Penta-aqua-[5,5'-(m-phenylene)ditetra-zolato-κN]manganese(II) dihydrate.

The title compound, [Mn(C(8)H(4)N(8))(2)(H(2)O)(5)]·2H(2)O, is the fourth transition metal complex containing the 1,3-di(2H-tetra-zol-5-yl)benzene ligand to be structurally characterized. The Mn^II^ cation has a distorted octahedral coordination geometry. The 1,3-di(tetra-zol-5-yl)benzene ligand is planar. All H atoms bonded to O atoms participate in hydrogen bonds, which link the mol-ecules into a framework structure.

Related literature

For similar complexes, see: Jiang et al. (2004 ▶); Hill et al. (1996 ▶).

Experimental

Crystal data

[Mn(C8H4N8)2(H2O)5]·2H2O

M = 393.24

Triclinic,

a = 6.5932 (1) Å

b = 10.0711 (2) Å

c = 12.9857 (3) Å

α = 68.296 (1)°

β = 77.213 (3)°

γ = 77.280 (5)°

V = 772.10 (3) Å3

Z = 2

Mo Kα radiation

μ = 0.91 mm−1

T = 296 (2) K

0.26 × 0.14 × 0.08 mm

Data collection

Bruker SMART CCD area-detector diffractometer

Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T min = 0.798, T max = 0.931

7710 measured reflections

3704 independent reflections

2846 reflections with I > 2σ(I)

R int = 0.022

Refinement

R[F 2 > 2σ(F 2)] = 0.038

wR(F 2) = 0.095

S = 1.02

3704 reflections

273 parameters

H atoms treated by a mixture of independent and constrained refinement

Δρmax = 0.36 e Å−3

Δρmin = −0.30 e Å−3

Data collection: SMART (Bruker, 2007 ▶); cell refinement: SMART; data reduction: SAINT-Plus (Bruker, 2007 ▶); 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. DOI: 10.1107/S1600536808028316/ez2139sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808028316/ez2139Isup2.hkl

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

[Mn(C8H4N8)2(H2O)5]·2H2O	Z = 2
Mr = 393.24	F(000) = 406
Triclinic, P1	Dx = 1.691 Mg m−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 6.5932 (1) Å	Cell parameters from 3628 reflections
b = 10.0711 (2) Å	θ = 2.7–27.9°
c = 12.9857 (3) Å	µ = 0.91 mm−1
α = 68.296 (1)°	T = 296 K
β = 77.213 (3)°	Plate, yellow
γ = 77.280 (5)°	0.26 × 0.14 × 0.08 mm
V = 772.10 (3) Å3

Bruker SMART CCD area-detector diffractometer	3704 independent reflections
Radiation source: fine-focus sealed tube	2846 reflections with I > 2σ(I)
graphite	Rint = 0.022
φ and ω scans	θmax = 28.1°, θmin = 1.7°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −8→6
Tmin = 0.798, Tmax = 0.931	k = −13→13
7710 measured reflections	l = −17→17

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)] = 0.038	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.095	H atoms treated by a mixture of independent and constrained refinement
S = 1.02	w = 1/[σ2(Fo2) + (0.0414P)2 + 0.3671P] where P = (Fo2 + 2Fc2)/3
3704 reflections	(Δ/σ)max = 0.001
273 parameters	Δρmax = 0.36 e Å−3
0 restraints	Δρmin = −0.30 e Å−3

