)	0.0204 (10)	0.0288 (11)	0.0016 (8)	−0.0013 (9)	−0.0045 (8)
C9	0.0156 (11)	0.0356 (12)	0.0425 (13)	0.0034 (9)	−0.0011 (10)	−0.0062 (10)
C10	0.0216 (12)	0.0350 (13)	0.074 (2)	−0.0046 (11)	−0.0066 (15)	−0.0078 (13)
N1	0.0142 (7)	0.0127 (8)	0.0136 (7)	0.0004 (6)	0.0014 (6)	−0.0001 (6)
N2	0.0200 (8)	0.0135 (8)	0.0229 (9)	0.0030 (6)	0.0073 (7)	0.0021 (7)
N3	0.0213 (9)	0.0119 (8)	0.0200 (8)	0.0004 (6)	0.0064 (7)	0.0032 (6)
N4	0.0166 (7)	0.0105 (7)	0.0140 (7)	0.0007 (6)	0.0007 (6)	0.0014 (6)
N5	0.0123 (8)	0.0124 (7)	0.0146 (7)	−0.0003 (6)	0.0014 (6)	−0.0006 (6)
N6	0.0132 (8)	0.0161 (8)	0.0195 (8)	−0.0045 (6)	0.0017 (7)	−0.0047 (7)
N7	0.0129 (8)	0.0194 (8)	0.0162 (8)	−0.0011 (6)	0.0027 (7)	−0.0027 (6)
N8	0.0124 (8)	0.0141 (7)	0.0143 (7)	−0.0016 (6)	0.0015 (6)	−0.0024 (6)

Zn1—N1	1.9923 (15)	C6—C7	1.487 (2)
Zn1—N5	1.9971 (14)	C7—C8	1.534 (3)
Zn1—N8i	2.0035 (14)	C7—H7A	0.9700
Zn1—N4ii	2.0085 (14)	C7—H7B	0.9700
C1—N4	1.331 (2)	C8—C9	1.536 (3)
C1—N1	1.336 (2)	C8—H8A	0.9700
C1—C2	1.489 (3)	C8—H8B	0.9700
C2—C3	1.525 (3)	C9—C10	1.521 (3)
C2—H2A	0.9700	C9—H9A	0.9700
C2—H2B	0.9700	C9—H9B	0.9700
C3—C4	1.547 (3)	C10—H10A	0.9600
C3—H3A	0.9700	C10—H10B	0.9600
C3—H3B	0.9700	C10—H10C	0.9600
C4—C5	1.484 (3)	N1—N2	1.363 (2)
C4—H4A	0.9700	N2—N3	1.286 (2)
C4—H4B	0.9700	N3—N4	1.366 (2)
C5—H5A	0.9600	N4—Zn1iii	2.0085 (14)
C5—H5B	0.9600	N5—N6	1.364 (2)
C5—H5C	0.9600	N6—N7	1.287 (2)
C6—N5	1.329 (2)	N7—N8	1.373 (2)
C6—N8	1.332 (2)	N8—Zn1iv	2.0035 (14)
N1—Zn1—N5	108.85 (6)	C8—C7—H7A	108.9
N1—Zn1—N8i	116.07 (6)	C6—C7—H7B	108.9
N5—Zn1—N8i	111.41 (6)	C8—C7—H7B	108.9
N1—Zn1—N4ii	106.79 (6)	H7A—C7—H7B	107.7
N5—Zn1—N4ii	104.18 (6)	C7—C8—C9	112.09 (17)
N8i—Zn1—N4ii	108.77 (6)	C7—C8—H8A	109.2
N4—C1—N1	108.82 (16)	C9—C8—H8A	109.2
N4—C1—C2	124.86 (16)	C7—C8—H8B	109.2
N1—C1—C2	126.30 (16)	C9—C8—H8B	109.2
C1—C2—C3	112.90 (17)	H8A—C8—H8B	107.9
C1—C2—H2A	109.0	C10—C9—C8	112.78 (18)
C3—C2—H2A	109.0	C10—C9—H9A	109.0
C1—C2—H2B	109.0	C8—C9—H9A	109.0
C3—C2—H2B	109.0	C10—C9—H9B	109.0
H2A—C2—H2B	107.8	C8—C9—H9B	109.0
