Diazido-bis(2,2'-biimidazole)iron(II).

In the title compound, [Fe(N(3))(2)(C(6)H(6)N(4))(2)], the Fe atom is bonded to two azide ions located in axial positions and to two equatorially positioned bidentate biimidazole ligands, forming a slightly distorterd octa-hedron. The non-H atoms of the equatorial plane are coplanar, with a mean deviation of 0.0355 (2) Å. The Fe(II) cation lies on an inversion centre. Thus, the asymmetric unit comprises one half-mol-ecule.

Related literature

For related literature, see: Caneschi et al. (1989 ▶); Tsukuda et al. (2002 ▶); Vostrikova et al. (2000 ▶); Kuchar et al. (2003 ▶).

Experimental

Crystal data

[Fe(N3)2(C6H6N4)2]

M = 404.17

Monoclinic,

a = 12.487 (3) Å

b = 9.012 (2) Å

c = 14.222 (3) Å

β = 91.91 (3)°

V = 1599.6 (6) Å3

Z = 4

Mo Kα radiation

μ = 0.98 mm−1

T = 293 (2) K

0.14 × 0.12 × 0.10 mm

Data collection

Bruker APEXII CCD diffractometer

Absorption correction: multi-scan (SADABS; Bruker, 2001 ▶) T min = 0.875, T max = 0.909

1964 measured reflections

1504 independent reflections

1250 reflections with I > 2σ(I)

R int = 0.022

Refinement

R[F 2 > 2σ(F 2)] = 0.038

wR(F 2) = 0.118

S = 1.00

1504 reflections

124 parameters

H-atom parameters constrained

Δρmax = 0.65 e Å−3

Δρmin = −0.26 e Å−3

Data collection: APEX2 (Bruker, 2004 ▶); cell refinement: SAINT-Plus (Bruker, 2001 ▶); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: SHELXTL (Sheldrick, 2008 ▶); software used to prepare material for publication: SHELXTL.

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536808018539/kp2177sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808018539/kp2177Isup2.hkl

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

[Fe(N3)2(C6H6N4)2]	F000 = 816
Mr = 404.17	Dx = 1.678 Mg m−3
Monoclinic, C2/c	Mo Kα radiation λ = 0.71073 Å
Hall symbol: -C 2yc	Cell parameters from 1504 reflections
a = 12.487 (3) Å	θ = 2.8–25.7º
b = 9.012 (2) Å	µ = 0.98 mm−1
c = 14.222 (3) Å	T = 293 (2) K
β = 91.91 (3)º	Block, colourless
V = 1599.6 (6) Å3	0.14 × 0.12 × 0.10 mm
Z = 4

Bruker APEXII CCD diffractometer	1504 independent reflections
Radiation source: fine-focus sealed tube	1250 reflections with I > 2σ(I)
Monochromator: graphite	Rint = 0.022
T = 293(2) K	θmax = 25.7º
φ and ω scans	θmin = 2.8º
Absorption correction: multi-scan(SADABS; Bruker, 2001)	h = −1→15
Tmin = 0.875, Tmax = 0.909	k = −1→10
1964 measured reflections	l = −17→17

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)] = 0.038	H-atom parameters constrained
wR(F2) = 0.118	w = 1/[σ2(Fo2) + (0.075P)2 + 1.004P] where P = (Fo2 + 2Fc2)/3
S = 1.00	(Δ/σ)max = 0.006
1504 reflections	Δρmax = 0.65 e Å−3
124 parameters	Δρmin = −0.25 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
Fe1	0.7500	1.2500	0.5000	0.0610 (9)
C1	0.6773 (3)	1.0317 (4)	0.3216 (2)	0.0554 (7)
H1	0.6279	1.0905	0.2883	0.067*
C2	0.7058 (3)	0.8903 (4)	0.2969 (2)	0.0583 (8)
H2	0.6805	0.8374	0.2446	0.070*
C3	0.9629 (2)	0.9250 (4)	0.6284 (2)	0.0555 (8)
H3	1.0126	0.8825	0.6704	0.067*
C4	0.9159 (2)	1.0612 (4)	0.63750 (19)	0.0543 (7)
H4	0.9290	1.1270	0.6869	0.065*
C5	0.7896 (2)	0.9564 (3)	0.42568 (19)	0.0456 (6)
C6	0.8539 (2)	0.9633 (3)	0.51069 (18)	0.0454 (6)
N1	0.60420 (19)	1.0322 (3)	0.57863 (17)	0.0519 (6)
N2	0.6173 (2)	1.1634 (3)	0.57318 (18)	0.0544 (6)
N3	0.5894 (2)	0.9020 (3)	0.5859 (2)	0.0697 (8)
N4	0.73154 (18)	1.0735 (3)	0.40187 (16)	0.0499 (6)
N5	0.84709 (18)	1.0851 (3)	0.56302 (15)	0.0491 (6)
N6	0.92402 (18)	0.8623 (3)	0.54644 (16)	0.0498 (6)
N7	0.7786 (2)	0.8422 (3)	0.36365 (16)	0.0517 (6)