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	0.11390 (6)	0.68638 (4)	0.58413 (3)	0.02732 (12)
O1	0.3923 (3)	0.7734 (2)	0.57901 (16)	0.0388 (4)
O2	−0.1155 (4)	0.8808 (2)	0.58408 (19)	0.0402 (5)
O3	0.0794 (3)	0.6043 (2)	0.76359 (15)	0.0361 (4)
O4	−0.1679 (4)	0.6027 (2)	0.59456 (18)	0.0411 (5)
O5	0.3064 (5)	0.4784 (2)	0.5795 (2)	0.0508 (6)
O6	0.2643 (3)	0.5392 (2)	0.12086 (18)	0.0370 (4)
O7	0.6605 (4)	0.3559 (3)	0.11514 (17)	0.0367 (4)
N1	0.1613 (3)	0.90491 (19)	0.31988 (14)	0.0244 (4)
N2	0.1633 (3)	0.76902 (19)	0.39242 (14)	0.0264 (4)
N3	0.1980 (3)	0.6792 (2)	0.33621 (15)	0.0300 (4)
N4	0.2200 (3)	0.75287 (19)	0.22651 (15)	0.0268 (4)
N5	0.3286 (3)	0.9471 (2)	−0.21040 (15)	0.0276 (4)
N6	0.3651 (3)	0.9732 (2)	−0.32077 (16)	0.0315 (4)
N7	0.3610 (3)	1.1128 (2)	−0.37435 (16)	0.0318 (4)
N8	0.3223 (3)	1.1812 (2)	−0.29911 (15)	0.0275 (4)
C1	0.1974 (3)	0.8914 (2)	0.21865 (17)	0.0205 (4)
C2	0.2128 (3)	1.0130 (2)	0.11148 (17)	0.0216 (4)
C3	0.2001 (4)	1.1526 (2)	0.11091 (19)	0.0306 (5)
H3	0.1796	1.1699	0.1783	0.037*
C4	0.2177 (4)	1.2662 (2)	0.0105 (2)	0.0380 (6)
H4	0.2077	1.3597	0.0105	0.046*
C5	0.2501 (4)	1.2411 (2)	−0.09028 (19)	0.0311 (5)
H5	0.2627	1.3178	−0.1576	0.037*
C6	0.2640 (3)	1.1024 (2)	−0.09143 (17)	0.0217 (4)
C7	0.2443 (3)	0.9883 (2)	0.00989 (17)	0.0214 (4)
H7	0.2523	0.8950	0.0098	0.026*
C8	0.3031 (3)	1.0766 (2)	−0.19900 (17)	0.0224 (4)
H1A	0.455 (5)	0.808 (3)	0.519 (3)	0.044 (9)*
H6A	0.254 (5)	0.602 (4)	0.148 (3)	0.053 (9)*
H4B	−0.180 (5)	0.511 (4)	0.613 (3)	0.063 (10)*
H7A	0.659 (5)	0.278 (4)	0.135 (3)	0.060 (12)*
H5B	0.306 (6)	0.402 (4)	0.620 (3)	0.068 (12)*
H1B	0.378 (5)	0.838 (4)	0.608 (3)	0.068 (11)*
H2B	−0.124 (5)	0.933 (4)	0.614 (3)	0.052 (10)*
H3B	−0.018 (5)	0.560 (3)	0.800 (3)	0.059 (10)*
H3A	0.149 (5)	0.615 (4)	0.806 (3)	0.065 (11)*
H4A	−0.261 (6)	0.645 (4)	0.597 (3)	0.076 (16)*
H2A	−0.179 (7)	0.908 (5)	0.539 (4)	0.105 (18)*
H6B	0.286 (8)	0.554 (5)	0.070 (4)	0.09 (2)*
H7B	0.588 (10)	0.394 (6)	0.126 (5)	0.11 (3)*
H5A	0.396 (10)	0.477 (7)	0.567 (5)	0.10 (3)*

