metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

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ISSN: 2056-9890

Hexa­aqua­magnesium(II) bis­­{[2-(1-phenyl-1H-tetra­zol-5-yl)sulfan­yl]acetate}

aCollege of Chemistry and Chemical Engineering, Guangxi Normal University, Guilin, 541004, People's Republic of China
*Correspondence e-mail: gxnuchem312@yahoo.com.cn

(Received 2 April 2010; accepted 10 May 2010; online 15 May 2010)

The asymmetric unit of the title compound, [Mg(H2O)6](C9H7N4O2S)2, contains one-half of a [Mg(H2O)6]2+ cation ([\overline{1}] symmetry) and one uncoordinated 2-[(1-phenyl-1H-tetra­zol-5-yl)sulfan­yl]acetate anion. The MgII cation is coordinated by six water mol­ecules, exhibiting a slightly distorted octa­hedral coordination. A two-dimensional network parallel to (001) is formed via extensive hydrogen-bonding inter­actions involving the water mol­ecules as donors and the tetra­zole N and carboxyl­ate O atoms of the anion as acceptors. The shortest distance between two adjacent parallel benzene rings is 3.315 (2) Å. The dihedral angle between the benzene ring and the tetra­zole ring is 40.98 (2)°.

Related literature

For general background, see: He et al. (2005[He, F., Tong, M.-L., Yu, X.-L. & Chen, X.-M. (2005). Inorg. Chem. 44, 559-565.]); Yang et al. (2008[Yang, G.-W., Li, Q.-Y., Zhou, Y., Sha, P., Ma, Y.-S. & Yuan, R.-X. (2008). Inorg. Chem. Commun. 11, 723-726.]). For synthetic details, see: D'Amico et al. (1957[D'Amico, J., Harman, M. & Cooper, R. H. (1957). J. Am. Chem. Soc. 79, 5270-5272.]). For related structures with [Mg(H2O)6]2+ cations, see: Zhang et al. (2006[Zhang, X.-F., Gao, S., Huo, L.-H. & Zhao, H. (2006). Acta Cryst. E62, m2898-m2900.]); Zhou et al. (2008[Zhou, Q.-P. Zhang, G.-F & She, J.-B. (2008). J. Coord. Chem. 61, 2601-2614.]).

[Scheme 1]

Experimental

Crystal data
  • [Mg(H2O)6](C9H7N4O2S)2

  • Mr = 602.92

  • Triclinic, [P \overline 1]

  • a = 6.8380 (14) Å

  • b = 7.5220 (15) Å

  • c = 13.556 (3) Å

  • α = 92.57 (3)°

  • β = 99.14 (3)°

  • γ = 100.07 (3)°

  • V = 675.9 (2) Å3

  • Z = 1

  • Mo Kα radiation

  • μ = 0.29 mm−1

  • T = 293 K

  • 0.25 × 0.13 × 0.08 mm

Data collection
  • Bruker SMART CCD area-detector diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2001[Bruker (2001). SMART, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.806, Tmax = 0.931

  • 3914 measured reflections

  • 2347 independent reflections

  • 1867 reflections with I > 2σ(I)

  • Rint = 0.026

Refinement
  • R[F2 > 2σ(F2)] = 0.047

  • wR(F2) = 0.122

  • S = 1.02

  • 2347 reflections

  • 202 parameters

  • H atoms treated by a mixture of independent and constrained refinement

  • Δρmax = 0.25 e Å−3

  • Δρmin = −0.30 e Å−3

Table 1
Selected bond lengths (Å)

Mg1—O3 2.039 (2)
Mg1—O5 2.061 (2)
Mg1—O4 2.093 (2)

Table 2
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A DA D—H⋯A
O3—H3A⋯O2 0.97 (5) 1.77 (6) 2.711 (3) 164 (5)
O3—H3B⋯O2i 0.75 (4) 2.00 (4) 2.727 (3) 162 (4)
O4—H4A⋯O1ii 0.77 (4) 2.13 (4) 2.899 (3) 172 (4)
O4—H4B⋯N4iii 0.92 (4) 2.01 (4) 2.882 (3) 158 (4)
O5—H5A⋯N3iii 0.84 (4) 2.08 (4) 2.896 (4) 164 (4)
O5—H5B⋯O1 0.84 (4) 1.85 (4) 2.682 (3) 172 (3)
Symmetry codes: (i) -x+2, -y+1, -z+2; (ii) x+1, y, z; (iii) x+1, y-1, z.

