Tetra-aqua-bis-[5-(pyridin-3-yl)tetra-zolido-κN⁵]manganese(II) tetra-hydrate.

The title compound, [Mn(C₆H₄N₅)₂(H₂O)₄]·4H₂O, was obtained by the solution reaction of MnCl₂ and 3-(2H-tetra-zol-5-yl)pyridine. The Mn(II) atom, located on an inversion center, shows a slightly distorted octa-hedral geometry and is coordinated by two pyridine N atoms from two 5-(pyridin-3-yl)tetra-zolide ligands occupying trans positions and four water mol-ecules. In the crystal, the mononuclear complex mol-ecules and solvent water mol-ecules are connected into a three-dimensional framework by O-H⋯N and O-H⋯O hydrogen bonds.

Related literature

For the synthesis and crystal structure of the isotypic zinc(II) complex [Zn(C6H4N5)2(H2O)4]·4H2O, see: Mu et al. (2010 ▶).

Experimental

Crystal data

[Mn(C6H4N5)2(H2O)4]·4H2O

M = 491.35

Triclinic,

a = 8.137 (8) Å

b = 8.629 (8) Å

c = 8.761 (8) Å

α = 84.878 (10)°

β = 65.347 (8)°

γ = 72.571 (10)°

V = 533.0 (9) Å3

Z = 1

Mo Kα radiation

μ = 0.68 mm−1

T = 293 K

0.15 × 0.10 × 0.10 mm

Data collection

Bruker APEXII CCD diffractometer

Absorption correction: multi-scan (SADABS; Sheldrick, 2007 ▶) T min = 0.922, T max = 0.934

2785 measured reflections

1850 independent reflections

1712 reflections with I > 2σ(I)

R int = 0.026

Refinement

R[F 2 > 2σ(F 2)] = 0.032

wR(F 2) = 0.080

S = 1.05

1850 reflections

143 parameters

H-atom parameters constrained

Δρmax = 0.23 e Å−3

Δρmin = −0.32 e Å−3

Data collection: APEX2 (Bruker, 2000 ▶); cell refinement: SAINT (Bruker, 2000 ▶); data reduction: SAINT; 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 datablock(s) I, global. DOI: 10.1107/S160053681202510X/gk2497sup1.cif

Structure factors: contains datablock(s) I. DOI: 10.1107/S160053681202510X/gk2497Isup2.hkl

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

[Mn(C6H4N5)2(H2O)4]·4H2O	Z = 1
Mr = 491.35	F(000) = 255
Triclinic, P1	Dx = 1.531 Mg m−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 8.137 (8) Å	Cell parameters from 1565 reflections
b = 8.629 (8) Å	θ = 2.5–27.3°
c = 8.761 (8) Å	µ = 0.68 mm−1
α = 84.878 (10)°	T = 293 K
β = 65.347 (8)°	Block, yellow
γ = 72.571 (10)°	0.15 × 0.10 × 0.10 mm
V = 533.0 (9) Å3

Bruker APEXII CCD diffractometer	1850 independent reflections
Radiation source: fine-focus sealed tube	1712 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.026
phi and ω scans	θmax = 25.0°, θmin = 2.5°
Absorption correction: multi-scan (SADABS; Sheldrick, 2007)	h = −7→9
Tmin = 0.922, Tmax = 0.934	k = −6→10
2785 measured reflections	l = −10→10

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)] = 0.032	H-atom parameters constrained
wR(F2) = 0.080	w = 1/[σ2(Fo2) + (0.0343P)2 + 0.2064P] where P = (Fo2 + 2Fc2)/3
S = 1.05	(Δ/σ)max < 0.001
1850 reflections	Δρmax = 0.23 e Å−3
143 parameters	Δρmin = −0.32 e Å−3
0 restraints	Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.063 (6)

