Diaqua-bis[5-(2-pyridylmeth-yl)tetra-zolato-κN,N]manganese(II).

The title complex, [Mn(C(7)H(6)N(5))(2)(H(2)O)(2)], was obtained by the in situ hydro-thermal reaction of MnCl(2) with 2-(2-pyrid-yl)acetonitrile in the presence of NaN(3). The Mn(II) atom, which is located on an inversion centre, has a distorted octa-hedral coordination geometry formed by two water mol-ecules and two chelating ligands. Inter-molecular hydrogen bonds and π-π inter-actions (3.452 Å) stabilize the crystal structure and lead to the formation of a three-dimensional network.

Related literature

For related literature, see: Demko & Sharpless (2001 ▶); Zhao et al. (2008 ▶). For the synthesis of similar complexes, see: Hu et al. (2007 ▶); Liu & Fan (2007 ▶).

Experimental

Crystal data

[Mn(C7H6N5)2(H2O)2]

M = 411.31

Monoclinic,

a = 6.638 (2) Å

b = 13.788 (5) Å

c = 8.771 (3) Å

β = 90.01 (5)°

V = 802.9 (4) Å3

Z = 2

Mo Kα radiation

μ = 0.86 mm−1

T = 293 (2) K

0.20 × 0.12 × 0.12 mm

Data collection

Rigaku Mercury2 diffractometer

Absorption correction: multi-scan (CrystalClear; Rigaku, 2005 ▶) T min = 0.802, T max = 1.000 (expected range = 0.723–0.902)

8070 measured reflections

1836 independent reflections

1550 reflections with I > 2σ(I)

R int = 0.057

Refinement

R[F 2 > 2σ(F 2)] = 0.058

wR(F 2) = 0.172

S = 1.13

1836 reflections

124 parameters

H-atom parameters constrained

Δρmax = 0.39 e Å−3

Δρmin = −0.73 e Å−3

Data collection: CrystalClear (Rigaku, 2005 ▶); 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: SHELXTL (Sheldrick, 2008 ▶); software used to prepare material for publication: SHELXTL.

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536808019272/hg2418sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808019272/hg2418Isup2.hkl

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

[Mn(C7H6N5)2(H2O)2]	F000 = 422
Mr = 411.31	Dx = 1.701 Mg m−3
Monoclinic, P21/n	Mo Kα radiation λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 2050 reflections
a = 6.639 (2) Å	θ = 2.8–27.5º
b = 13.788 (5) Å	µ = 0.86 mm−1
c = 8.771 (3) Å	T = 293 (2) K
β = 90.01 (5)º	Prism, colorless
V = 802.9 (4) Å3	0.20 × 0.12 × 0.12 mm
Z = 2

Rigaku Mercury2) diffractometer	1836 independent reflections
Radiation source: fine-focus sealed tube	1550 reflections with I > 2σ(I)
Monochromator: graphite	Rint = 0.057
Detector resolution: 13.6612 pixels mm-1	θmax = 27.5º
T = 293(2) K	θmin = 3.0º
CCD_Profile_fitting scans	h = −8→8
Absorption correction: multi-scan(CrystalClear; Rigaku, 2005)	k = −17→17
Tmin = 0.802, Tmax = 1.000	l = −11→11
8070 measured reflections