Data collection: SMART (Bruker, 2001[Bruker (2001). SMART, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2001[Bruker (2001). SMART, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); software used to prepare material for publication: SHELXTL.

Supporting information


Comment top

The design and synthesis of supramolecular complexes with a high-nuclearity and N-containing carboxylate ligands, especially tetrazole-containing ligands, has been a rapidly growing area of research due to their fascinating structures and interesting physical properties (He et al., 2005). Several transition metal and rare earths metal complexes with similar ligand systems were reported (Yang et al., 2008).

We are interested in the solid-state coordination chemistry of ligands derived from 2-(1-phenyl-1H-tetrazol-5-ylthio)acetic acid (HPsta). In order to understand the behavior of alkali earth metals with the HPsta ligand, we prepared the title compound, [Mg(H2O)6](Psta)2, (I), the synthesis and structure of which are reported here.

As shown in Fig. 1, the asymmetric unit of (I) consists of one-half of a [Mg(H2O)6]2+ cation (site symmetry 1) and an uncoordinated 2-(1-phenyl-1H-tetrazol-5-ylthio)acetate monoanion. The MgII atom is coordinated by six water molecules in a slightly distorted octahedral coordination. The corresponding Mg—O distances (Table 1) are in agreement with similar complexes containing the [Mg(H2O)]2+ cation (Zhang et al., 2006; Zhou et al., 2008). The dihedral angle between the benzene ring and the tetrazole ring is 40.98 (2) °. In the crystal structure, the two Psta groups are involved in a number of intermolecular hydrogen bonds (Table 2) involving the O and N atoms as acceptors and the coordinated water molecules as donor groups (Fig. 2; Table 2), leading to a layer structure extending parallel to (001). In addition, ππ stacking is observed with a shortest distance between two adjacent parallel benzene rings of 3.315 (2) Å.

Related literature top

For general background, see: He et al. (2005); Yang et al. (2008). For synthetic details, see: D'Amico et al. (1957). For related structures with [Mg(H2O)6]2+ cations, see: Zhang et al. (2006); Zhou et al. (2008).

Experimental top

The ligand 2-(1-phenyl-1H-tetrazol-5-ylthio)acetic acid (HPsta) was synthesized according to the literature method (D'Amico et al., 1957). To prepare the title complex, the ligand HPsta (0.4 mmol,0.0944 g) was dissolved in methanol (6 ml) at 348 K and an aqueous solution (4 ml) containing MgCO3 (0.0336 g, 0.4 mmol) was added. The resulting solution was stirred at 348 K for 4 h, then cooled to room temperature and filtered. Colorless, prismatic crystals suitable for X-ray diffraction were obtained by slow evaporation over several days, with a yield of 61%. Elemental analysis, found (%):C, 35.79; H, 4.38; O, 26.65; N, 18.52; S, 10.66 calc(%): 35.88; H, 4.32; O, 26.58; N, 18.60; S, 10.63.

Refinement top

Water H atoms were located in a difference Fourier map and refined freely. All other H atoms were placed in their calculated positions and refined as riding with Uiso(H) = 1.2Ueq(C).

Structure description top

The design and synthesis of supramolecular complexes with a high-nuclearity and N-containing carboxylate ligands, especially tetrazole-containing ligands, has been a rapidly growing area of research due to their fascinating structures and interesting physical properties (He et al., 2005). Several transition metal and rare earths metal complexes with similar ligand systems were reported (Yang et al., 2008).

We are interested in the solid-state coordination chemistry of ligands derived from 2-(1-phenyl-1H-tetrazol-5-ylthio)acetic acid (HPsta). In order to understand the behavior of alkali earth metals with the HPsta ligand, we prepared the title compound, [Mg(H2O)6](Psta)2, (I), the synthesis and structure of which are reported here.

