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

In the title compound, [Mn(N(3))(2)(C(6)H(6)N(4))(2)], the Mn atom (site symmetry ) is bonded to two azide ions and two bidentate biimidizole ligands, resulting in a slightly distorted octa-hedral MnN(6) geometry for the metal ion. In the crystal structure, N-H⋯N hydrogen bonds help to consolidate the packing.

Related literature

For a related structure, see: Hester et al. (1997 ▶).

Experimental

Crystal data

[Mn(N3)2(C6H6N4)2]

M = 407.30

Monoclinic,

a = 12.5097 (10) Å

b = 8.9728 (5) Å

c = 14.1416 (10) Å

β = 91.883 (10)°

V = 1586.50 (19) Å3

Z = 4

Mo Kα radiation

μ = 0.87 mm−1

T = 293 (2) K

0.40 × 0.26 × 0.20 mm

Data collection

Bruker APEXII CCD diffractometer

Absorption correction: multi-scan (SADABS; Bruker, 2004 ▶) T min = 0.723, T max = 0.846

1966 measured reflections

1505 independent reflections

1250 reflections with I > 2σ(I)

R int = 0.022

Refinement

R[F 2 > 2σ(F 2)] = 0.038

wR(F 2) = 0.131

S = 1.00

1505 reflections

131 parameters

2 restraints

H atoms treated by a mixture of independent and constrained refinement

Δρmax = 0.49 e Å−3

Δρmin = −0.25 e Å−3

Data collection: APEX2 (Bruker, 2004 ▶); cell refinement: SAINT-Plus (Bruker, 2004 ▶); 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/S1600536808017984/hb2744sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808017984/hb2744Isup2.hkl

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

[Mn(N3)2(C6H6N4)2]	F000 = 828
Mr = 407.30	Dx = 1.705 Mg m−3
Monoclinic, C2/c	Mo Kα radiation λ = 0.71073 Å
Hall symbol: -C 2yc	Cell parameters from 1505 reflections
a = 12.5097 (10) Å	θ = 2.8–25.9º
b = 8.9728 (5) Å	µ = 0.87 mm−1
c = 14.1416 (10) Å	T = 293 (2) K
β = 91.883 (10)º	Block, yellow
V = 1586.50 (19) Å3	0.40 × 0.26 × 0.20 mm
Z = 4

Bruker APEXII CCD diffractometer	1505 independent reflections
Radiation source: fine-focus sealed tube	1250 reflections with I > 2σ(I)
Monochromator: graphite	Rint = 0.022
T = 293(2) K	θmax = 25.9º
φ and ω scans	θmin = 2.8º
Absorption correction: multi-scan(SADABS; Bruker, 2004)	h = −1→15
Tmin = 0.723, Tmax = 0.846	k = −1→10
1966 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 atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.131	w = 1/[σ2(Fo2) + (0.081P)2 + 1.7249P] where P = (Fo2 + 2Fc2)/3
S = 1.00	(Δ/σ)max = 0.024
1505 reflections	Δρmax = 0.49 e Å−3
131 parameters	Δρmin = −0.25 e Å−3
2 restraints	Extinction correction: none
Primary atom site location: structure-invariant direct methods

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
Mn1	0.7500	0.7500	0.5000	0.0486 (5)
C1	0.5842 (3)	0.5617 (4)	0.3628 (2)	0.0572 (8)
H1	0.5711	0.6280	0.3132	0.069*
C2	0.5366 (3)	0.4245 (4)	0.3721 (2)	0.0585 (9)
H2	0.4865	0.3819	0.3303	0.070*
C3	0.6462 (2)	0.4631 (4)	0.4891 (2)	0.0482 (7)
C4	0.7106 (2)	0.4562 (4)	0.5744 (2)	0.0489 (7)
C5	0.8223 (3)	0.5322 (4)	0.6783 (2)	0.0580 (8)
H5	0.8713	0.5915	0.7118	0.070*
C6	0.7940 (3)	0.3903 (4)	0.7030 (2)	0.0610 (9)
H6	0.8195	0.3369	0.7554	0.073*
N1	0.5763 (2)	0.3633 (3)	0.45300 (18)	0.0534 (7)
H1A	0.546 (3)	0.270 (3)	0.474 (3)	0.064*
N2	0.6529 (2)	0.5851 (3)	0.43706 (17)	0.0520 (7)
N3	0.7688 (2)	0.5733 (3)	0.59802 (18)	0.0525 (7)
N4	0.7220 (2)	0.3432 (3)	0.63640 (19)	0.0551 (7)
H4	0.680 (3)	0.255 (3)	0.634 (3)	0.066*
N5	0.8833 (2)	0.6634 (3)	0.4268 (2)	0.0529 (7)
N6	0.8963 (2)	0.5320 (3)	0.4212 (2)	0.0552 (7)
N7	0.9109 (3)	0.4018 (3)	0.4143 (2)	0.0723 (9)

