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Acta Crystallogr Sect E Struct Rep Online. 2010 August 1; 66(Pt 8): m979.
Published online 2010 July 21. doi:  10.1107/S1600536810027625
PMCID: PMC3007222

Tetra­aqua­bis­(tetra­zolido-κN 1)magnesium

Abstract

In the crystal structure of the title compound, [Mg(CHN4)2(H2O)4], the MgII atom is six-coordinated by two N atoms from two tetra­zolide anions and four O atoms from four coordinated water mol­ecules in a slightly distorted octa­hedral geometry. The Mg atom is located on centres of inversion whereas the tetra­zolide anion and the water mol­ecules occupy general positions. The crystal packing is stabilized by intermolecular O—H(...)N hydrogen bonding between the tetra­zolide anions and the coordinated water mol­ecules.

Related literature

For metal complexes with tetra­zolide anions, see: Zhang et al. (2007 [triangle]); He et al. (2006 [triangle]).

An external file that holds a picture, illustration, etc.
Object name is e-66-0m979-scheme1.jpg

Experimental

Crystal data

  • [Mg(CHN4)2(H2O)4]
  • M r = 234.49
  • Monoclinic, An external file that holds a picture, illustration, etc.
Object name is e-66-0m979-efi1.jpg
  • a = 5.7570 (19) Å
  • b = 11.638 (4) Å
  • c = 6.963 (2) Å
  • β = 99.785 (5)°
  • V = 459.7 (3) Å3
  • Z = 2
  • Mo Kα radiation
  • μ = 0.21 mm−1
  • T = 173 K
  • 0.36 × 0.28 × 0.22 mm

Data collection

  • Bruker SMART CCD area-detector diffractometer
  • Absorption correction: multi-scan (SADABS; Bruker, 1998 [triangle]) T min = 0.929, T max = 0.955
  • 1806 measured reflections
  • 792 independent reflections
  • 709 reflections with I > 2σ(I)
  • R int = 0.015

Refinement

  • R[F 2 > 2σ(F 2)] = 0.033
  • wR(F 2) = 0.097
  • S = 1.01
  • 792 reflections
  • 86 parameters
  • 6 restraints
  • H atoms treated by a mixture of independent and constrained refinement
  • Δρmax = 0.35 e Å−3
  • Δρmin = −0.25 e Å−3

Data collection: SMART (Bruker, 1998 [triangle]); cell refinement: SAINT (Bruker, 1998 [triangle]); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 [triangle]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 [triangle]); molecular graphics: SHELXTL (Sheldrick, 2008 [triangle]); software used to prepare material for publication: SHELXTL.

Table 1
Hydrogen-bond geometry (Å, °)

Supplementary Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536810027625/nc2193sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536810027625/nc2193Isup2.hkl

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

supplementary crystallographic information

Comment

Tetrazolide anions are found in a number of metal complexes as ligands and the crystal structures and properties of several of such metal complexes have been reported in literature (Zhang et al., 2007; He et al., 2006) In the present contribution we report the synthesis and crystal structure of it's magnesium(II) complex. In the crystal structure of the title compound the Mg atoms are six-coordinated by two N atoms from two symmetry equivalent tetrazolide anions and four O atoms of two pairs of symmetry equivalent water molecules. The coordination polyhedra around the Mg atoms can be described as slightly distorted tetrahedra (Fig. 1). In the crystal structure the complexes are connected by intermolecular O—H···N hydrogen bonding into a three-dimensional network (Fig. 2 and Tab. 1).

Experimental

A solution of MgCl2 2H2O (1 mmol) in water (5 ml) was slowly added to a solution of tetrazole (1 mmol) in water (14 ml) with continuous stirring at room temperature. After 30 minutes, the mixture was sealed in a 25 ml Teflon-lined stainless steel vessel and heated under autogenous pressure at 160 °C for 4 days, then slowly cooled to room temperature. The colorless crystals were collected by filtration, washed with distilled water and dried in air. Yield: 60% (based on Mg).

Refinement

The H atoms of the tetrazole ligands were placed in geometrically idealized positions with C—H distances of 0.95 Å and were refined isotropic using a riding model with Uiso(H) = 1.2Ueq(C). The H atoms of the coordinated water molecules were located in the difference Fourier maps and refined isotropic with varying coordinates.

Figures

Fig. 1.
The structure of (I), showing 30% probability displacement ellipsoids and the atom-labeling scheme. Symmetry code: i = x,y,z.
Fig. 2.
Crystal structure of title compound with view along the a axis. Hydrogen bonding is shown as dashed lines.

Crystal data

[Mg(CHN4)2(H2O)4]F(000) = 244
Mr = 234.49Dx = 1.694 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 1468 reflections
a = 5.7570 (19) Åθ = 3.5–26.9°
b = 11.638 (4) ŵ = 0.21 mm1
c = 6.963 (2) ÅT = 173 K
β = 99.785 (5)°Block, colorless
V = 459.7 (3) Å30.36 × 0.28 × 0.22 mm
Z = 2

Data collection

Bruker SMART CCD area-detector diffractometer792 independent reflections
Radiation source: fine-focus sealed tube709 reflections with I > 2σ(I)
graphiteRint = 0.015
phi and ω scansθmax = 25.0°, θmin = 3.5°
Absorption correction: multi-scan (SADABS; Bruker, 1998)h = −5→6
Tmin = 0.929, Tmax = 0.955k = −13→12
1806 measured reflectionsl = −7→8

