Dibromido(di-2-pyridyl disulfide-κN,N')zinc(II).

The molecular structure of the title compound, [ZnBr(2)(C(10)H(8)N(2)S(2))], contains a seven-membered chelate ring in which the zinc atom is coordinated by two bromide ions and by the two pyridyl N atoms of a single 2,2'-dipyridyldisulfide (dpds) ligand within a slightly distorted tetra-hedron. As is usual for this type of complex, the disulfide group does not participate in zinc coordination. The chelate complexes are connected via weak inter-molecular C-H⋯Br hydrogen bonding into chains, which extend in the [010] direction.

Related literature

For related literature, see: Bhosekar et al. (2007 ▶); Kinoshita et al. (2003 ▶); Kadooka et al. (1976 ▶); Kubo et al. (1998 ▶); Näther & Jess (2006 ▶); n class="Chemical">Näther et al. (2003 ▶); Pickardt et al. (2005 ▶); Raghavan & Seff (1977 ▶).

Experimental

Crystal data

[ZnBr2(C10n class="Species">H8N2S2)]

M = 445.49

Triclinic,

a = 7.7610 (8) Å

b = 8.2962 (8) Å

c = 12.3576 (13) Å

α = 95.488 (12)°

β = 107.161 (12)°

γ = 112.950 (11)°

V = 679.70 (12) Å3

Z = 2

Mo Kα radiation

μ = 7.97 mm−1

T = 170 (2) K

0.09 × 0.09 × 0.08 mm

Data collection

Stoe IPDS-1 diffractometer

Absorption correction: none

6076 measured reflections

2609 independent reflections

2167 reflections with I > 2σ(I)

R int = 0.054

Refinement

R[F 2 > 2σ(F 2)] = 0.046

wR(F 2) = 0.120

S = 1.06

2609 reflections

155 parameters

H-atom parameters constrained

Δρmax = 1.31 e Å−3

Δρmin = −1.43 e Å−3

Data collection: IPDS Program Package (Stoe, 1998 ▶); cell refinement: IPDS Program Package; data reduction: IPDS Program Package; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997 ▶; program(s) used to refine structure: SHELXL97 (Sheldrick, 1997 ▶); molecular graphics: XP in SHELXTL (Bruker, 1998 ▶); software used to prepare material for publication: n class="Chemical">CIFTAB in SHELXTL.

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536807063556/si2061sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536807063556/si2061Isup2.hkl

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

[ZnBr2(C10H8N2S2)]	Z = 2
Mr = 445.49	F000 = 428
Triclinic, P1	Dx = 2.177 Mg m−3
a = 7.7610 (8) Å	Mo Kα radiation λ = 0.71073 Å
b = 8.2962 (8) Å	Cell parameters from 8000 reflections
c = 12.3576 (13) Å	θ = 2.9–28.1º
α = 95.488 (12)º	µ = 7.97 mm−1
β = 107.161 (12)º	T = 170 (2) K
γ = 112.950 (11)º	Block, colourless
V = 679.70 (12) Å3	0.09 × 0.09 × 0.08 mm

STOE IPDS-1 diffractometer	2167 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.054
Monochromator: graphite	θmax = 26.0º
T = 170(2) K	θmin = 2.9º
Phi scans	h = −9→9
Absorption correction: none	k = −10→10
6076 measured reflections	l = −15→15
2609 independent reflections

Refinement on F2	Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: full	H-atom parameters constrained
R[F2 > 2σ(F2)] = 0.046	w = 1/[σ2(Fo2) + (0.0684P)2 + 2.046P] where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.120	(Δ/σ)max < 0.001
S = 1.06	Δρmax = 1.31 e Å−3
2609 reflections	Δρmin = −1.43 e Å−3
155 parameters	Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0071 (16)
Secondary atom site location: difference Fourier map

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
Br1	0.99364 (9)	0.75728 (8)	0.23015 (6)	0.0193 (2)
Br2	0.38203 (9)	0.48414 (9)	0.12968 (6)	0.0197 (2)
Zn1	0.70460 (10)	0.50584 (9)	0.22904 (6)	0.0143 (2)
S1	0.7276 (3)	0.2365 (2)	0.44635 (15)	0.0223 (4)
N1	0.7378 (8)	0.5577 (7)	0.4048 (5)	0.0167 (11)
C2	0.7679 (9)	0.5176 (10)	0.5987 (6)	0.0222 (14)
H2	0.7685	0.4418	0.6517	0.027*
C5	0.7566 (10)	0.7263 (9)	0.4404 (5)	0.0190 (13)
H5	0.7473	0.7974	0.3850	0.023*
C1	0.7414 (9)	0.4556 (9)	0.4828 (5)	0.0166 (13)
C3	0.7933 (10)	0.6913 (10)	0.6347 (6)	0.0248 (15)
H3	0.8134	0.7373	0.7131	0.030*
C4	0.7888 (10)	0.7975 (10)	0.5545 (7)	0.0263 (15)
H4	0.8077	0.9175	0.5777	0.032*
S2	0.5117 (2)	0.1119 (2)	0.28313 (15)	0.0213 (4)
N11	0.7411 (7)	0.2888 (7)	0.1671 (5)	0.0151 (10)
C15	0.8390 (9)	0.2991 (9)	0.0928 (5)	0.0183 (13)
H15	0.9064	0.4133	0.0785	0.022*
C11	0.6512 (9)	0.1280 (8)	0.1897 (5)	0.0156 (12)
C14	0.8465 (10)	0.1511 (10)	0.0359 (6)	0.0237 (15)
H14	0.9146	0.1632	−0.0175	0.028*
C13	0.7523 (10)	−0.0148 (9)	0.0587 (6)	0.0225 (14)
H13	0.7544	−0.1189	0.0209	0.027*
C12	0.6535 (10)	−0.0270 (9)	0.1385 (6)	0.0227 (14)
H12	0.5899	−0.1386	0.1570	0.027*