As shown in Fig. 1, the asymmetric unit of (I) consists of one-half of a [Mg(H2O)6]2+ cation (site symmetry 1) and an uncoordinated 2-(1-phenyl-1H-tetrazol-5-ylthio)acetate monoanion. The MgII atom is coordinated by six water molecules in a slightly distorted octahedral coordination. The corresponding Mg—O distances (Table 1) are in agreement with similar complexes containing the [Mg(H2O)]2+ cation (Zhang et al., 2006; Zhou et al., 2008). The dihedral angle between the benzene ring and the tetrazole ring is 40.98 (2) °. In the crystal structure, the two Psta groups are involved in a number of intermolecular hydrogen bonds (Table 2) involving the O and N atoms as acceptors and the coordinated water molecules as donor groups (Fig. 2; Table 2), leading to a layer structure extending parallel to (001). In addition, ππ stacking is observed with a shortest distance between two adjacent parallel benzene rings of 3.315 (2) Å.

For general background, see: He et al. (2005); Yang et al. (2008). For synthetic details, see: D'Amico et al. (1957). For related structures with [Mg(H2O)6]2+ cations, see: Zhang et al. (2006); Zhou et al. (2008).

Computing details top

Data collection: SMART (Bruker, 2001); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT (Bruker, 2001); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXS97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. The molecular moieties of (I), showing the atom-numbering scheme. Symmetry code: A -x+2,-y,-z+2. Probability function is drawn at the 50% level.
[Figure 2] Fig. 2. Packing of (I), viewed down the a axis. Hydrogen bonding interactions are shown by dashed lines.
Hexaaquamagnesium(II) bis{[2-(1-phenyl-1H-tetrazol-5-yl)sulfanyl]acetate} top
Crystal data top
[Mg(H2O)6](C9H7N4O2S)2Z = 1
Mr = 602.92F(000) = 314.0
Triclinic, P1Dx = 1.481 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 6.8380 (14) ÅCell parameters from 1867 reflections
b = 7.5220 (15) Åθ = 2.0–25.0°
c = 13.556 (3) ŵ = 0.29 mm1
α = 92.57 (3)°T = 293 K
β = 99.14 (3)°Prism, colourless
γ = 100.07 (3)°0.25 × 0.13 × 0.08 mm
V = 675.9 (2) Å3
Data collection top
Bruker SMART CCD area-detector
diffractometer
2347 independent reflections
Radiation source: fine-focus sealed tube1867 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.026
phi and ω scansθmax = 25.0°, θmin = 3.1°
Absorption correction: multi-scan
(SADABS; Bruker, 2001)
h = 87
Tmin = 0.806, Tmax = 0.931k = 88
3914 measured reflectionsl = 1616
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.047Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.122H atoms treated by a mixture of independent and constrained refinement
S = 1.02 w = 1/[σ2(Fo2) + (0.067P)2 + 0.250P]
where P = (Fo2 + 2Fc2)/3
2347 reflections(Δ/σ)max < 0.001
202 parametersΔρmax = 0.25 e Å3
0 restraintsΔρmin = 0.30 e Å3
Crystal data top
[Mg(H2O)6](C9H7N4O2S)2γ = 100.07 (3)°
Mr = 602.92V = 675.9 (2) Å3
Triclinic, P1Z = 1
a = 6.8380 (14) ÅMo Kα radiation
b = 7.5220 (15) ŵ = 0.29 mm1
c = 13.556 (3) ÅT = 293 K
α = 92.57 (3)°0.25 × 0.13 × 0.08 mm
β = 99.14 (3)°
Data collection top
Bruker SMART CCD area-detector
diffractometer
2347 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2001)
1867 reflections with I > 2σ(I)
Tmin = 0.806, Tmax = 0.931Rint = 0.026
3914 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0470 restraints
wR(F2) = 0.122H atoms treated by a mixture of independent and constrained refinement
S = 1.02Δρmax = 0.25 e Å3
2347 reflectionsΔρmin = 0.30 e Å3
202 parameters
Special details top