	U11	U22	U33	U12	U13	U23
Fe1	0.064 (2)	0.067 (2)	0.0510 (18)	−0.0005 (18)	−0.0087 (15)	0.0092 (16)
C1	0.0573 (17)	0.0577 (18)	0.0505 (15)	0.0058 (14)	−0.0099 (13)	−0.0031 (14)
C2	0.0618 (18)	0.064 (2)	0.0489 (16)	−0.0009 (16)	−0.0092 (14)	−0.0094 (14)
C3	0.0499 (16)	0.069 (2)	0.0472 (15)	0.0174 (15)	−0.0050 (12)	0.0040 (14)
C4	0.0513 (16)	0.0661 (19)	0.0448 (14)	0.0160 (15)	−0.0081 (12)	−0.0049 (13)
C5	0.0440 (14)	0.0452 (15)	0.0473 (14)	0.0058 (12)	0.0004 (11)	−0.0026 (12)
C6	0.0454 (14)	0.0474 (16)	0.0435 (13)	0.0084 (12)	0.0018 (11)	−0.0004 (11)
N1	0.0492 (14)	0.0514 (16)	0.0547 (14)	0.0132 (11)	−0.0061 (11)	−0.0075 (11)
N2	0.0528 (14)	0.0487 (16)	0.0614 (15)	0.0104 (12)	−0.0006 (11)	−0.0037 (12)
N3	0.0706 (18)	0.0500 (17)	0.088 (2)	0.0088 (14)	−0.0093 (15)	−0.0077 (15)
N4	0.0497 (13)	0.0521 (15)	0.0474 (12)	0.0085 (11)	−0.0060 (10)	−0.0052 (11)
N5	0.0462 (13)	0.0545 (15)	0.0463 (12)	0.0117 (11)	−0.0042 (10)	−0.0045 (11)
N6	0.0476 (13)	0.0525 (14)	0.0491 (12)	0.0130 (11)	0.0005 (10)	0.0034 (11)
N7	0.0553 (14)	0.0513 (15)	0.0482 (12)	0.0048 (12)	−0.0012 (10)	−0.0068 (11)

Fe1—N5	2.100 (2)	C3—C4	1.368 (4)
Fe1—N5i	2.100 (2)	C3—H3	0.9300
Fe1—N4i	2.123 (2)	C4—N5	1.359 (3)
Fe1—N4	2.123 (2)	C4—H4	0.9300
Fe1—N2i	2.134 (3)	C5—N4	1.318 (4)
Fe1—N2	2.134 (3)	C5—N7	1.360 (4)
C1—N4	1.361 (4)	C5—C6	1.430 (4)
C1—C2	1.373 (4)	C6—N5	1.330 (4)
C1—H1	0.9300	C6—N6	1.351 (4)
C2—N7	1.363 (4)	N1—N3	1.193 (4)
C2—H2	0.9300	N1—N2	1.197 (3)
C3—N6	1.369 (4)
N5—Fe1—N5i	180.000 (1)	N6—C3—H3	126.0
N5—Fe1—N4i	101.60 (9)	C4—C3—H3	126.0
N5i—Fe1—N4i	78.40 (9)	N5—C4—C3	109.3 (3)
N5—Fe1—N4	78.40 (9)	N5—C4—H4	125.4
N5i—Fe1—N4	101.60 (9)	C3—C4—H4	125.4
N4i—Fe1—N4	180.000 (1)	N4—C5—N7	113.3 (2)
N5—Fe1—N2i	91.16 (10)	N4—C5—C6	118.1 (2)
N5i—Fe1—N2i	88.84 (10)	N7—C5—C6	128.6 (3)
N4i—Fe1—N2i	88.71 (10)	N5—C6—N6	113.4 (2)
N4—Fe1—N2i	91.29 (10)	N5—C6—C5	117.7 (2)
N5—Fe1—N2	88.84 (10)	N6—C6—C5	128.9 (3)
N5i—Fe1—N2	91.16 (10)	N3—N1—N2	178.3 (3)
N4i—Fe1—N2	91.29 (10)	N1—N2—Fe1	120.2 (2)
N4—Fe1—N2	88.71 (10)	C5—N4—C1	104.4 (2)
N2i—Fe1—N2	180.0	C5—N4—Fe1	112.58 (18)
N4—C1—C2	110.2 (3)	C1—N4—Fe1	143.0 (2)
N4—C1—H1	124.9	C6—N5—C4	104.8 (2)
C2—C1—H1	124.9	C6—N5—Fe1	113.05 (17)
N7—C2—C1	106.8 (3)	C4—N5—Fe1	141.8 (2)
N7—C2—H2	126.6	C6—N6—C3	104.4 (2)
C1—C2—H2	126.6	C5—N7—C2	105.2 (2)
N6—C3—C4	108.0 (2)

Fe1—N5	2.100 (2)
Fe1—N4	2.123 (2)
Fe1—N2	2.134 (3)

N5—Fe1—N5i	180
N5—Fe1—N4	78.40 (9)
N5—Fe1—N2	88.84 (10)
N4—Fe1—N4i
N4—Fe1—N2	88.71 (10)
N2i—Fe1—N2	180

Symmetry code: (i) .