	U11	U22	U33	U12	U13	U23
Mn1	0.0504 (12)	0.0400 (13)	0.0550 (13)	0.0096 (10)	−0.0016 (10)	−0.0034 (10)
C1	0.0542 (18)	0.069 (2)	0.0481 (17)	−0.0156 (16)	−0.0081 (14)	0.0038 (15)
C2	0.0551 (18)	0.070 (2)	0.0495 (17)	−0.0171 (16)	−0.0056 (14)	−0.0031 (15)
C3	0.0485 (16)	0.0500 (18)	0.0462 (15)	−0.0087 (13)	0.0012 (12)	−0.0003 (13)
C4	0.0481 (15)	0.0480 (17)	0.0503 (16)	−0.0051 (13)	0.0012 (13)	0.0026 (13)
C5	0.0598 (19)	0.061 (2)	0.0527 (17)	−0.0041 (16)	−0.0095 (14)	0.0033 (15)
C6	0.064 (2)	0.067 (2)	0.0510 (18)	−0.0005 (18)	−0.0087 (15)	0.0092 (16)
N1	0.0539 (15)	0.0539 (16)	0.0525 (15)	−0.0158 (13)	0.0020 (12)	−0.0012 (12)
N2	0.0512 (14)	0.0569 (17)	0.0477 (14)	−0.0117 (13)	−0.0035 (11)	0.0045 (12)
N3	0.0519 (15)	0.0543 (16)	0.0508 (14)	−0.0088 (13)	−0.0063 (11)	0.0042 (12)
N4	0.0600 (16)	0.0524 (16)	0.0524 (14)	−0.0079 (13)	−0.0021 (12)	0.0077 (12)
N5	0.0585 (16)	0.0552 (17)	0.0444 (14)	−0.0006 (14)	−0.0080 (12)	−0.0089 (12)
N6	0.0525 (15)	0.0540 (18)	0.0585 (16)	−0.0129 (13)	−0.0071 (12)	0.0069 (13)
N7	0.073 (2)	0.0512 (18)	0.092 (2)	−0.0078 (15)	−0.0108 (17)	0.0073 (16)

Mn1—N2	2.094 (3)	C3—C4	1.430 (4)
Mn1—N2i	2.094 (3)	C4—N3	1.315 (4)
Mn1—N3i	2.114 (3)	C4—N4	1.345 (4)
Mn1—N3	2.114 (3)	C5—N3	1.350 (4)
Mn1—N5	2.138 (3)	C5—C6	1.370 (5)
Mn1—N5i	2.138 (3)	C5—H5	0.9300
C1—N2	1.351 (4)	C6—N4	1.350 (4)
C1—C2	1.375 (5)	C6—H6	0.9300
C1—H1	0.9300	N1—H1A	0.966 (18)
C2—N1	1.349 (4)	N4—H4	0.952 (19)
C2—H2	0.9300	N5—N6	1.193 (4)
C3—N2	1.323 (4)	N6—N7	1.187 (4)
C3—N1	1.340 (4)
N2—Mn1—N2i	180.0)	N3—C4—N4	113.0 (3)
N2—Mn1—N3i	101.59 (10)	N3—C4—C3	118.2 (3)
N2i—Mn1—N3i	78.41 (10)	N4—C4—C3	128.8 (3)
N2—Mn1—N3	78.41 (10)	N3—C5—C6	110.1 (3)
N2i—Mn1—N3	101.59 (10)	N3—C5—H5	125.0
N3i—Mn1—N3	180.0	C6—C5—H5	125.0
N2—Mn1—N5	89.31 (11)	N4—C6—C5	106.5 (3)
N2i—Mn1—N5	90.69 (11)	N4—C6—H6	126.7
N3i—Mn1—N5	91.53 (11)	C5—C6—H6	126.7
N3—Mn1—N5	88.47 (11)	C3—N1—C2	105.6 (3)
N2—Mn1—N5i	90.69 (11)	C3—N1—H1A	135 (3)
N2i—Mn1—N5i	89.31 (11)	C2—N1—H1A	119 (3)
N3i—Mn1—N5i	88.47 (11)	C3—N2—C1	104.7 (3)
N3—Mn1—N5i	91.53 (11)	C3—N2—Mn1	113.26 (19)
N5—Mn1—N5i	180.0	C1—N2—Mn1	141.7 (2)
N2—C1—C2	109.3 (3)	C4—N3—C5	104.5 (3)
N2—C1—H1	125.3	C4—N3—Mn1	112.6 (2)
C2—C1—H1	125.3	C5—N3—Mn1	142.9 (2)
N1—C2—C1	107.3 (3)	C4—N4—C6	105.8 (3)
N1—C2—H2	126.4	C4—N4—H4	124 (3)
C1—C2—H2	126.4	C6—N4—H4	130 (3)
N2—C3—N1	113.1 (3)	N6—N5—Mn1	120.1 (2)
N2—C3—C4	117.4 (3)	N7—N6—N5	178.6 (4)
N1—C3—C4	129.5 (3)

D—H···A	D—H	H···A	D···A	D—H···A
N1—H1A···N7ii	0.966 (18)	2.26 (3)	3.031 (4)	136 (3)
N1—H1A···N5iii	0.966 (18)	2.33 (4)	3.021 (4)	127 (3)
N4—H4···N7ii	0.952 (19)	1.92 (2)	2.834 (4)	160 (4)

Table 1

Selected bond lengths (Å)

Mn1—N2	2.094 (3)
Mn1—N3	2.114 (3)
Mn1—N5	2.138 (3)

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
N1—H1A⋯N7i	0.966 (18)	2.26 (3)	3.031 (4)	136 (3)
N1—H1A⋯N5ii	0.966 (18)	2.33 (4)	3.021 (4)	127 (3)
N4—H4⋯N7i	0.952 (19)	1.92 (2)	2.834 (4)	160 (4)

Symmetry codes: (i) ; (ii) .