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
C1	0.4972 (3)	0.8406 (3)	0.1955 (2)	0.0309 (5)
H1	0.3863	0.8330	0.2844	0.037*
C2	0.5378 (3)	0.7784 (2)	0.0396 (2)	0.0250 (4)
C3	0.7038 (3)	0.7881 (3)	−0.0919 (2)	0.0312 (4)
H3	0.7369	0.7485	−0.1993	0.037*
C4	0.8196 (3)	0.8579 (3)	−0.0606 (3)	0.0367 (5)
H4	0.9326	0.8647	−0.1468	0.044*
C5	0.7665 (3)	0.9175 (2)	0.0990 (3)	0.0313 (4)
H5	0.8457	0.9643	0.1180	0.038*
C6	0.4027 (3)	0.7086 (2)	0.0214 (2)	0.0253 (4)
Mn1	0.5000	1.0000	0.5000	0.02565 (17)
N1	0.6059 (2)	0.9108 (2)	0.22757 (19)	0.0291 (4)
N2	0.2536 (2)	0.6822 (2)	0.1516 (2)	0.0316 (4)
N3	0.1654 (2)	0.6214 (2)	0.0825 (2)	0.0345 (4)
N4	0.2572 (2)	0.6120 (2)	−0.0813 (2)	0.0335 (4)
N5	0.4088 (2)	0.6669 (2)	−0.12397 (19)	0.0293 (4)
O1	0.4248 (2)	1.25174 (18)	0.44974 (18)	0.0465 (4)
H1B	0.3486	1.3288	0.5213	0.056*
H1A	0.4587	1.2950	0.3548	0.056*
O2	0.79389 (19)	0.99831 (18)	0.44105 (18)	0.0364 (4)
H2A	0.8730	0.9173	0.4589	0.044*
H2B	0.8229	1.0820	0.4526	0.044*
O3	0.0823 (2)	0.75323 (18)	0.49811 (18)	0.0372 (4)
H3B	0.0942	0.6696	0.5562	0.045*
H3A	0.1346	0.7196	0.3958	0.045*
O4	0.1519 (2)	0.48719 (18)	0.69383 (17)	0.0359 (4)
H4B	0.0608	0.4519	0.7598	0.043*
H4A	0.1855	0.5271	0.7575	0.043*

	U11	U22	U33	U12	U13	U23
C1	0.0302 (10)	0.0403 (11)	0.0217 (10)	−0.0155 (9)	−0.0058 (8)	−0.0023 (8)
C2	0.0279 (10)	0.0230 (9)	0.0239 (10)	−0.0064 (8)	−0.0108 (8)	−0.0002 (7)
C3	0.0317 (10)	0.0378 (11)	0.0216 (10)	−0.0100 (9)	−0.0071 (8)	−0.0061 (8)
C4	0.0286 (10)	0.0506 (13)	0.0277 (11)	−0.0162 (10)	−0.0043 (8)	−0.0034 (9)
C5	0.0277 (10)	0.0374 (11)	0.0320 (11)	−0.0116 (8)	−0.0134 (8)	−0.0010 (9)
C6	0.0292 (10)	0.0226 (9)	0.0234 (10)	−0.0065 (8)	−0.0104 (8)	−0.0011 (7)
Mn1	0.0264 (2)	0.0299 (3)	0.0210 (2)	−0.00911 (17)	−0.00862 (17)	−0.00332 (16)
N1	0.0311 (9)	0.0351 (9)	0.0230 (8)	−0.0125 (7)	−0.0105 (7)	−0.0017 (7)
N2	0.0307 (9)	0.0386 (10)	0.0264 (9)	−0.0142 (7)	−0.0091 (7)	−0.0018 (7)
N3	0.0341 (9)	0.0405 (10)	0.0320 (9)	−0.0165 (8)	−0.0122 (7)	−0.0018 (8)
N4	0.0370 (9)	0.0370 (10)	0.0314 (9)	−0.0153 (8)	−0.0152 (8)	−0.0008 (7)
N5	0.0348 (9)	0.0320 (9)	0.0237 (9)	−0.0141 (7)	−0.0109 (7)	−0.0014 (7)
O1	0.0623 (10)	0.0321 (8)	0.0252 (8)	−0.0059 (7)	−0.0044 (7)	0.0003 (6)
O2	0.0302 (7)	0.0385 (8)	0.0429 (9)	−0.0084 (6)	−0.0166 (6)	−0.0071 (6)
O3	0.0407 (8)	0.0377 (8)	0.0292 (8)	−0.0113 (7)	−0.0100 (6)	−0.0011 (6)
O4	0.0401 (8)	0.0413 (8)	0.0273 (8)	−0.0177 (7)	−0.0094 (6)	−0.0044 (6)