	U11	U22	U33	U12	U13	U23
Mn1	0.0377 (2)	0.02288 (18)	0.02168 (18)	−0.00688 (14)	−0.00202 (14)	−0.00808 (13)
O1	0.0537 (12)	0.0406 (10)	0.0275 (9)	−0.0234 (9)	0.0075 (8)	−0.0164 (8)
O2	0.0540 (13)	0.0266 (9)	0.0423 (11)	0.0024 (8)	−0.0102 (10)	−0.0174 (9)
O3	0.0426 (11)	0.0429 (11)	0.0241 (9)	−0.0157 (9)	−0.0046 (8)	−0.0078 (8)
O4	0.0460 (13)	0.0253 (10)	0.0564 (13)	−0.0068 (9)	−0.0170 (10)	−0.0128 (9)
O5	0.0666 (16)	0.0254 (11)	0.0400 (12)	0.0045 (10)	0.0116 (11)	−0.0056 (9)
O6	0.0484 (11)	0.0342 (10)	0.0310 (10)	−0.0101 (8)	−0.0005 (9)	−0.0150 (8)
O7	0.0479 (12)	0.0276 (10)	0.0350 (10)	−0.0079 (9)	−0.0089 (8)	−0.0082 (8)
N1	0.0311 (10)	0.0217 (9)	0.0191 (8)	−0.0043 (7)	−0.0027 (7)	−0.0059 (7)
N2	0.0347 (10)	0.0215 (9)	0.0209 (9)	−0.0044 (8)	−0.0021 (8)	−0.0062 (7)
N3	0.0428 (12)	0.0239 (9)	0.0223 (9)	−0.0070 (8)	−0.0005 (8)	−0.0083 (7)
N4	0.0356 (11)	0.0240 (9)	0.0203 (9)	−0.0063 (8)	−0.0011 (8)	−0.0077 (7)
N5	0.0333 (10)	0.0258 (9)	0.0236 (9)	−0.0052 (8)	−0.0022 (8)	−0.0092 (8)
N6	0.0375 (11)	0.0343 (11)	0.0247 (10)	−0.0074 (9)	−0.0005 (8)	−0.0135 (8)
N7	0.0380 (11)	0.0333 (11)	0.0219 (9)	−0.0072 (9)	0.0009 (8)	−0.0088 (8)
N8	0.0338 (10)	0.0269 (10)	0.0193 (9)	−0.0048 (8)	0.0001 (8)	−0.0072 (7)
C1	0.0197 (10)	0.0214 (10)	0.0202 (10)	−0.0028 (8)	−0.0008 (8)	−0.0083 (8)
C2	0.0207 (10)	0.0219 (10)	0.0203 (10)	−0.0010 (8)	−0.0028 (8)	−0.0066 (8)
C3	0.0427 (14)	0.0259 (11)	0.0222 (11)	−0.0016 (10)	−0.0027 (10)	−0.0105 (9)
C4	0.0638 (18)	0.0197 (11)	0.0301 (12)	−0.0058 (11)	−0.0040 (12)	−0.0101 (9)
C5	0.0448 (14)	0.0199 (10)	0.0230 (11)	−0.0015 (10)	−0.0051 (10)	−0.0028 (9)
C6	0.0206 (10)	0.0238 (10)	0.0203 (10)	−0.0029 (8)	−0.0022 (8)	−0.0076 (8)
C7	0.0223 (10)	0.0186 (10)	0.0228 (10)	−0.0027 (8)	−0.0022 (8)	−0.0073 (8)
C8	0.0206 (10)	0.0235 (10)	0.0213 (10)	−0.0039 (8)	−0.0024 (8)	−0.0058 (8)

