Diaqua-bis(tetra-zolo[1,5-a]pyridine-8-carboxyl-ato-κN,O)manganese(II) dihydrate.

In the title compound, [Mn(C(6)H(3)N(4)O(2))(2)(H(2)O)(2)]·2H(2)O, the Mn(II) atom is located on a twofold rotation axis and is octa-hedrally coordinated by the N and O atoms of the chelating tetra-zolo[1,5-a]pyridine-8-carboxyl-ate anions and the O atoms of two water mol-ecules. Hydrogen bonds of the O-H⋯O and O-H⋯N types lead to the formation of layers parallel to (100).

Related literature

For background to coordination compounds, see: Kulynych & Shimizu (2002 ▶); Liu et al. (2001 ▶); Xue & Liu (2009 ▶).

Experimental

Crystal data

[Mn(C6H3N4O2)2(H2O)2]·2H2O

M = 453.25

Orthorhombic,

a = 19.041 (4) Å

b = 11.694 (2) Å

c = 7.5371 (15) Å

V = 1678.3 (6) Å3

Z = 4

Mo Kα radiation

μ = 0.85 mm−1

T = 293 K

0.5 × 0.5 × 0.5 mm

Data collection

Rigaku SCXmini diffractometer

Absorption correction: multi-scan (ABSCOR; Higashi, 1995 ▶) T min = 0.60, T max = 0.662

16422 measured reflections

1925 independent reflections

1755 reflections with I > 2σ(I)

R int = 0.029

Refinement

R[F 2 > 2σ(F 2)] = 0.032

wR(F 2) = 0.081

S = 1.20

1925 reflections

132 parameters

H-atom parameters constrained

Δρmax = 0.26 e Å−3

Δρmin = −0.34 e Å−3

Data collection: SCXmini (Rigaku, 2006 ▶); cell refinement: PROCESS-AUTO (Rigaku, 1998 ▶); data reduction: PROCESS-AUTO; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: ORTEPIII (Burnett & Johnson, 1996 ▶), ORTEP-3 for Windows (Farrugia, 1997 ▶) and PLATON (Spek, 2009 ▶); software used to prepare material for publication: SHELXTL (Sheldrick, 2008 ▶).

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536809023253/dn2463sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809023253/dn2463Isup2.hkl

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

[Mn(C6H3N4O2)2(H2O)2]·2H2O	F(000) = 924
Mr = 453.25	Dx = 1.794 Mg m−3
Orthorhombic, Pnna	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2a 2bc	Cell parameters from 15650 reflections
a = 19.041 (4) Å	θ = 3.2–27.9°
b = 11.694 (2) Å	µ = 0.85 mm−1
c = 7.5371 (15) Å	T = 293 K
V = 1678.3 (6) Å3	Block, yellow
Z = 4	0.5 × 0.5 × 0.5 mm

Rigaku SCXmini diffractometer	1925 independent reflections
Radiation source: fine-focus sealed tube	1755 reflections with I > 2σ(I)
graphite	Rint = 0.029
ω scans	θmax = 27.5°, θmin = 3.2°
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	h = −24→24
Tmin = 0.60, Tmax = 0.662	k = −15→15
16422 measured reflections	l = −9→9

Refinement on F2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.032	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.081	H-atom parameters constrained
S = 1.20	w = 1/[σ2(Fo2) + (0.0386P)2 + 0.6168P] where P = (Fo2 + 2Fc2)/3
1925 reflections	(Δ/σ)max = 0.001
132 parameters	Δρmax = 0.26 e Å−3
0 restraints	Δρmin = −0.34 e Å−3

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 > 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	0.2500	0.0000	0.86700 (4)	0.01925 (12)
O1	0.19724 (6)	0.09901 (10)	0.66846 (16)	0.0263 (3)
O1W	0.21023 (6)	0.11467 (10)	1.06874 (17)	0.0294 (3)
H11	0.1888	0.1746	1.0359	0.044*
H12	0.2351	0.1270	1.1599	0.044*
O2	0.12016 (6)	0.21215 (10)	0.53402 (17)	0.0306 (3)
N1	0.14757 (7)	−0.09265 (11)	0.85974 (18)	0.0233 (3)
N2	0.12692 (8)	−0.18779 (12)	0.9450 (2)	0.0279 (3)
N3	0.05962 (8)	−0.20081 (12)	0.9411 (2)	0.0285 (3)
N4	0.03454 (7)	−0.10924 (11)	0.84998 (17)	0.0212 (3)
C1	0.13563 (9)	0.13028 (13)	0.6301 (2)	0.0201 (3)
C2	0.07619 (8)	0.05909 (13)	0.7039 (2)	0.0194 (3)
C3	0.00732 (9)	0.08539 (14)	0.6756 (2)	0.0244 (3)
H3	−0.0036	0.1528	0.6161	0.029*
C4	−0.04836 (9)	0.01396 (14)	0.7335 (2)	0.0276 (4)
H4	−0.0946	0.0355	0.7122	0.033*
C5	−0.03481 (9)	−0.08466 (15)	0.8190 (2)	0.0261 (4)
H5	−0.0706	−0.1336	0.8551	0.031*
C6	0.08933 (8)	−0.04294 (13)	0.7994 (2)	0.0185 (3)
O2W	0.28824 (7)	0.12927 (11)	0.37555 (17)	0.0354 (3)
H21	0.2590	0.1132	0.4635	0.053*
H22	0.3103	0.1791	0.4079	0.053*

