Poly[μ-azido-(μ(3)-nicotinato N-oxide)zinc(II)].

The title compound, [Zn(C(6)H(4)NO(3))(N(3))], has been prepared by the reaction of nicotinate N-oxide acid, zinc(II) nitrate and sodium azide. The Zn atom is five coordinated by two azide anions and three nicotinate N-oxide ligands. Each nicotinate N-oxide bridges three Zn atoms, whereas the azide bridges two Zn atoms, resulting in the formation of a two-dimensional metal-organic polymer developing parallel to (100).

Related literature

For background to metal–azide complexes, see: Escuer et al. (1997 ▶); Liu et al. (2005 ▶); Monfort et al. (2000 ▶); Shen et al. (2000 ▶).

Experimental

Crystal data

[Zn(C6H4NO3)(N3)]

M = 245.50

Monoclinic,

a = 8.1132 (16) Å

b = 6.1342 (12) Å

c = 15.786 (3) Å

β = 101.19 (3)°

V = 770.7 (3) Å3

Z = 4

Mo Kα radiation

μ = 3.17 mm−1

T = 293 (2) K

0.20 × 0.18 × 0.15 mm

Data collection

Rigaku SCXmini diffractometer

Absorption correction: multi-scan (ABSCOR; Higashi, 1995 ▶) T min = 0.786, T max = 1.000 (expected range = 0.489–0.622)

7629 measured reflections

1761 independent reflections

1293 reflections with I > 2σ(I)

R int = 0.091

Refinement

R[F 2 > 2σ(F 2)] = 0.065

wR(F 2) = 0.122

S = 1.12

1761 reflections

127 parameters

H-atom parameters constrained

Δρmax = 0.50 e Å−3

Δρmin = −0.52 e Å−3

Data collection: CrystalClear (Rigaku, 2007 ▶); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: ORTEPIII (Burnett & Johnson, 1996 ▶) and PLATON (Spek, 2003 ▶); software used to prepare material for publication: SHELXTL (Sheldrick, 2008 ▶).

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536808039275/dn2407sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808039275/dn2407Isup2.hkl

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

[Zn(C6H4NO3)(N3)]	F000 = 488
Mr = 245.50	Dx = 2.116 Mg m−3
Monoclinic, P21/c	Mo Kα radiation λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 6677 reflections
a = 8.1132 (16) Å	θ = 3.1–27.6º
b = 6.1342 (12) Å	µ = 3.17 mm−1
c = 15.786 (3) Å	T = 293 (2) K
β = 101.19 (3)º	Block, pink
V = 770.7 (3) Å3	0.20 × 0.18 × 0.15 mm
Z = 4

Rigaku SCXmini diffractometer	1761 independent reflections
Radiation source: fine-focus sealed tube	1293 reflections with I > 2σ(I)
Monochromator: graphite	Rint = 0.091
T = 293(2) K	θmax = 27.5º
ω scans	θmin = 3.3º
Absorption correction: multi-scan(ABSCOR; Higashi, 1995)	h = −10→10
Tmin = 0.786, Tmax = 1.000	k = −7→7
7629 measured reflections	l = −20→20

Refinement on F2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.065	H-atom parameters constrained
wR(F2) = 0.122	w = 1/[σ2(Fo2) + (0.0419P)2 + 1.4372P] where P = (Fo2 + 2Fc2)/3
S = 1.12	(Δ/σ)max < 0.001
1761 reflections	Δρmax = 0.50 e Å−3
127 parameters	Δρmin = −0.52 e Å−3
Primary atom site location: structure-invariant direct methods	Extinction correction: none

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	0.92049 (8)	1.07685 (11)	0.77114 (4)	0.0250 (2)
N2	1.2498 (6)	0.9185 (8)	0.8332 (3)	0.0259 (10)
O3	0.9850 (5)	0.8093 (6)	1.1049 (2)	0.0246 (9)
O2	0.8412 (5)	0.5276 (7)	1.1413 (3)	0.0396 (11)
O1	0.7173 (5)	0.9338 (8)	0.7978 (2)	0.0395 (11)
N4	0.7150 (5)	0.7746 (8)	0.8558 (3)	0.0261 (11)
C6	0.8023 (7)	0.7911 (9)	0.9367 (3)	0.0229 (12)
H6A	0.8716	0.9110	0.9526	0.028*
N1	1.1263 (6)	0.8822 (7)	0.7773 (3)	0.0268 (11)
C5	0.6141 (6)	0.6031 (10)	0.8310 (3)	0.0263 (13)
H5A	0.5543	0.5953	0.7745	0.032*
C4	0.5987 (7)	0.4421 (10)	0.8872 (4)	0.0308 (14)
H4A	0.5276	0.3247	0.8700	0.037*
C2	0.7901 (7)	0.6329 (9)	0.9958 (3)	0.0208 (12)
N3	1.3654 (6)	0.9564 (8)	0.8842 (3)	0.0361 (13)
C3	0.6906 (7)	0.4538 (10)	0.9712 (4)	0.0299 (14)
H3A	0.6847	0.3418	1.0103	0.036*
C1	0.8807 (7)	0.6564 (9)	1.0894 (4)	0.0232 (12)