Refinement

Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.033Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.097H atoms treated by a mixture of independent and constrained refinement
S = 1.01w = 1/[σ2(Fo2) + (0.0716P)2 + 0.1838P] where P = (Fo2 + 2Fc2)/3
792 reflections(Δ/σ)max < 0.001
86 parametersΔρmax = 0.35 e Å3
6 restraintsΔρmin = −0.25 e Å3

Special details

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2)

xyzUiso*/Ueq
Mg10.50000.50000.00000.0139 (3)
N10.8863 (2)0.31027 (12)0.0878 (2)0.0188 (4)
N20.6554 (2)0.32630 (12)0.02230 (19)0.0154 (4)
C10.5683 (3)0.22168 (15)−0.0099 (2)0.0184 (4)
H10.40700.2058−0.05750.022*
N40.7331 (2)0.14132 (12)0.0322 (2)0.0199 (4)
O10.2683 (2)0.45460 (11)0.18011 (19)0.0187 (3)
O20.7258 (2)0.54196 (11)0.25064 (18)0.0196 (4)
N30.9328 (3)0.20068 (12)0.0938 (2)0.0200 (4)
H2A0.729 (4)0.4945 (18)0.341 (3)0.033 (6)*
H1A0.256 (4)0.5042 (18)0.260 (3)0.037 (7)*
H1B0.136 (4)0.417 (2)0.150 (3)0.043 (7)*
H2B0.819 (4)0.594 (2)0.293 (4)0.045 (7)*

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
Mg10.0152 (4)0.0058 (5)0.0200 (5)−0.0001 (3)0.0007 (3)−0.0002 (3)
N10.0187 (8)0.0104 (8)0.0262 (8)0.0028 (6)0.0011 (6)0.0006 (6)
N20.0170 (7)0.0095 (8)0.0194 (8)0.0003 (6)0.0017 (6)−0.0003 (5)
C10.0192 (8)0.0115 (9)0.0235 (9)−0.0005 (7)0.0006 (7)−0.0002 (7)
N40.0242 (8)0.0090 (8)0.0255 (9)0.0007 (6)0.0015 (6)−0.0007 (6)
O10.0201 (7)0.0106 (7)0.0260 (7)−0.0027 (5)0.0053 (5)−0.0036 (5)
O20.0237 (7)0.0105 (7)0.0221 (7)−0.0051 (5)−0.0034 (5)0.0019 (5)
N30.0227 (8)0.0108 (7)0.0256 (8)0.0026 (6)0.0014 (6)−0.0002 (6)

Geometric parameters (Å, °)

Mg1—O1i2.0492 (13)N2—C11.321 (2)
Mg1—O12.0492 (13)C1—N41.329 (2)
Mg1—O2i2.0499 (13)C1—H10.9500
Mg1—O22.0499 (13)N4—N31.347 (2)
Mg1—N22.2053 (15)O1—H1A0.812 (19)
Mg1—N2i2.2053 (15)O1—H1B0.876 (19)
N1—N31.302 (2)O2—H2A0.83 (2)
N1—N21.343 (2)O2—H2B0.83 (2)
O1i—Mg1—O1180.00 (7)N3—N1—N2109.45 (13)
O1i—Mg1—O2i85.69 (6)C1—N2—N1104.74 (13)
O1—Mg1—O2i94.31 (6)C1—N2—Mg1134.05 (11)
O1i—Mg1—O294.31 (6)N1—N2—Mg1121.16 (10)
O1—Mg1—O285.69 (6)N2—C1—N4112.04 (15)
O2i—Mg1—O2180.00 (7)N2—C1—H1124.0
O1i—Mg1—N288.91 (5)N4—C1—H1124.0
O1—Mg1—N291.09 (5)C1—N4—N3104.34 (15)
O2i—Mg1—N291.86 (5)Mg1—O1—H1A112.3 (16)
O2—Mg1—N288.14 (5)Mg1—O1—H1B128.1 (16)
O1i—Mg1—N2i91.09 (5)H1A—O1—H1B110 (2)
O1—Mg1—N2i88.91 (5)Mg1—O2—H2A114.5 (16)
O2i—Mg1—N2i88.14 (5)Mg1—O2—H2B139.2 (17)
O2—Mg1—N2i91.86 (5)H2A—O2—H2B106 (2)
N2—Mg1—N2i180.0N1—N3—N4109.42 (14)

Symmetry codes: (i) −x+1, −y+1, −z.

Hydrogen-bond geometry (Å, °)

D—H···AD—HH···AD···AD—H···A
O2—H2B···N3ii0.83 (2)1.96 (2)2.7797 (19)173 (2)
O1—H1B···N1iii0.88 (2)1.89 (2)2.755 (2)169 (2)
O1—H1A···N4iv0.81 (2)2.15 (2)2.956 (2)173 (2)
O2—H2A···N4v0.83 (2)2.06 (2)2.892 (2)171 (2)

Symmetry codes: (ii) −x+2, y+1/2, −z+1/2; (iii) x−1, y, z; (iv) −x+1, y+1/2, −z+1/2; (v) x, −y+1/2, z+1/2.

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: NC2193).

References

  • Bruker (1998). SMART, SAINT and SADABS Bruker AXS Inc., Madison, Wisconsin, USA.
  • He, X., Lu, C.-Z. & Yuan, D.-Q. (2006). Inorg. Chem.15, 5760–5766. [PubMed]
  • Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. [PubMed]
  • Zhang, X.-M., Zhao, Y.-F., Zhang, W.-X. & Chen, X.-M. (2007). Adv. Mater.19, 2843–2846.

Articles from Acta Crystallographica Section E: Structure Reports Online are provided here courtesy of International Union of Crystallography