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Mg11.00000.00001.00000.0290 (3)
C10.5668 (4)0.3487 (4)0.8626 (2)0.0316 (6)
C20.4066 (4)0.4641 (4)0.8376 (2)0.0334 (7)
H2A0.46550.57920.81550.040*
H2B0.34720.48740.89620.040*
C30.0428 (4)0.4804 (4)0.72657 (19)0.0292 (6)
C40.1942 (4)0.3060 (4)0.5768 (2)0.0321 (7)
C50.1784 (4)0.1299 (4)0.5934 (2)0.0393 (7)
H50.13090.09850.65720.047*
C60.2343 (4)0.0001 (4)0.5137 (3)0.0491 (9)
H6A0.22060.11910.52320.059*
C70.3105 (5)0.0470 (5)0.4198 (2)0.0503 (9)
H7A0.34770.04070.36640.060*
C80.3314 (5)0.2215 (5)0.4051 (2)0.0526 (9)
H8A0.38610.25110.34200.063*
C90.2721 (5)0.3546 (4)0.4831 (2)0.0431 (8)
H9A0.28420.47400.47300.052*
N10.1273 (3)0.4464 (3)0.65654 (16)0.0326 (6)
N20.2303 (4)0.5835 (4)0.66553 (19)0.0449 (7)
N30.1245 (4)0.6943 (4)0.73682 (19)0.0465 (7)
N40.0470 (4)0.6354 (3)0.77710 (17)0.0364 (6)
O10.5227 (3)0.1854 (3)0.83268 (16)0.0427 (6)
O20.7301 (3)0.4261 (3)0.91271 (18)0.0550 (7)
O31.0502 (3)0.2699 (3)0.97908 (17)0.0371 (5)
O41.2154 (4)0.0513 (3)0.91404 (18)0.0453 (6)
O50.7751 (3)0.0466 (3)0.87611 (17)0.0465 (6)
S10.21753 (11)0.33953 (10)0.73900 (5)0.0384 (2)
H5B0.700 (5)0.027 (5)0.857 (2)0.050 (10)*
H3B1.122 (5)0.338 (5)1.016 (3)0.048 (11)*
H5A0.793 (6)0.110 (5)0.827 (3)0.069 (12)*
H4B1.194 (6)0.160 (6)0.877 (3)0.088 (14)*
H4A1.291 (6)0.020 (5)0.893 (3)0.058 (13)*
H3A0.935 (8)0.313 (7)0.944 (4)0.13 (2)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mg10.0306 (7)0.0222 (6)0.0334 (7)0.0083 (5)0.0007 (5)0.0019 (5)
C10.0297 (15)0.0306 (15)0.0319 (14)0.0047 (12)0.0013 (12)0.0008 (12)
C20.0324 (16)0.0308 (14)0.0343 (15)0.0082 (12)0.0033 (12)0.0029 (12)
C30.0292 (15)0.0322 (15)0.0266 (13)0.0097 (12)0.0018 (11)0.0003 (12)
C40.0255 (15)0.0358 (16)0.0339 (15)0.0065 (12)0.0024 (11)0.0041 (12)
C50.0311 (16)0.0384 (17)0.0465 (17)0.0091 (13)0.0016 (13)0.0013 (14)
C60.0349 (18)0.0360 (17)0.073 (2)0.0084 (14)0.0021 (16)0.0108 (16)
C70.0375 (18)0.057 (2)0.053 (2)0.0069 (15)0.0059 (15)0.0239 (17)
C80.051 (2)0.069 (2)0.0327 (16)0.0058 (17)0.0001 (14)0.0053 (16)
C90.0505 (19)0.0411 (17)0.0350 (16)0.0109 (14)0.0037 (14)0.0036 (14)
N10.0326 (13)0.0342 (13)0.0319 (12)0.0148 (10)0.0002 (10)0.0021 (10)
N20.0429 (15)0.0470 (15)0.0463 (15)0.0262 (12)0.0046 (12)0.0083 (13)
N30.0496 (16)0.0457 (16)0.0458 (15)0.0250 (13)0.0013 (12)0.0113 (13)
N40.0380 (14)0.0347 (13)0.0375 (13)0.0167 (11)0.0007 (11)0.0051 (11)
O10.0356 (12)0.0297 (11)0.0581 (13)0.0117 (9)0.0097 (10)0.0065 (10)
O20.0371 (13)0.0327 (12)0.0827 (17)0.0054 (9)0.0239 (12)0.0032 (11)
O30.0390 (13)0.0231 (10)0.0454 (12)0.0059 (9)0.0035 (10)0.0018 (10)
O40.0471 (15)0.0331 (12)0.0552 (14)0.0001 (11)0.0188 (12)0.0099 (11)
