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

Fu, C.-H.; Zhou, X.; Yu, Q.; Bian, H.-D.

doi:10.1107/S1600536810016983

metal-organic compounds

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ISSN: 2056-9890

Volume 66| Part 6| June 2010| Page m657

https://doi.org/10.1107/S1600536810016983

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

Chun-Hua Fu,^a Xiang Zhou,^a Qing Yu ^a ^* and He-Dong Bian ^a

^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 Mg^II 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 ); 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

Crystal data

[Mg(H₂O)₆](C₉H₇N₄O₂S)₂
M_r = 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 ) T_min = 0.806, T_max = 0.931
3914 measured reflections
2347 independent reflections
1867 reflections with I > 2σ(I)
R_int = 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
Δρ_max = 0.25 e Å⁻³
Δρ_min = −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	D⋯A	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); cell refinement: SAINT (Bruker, 2001); 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.

Supporting information

Crystal structure: contains datablocks I, global. DOI: https://doi.org/10.1107/S1600536810016983/wm2320sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536810016983/wm2320Isup2.hkl

checkCIF report

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 Mg^II 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, π—π 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.

Structure description 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).

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

	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.
	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)₂	Z = 1
M_r = 602.92	F(000) = 314.0
Triclinic, P1	D_x = 1.481 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 6.8380 (14) Å	Cell parameters from 1867 reflections
b = 7.5220 (15) Å	θ = 2.0–25.0°
c = 13.556 (3) Å	µ = 0.29 mm⁻¹
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 tube	1867 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.026
phi and ω scans	θ_max = 25.0°, θ_min = 3.1°
Absorption correction: multi-scan (SADABS; Bruker, 2001)	h = −8→7
T_min = 0.806, T_max = 0.931	k = −8→8
3914 measured reflections	l = −16→16

Refinement top

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)] = 0.047	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.122	H atoms treated by a mixture of independent and constrained refinement
S = 1.02	w = 1/[σ²(F_o²) + (0.067P)² + 0.250P] where P = (F_o² + 2F_c²)/3
2347 reflections	(Δ/σ)_max < 0.001
202 parameters	Δρ_max = 0.25 e Å⁻³
0 restraints	Δρ_min = −0.30 e Å⁻³

Crystal data top

[Mg(H₂O)₆](C₉H₇N₄O₂S)₂	γ = 100.07 (3)°
M_r = 602.92	V = 675.9 (2) Å³
Triclinic, P1	Z = 1
a = 6.8380 (14) Å	Mo Kα radiation
b = 7.5220 (15) Å	µ = 0.29 mm⁻¹
c = 13.556 (3) Å	T = 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)
T_min = 0.806, T_max = 0.931	R_int = 0.026
3914 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.047	0 restraints
wR(F²) = 0.122	H atoms treated by a mixture of independent and constrained refinement
S = 1.02	Δρ_max = 0.25 e Å⁻³
2347 reflections	Δρ_min = −0.30 e Å⁻³
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

