Di-μ(1,1)-azido-bis-[azido-(5,5'-dimethyl-2,2'-bipyridine)nickel(II)].

In the title azide-bridged dinuclear centrosymmetric nickel(II) complex, [Ni(2)(N(3))(4)(C(12)H(12)N(2))(2)], the Ni(II) atom is five-coordinated by two N atoms of the 5,5'-dimethyl-2,2'-bipyridine ligand and three N atoms from three azide ligands in a distorted trigonal-bipyramidal geometry. The Ni⋯Ni distance is 3.2398 (12) Å.

Related literature

For general background, see: Abramo et al. (2002 ▶); Dey et al. (2007 ▶); Jiang et al. (2005 ▶). For related structures, see: Fu et al. (2005 ▶); Song et al. (2007 ▶).

Experimental

Crystal data

[Ni2(N3)4(C12H12N2)2]

M = 654.01

Monoclinic,

a = 7.938 (2) Å

b = 15.067 (3) Å

c = 11.755 (2) Å

β = 91.650 (2)°

V = 1405.3 (5) Å3

Z = 2

Mo Kα radiation

μ = 1.39 mm−1

T = 298 (2) K

0.13 × 0.10 × 0.08 mm

Data collection

Bruker SMART CCD area-detector diffractometer

Absorption correction: multi-scan (SADABS; Bruker, 2001 ▶) T min = 0.840, T max = 0.897

11588 measured reflections

3060 independent reflections

2165 reflections with I > 2σ(I)

R int = 0.063

Refinement

R[F 2 > 2σ(F 2)] = 0.056

wR(F 2) = 0.149

S = 1.03

3060 reflections

192 parameters

14 restraints

H-atom parameters constrained

Δρmax = 0.67 e Å−3

Δρmin = −0.77 e Å−3

Data collection: SMART (Bruker, 2007 ▶); cell refinement: SAINT (Bruker, 2007 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536808037902/ci2712sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808037902/ci2712Isup2.hkl

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

[Ni2(N3)4(C12H12N2)2]	F000 = 672
Mr = 654.01	Dx = 1.546 Mg m−3
Monoclinic, P21/n	Mo Kα radiation λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 1576 reflections
a = 7.938 (2) Å	θ = 2.3–25.1º
b = 15.067 (3) Å	µ = 1.39 mm−1
c = 11.755 (2) Å	T = 298 (2) K
β = 91.650 (2)º	Block, green
V = 1405.3 (5) Å3	0.13 × 0.10 × 0.08 mm
Z = 2

Bruker SMART CCD area-detector diffractometer	3060 independent reflections
Radiation source: fine-focus sealed tube	2165 reflections with I > 2σ(I)
Monochromator: graphite	Rint = 0.063
T = 298(2) K	θmax = 27.0º
φ and ω scan	θmin = 2.2º
Absorption correction: multi-scan(SADABS; Bruker, 2001)	h = −10→10
Tmin = 0.840, Tmax = 0.897	k = −19→19
11588 measured reflections	l = −15→15

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)] = 0.056	H-atom parameters constrained
wR(F2) = 0.149	w = 1/[σ2(Fo2) + (0.0643P)2 + 1.1062P] where P = (Fo2 + 2Fc2)/3
S = 1.03	(Δ/σ)max = 0.001
3060 reflections	Δρmax = 0.67 e Å−3
192 parameters	Δρmin = −0.77 e Å−3
14 restraints	Extinction correction: none
Primary atom site location: structure-invariant direct methods

