Tetra­aqua­(2-hy­droxy­acetato-κ2O1,O2)magnesium nitrate

Liu, W.-J.; Wei, Z.-Q.; Yue, S.-T.

doi:10.1107/S1600536811006611

metal-organic compounds

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ISSN: 2056-9890

Volume 67| Part 3| March 2011| Page m374

doi:10.1107/S1600536811006611

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Tetraaqua(2-hydroxyacetato-κ²O¹,O²)magnesium nitrate

Wen-Jing Liu,^a Zhi-Qiang Wei ^a and Shan-Tang Yue ^a ^*

^aSchool of Chemistry and Environment, South China Normal University, Guangzhou 510006, People's Republic of China
^*Correspondence e-mail: yuesht@scnu.edu.cn

(Received 15 February 2011; accepted 21 February 2011; online 26 February 2011)

In the title complex, [Mg(C₂H₃O₃)(H₂O)₄]NO₃, the Mg^II cation is hexacoordinated by four O atoms from water molecules and two O atoms from a 2-hydroxyacetate ligand in a distorted octahedral coordination geometry. The structure exhibits a three-dimensional supramolecular network, which is stabilized by nine different O—H⋯O hydrogen bonds.

Related literature

For related magnesium complexes, see: Erxleben & Schumacher (2001 ).

Experimental

Crystal data

[Mg(C₂H₃O₃)(H₂O)₄]NO₃
M_r = 233.43
Monoclinic, P 2₁ /n
a = 5.777 (2) Å
b = 7.171 (3) Å
c = 23.045 (8) Å
β = 92.839 (4)°
V = 953.5 (6) Å³
Z = 4
Mo Kα radiation
μ = 0.23 mm⁻¹
T = 298 K
0.20 × 0.18 × 0.18 mm

Data collection

Bruker SMART CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2001 ) T_min = 0.956, T_max = 0.960
4632 measured reflections
1713 independent reflections
1424 reflections with I > 2σ(I)
R_int = 0.027

Refinement

R[F² > 2σ(F²)] = 0.044
wR(F²) = 0.115
S = 1.06
1713 reflections
141 parameters
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 0.29 e Å⁻³
Δρ_min = −0.18 e Å⁻³

Table 1
Selected bond lengths (Å)

Mg1—O3W	2.021 (2)
Mg1—O1W	2.033 (2)
Mg1—O2	2.0467 (19)
Mg1—O4W	2.052 (2)
Mg1—O2W	2.058 (2)
Mg1—O1	2.069 (2)

Table 2
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O3W—H3W1⋯O2ⁱ	0.85	1.88	2.719 (3)	167
O3W—H3W2⋯O6ⁱⁱ	0.85	2.05	2.860 (3)	160
O1—H3⋯O3ⁱ	0.88 (3)	1.76 (3)	2.638 (3)	172 (3)
O1W—H1W2⋯O4ⁱⁱⁱ	0.85	1.90	2.747 (3)	173
O1W—H1W1⋯O6^iv	0.85	2.06	2.905 (3)	174
O4W—H4W1⋯O3^v	0.85	1.85	2.687 (3)	166
O4W—H4W2⋯O4^vi	0.85	2.31	3.014 (3)	141
O2W—H2W1⋯O4	0.85	2.02	2.860 (3)	169
O2W—H2W2⋯O5^vii	0.85	2.00	2.826 (3)	166
Symmetry codes: (i) x+1, y, z; (ii) -x+1, -y+1, -z; (iii) -x, -y+1, -z; (iv) x-1, y-1, z; (v) $[-x-{\script{1\over 2}}, y-{\script{1\over 2}}, -z+{\script{1\over 2}}]$ ; (vi) x, y-1, z; (vii) x-1, y, z.

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

Supporting information

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536811006611/go2005sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536811006611/go2005Isup2.hkl

checkCIF report

Comment top

The compound crystallizes in the monoclinic system, space group P2₁/n, an ORTEP view is shown in Fig. 1. The Mg^II ion is hexa-coordinated by four oxygen atoms from water and two oxygen atoms from 2-hydroxyacetato ions. The Mg—O distances are in the range of 2.021 (2)—2.069 (2) Å. The O—Mg—O bond angles fall in the range of 76.73 (8)—171.89 (10) °. The C—O distances of HOCH₂COO^- are within the range of 1.247 (3) Å to 1.413 (3) Å. This molecular complex exhibits a 3D structure via O—H···O hydrogen bonding interactions (Fig. 2).

Related literature top

For related magnesium complexes, see: Erxleben & Schumacher (2001).

Experimental top

A mixture of 2-hydroxyacetic acid (0.038 g, 0.5 mmol), Mg(NO₃)₂.6H₂O (0.064 g, 0.25 mmol) and H₂O (7 mL) was heated to 180 °C for 72 h in a 15 ml Teflon-lined stainless-steel autoclave and then cooled to room temperature at a rate of 5 °C/h. Colorless block crystals were collected and dried in air in ca. 48% yield based on Mg.

Computing details top

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

Figures top

	Fig. 1. Displacement ellipsoid plot (40% probability level) of the title compound.
	Fig. 2. The packing diagram of the title compound.