	x	y	z	U_iso*/U_eq
Mg1	1.0000	0.0000	1.0000	0.0290 (3)
C1	0.5668 (4)	0.3487 (4)	0.8626 (2)	0.0316 (6)
C2	0.4066 (4)	0.4641 (4)	0.8376 (2)	0.0334 (7)
H2A	0.4655	0.5792	0.8155	0.040*
H2B	0.3472	0.4874	0.8962	0.040*
C3	0.0428 (4)	0.4804 (4)	0.72657 (19)	0.0292 (6)
C4	−0.1942 (4)	0.3060 (4)	0.5768 (2)	0.0321 (7)
C5	−0.1784 (4)	0.1299 (4)	0.5934 (2)	0.0393 (7)
H5	−0.1309	0.0985	0.6572	0.047*
C6	−0.2343 (4)	0.0001 (4)	0.5137 (3)	0.0491 (9)
H6A	−0.2206	−0.1191	0.5232	0.059*
C7	−0.3105 (5)	0.0470 (5)	0.4198 (2)	0.0503 (9)
H7A	−0.3477	−0.0407	0.3664	0.060*
C8	−0.3314 (5)	0.2215 (5)	0.4051 (2)	0.0526 (9)
H8A	−0.3861	0.2511	0.3420	0.063*
C9	−0.2721 (5)	0.3546 (4)	0.4831 (2)	0.0431 (8)
H9A	−0.2842	0.4740	0.4730	0.052*
N1	−0.1273 (3)	0.4464 (3)	0.65654 (16)	0.0326 (6)
N2	−0.2303 (4)	0.5835 (4)	0.66553 (19)	0.0449 (7)
N3	−0.1245 (4)	0.6943 (4)	0.73682 (19)	0.0465 (7)
N4	0.0470 (4)	0.6354 (3)	0.77710 (17)	0.0364 (6)
O1	0.5227 (3)	0.1854 (3)	0.83268 (16)	0.0427 (6)
O2	0.7301 (3)	0.4261 (3)	0.91271 (18)	0.0550 (7)
O3	1.0502 (3)	0.2699 (3)	0.97908 (17)	0.0371 (5)
O4	1.2154 (4)	−0.0513 (3)	0.91404 (18)	0.0453 (6)
O5	0.7751 (3)	−0.0466 (3)	0.87611 (17)	0.0465 (6)
S1	0.21753 (11)	0.33953 (10)	0.73900 (5)	0.0384 (2)
H5B	0.700 (5)	0.027 (5)	0.857 (2)	0.050 (10)*
H3B	1.122 (5)	0.338 (5)	1.016 (3)	0.048 (11)*
H5A	0.793 (6)	−0.110 (5)	0.827 (3)	0.069 (12)*
H4B	1.194 (6)	−0.160 (6)	0.877 (3)	0.088 (14)*
H4A	1.291 (6)	0.020 (5)	0.893 (3)	0.058 (13)*
H3A	0.935 (8)	0.313 (7)	0.944 (4)	0.13 (2)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Mg1	0.0306 (7)	0.0222 (6)	0.0334 (7)	0.0083 (5)	0.0007 (5)	−0.0019 (5)
C1	0.0297 (15)	0.0306 (15)	0.0319 (14)	0.0047 (12)	−0.0013 (12)	0.0008 (12)
C2	0.0324 (16)	0.0308 (14)	0.0343 (15)	0.0082 (12)	−0.0033 (12)	−0.0029 (12)
C3	0.0292 (15)	0.0322 (15)	0.0266 (13)	0.0097 (12)	0.0018 (11)	−0.0003 (12)
C4	0.0255 (15)	0.0358 (16)	0.0339 (15)	0.0065 (12)	0.0024 (11)	−0.0041 (12)
C5	0.0311 (16)	0.0384 (17)	0.0465 (17)	0.0091 (13)	−0.0016 (13)	0.0013 (14)
C6	0.0349 (18)	0.0360 (17)	0.073 (2)	0.0084 (14)	0.0021 (16)	−0.0108 (16)
C7	0.0375 (18)	0.057 (2)	0.053 (2)	0.0069 (15)	0.0059 (15)	−0.0239 (17)
C8	0.051 (2)	0.069 (2)	0.0327 (16)	0.0058 (17)	−0.0001 (14)	−0.0053 (16)
C9	0.0505 (19)	0.0411 (17)	0.0350 (16)	0.0109 (14)	−0.0037 (14)	0.0036 (14)
N1	0.0326 (13)	0.0342 (13)	0.0319 (12)	0.0148 (10)	−0.0002 (10)	−0.0021 (10)
N2	0.0429 (15)	0.0470 (15)	0.0463 (15)	0.0262 (12)	−0.0046 (12)	−0.0083 (13)
N3	0.0496 (16)	0.0457 (16)	0.0458 (15)	0.0250 (13)	−0.0013 (12)	−0.0113 (13)
N4	0.0380 (14)	0.0347 (13)	0.0375 (13)	0.0167 (11)	0.0007 (11)	−0.0051 (11)
O1	0.0356 (12)	0.0297 (11)	0.0581 (13)	0.0117 (9)	−0.0097 (10)	−0.0065 (10)
O2	0.0371 (13)	0.0327 (12)	0.0827 (17)	0.0054 (9)	−0.0239 (12)	−0.0032 (11)
O3	0.0390 (13)	0.0231 (10)	0.0454 (12)	0.0059 (9)	−0.0035 (10)	−0.0018 (10)
O4	0.0471 (15)	0.0331 (12)	0.0552 (14)	−0.0001 (11)	0.0188 (12)	−0.0099 (11)
O5	0.0509 (14)	0.0469 (14)	0.0413 (13)	0.0279 (11)	−0.0094 (10)	−0.0129 (11)
S1	0.0359 (4)	0.0357 (4)	0.0410 (4)	0.0180 (3)	−0.0097 (3)	−0.0103 (3)