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 > 2sigma(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
Ni1	0.03235 (7)	0.44079 (4)	0.11356 (5)	0.0386 (2)
N1	0.2280 (5)	0.3549 (3)	0.1785 (4)	0.0491 (10)
N2	−0.0777 (5)	0.3158 (3)	0.0994 (3)	0.0416 (9)
N3	0.0029 (5)	0.5108 (3)	0.2626 (4)	0.0459 (11)
N4	0.0958 (8)	0.5106 (4)	0.3252 (5)	0.0857 (18)
N5	0.1983 (12)	0.5160 (6)	0.4040 (7)	0.144 (3)
N6	0.1668 (5)	0.4913 (3)	−0.0170 (4)	0.0583 (12)
N7	0.2901 (6)	0.4579 (3)	−0.0571 (4)	0.0594 (12)
N8	0.4096 (8)	0.4282 (4)	−0.0950 (6)	0.094 (2)
C1	0.1794 (6)	0.2706 (3)	0.1926 (4)	0.0445 (11)
C2	0.2820 (7)	0.2113 (4)	0.2525 (5)	0.0573 (14)
H2	0.2475	0.1529	0.2628	0.069*
C3	0.4356 (7)	0.2398 (4)	0.2967 (5)	0.0632 (16)
H3	0.5057	0.2000	0.3357	0.076*
C4	0.4857 (6)	0.3259 (4)	0.2836 (5)	0.0575 (14)
C5	0.3771 (6)	0.3811 (4)	0.2219 (5)	0.0570 (14)
H5	0.4100	0.4396	0.2102	0.068*
C6	0.6485 (7)	0.3623 (5)	0.3348 (5)	0.085 (2)
H6A	0.6289	0.3847	0.4097	0.128*
H6B	0.6886	0.4095	0.2878	0.128*
H6C	0.7312	0.3159	0.3393	0.128*
C7	0.0139 (6)	0.2474 (3)	0.1428 (4)	0.0442 (12)
C8	−0.0506 (7)	0.1625 (4)	0.1383 (5)	0.0626 (15)
H8	0.0127	0.1155	0.1680	0.075*
C9	−0.2070 (8)	0.1468 (4)	0.0904 (5)	0.0652 (16)
H9	−0.2501	0.0894	0.0893	0.078*
C10	−0.3023 (6)	0.2160 (4)	0.0433 (5)	0.0530 (13)
C11	−0.2308 (6)	0.2993 (3)	0.0520 (4)	0.0477 (12)
H11	−0.2925	0.3472	0.0233	0.057*
C12	−0.4711 (7)	0.2026 (4)	−0.0126 (5)	0.0657 (16)
H12A	−0.5490	0.1824	0.0427	0.098*
H12B	−0.4629	0.1591	−0.0719	0.098*
H12C	−0.5103	0.2577	−0.0448	0.098*

	U11	U22	U33	U12	U13	U23
Ni1	0.0339 (3)	0.0328 (3)	0.0487 (4)	−0.0009 (3)	−0.0026 (2)	0.0057 (3)
N1	0.039 (2)	0.048 (3)	0.060 (3)	0.0018 (19)	−0.003 (2)	0.004 (2)
N2	0.039 (2)	0.040 (2)	0.046 (2)	0.0000 (17)	−0.0016 (18)	−0.0013 (17)
N3	0.035 (2)	0.036 (2)	0.067 (3)	0.0025 (18)	−0.006 (2)	−0.012 (2)
N4	0.119 (5)	0.043 (3)	0.097 (5)	0.001 (4)	0.045 (4)	−0.006 (3)
N5	0.165 (7)	0.149 (6)	0.115 (6)	−0.004 (6)	−0.029 (5)	0.002 (5)
N6	0.038 (2)	0.066 (3)	0.072 (3)	0.010 (2)	0.005 (2)	0.021 (2)
N7	0.051 (3)	0.056 (3)	0.070 (3)	0.005 (2)	−0.002 (2)	0.016 (2)
N8	0.071 (4)	0.105 (5)	0.108 (5)	0.037 (3)	0.020 (3)	0.011 (4)
C1	0.048 (3)	0.043 (3)	0.043 (3)	0.009 (2)	0.004 (2)	0.001 (2)
C2	0.065 (4)	0.048 (3)	0.058 (3)	0.010 (3)	0.002 (3)	0.002 (3)
C3	0.058 (4)	0.084 (4)	0.047 (3)	0.025 (3)	−0.009 (3)	0.004 (3)
C4	0.041 (3)	0.080 (4)	0.051 (3)	0.008 (3)	0.001 (2)	−0.001 (3)
C5	0.044 (3)	0.064 (4)	0.063 (4)	−0.003 (3)	−0.001 (3)	0.002 (3)
C6	0.049 (3)	0.131 (7)	0.074 (4)	−0.001 (4)	−0.014 (3)	0.003 (4)
C7	0.049 (3)	0.038 (3)	0.046 (3)	0.003 (2)	0.004 (2)	0.001 (2)
C8	0.060 (4)	0.047 (3)	0.080 (4)	0.003 (3)	−0.002 (3)	0.013 (3)
C9	0.067 (4)	0.047 (3)	0.081 (4)	−0.016 (3)	−0.001 (3)	0.004 (3)
C10	0.049 (3)	0.056 (3)	0.054 (3)	−0.008 (3)	0.006 (2)	−0.004 (3)
C11	0.045 (3)	0.047 (3)	0.050 (3)	0.001 (2)	0.001 (2)	0.002 (2)
C12	0.054 (3)	0.075 (4)	0.068 (4)	−0.020 (3)	−0.002 (3)	−0.009 (3)