C2—C3—C4	111.6 (2)	H9A—C9—H9B	107.8
C2—C3—H3A	109.3	C9—C10—H10A	109.5
C4—C3—H3A	109.3	C9—C10—H10B	109.5
C2—C3—H3B	109.3	H10A—C10—H10B	109.5
C4—C3—H3B	109.3	C9—C10—H10C	109.5
H3A—C3—H3B	108.0	H10A—C10—H10C	109.5
C5—C4—C3	111.4 (2)	H10B—C10—H10C	109.5
C5—C4—H4A	109.4	C1—N1—N2	106.75 (14)
C3—C4—H4A	109.4	C1—N1—Zn1	134.64 (12)
C5—C4—H4B	109.4	N2—N1—Zn1	118.57 (11)
C3—C4—H4B	109.4	N3—N2—N1	108.85 (14)
H4A—C4—H4B	108.0	N2—N3—N4	108.89 (14)
C4—C5—H5A	109.5	C1—N4—N3	106.68 (14)
C4—C5—H5B	109.5	C1—N4—Zn1iii	139.52 (13)
H5A—C5—H5B	109.5	N3—N4—Zn1iii	113.61 (11)
C4—C5—H5C	109.5	C6—N5—N6	106.99 (14)
H5A—C5—H5C	109.5	C6—N5—Zn1	131.52 (12)
H5B—C5—H5C	109.5	N6—N5—Zn1	121.40 (11)
N5—C6—N8	108.99 (15)	N7—N6—N5	108.83 (14)
N5—C6—C7	124.24 (15)	N6—N7—N8	108.60 (14)
N8—C6—C7	126.77 (16)	C6—N8—N7	106.59 (14)
C6—C7—C8	113.35 (16)	C6—N8—Zn1iv	139.87 (13)
C6—C7—H7A	108.9	N7—N8—Zn1iv	113.40 (11)
N4—C1—C2—C3	60.4 (3)	N1—C1—N4—Zn1iii	174.28 (14)
N1—C1—C2—C3	−121.4 (2)	C2—C1—N4—Zn1iii	−7.2 (3)
C1—C2—C3—C4	−168.7 (2)	N2—N3—N4—C1	−0.44 (19)
C2—C3—C4—C5	173.6 (2)	N2—N3—N4—Zn1iii	−176.38 (12)
N5—C6—C7—C8	114.1 (2)	N8—C6—N5—N6	−0.20 (19)
N8—C6—C7—C8	−64.9 (2)	C7—C6—N5—N6	−179.41 (16)
C6—C7—C8—C9	−179.85 (16)	N8—C6—N5—Zn1	176.40 (12)
C7—C8—C9—C10	65.2 (2)	C7—C6—N5—Zn1	−2.8 (3)
N4—C1—N1—N2	0.4 (2)	N1—Zn1—N5—C6	−166.75 (15)
C2—C1—N1—N2	−178.09 (17)	N8i—Zn1—N5—C6	64.01 (17)
N4—C1—N1—Zn1	177.93 (12)	N4ii—Zn1—N5—C6	−53.10 (16)
C2—C1—N1—Zn1	−0.5 (3)	N1—Zn1—N5—N6	9.43 (14)
N5—Zn1—N1—C1	46.63 (19)	N8i—Zn1—N5—N6	−119.81 (13)
N8i—Zn1—N1—C1	173.24 (16)	N4ii—Zn1—N5—N6	123.08 (13)
N4ii—Zn1—N1—C1	−65.30 (18)	C6—N5—N6—N7	0.2 (2)
N5—Zn1—N1—N2	−136.05 (13)	Zn1—N5—N6—N7	−176.78 (11)
N8i—Zn1—N1—N2	−9.44 (15)	N5—N6—N7—N8	−0.18 (19)
N4ii—Zn1—N1—N2	112.02 (13)	N5—C6—N8—N7	0.09 (18)
C1—N1—N2—N3	−0.7 (2)	C7—C6—N8—N7	179.28 (17)
Zn1—N1—N2—N3	−178.68 (12)	N5—C6—N8—Zn1iv	175.30 (14)
N1—N2—N3—N4	0.7 (2)	C7—C6—N8—Zn1iv	−5.5 (3)
N1—C1—N4—N3	0.01 (19)	N6—N7—N8—C6	0.06 (18)
C2—C1—N4—N3	178.52 (17)	N6—N7—N8—Zn1iv	−176.58 (12)