Mn1—O3	2.1423 (18)	N1—N2	1.343 (2)
Mn1—O4	2.162 (2)	N2—N3	1.314 (2)
Mn1—O1	2.1797 (19)	N3—N4	1.332 (2)
Mn1—O2	2.1946 (19)	N4—C1	1.338 (3)
Mn1—O5	2.212 (2)	N5—N6	1.333 (3)
Mn1—N2	2.2857 (17)	N5—C8	1.336 (3)
O1—H1A	0.78 (3)	N6—N7	1.315 (3)
O1—H1B	0.85 (4)	N7—N8	1.343 (3)
O2—H2B	0.75 (3)	N8—C8	1.338 (3)
O2—H2A	0.73 (5)	C1—C2	1.476 (3)
O3—H3B	0.82 (3)	C2—C3	1.387 (3)
O3—H3A	0.84 (4)	C2—C7	1.394 (3)
O4—H4B	0.88 (4)	C3—C4	1.382 (3)
O4—H4A	0.67 (4)	C3—H3	0.9300
O5—H5B	0.75 (4)	C4—C5	1.385 (3)
O5—H5A	0.57 (6)	C4—H4	0.9300
O6—H6A	0.82 (3)	C5—C6	1.385 (3)
O6—H6B	0.61 (5)	C5—H5	0.9300
O7—H7A	0.73 (4)	C6—C7	1.393 (3)
O7—H7B	0.57 (6)	C6—C8	1.472 (3)
N1—C1	1.335 (3)	C7—H7	0.9300
O3—Mn1—O4	88.99 (8)	N3—N2—N1	109.26 (16)
O3—Mn1—O1	89.37 (8)	N3—N2—Mn1	120.96 (13)
O4—Mn1—O1	177.83 (8)	N1—N2—Mn1	129.79 (13)
O3—Mn1—O2	92.33 (8)	N2—N3—N4	109.71 (17)
O4—Mn1—O2	81.61 (9)	N3—N4—C1	104.97 (17)
O1—Mn1—O2	97.05 (8)	N6—N5—C8	105.15 (17)
O3—Mn1—O5	89.42 (8)	N7—N6—N5	109.76 (17)
O4—Mn1—O5	90.03 (11)	N6—N7—N8	109.04 (17)
O1—Mn1—O5	91.36 (10)	C8—N8—N7	105.04 (18)
O2—Mn1—O5	171.42 (11)	N1—C1—N4	111.28 (17)
O3—Mn1—N2	177.82 (7)	N1—C1—C2	124.65 (18)
O4—Mn1—N2	92.24 (8)	N4—C1—C2	124.07 (18)
O1—Mn1—N2	89.44 (7)	C3—C2—C7	119.41 (19)
O2—Mn1—N2	89.63 (8)	C3—C2—C1	120.24 (19)
O5—Mn1—N2	88.78 (8)	C7—C2—C1	120.34 (18)
Mn1—O1—H1A	116 (2)	C4—C3—C2	120.2 (2)
Mn1—O1—H1B	118 (2)	C4—C3—H3	119.9
H1A—O1—H1B	102 (3)	C2—C3—H3	119.9
Mn1—O2—H2B	131 (3)	C3—C4—C5	120.2 (2)
Mn1—O2—H2A	115 (4)	C3—C4—H4	119.9
H2B—O2—H2A	113 (4)	C5—C4—H4	119.9
Mn1—O3—H3B	120 (2)	C6—C5—C4	120.4 (2)
Mn1—O3—H3A	129 (2)	C6—C5—H5	119.8
H3B—O3—H3A	110 (3)	C4—C5—H5	119.8
Mn1—O4—H4B	127 (2)	C5—C6—C7	119.31 (19)
Mn1—O4—H4A	119 (4)	C5—C6—C8	119.95 (19)
H4B—O4—H4A	113 (4)	C7—C6—C8	120.73 (18)
Mn1—O5—H5B	132 (3)	C6—C7—C2	120.44 (19)
Mn1—O5—H5A	117 (7)	C6—C7—H7	119.8
H5B—O5—H5A	99 (7)	C2—C7—H7	119.8
H6A—O6—H6B	119 (5)	N5—C8—N8	111.01 (18)
H7A—O7—H7B	120 (6)	N5—C8—C6	125.20 (18)
C1—N1—N2	104.79 (16)	N8—C8—C6	123.78 (19)
C1—N1—N2—N3	−0.3 (2)	N4—C1—C2—C3	−176.0 (2)
C1—N1—N2—Mn1	−179.63 (15)	N1—C1—C2—C7	−177.9 (2)
O4—Mn1—N2—N3	−62.82 (18)	N4—C1—C2—C7	2.7 (3)
O1—Mn1—N2—N3	118.54 (17)	C7—C2—C3—C4	0.2 (4)
O2—Mn1—N2—N3	−144.41 (18)	C1—C2—C3—C4	179.0 (2)
O5—Mn1—N2—N3	27.16 (18)	C2—C3—C4—C5	−0.6 (4)
O3—Mn1—N2—N1	−119.2 (19)	C3—C4—C5—C6	0.4 (4)
O4—Mn1—N2—N1	116.41 (19)	C4—C5—C6—C7	0.2 (4)
O1—Mn1—N2—N1	−62.23 (19)	C4—C5—C6—C8	−178.7 (2)
O2—Mn1—N2—N1	34.82 (19)	C5—C6—C7—C2	−0.5 (3)
O5—Mn1—N2—N1	−153.6 (2)	C8—C6—C7—C2	178.31 (19)
N1—N2—N3—N4	0.2 (2)	C3—C2—C7—C6	0.3 (3)
Mn1—N2—N3—N4	179.52 (14)	C1—C2—C7—C6	−178.46 (19)
N2—N3—N4—C1	0.1 (2)	N6—N5—C8—N8	0.2 (2)
C8—N5—N6—N7	−0.3 (2)	N6—N5—C8—C6	−178.4 (2)
N5—N6—N7—N8	0.4 (3)	N7—N8—C8—N5	0.0 (2)
N6—N7—N8—C8	−0.2 (2)	N7—N8—C8—C6	178.67 (19)
N2—N1—C1—N4	0.4 (2)	C5—C6—C8—N5	176.9 (2)
N2—N1—C1—C2	−179.00 (19)	C7—C6—C8—N5	−1.9 (3)
N3—N4—C1—N1	−0.3 (2)	C5—C6—C8—N8	−1.6 (3)
N3—N4—C1—C2	179.09 (19)	C7—C6—C8—N8	179.6 (2)
N1—C1—C2—C3	3.3 (3)