	U11	U22	U33	U12	U13	U23
Zn1	0.0290 (4)	0.0231 (4)	0.0213 (3)	0.0007 (3)	0.0006 (2)	0.0007 (3)
N2	0.030 (3)	0.019 (2)	0.030 (3)	−0.001 (2)	0.008 (2)	0.000 (2)
O3	0.028 (2)	0.024 (2)	0.021 (2)	−0.0054 (17)	0.0008 (16)	−0.0007 (17)
O2	0.047 (3)	0.046 (3)	0.021 (2)	−0.024 (2)	−0.0064 (18)	0.011 (2)
O1	0.032 (2)	0.055 (3)	0.027 (2)	−0.014 (2)	−0.0085 (17)	0.025 (2)
N4	0.024 (3)	0.033 (3)	0.021 (2)	−0.002 (2)	0.002 (2)	0.005 (2)
C6	0.026 (3)	0.023 (3)	0.019 (3)	−0.006 (2)	0.000 (2)	−0.002 (2)
N1	0.025 (3)	0.025 (3)	0.026 (3)	0.004 (2)	−0.006 (2)	−0.007 (2)
C5	0.022 (3)	0.035 (4)	0.020 (3)	−0.007 (3)	−0.002 (2)	−0.004 (3)
C4	0.035 (3)	0.027 (3)	0.027 (3)	−0.012 (3)	−0.001 (2)	−0.008 (3)
C2	0.023 (3)	0.023 (3)	0.018 (3)	0.001 (2)	0.004 (2)	−0.002 (2)
N3	0.029 (3)	0.036 (3)	0.039 (3)	−0.006 (2)	−0.004 (2)	−0.004 (3)
C3	0.039 (4)	0.026 (3)	0.024 (3)	−0.010 (3)	0.004 (3)	0.002 (3)
C1	0.025 (3)	0.024 (3)	0.020 (3)	0.002 (2)	0.002 (2)	−0.003 (2)

Zn1—O1	1.983 (4)	N4—C5	1.344 (7)
Zn1—N1i	2.031 (5)	C6—C2	1.363 (7)
Zn1—N1	2.040 (4)	C6—H6A	0.9300
Zn1—O3ii	2.079 (4)	C5—C4	1.349 (8)
Zn1—O2iii	2.125 (4)	C5—H5A	0.9300
N2—N3	1.134 (6)	C4—C3	1.392 (7)
N2—N1	1.220 (6)	C4—H4A	0.9300
O3—C1	1.255 (6)	C2—C3	1.374 (8)
O2—C1	1.225 (7)	C2—C1	1.523 (7)
O1—N4	1.342 (6)	C3—H3A	0.9300
N4—C6	1.338 (6)
O1—Zn1—N1i	112.69 (19)	C2—C6—H6A	119.9
O1—Zn1—N1	115.93 (19)	N2—N1—Zn1v	120.5 (4)
N1i—Zn1—N1	130.49 (12)	N2—N1—Zn1	118.5 (4)
O1—Zn1—O3ii	96.82 (16)	Zn1v—N1—Zn1	115.5 (2)
N1i—Zn1—O3ii	93.02 (17)	N4—C5—C4	120.7 (5)
N1—Zn1—O3ii	90.14 (16)	N4—C5—H5A	119.7
O1—Zn1—O2iii	87.86 (18)	C4—C5—H5A	119.7
N1i—Zn1—O2iii	85.13 (18)	C5—C4—C3	119.2 (5)
N1—Zn1—O2iii	87.80 (17)	C5—C4—H4A	120.4
O3ii—Zn1—O2iii	175.31 (17)	C3—C4—H4A	120.4
N3—N2—N1	178.4 (6)	C6—C2—C3	119.5 (5)
C1—O3—Zn1ii	123.1 (4)	C6—C2—C1	120.7 (5)
C1—O2—Zn1iv	140.4 (4)	C3—C2—C1	119.7 (5)
N4—O1—Zn1	126.1 (3)	C2—C3—C4	119.1 (5)
C6—N4—O1	121.4 (5)	C2—C3—H3A	120.4
C6—N4—C5	121.1 (5)	C4—C3—H3A	120.4
O1—N4—C5	117.3 (4)	O2—C1—O3	127.3 (5)
N4—C6—C2	120.3 (5)	O2—C1—C2	116.6 (5)
N4—C6—H6A	119.9	O3—C1—C2	116.1 (5)