	U11	U22	U33	U12	U13	U23
Br1	0.0160 (3)	0.0134 (4)	0.0251 (4)	0.0025 (3)	0.0079 (3)	0.0054 (2)
Br2	0.0136 (3)	0.0182 (4)	0.0257 (4)	0.0065 (3)	0.0050 (3)	0.0070 (3)
Zn1	0.0137 (4)	0.0105 (4)	0.0198 (4)	0.0056 (3)	0.0067 (3)	0.0045 (3)
S1	0.0257 (9)	0.0218 (9)	0.0254 (9)	0.0145 (7)	0.0097 (7)	0.0113 (7)
N1	0.015 (3)	0.018 (3)	0.019 (3)	0.008 (2)	0.006 (2)	0.006 (2)
C2	0.016 (3)	0.035 (4)	0.017 (3)	0.013 (3)	0.006 (3)	0.007 (3)
C5	0.025 (3)	0.018 (3)	0.017 (3)	0.012 (3)	0.008 (3)	0.005 (3)
C1	0.011 (3)	0.021 (3)	0.021 (3)	0.009 (3)	0.005 (2)	0.007 (3)
C3	0.022 (3)	0.038 (4)	0.013 (3)	0.013 (3)	0.006 (3)	0.001 (3)
C4	0.020 (3)	0.021 (4)	0.040 (4)	0.010 (3)	0.013 (3)	0.006 (3)
S2	0.0147 (8)	0.0164 (8)	0.0303 (9)	0.0024 (6)	0.0108 (7)	0.0054 (7)
N11	0.012 (2)	0.011 (3)	0.021 (3)	0.005 (2)	0.004 (2)	0.003 (2)
C15	0.016 (3)	0.020 (3)	0.020 (3)	0.009 (3)	0.008 (3)	0.005 (3)
C11	0.009 (3)	0.014 (3)	0.021 (3)	0.005 (2)	0.001 (2)	0.006 (2)
C14	0.020 (3)	0.026 (4)	0.028 (4)	0.014 (3)	0.009 (3)	0.003 (3)
C13	0.023 (3)	0.023 (4)	0.018 (3)	0.013 (3)	0.003 (3)	−0.006 (3)
C12	0.025 (4)	0.015 (3)	0.025 (3)	0.010 (3)	0.004 (3)	0.004 (3)

Br1—Zn1	2.3897 (10)	C3—H3	0.9500
Br2—Zn1	2.3664 (10)	C4—H4	0.9500
Zn1—N11	2.042 (5)	S2—C11	1.783 (6)
Zn1—N1	2.091 (5)	N11—C11	1.343 (8)
S1—C1	1.784 (7)	N11—C15	1.344 (8)
S1—S2	2.050 (3)	C15—C14	1.385 (9)
N1—C1	1.344 (8)	C15—H15	0.9500
N1—C5	1.362 (8)	C11—C12	1.387 (9)
C2—C3	1.385 (10)	C14—C13	1.386 (11)
C2—C1	1.401 (9)	C14—H14	0.9500
C2—H2	0.9500	C13—C12	1.406 (10)
C5—C4	1.385 (10)	C13—H13	0.9500
C5—H5	0.9500	C12—H12	0.9500
C3—C4	1.389 (11)
N11—Zn1—N1	117.2 (2)	C5—C4—C3	119.2 (6)
N11—Zn1—Br2	112.77 (15)	C5—C4—H4	120.4
N1—Zn1—Br2	103.61 (14)	C3—C4—H4	120.4
N11—Zn1—Br1	103.35 (15)	C11—S2—S1	104.0 (2)
N1—Zn1—Br1	100.99 (15)	C11—N11—C15	118.2 (5)
Br2—Zn1—Br1	119.06 (4)	C11—N11—Zn1	121.2 (4)
C1—S1—S2	106.7 (2)	C15—N11—Zn1	120.3 (4)
C1—N1—C5	118.1 (5)	N11—C15—C14	123.2 (6)
C1—N1—Zn1	131.4 (4)	N11—C15—H15	118.4
C5—N1—Zn1	110.4 (4)	C14—C15—H15	118.4
C3—C2—C1	118.8 (6)	N11—C11—C12	122.8 (6)
C3—C2—H2	120.6	N11—C11—S2	118.3 (4)
C1—C2—H2	120.6	C12—C11—S2	118.8 (5)
N1—C5—C4	122.2 (6)	C15—C14—C13	118.5 (6)
N1—C5—H5	118.9	C15—C14—H14	120.8
C4—C5—H5	118.9	C13—C14—H14	120.8
N1—C1—C2	122.5 (6)	C14—C13—C12	119.1 (6)
N1—C1—S1	121.5 (5)	C14—C13—H13	120.5
C2—C1—S1	115.9 (5)	C12—C13—H13	120.5
C2—C3—C4	119.1 (6)	C11—C12—C13	118.3 (6)
C2—C3—H3	120.5	C11—C12—H12	120.9
C4—C3—H3	120.5	C13—C12—H12	120.9

Br1—Zn1	2.3897 (10)
Br2—Zn1	2.3664 (10)
Zn1—N11	2.042 (5)
Zn1—N1	2.091 (5)

N11—Zn1—N1	117.2 (2)
N11—Zn1—Br2	112.77 (15)
N1—Zn1—Br2	103.61 (14)
N11—Zn1—Br1	103.35 (15)
N1—Zn1—Br1	100.99 (15)
Br2—Zn1—Br1	119.06 (4)