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)] = 0.058	H-atom parameters constrained
wR(F2) = 0.173	w = 1/[σ2(Fo2) + (0.0834P)2 + 0.8368P] where P = (Fo2 + 2Fc2)/3
S = 1.13	(Δ/σ)max < 0.001
1836 reflections	Δρmax = 0.39 e Å−3
124 parameters	Δρmin = −0.73 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
Mn1	0.0000	1.0000	1.0000	0.0261 (3)
N5	0.4367 (4)	0.7962 (2)	0.8387 (3)	0.0354 (7)
O1	0.2353 (4)	1.10029 (18)	0.9172 (3)	0.0382 (6)
H1B	0.3241	1.1164	0.9997	0.057*
H1C	0.1730	1.1583	0.8792	0.057*
N3	0.1879 (4)	0.88112 (19)	0.9162 (3)	0.0299 (6)
C7	0.1284 (5)	0.8238 (2)	0.8048 (4)	0.0275 (7)
N2	0.3843 (4)	0.8625 (2)	0.9339 (3)	0.0346 (7)
N4	0.2778 (4)	0.7701 (2)	0.7545 (3)	0.0332 (6)
C6	−0.0793 (5)	0.8223 (2)	0.7415 (4)	0.0317 (7)
H6A	−0.1720	0.8028	0.8214	0.038*
H6B	−0.0860	0.7738	0.6614	0.038*
C5	−0.1465 (5)	0.9175 (2)	0.6782 (4)	0.0289 (7)
C4	−0.2173 (5)	0.9233 (3)	0.5316 (4)	0.0359 (8)
H4A	−0.2262	0.8677	0.4720	0.043*
C3	−0.2743 (6)	1.0105 (3)	0.4737 (4)	0.0371 (8)
H3A	−0.3202	1.0155	0.3738	0.045*
C2	−0.2628 (6)	1.0907 (3)	0.5649 (4)	0.0377 (8)
H2A	−0.3022	1.1513	0.5290	0.045*
C1	−0.1925 (5)	1.0797 (2)	0.7089 (4)	0.0340 (8)
H1A	−0.1832	1.1345	0.7704	0.041*
N1	−0.1363 (4)	0.99533 (17)	0.7671 (3)	0.0273 (6)

	U11	U22	U33	U12	U13	U23
Mn1	0.0329 (4)	0.0185 (4)	0.0270 (4)	0.0025 (2)	−0.0001 (3)	−0.0016 (2)
N5	0.0353 (15)	0.0297 (15)	0.0413 (16)	0.0058 (12)	−0.0018 (12)	−0.0047 (12)
O1	0.0381 (13)	0.0326 (13)	0.0439 (14)	−0.0103 (10)	−0.0061 (11)	0.0116 (11)
N3	0.0341 (15)	0.0230 (13)	0.0326 (14)	0.0049 (11)	−0.0004 (11)	−0.0030 (11)
C7	0.0324 (16)	0.0155 (13)	0.0345 (16)	0.0003 (11)	0.0025 (13)	−0.0007 (12)
N2	0.0328 (15)	0.0265 (14)	0.0446 (16)	0.0041 (11)	−0.0027 (12)	−0.0019 (12)
N4	0.0371 (15)	0.0253 (13)	0.0371 (16)	0.0054 (11)	−0.0003 (12)	−0.0037 (12)
C6	0.0339 (17)	0.0217 (15)	0.0395 (17)	−0.0018 (12)	−0.0022 (14)	−0.0058 (13)
C5	0.0271 (15)	0.0245 (15)	0.0349 (17)	−0.0007 (12)	−0.0006 (13)	−0.0032 (13)
C4	0.0334 (17)	0.0372 (19)	0.0373 (18)	0.0010 (14)	−0.0045 (14)	−0.0081 (15)
C3	0.0299 (18)	0.051 (2)	0.0303 (17)	−0.0013 (14)	−0.0013 (14)	0.0029 (15)
C2	0.0399 (19)	0.0357 (18)	0.0376 (18)	0.0039 (15)	−0.0015 (15)	0.0079 (15)
C1	0.0417 (19)	0.0246 (16)	0.0357 (17)	0.0038 (13)	0.0001 (14)	0.0003 (13)
N1	0.0289 (14)	0.0239 (14)	0.0291 (14)	0.0009 (9)	0.0012 (11)	0.0003 (10)