	U11	U22	U33	U12	U13	U23
Mn1	0.01548 (18)	0.02138 (19)	0.02089 (19)	0.00086 (12)	0.000	0.000
O1	0.0199 (6)	0.0302 (6)	0.0287 (6)	−0.0007 (5)	−0.0003 (5)	0.0108 (5)
O1W	0.0325 (7)	0.0280 (6)	0.0277 (6)	0.0091 (5)	−0.0033 (5)	−0.0048 (5)
O2	0.0297 (6)	0.0260 (6)	0.0362 (7)	−0.0035 (5)	−0.0053 (6)	0.0141 (5)
N1	0.0222 (7)	0.0181 (6)	0.0295 (7)	−0.0005 (5)	−0.0016 (5)	0.0066 (5)
N2	0.0295 (7)	0.0215 (7)	0.0326 (8)	−0.0017 (6)	0.0003 (6)	0.0083 (6)
N3	0.0312 (8)	0.0219 (7)	0.0324 (8)	−0.0038 (6)	0.0002 (6)	0.0079 (6)
N4	0.0215 (7)	0.0194 (6)	0.0226 (7)	−0.0044 (5)	0.0011 (5)	0.0018 (5)
C1	0.0230 (8)	0.0190 (7)	0.0185 (7)	−0.0021 (6)	−0.0002 (6)	0.0016 (6)
C2	0.0224 (8)	0.0175 (7)	0.0183 (7)	−0.0011 (6)	0.0004 (6)	0.0007 (6)
C3	0.0248 (8)	0.0245 (8)	0.0239 (8)	0.0018 (6)	−0.0025 (6)	0.0016 (6)
C4	0.0171 (7)	0.0369 (9)	0.0289 (9)	0.0015 (7)	−0.0009 (7)	−0.0018 (7)
C5	0.0178 (8)	0.0326 (9)	0.0279 (8)	−0.0068 (7)	0.0027 (7)	−0.0021 (7)
C6	0.0177 (7)	0.0187 (7)	0.0190 (7)	−0.0023 (6)	0.0001 (6)	−0.0003 (6)
O2W	0.0383 (8)	0.0386 (7)	0.0293 (7)	−0.0081 (6)	0.0032 (5)	−0.0043 (5)

Mn1—O1	2.1422 (12)	N3—N4	1.3588 (19)
Mn1—O1i	2.1422 (12)	N4—C6	1.3546 (19)
Mn1—O1W	2.1642 (12)	N4—C5	1.372 (2)
Mn1—O1Wi	2.1642 (12)	C1—C2	1.511 (2)
Mn1—N1	2.2317 (14)	C2—C3	1.364 (2)
Mn1—N1i	2.2317 (14)	C2—C6	1.416 (2)
O1—C1	1.262 (2)	C3—C4	1.418 (2)
O1W—H11	0.8477	C3—H3	0.9300
O1W—H12	0.8471	C4—C5	1.346 (2)
O2—C1	1.2362 (19)	C4—H4	0.9300
N1—C6	1.332 (2)	C5—H5	0.9300
N1—N2	1.3438 (19)	O2W—H21	0.8853
N2—N3	1.291 (2)	O2W—H22	0.7585
O1—Mn1—O1i	91.38 (7)	N2—N3—N4	105.51 (12)
O1—Mn1—O1W	89.53 (5)	C6—N4—N3	108.82 (13)
O1i—Mn1—O1W	171.80 (5)	C6—N4—C5	125.01 (14)
O1—Mn1—O1Wi	171.80 (5)	N3—N4—C5	126.13 (14)
O1i—Mn1—O1Wi	89.53 (5)	O2—C1—O1	125.44 (15)
O1W—Mn1—O1Wi	90.73 (7)	O2—C1—C2	117.64 (14)
O1—Mn1—N1	80.53 (5)	O1—C1—C2	116.89 (13)
O1i—Mn1—N1	97.49 (5)	C3—C2—C6	116.08 (14)
O1W—Mn1—N1	90.70 (5)	C3—C2—C1	122.57 (14)
O1Wi—Mn1—N1	91.27 (5)	C6—C2—C1	121.27 (14)
O1—Mn1—N1i	97.49 (5)	C2—C3—C4	122.53 (15)
O1i—Mn1—N1i	80.53 (5)	C2—C3—H3	118.7
O1W—Mn1—N1i	91.27 (5)	C4—C3—H3	118.7
O1Wi—Mn1—N1i	90.70 (5)	C5—C4—C3	120.56 (16)
N1—Mn1—N1i	177.19 (7)	C5—C4—H4	119.7
C1—O1—Mn1	138.78 (10)	C3—C4—H4	119.7
Mn1—O1W—H11	118.4	C4—C5—N4	116.47 (15)
Mn1—O1W—H12	118.7	C4—C5—H5	121.8
H11—O1W—H12	111.4	N4—C5—H5	121.8
C6—N1—N2	106.31 (13)	N1—C6—N4	107.18 (13)
C6—N1—Mn1	121.61 (10)	N1—C6—C2	133.50 (14)
N2—N1—Mn1	130.24 (11)	N4—C6—C2	119.29 (14)
N3—N2—N1	112.16 (13)	H21—O2W—H22	105.7

D—H···A	D—H	H···A	D···A	D—H···A
O1W—H11···O2ii	0.85	1.93	2.7644 (17)	166
O1W—H12···O2Wiii	0.85	1.91	2.7538 (19)	171
O2W—H21···O1	0.89	1.95	2.8287 (18)	172
O2W—H22···N2iv	0.76	2.25	3.003 (2)	169

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1W—H11⋯O2i	0.85	1.93	2.7644 (17)	166
O1W—H12⋯O2Wii	0.85	1.91	2.7538 (19)	171
O2W—H21⋯O1	0.89	1.95	2.8287 (18)	172
O2W—H22⋯N2iii	0.76	2.25	3.003 (2)	169

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