Ni1—N1	2.145 (4)	C3—H3	0.93
Ni1—N2	2.081 (4)	C4—C5	1.387 (7)
Ni1—N3	2.064 (5)	C4—C6	1.512 (8)
Ni1—N6	2.041 (4)	C5—H5	0.93
Ni1—N6i	2.175 (4)	C6—H6A	0.96
N1—C5	1.336 (6)	C6—H6B	0.96
N1—C1	1.339 (6)	C6—H6C	0.96
N2—C11	1.345 (6)	C7—C8	1.379 (7)
N2—C7	1.352 (6)	C8—C9	1.369 (8)
N3—N4	1.027 (6)	C8—H8	0.93
N4—N5	1.217 (7)	C9—C10	1.394 (8)
N6—N7	1.209 (6)	C9—H9	0.93
N6—Ni1i	2.175 (4)	C10—C11	1.380 (7)
N7—N8	1.149 (7)	C10—C12	1.489 (7)
C1—C2	1.387 (7)	C11—H11	0.93
C1—C7	1.465 (7)	C12—H12A	0.96
C2—C3	1.380 (8)	C12—H12B	0.96
C2—H2	0.93	C12—H12C	0.96
C3—C4	1.367 (8)
N6—Ni1—N3	121.5 (2)	C3—C4—C6	123.2 (5)
N6—Ni1—N2	120.32 (18)	C5—C4—C6	120.1 (6)
N3—Ni1—N2	118.23 (17)	N1—C5—C4	123.5 (5)
N6—Ni1—N1	95.97 (17)	N1—C5—H5	118.2
N3—Ni1—N1	96.02 (17)	C4—C5—H5	118.2
N2—Ni1—N1	77.30 (15)	C4—C6—H6A	109.5
N6—Ni1—N6i	79.63 (18)	C4—C6—H6B	109.5
N3—Ni1—N6i	95.99 (18)	H6A—C6—H6B	109.5
N2—Ni1—N6i	94.98 (16)	C4—C6—H6C	109.5
N1—Ni1—N6i	167.78 (18)	H6A—C6—H6C	109.5
C5—N1—C1	119.3 (5)	H6B—C6—H6C	109.5
C5—N1—Ni1	125.6 (4)	N2—C7—C8	119.8 (5)
C1—N1—Ni1	114.1 (3)	N2—C7—C1	115.8 (4)
C11—N2—C7	119.0 (4)	C8—C7—C1	124.3 (5)
C11—N2—Ni1	124.9 (3)	C9—C8—C7	120.5 (5)
C7—N2—Ni1	116.1 (3)	C9—C8—H8	119.8
N4—N3—Ni1	120.7 (5)	C7—C8—H8	119.8
N3—N4—N5	174.4 (8)	C8—C9—C10	120.6 (5)
N7—N6—Ni1	125.8 (4)	C8—C9—H9	119.7
N7—N6—Ni1i	125.2 (4)	C10—C9—H9	119.7
Ni1—N6—Ni1i	100.37 (18)	C11—C10—C9	115.7 (5)
N8—N7—N6	178.1 (6)	C11—C10—C12	121.3 (5)
N1—C1—C2	120.5 (5)	C9—C10—C12	123.0 (5)
N1—C1—C7	115.8 (4)	N2—C11—C10	124.3 (5)
C2—C1—C7	123.8 (5)	N2—C11—H11	117.8
C3—C2—C1	119.3 (5)	C10—C11—H11	117.8
C3—C2—H2	120.3	C10—C12—H12A	109.5
C1—C2—H2	120.3	C10—C12—H12B	109.5
C4—C3—C2	120.7 (5)	H12A—C12—H12B	109.5
C4—C3—H3	119.7	C10—C12—H12C	109.5
C2—C3—H3	119.7	H12A—C12—H12C	109.5
C3—C4—C5	116.7 (5)	H12B—C12—H12C	109.5

Table 1

Selected bond lengths (Å)

Ni1—N1	2.145 (4)
Ni1—N2	2.081 (4)
Ni1—N3	2.064 (5)
Ni1—N6	2.041 (4)
Ni1—N6i	2.175 (4)

Symmetry code: (i) .