D—H···A	D—H	H···A	D···A	D—H···A
O7—H7B···O6	0.57 (6)	2.31 (6)	2.852 (3)	162 (8)
O5—H5A···O5i	0.57 (6)	2.41 (5)	2.910 (6)	148 (9)
O6—H6B···O7ii	0.61 (5)	2.21 (5)	2.814 (3)	171 (6)
O4—H4A···O1iii	0.67 (4)	2.38 (4)	3.035 (3)	167 (5)
O3—H3A···O7i	0.84 (4)	1.91 (4)	2.747 (3)	171 (3)
O3—H3B···O6iv	0.82 (3)	1.98 (3)	2.794 (3)	176 (3)
O2—H2B···N1v	0.75 (3)	2.06 (3)	2.800 (3)	173 (3)
O1—H1B···N6vi	0.85 (4)	1.89 (4)	2.730 (3)	176 (3)
O5—H5B···N8vii	0.75 (4)	2.07 (4)	2.810 (3)	168 (4)
O7—H7A···N5ii	0.73 (4)	2.10 (4)	2.828 (3)	173 (4)
O4—H4B···N3iv	0.88 (4)	1.80 (4)	2.681 (3)	175 (3)
O6—H6A···N4	0.82 (3)	2.07 (4)	2.886 (3)	176 (3)
O1—H1A···N7viii	0.78 (3)	1.99 (3)	2.771 (3)	175 (3)

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O7—H7B⋯O6	0.57 (6)	2.31 (6)	2.852 (3)	162 (8)
O5—H5A⋯O5i	0.57 (6)	2.41 (5)	2.910 (6)	148 (9)
O6—H6B⋯O7ii	0.61 (5)	2.21 (5)	2.814 (3)	171 (6)
O4—H4A⋯O1iii	0.67 (4)	2.38 (4)	3.035 (3)	167 (5)
O3—H3A⋯O7i	0.84 (4)	1.91 (4)	2.747 (3)	171 (3)
O3—H3B⋯O6iv	0.82 (3)	1.98 (3)	2.794 (3)	176 (3)
O2—H2B⋯N1v	0.75 (3)	2.06 (3)	2.800 (3)	173 (3)
O1—H1B⋯N6vi	0.85 (4)	1.89 (4)	2.730 (3)	176 (3)
O5—H5B⋯N8vii	0.75 (4)	2.07 (4)	2.810 (3)	168 (4)
O7—H7A⋯N5ii	0.73 (4)	2.10 (4)	2.828 (3)	173 (4)
O4—H4B⋯N3iv	0.88 (4)	1.80 (4)	2.681 (3)	175 (3)
O6—H6A⋯N4	0.82 (3)	2.07 (4)	2.886 (3)	176 (3)
O1—H1A⋯N7viii	0.78 (3)	1.99 (3)	2.771 (3)	175 (3)

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