Geometric parameters (Å, º) top

Mg1—O3ⁱ	2.039 (2)	C5—C6	1.383 (4)
Mg1—O3	2.039 (2)	C5—H5	0.9300
Mg1—O5ⁱ	2.061 (2)	C6—C7	1.382 (5)
Mg1—O5	2.061 (2)	C6—H6A	0.9300
Mg1—O4	2.093 (2)	C7—C8	1.365 (5)
Mg1—O4ⁱ	2.093 (2)	C7—H7A	0.9300
C1—O2	1.242 (3)	C8—C9	1.383 (4)
C1—O1	1.246 (3)	C8—H8A	0.9300
C1—C2	1.519 (4)	C9—H9A	0.9300
C2—S1	1.803 (3)	N1—N2	1.358 (3)
C2—H2A	0.9700	N2—N3	1.284 (3)
C2—H2B	0.9700	N3—N4	1.367 (3)
C3—N4	1.319 (3)	O3—H3B	0.75 (4)
C3—N1	1.358 (3)	O3—H3A	0.97 (6)
C3—S1	1.725 (3)	O4—H4B	0.91 (5)
C4—C5	1.373 (4)	O4—H4A	0.77 (4)
C4—C9	1.388 (4)	O5—H5B	0.84 (4)
C4—N1	1.438 (3)	O5—H5A	0.84 (4)

O3ⁱ—Mg1—O3	180.000 (1)	C4—C5—H5	120.6
O3ⁱ—Mg1—O5ⁱ	90.36 (10)	C6—C5—H5	120.6
O3—Mg1—O5ⁱ	89.64 (10)	C7—C6—C5	120.1 (3)
O3ⁱ—Mg1—O5	89.64 (10)	C7—C6—H6A	119.9
O3—Mg1—O5	90.36 (10)	C5—C6—H6A	119.9
O5ⁱ—Mg1—O5	180.000 (1)	C8—C7—C6	120.4 (3)
O3ⁱ—Mg1—O4	87.11 (10)	C8—C7—H7A	119.8
O3—Mg1—O4	92.89 (10)	C6—C7—H7A	119.8
O5ⁱ—Mg1—O4	88.33 (10)	C7—C8—C9	120.6 (3)
O5—Mg1—O4	91.67 (10)	C7—C8—H8A	119.7
O3ⁱ—Mg1—O4ⁱ	92.89 (10)	C9—C8—H8A	119.7
O3—Mg1—O4ⁱ	87.11 (10)	C8—C9—C4	118.5 (3)
O5ⁱ—Mg1—O4ⁱ	91.67 (10)	C8—C9—H9A	120.8
O5—Mg1—O4ⁱ	88.33 (10)	C4—C9—H9A	120.8
O4—Mg1—O4ⁱ	180.000 (1)	N2—N1—C3	108.3 (2)
O2—C1—O1	125.7 (3)	N2—N1—C4	120.9 (2)
O2—C1—C2	116.6 (2)	C3—N1—C4	130.5 (2)
O1—C1—C2	117.6 (2)	N3—N2—N1	106.2 (2)
C1—C2—S1	107.16 (18)	N2—N3—N4	111.7 (2)
C1—C2—H2A	110.3	C3—N4—N3	105.8 (2)
S1—C2—H2A	110.3	Mg1—O3—H3B	123 (3)
C1—C2—H2B	110.3	Mg1—O3—H3A	115 (3)
S1—C2—H2B	110.3	H3B—O3—H3A	115 (4)
H2A—C2—H2B	108.5	Mg1—O4—H4B	119 (3)
N4—C3—N1	108.1 (2)	Mg1—O4—H4A	127 (3)
N4—C3—S1	129.0 (2)	H4B—O4—H4A	111 (4)
N1—C3—S1	122.93 (19)	Mg1—O5—H5B	125 (2)
C5—C4—C9	121.5 (3)	Mg1—O5—H5A	118 (3)
C5—C4—N1	120.5 (2)	H5B—O5—H5A	110 (3)
C9—C4—N1	118.0 (3)	C3—S1—C2	100.91 (12)
C4—C5—C6	118.9 (3)