O50.0509 (14)0.0469 (14)0.0413 (13)0.0279 (11)0.0094 (10)0.0129 (11)
S10.0359 (4)0.0357 (4)0.0410 (4)0.0180 (3)0.0097 (3)0.0103 (3)
Geometric parameters (Å, º) top
Mg1—O3i2.039 (2)C5—C61.383 (4)
Mg1—O32.039 (2)C5—H50.9300
Mg1—O5i2.061 (2)C6—C71.382 (5)
Mg1—O52.061 (2)C6—H6A0.9300
Mg1—O42.093 (2)C7—C81.365 (5)
Mg1—O4i2.093 (2)C7—H7A0.9300
C1—O21.242 (3)C8—C91.383 (4)
C1—O11.246 (3)C8—H8A0.9300
C1—C21.519 (4)C9—H9A0.9300
C2—S11.803 (3)N1—N21.358 (3)
C2—H2A0.9700N2—N31.284 (3)
C2—H2B0.9700N3—N41.367 (3)
C3—N41.319 (3)O3—H3B0.75 (4)
C3—N11.358 (3)O3—H3A0.97 (6)
C3—S11.725 (3)O4—H4B0.91 (5)
C4—C51.373 (4)O4—H4A0.77 (4)
C4—C91.388 (4)O5—H5B0.84 (4)
C4—N11.438 (3)O5—H5A0.84 (4)
O3i—Mg1—O3180.000 (1)C4—C5—H5120.6
O3i—Mg1—O5i90.36 (10)C6—C5—H5120.6
O3—Mg1—O5i89.64 (10)C7—C6—C5120.1 (3)
O3i—Mg1—O589.64 (10)C7—C6—H6A119.9
O3—Mg1—O590.36 (10)C5—C6—H6A119.9
O5i—Mg1—O5180.000 (1)C8—C7—C6120.4 (3)
O3i—Mg1—O487.11 (10)C8—C7—H7A119.8
O3—Mg1—O492.89 (10)C6—C7—H7A119.8
O5i—Mg1—O488.33 (10)C7—C8—C9120.6 (3)
O5—Mg1—O491.67 (10)C7—C8—H8A119.7
O3i—Mg1—O4i92.89 (10)C9—C8—H8A119.7
O3—Mg1—O4i87.11 (10)C8—C9—C4118.5 (3)
O5i—Mg1—O4i91.67 (10)C8—C9—H9A120.8
O5—Mg1—O4i88.33 (10)C4—C9—H9A120.8
O4—Mg1—O4i180.000 (1)N2—N1—C3108.3 (2)
O2—C1—O1125.7 (3)N2—N1—C4120.9 (2)
O2—C1—C2116.6 (2)C3—N1—C4130.5 (2)
O1—C1—C2117.6 (2)N3—N2—N1106.2 (2)
C1—C2—S1107.16 (18)N2—N3—N4111.7 (2)
C1—C2—H2A110.3C3—N4—N3105.8 (2)
S1—C2—H2A110.3Mg1—O3—H3B123 (3)
C1—C2—H2B110.3Mg1—O3—H3A115 (3)
S1—C2—H2B110.3H3B—O3—H3A115 (4)
H2A—C2—H2B108.5Mg1—O4—H4B119 (3)
N4—C3—N1108.1 (2)Mg1—O4—H4A127 (3)
N4—C3—S1129.0 (2)H4B—O4—H4A111 (4)
N1—C3—S1122.93 (19)Mg1—O5—H5B125 (2)
C5—C4—C9121.5 (3)Mg1—O5—H5A118 (3)
C5—C4—N1120.5 (2)H5B—O5—H5A110 (3)
C9—C4—N1118.0 (3)C3—S1—C2100.91 (12)
C4—C5—C6118.9 (3)
O2—C1—C2—S1164.8 (2)C5—C4—N1—N2142.3 (3)
O1—C1—C2—S116.2 (3)C9—C4—N1—N238.4 (4)
C9—C4—C5—C62.6 (4)C5—C4—N1—C344.2 (4)
N1—C4—C5—C6176.6 (3)C9—C4—N1—C3135.0 (3)
C4—C5—C6—C72.0 (5)C3—N1—N2—N30.7 (3)
C5—C6—C7—C80.1 (5)C4—N1—N2—N3174.0 (3)
C6—C7—C8—C91.6 (5)N1—N2—N3—N40.5 (4)
C7—C8—C9—C41.0 (5)N1—C3—N4—N30.3 (3)
C5—C4—C9—C81.1 (5)S1—C3—N4—N3178.7 (2)
N1—C4—C9—C8178.1 (3)N2—N3—N4—C30.1 (4)
N4—C3—N1—N20.7 (3)N4—C3—S1—C20.9 (3)
S1—C3—N1—N2179.1 (2)N1—C3—S1—C2177.1 (2)
N4—C3—N1—C4173.4 (3)C1—C2—S1—C3176.0 (2)
S1—C3—N1—C45.0 (4)
Symmetry code: (i) x+2, y, z+2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O3—H3A···O20.97 (5)1.77 (6)2.711 (3)164 (5)
O3—H3B···O2ii0.75 (4)2.00 (4)2.727 (3)162 (4)
O4—H4A···O1iii0.77 (4)2.13 (4)2.899 (3)172 (4)
O4—H4B···N4iv0.92 (4)2.01 (4)2.882 (3)158 (4)
O5—H5A···N3iv0.84 (4)2.08 (4)2.896 (4)164 (4)
O5—H5B···O10.84 (4)1.85 (4)2.682 (3)172 (3)
Symmetry codes: (ii) x+2, y+1, z+2; (iii) x+1, y, z; (iv) x+1, y1, z.