Mn1—N3	2.187 (5)	C6—H6A	0.9700
Mn1—O1	2.209 (5)	C6—H6B	0.9700
Mn1—N1	2.235 (3)	C5—N1	1.328 (5)
N5—N2	1.286 (5)	C5—C4	1.371 (6)
N5—N4	1.337 (5)	C4—C3	1.359 (6)
O1—H1B	0.9600	C4—H4A	0.9300
O1—H1C	0.9600	C3—C2	1.367 (6)
N3—C7	1.317 (5)	C3—H3A	0.9300
N3—N2	1.338 (6)	C2—C1	1.355 (6)
C7—N4	1.314 (5)	C2—H2A	0.9300
C7—C6	1.487 (6)	C1—N1	1.324 (5)
C6—C5	1.494 (6)	C1—H1A	0.9300
N3—Mn1—O1	87.43 (11)	C7—C6—H6B	108.8
N3i—Mn1—O1	92.57 (5)	C5—C6—H6B	108.8
N3—Mn1—N1	84.39 (17)	H6A—C6—H6B	107.7
N3i—Mn1—N1	95.61 (17)	N1—C5—C4	121.4 (3)
O1i—Mn1—N1	89.79 (18)	N1—C5—C6	118.5 (4)
O1—Mn1—N1	90.21 (18)	C4—C5—C6	120.1 (3)
N2—N5—N4	109.6 (3)	C3—C4—C5	119.9 (3)
Mn1—O1—H1B	109.3	C3—C4—H4A	120.1
Mn1—O1—H1C	109.3	C5—C4—H4A	120.1
H1B—O1—H1C	109.5	C4—C3—C2	118.8 (4)
C7—N3—N2	105.3 (3)	C4—C3—H3A	120.6
C7—N3—Mn1	121.9 (3)	C2—C3—H3A	120.6
N2—N3—Mn1	131.4 (2)	C1—C2—C3	118.3 (4)
N3—C7—N4	111.1 (3)	C1—C2—H2A	120.9
N3—C7—C6	124.3 (3)	C3—C2—H2A	120.9
N4—C7—C6	124.5 (3)	N1—C1—C2	123.7 (3)
N5—N2—N3	109.0 (3)	N1—C1—H1A	118.2
C7—N4—N5	105.0 (3)	C2—C1—H1A	118.2
C7—C6—C5	113.8 (3)	C1—N1—C5	118.0 (4)
C7—C6—H6A	108.8	C1—N1—Mn1	116.2 (2)
C5—C6—H6A	108.8	C5—N1—Mn1	125.5 (2)
O1i—Mn1—N3—C7	64.4 (3)	C7—C6—C5—C4	125.9 (3)
O1—Mn1—N3—C7	−115.6 (3)	N1—C5—C4—C3	1.5 (5)
N1—Mn1—N3—C7	−25.2 (3)	C6—C5—C4—C3	−178.6 (3)
O1i—Mn1—N3—N2	−131.9 (3)	C5—C4—C3—C2	−1.1 (6)
O1—Mn1—N3—N2	48.1 (3)	C4—C3—C2—C1	0.8 (6)
N1—Mn1—N3—N2	138.5 (3)	C3—C2—C1—N1	−0.8 (6)
N1i—Mn1—N3—N2	−41.5 (3)	C2—C1—N1—C5	1.1 (5)
N2—N3—C7—N4	0.8 (4)	C2—C1—N1—Mn1	174.6 (3)
Mn1—N3—C7—N4	168.2 (2)	C4—C5—N1—C1	−1.5 (5)
N2—N3—C7—C6	−177.6 (3)	C6—C5—N1—C1	178.7 (3)
Mn1—N3—C7—C6	−10.2 (4)	C4—C5—N1—Mn1	−174.3 (2)
N4—N5—N2—N3	0.7 (4)	C6—C5—N1—Mn1	5.9 (4)
C7—N3—N2—N5	−0.9 (4)	N3—Mn1—N1—C1	−145.1 (3)
Mn1—N3—N2—N5	−166.6 (2)	N3i—Mn1—N1—C1	34.9 (3)
N3—C7—N4—N5	−0.3 (4)	O1i—Mn1—N1—C1	122.3 (3)
C6—C7—N4—N5	178.0 (3)	O1—Mn1—N1—C1	−57.7 (3)
N2—N5—N4—C7	−0.3 (4)	N3—Mn1—N1—C5	27.8 (3)
N3—C7—C6—C5	59.0 (5)	N3i—Mn1—N1—C5	−152.2 (3)
N4—C7—C6—C5	−119.2 (4)	O1i—Mn1—N1—C5	−64.8 (3)
C7—C6—C5—N1	−54.2 (4)	O1—Mn1—N1—C5	115.2 (3)

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1B···N2ii	0.96	2.04	2.889 (8)	146
O1—H1B···N5ii	0.96	2.45	3.371 (8)	162
O1—H1C···N4iii	0.96	1.96	2.786 (8)	142
C6—H6A···N5iv	0.97	2.60	3.343 (5)	133

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1—H1B⋯N2i	0.96	2.04	2.889 (8)	146
O1—H1B⋯N5i	0.96	2.45	3.371 (8)	162
O1—H1C⋯N4ii	0.96	1.96	2.786 (8)	142
C6—H6A⋯N5iii	0.97	2.60	3.343 (5)	133

Symmetry codes: (i) ; (ii) ; (iii) .