O2—C1—C2—S1	164.8 (2)	C5—C4—N1—N2	−142.3 (3)
O1—C1—C2—S1	−16.2 (3)	C9—C4—N1—N2	38.4 (4)
C9—C4—C5—C6	2.6 (4)	C5—C4—N1—C3	44.2 (4)
N1—C4—C5—C6	−176.6 (3)	C9—C4—N1—C3	−135.0 (3)
C4—C5—C6—C7	−2.0 (5)	C3—N1—N2—N3	0.7 (3)
C5—C6—C7—C8	−0.1 (5)	C4—N1—N2—N3	−174.0 (3)
C6—C7—C8—C9	1.6 (5)	N1—N2—N3—N4	−0.5 (4)
C7—C8—C9—C4	−1.0 (5)	N1—C3—N4—N3	0.3 (3)
C5—C4—C9—C8	−1.1 (5)	S1—C3—N4—N3	178.7 (2)
N1—C4—C9—C8	178.1 (3)	N2—N3—N4—C3	0.1 (4)
N4—C3—N1—N2	−0.7 (3)	N4—C3—S1—C2	−0.9 (3)
S1—C3—N1—N2	−179.1 (2)	N1—C3—S1—C2	177.1 (2)
N4—C3—N1—C4	173.4 (3)	C1—C2—S1—C3	176.0 (2)
S1—C3—N1—C4	−5.0 (4)

Symmetry code: (i) −x+2, −y, −z+2.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O3—H3A···O2	0.97 (5)	1.77 (6)	2.711 (3)	164 (5)
O3—H3B···O2ⁱⁱ	0.75 (4)	2.00 (4)	2.727 (3)	162 (4)
O4—H4A···O1ⁱⁱⁱ	0.77 (4)	2.13 (4)	2.899 (3)	172 (4)
O4—H4B···N4^iv	0.92 (4)	2.01 (4)	2.882 (3)	158 (4)
O5—H5A···N3^iv	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: (ii) −x+2, −y+1, −z+2; (iii) x+1, y, z; (iv) x+1, y−1, z.

Experimental details

Crystal data
Chemical formula	[Mg(H₂O)₆](C₉H₇N₄O₂S)₂
M_r	602.92
Crystal system, space group	Triclinic, 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)
V (Å³)	675.9 (2)
Z	1
Radiation type	Mo Kα
µ (mm⁻¹)	0.29
Crystal size (mm)	0.25 × 0.13 × 0.08

Data collection
Diffractometer	Bruker SMART CCD area-detector
Absorption correction	Multi-scan (SADABS; Bruker, 2001)
T_min, T_max	0.806, 0.931
No. of measured, independent and observed [I > 2σ(I)] reflections	3914, 2347, 1867
R_int	0.026
(sin θ/λ)_max (Å⁻¹)	0.595

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.047, 0.122, 1.02
No. of reflections	2347
No. of parameters	202
H-atom treatment	H atoms treated by a mixture of independent and constrained refinement
Δρ_max, Δρ_min (e Å⁻³)	0.25, −0.30

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

Selected bond lengths (Å) top

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	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.

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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