C1—N1	1.337 (3)	Mn1—O2i	2.222 (3)
C1—C2	1.382 (3)	Mn1—O2	2.222 (3)
C1—H1	0.9300	Mn1—N1	2.290 (3)
C2—C3	1.383 (3)	Mn1—N1i	2.290 (3)
C2—C6	1.468 (3)	N2—N3	1.342 (2)
C3—C4	1.382 (3)	N3—N4	1.309 (3)
C3—H3	0.9300	N4—N5	1.349 (3)
C4—C5	1.377 (3)	O1—H1B	0.8500
C4—H4	0.9300	O1—H1A	0.8500
C5—N1	1.336 (3)	O2—H2A	0.8500
C5—H5	0.9300	O2—H2B	0.8501
C6—N5	1.331 (3)	O3—H3B	0.8500
C6—N2	1.338 (3)	O3—H3A	0.8501
Mn1—O1	2.132 (2)	O4—H4B	0.8500
Mn1—O1i	2.132 (2)	O4—H4A	0.8501
N1—C1—C2	124.70 (17)	O1—Mn1—N1	95.02 (7)
N1—C1—H1	117.6	O1i—Mn1—N1	84.98 (7)
C2—C1—H1	117.6	O2i—Mn1—N1	92.50 (6)
C1—C2—C3	117.48 (18)	O2—Mn1—N1	87.50 (6)
C1—C2—C6	118.90 (17)	O1—Mn1—N1i	84.98 (7)
C3—C2—C6	123.61 (18)	O1i—Mn1—N1i	95.02 (7)
C4—C3—C2	118.66 (19)	O2i—Mn1—N1i	87.50 (5)
C4—C3—H3	120.7	O2—Mn1—N1i	92.50 (6)
C2—C3—H3	120.7	N1—Mn1—N1i	179.999 (1)
C5—C4—C3	119.62 (19)	C5—N1—C1	116.74 (18)
C5—C4—H4	120.2	C5—N1—Mn1	127.06 (13)
C3—C4—H4	120.2	C1—N1—Mn1	116.17 (13)
N1—C5—C4	122.78 (19)	C6—N2—N3	104.94 (17)
N1—C5—H5	118.6	N4—N3—N2	109.54 (17)
C4—C5—H5	118.6	N3—N4—N5	109.28 (15)
N5—C6—N2	111.27 (17)	C6—N5—N4	104.97 (15)
N5—C6—C2	125.30 (17)	Mn1—O1—H1B	126.3
N2—C6—C2	123.42 (17)	Mn1—O1—H1A	127.6
O1—Mn1—O1i	180.0	H1B—O1—H1A	106.1
O1—Mn1—O2i	88.59 (7)	Mn1—O2—H2A	122.5
O1i—Mn1—O2i	91.41 (7)	Mn1—O2—H2B	123.2
O1—Mn1—O2	91.41 (7)	H2A—O2—H2B	106.1
O1i—Mn1—O2	88.59 (7)	H3B—O3—H3A	106.7
O2i—Mn1—O2	180.000 (1)	H4B—O4—H4A	105.2

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1B···O4ii	0.85	1.94	2.783 (3)	172
O1—H1A···N5iii	0.85	1.91	2.731 (3)	163
O2—H2A···O3iv	0.85	1.99	2.836 (3)	171
O2—H2B···O3i	0.85	1.96	2.800 (3)	169
O3—H3B···O4	0.85	1.96	2.803 (3)	171
O3—H3A···N2	0.85	1.96	2.797 (3)	170
O4—H4B···N3v	0.85	2.03	2.878 (3)	177
O4—H4A···N4vi	0.85	2.00	2.849 (3)	176

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1—H1B⋯O4i	0.85	1.94	2.783 (3)	172
O1—H1A⋯N5ii	0.85	1.91	2.731 (3)	163
O2—H2A⋯O3iii	0.85	1.99	2.836 (3)	171
O2—H2B⋯O3iv	0.85	1.96	2.800 (3)	169
O3—H3B⋯O4	0.85	1.96	2.803 (3)	171
O3—H3A⋯N2	0.85	1.96	2.797 (3)	170
O4—H4B⋯N3v	0.85	2.03	2.878 (3)	177
O4—H4A⋯N4vi	0.85	2.00	2.849 (3)	176

Symmetry codes: (i) ; (ii) ; (iii) ; (iv) ; (v) ; (vi) .