Experimental details

Crystal data
Chemical formula[Mg(H2O)6](C9H7N4O2S)2
Mr602.92
Crystal system, space groupTriclinic, P1
Temperature (K)293
a, b, c (Å)6.8380 (14), 7.5220 (15), 13.556 (3)
α, β, γ (°)92.57 (3), 99.14 (3), 100.07 (3)
V3)675.9 (2)
Z1
Radiation typeMo Kα
µ (mm1)0.29
Crystal size (mm)0.25 × 0.13 × 0.08
Data collection
DiffractometerBruker SMART CCD area-detector
Absorption correctionMulti-scan
(SADABS; Bruker, 2001)
Tmin, Tmax0.806, 0.931
No. of measured, independent and
observed [I > 2σ(I)] reflections
3914, 2347, 1867
Rint0.026
(sin θ/λ)max1)0.595
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.047, 0.122, 1.02
No. of reflections2347
No. of parameters202
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)0.25, 0.30

Computer programs: SMART (Bruker, 2001), SAINT (Bruker, 2001), SHELXS97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

Selected bond lengths (Å) top
Mg1—O32.039 (2)Mg1—O42.093 (2)
Mg1—O52.061 (2)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O3—H3A···O20.97 (5)1.77 (6)2.711 (3)164 (5)
O3—H3B···O2i0.75 (4)2.00 (4)2.727 (3)162 (4)
O4—H4A···O1ii0.77 (4)2.13 (4)2.899 (3)172 (4)
O4—H4B···N4iii0.92 (4)2.01 (4)2.882 (3)158 (4)
O5—H5A···N3iii0.84 (4)2.08 (4)2.896 (4)164 (4)
O5—H5B···O10.84 (4)1.85 (4)2.682 (3)172 (3)
Symmetry codes: (i) x+2, y+1, z+2; (ii) x+1, y, z; (iii) x+1, y1, z.
 

Acknowledgements

We gratefully acknowledge the Natural Science Foundation of Guangxi (0832098) and the Program of Educational Innovation of Graduate Students (06020703M242).

References

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First citationZhou, Q.-P. Zhang, G.-F & She, J.-B. (2008). J. Coord. Chem. 61, 2601–2614.  Web of Science CSD CrossRef CAS Google Scholar

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