Tetraaqua(2-hydroxyacetato-κ²O¹,O²)magnesium nitrate top

Crystal data top

[Mg(C₂H₃O₃)(H₂O)₄]NO₃	F(000) = 488
M_r = 233.43	D_x = 1.626 Mg m⁻³ D_m = 1.626 Mg m⁻³ D_m measured by not measured
Monoclinic, P2₁/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 1638 reflections
a = 5.777 (2) Å	θ = 2.8–26.0°
b = 7.171 (3) Å	µ = 0.23 mm⁻¹
c = 23.045 (8) Å	T = 298 K
β = 92.839 (4)°	Block, colorless
V = 953.5 (6) Å³	0.20 × 0.18 × 0.18 mm
Z = 4

Data collection top

Bruker SMART CCD area-detector diffractometer	1713 independent reflections
Radiation source: fine-focus sealed tube	1424 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.027
ϕ and ω scans	θ_max = 25.2°, θ_min = 1.8°
Absorption correction: multi-scan (SADABS; Bruker, 2001)	h = −6→6
T_min = 0.956, T_max = 0.960	k = −8→6
4632 measured reflections	l = −27→27

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)] = 0.044	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.115	H atoms treated by a mixture of independent and constrained refinement
S = 1.06	w = 1/[σ²(F_o²) + (0.0488P)² + 0.7836P] where P = (F_o² + 2F_c²)/3
1713 reflections	(Δ/σ)_max < 0.001
141 parameters	Δρ_max = 0.29 e Å⁻³
0 restraints	Δρ_min = −0.18 e Å⁻³

Crystal data top

[Mg(C₂H₃O₃)(H₂O)₄]NO₃	V = 953.5 (6) Å³
M_r = 233.43	Z = 4
Monoclinic, P2₁/n	Mo Kα radiation
a = 5.777 (2) Å	µ = 0.23 mm⁻¹
b = 7.171 (3) Å	T = 298 K
c = 23.045 (8) Å	0.20 × 0.18 × 0.18 mm
β = 92.839 (4)°

Data collection top

Bruker SMART CCD area-detector diffractometer	1713 independent reflections
Absorption correction: multi-scan (SADABS; Bruker, 2001)	1424 reflections with I > 2σ(I)
T_min = 0.956, T_max = 0.960	R_int = 0.027
4632 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.044	0 restraints
wR(F²) = 0.115	H atoms treated by a mixture of independent and constrained refinement
S = 1.06	Δρ_max = 0.29 e Å⁻³
1713 reflections	Δρ_min = −0.18 e Å⁻³
141 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.

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 > 2sigma(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) top

	x	y	z	U_iso*/U_eq
Mg1	0.03285 (14)	0.16089 (12)	0.12732 (3)	0.0330 (3)
O2	−0.2625 (3)	0.1820 (3)	0.17242 (7)	0.0381 (5)
O3W	0.3575 (3)	0.1539 (3)	0.09850 (8)	0.0480 (5)
H3W1	0.4864	0.1697	0.1172	0.080 (13)*
H3W2	0.3969	0.1891	0.0652	0.054 (9)*
O1	0.1570 (3)	0.2201 (4)	0.21105 (8)	0.0507 (6)
O1W	−0.1370 (3)	0.0888 (3)	0.05123 (8)	0.0431 (5)
H1W2	−0.1878	0.1479	0.0213	0.065*
H1W1	−0.1967	−0.0171	0.0433	0.065*
O4W	0.0493 (4)	−0.1211 (3)	0.14223 (9)	0.0520 (6)
H4W1	0.0047	−0.1825	0.1712	0.078*
H4W2	0.1424	−0.2007	0.1291	0.078*
O2W	−0.0052 (4)	0.4340 (3)	0.10109 (10)	0.0557 (6)
H2W1	0.0818	0.4998	0.0805	0.083*
H2W2	−0.1280	0.4991	0.0973	0.083*
N1	0.4889 (4)	0.6773 (3)	0.05397 (10)	0.0436 (6)
O4	0.2764 (4)	0.6940 (3)	0.04229 (10)	0.0606 (6)
O6	0.6310 (4)	0.7402 (3)	0.02097 (9)	0.0599 (6)
O5	0.5496 (4)	0.5979 (5)	0.09917 (11)	0.0840 (9)
C2	−0.0077 (5)	0.2379 (5)	0.25407 (12)	0.0396 (6)
C1	−0.2471 (4)	0.2188 (4)	0.22541 (11)	0.0337 (6)
O3	−0.4157 (3)	0.2385 (3)	0.25663 (8)	0.0503 (6)
H1	0.004 (5)	0.352 (5)	0.2734 (14)	0.052 (9)*
H3	0.294 (6)	0.232 (4)	0.2291 (13)	0.048 (8)*
H2	0.019 (5)	0.144 (5)	0.2852 (14)	0.055 (9)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Mg1	0.0246 (4)	0.0441 (5)	0.0305 (4)	−0.0018 (4)	0.0053 (3)	−0.0009 (4)
O2	0.0242 (9)	0.0586 (12)	0.0315 (9)	−0.0037 (8)	0.0030 (7)	−0.0057 (8)
O3W	0.0260 (10)	0.0799 (15)	0.0387 (11)	−0.0066 (9)	0.0068 (8)	0.0017 (10)
O1	0.0214 (10)	0.0941 (17)	0.0368 (10)	−0.0028 (10)	0.0024 (8)	−0.0129 (10)
O1W	0.0464 (11)	0.0480 (11)	0.0342 (10)	−0.0048 (9)	−0.0040 (8)	0.0008 (8)
O4W	0.0674 (14)	0.0443 (12)	0.0464 (11)	0.0072 (10)	0.0232 (10)	0.0089 (9)
O2W	0.0463 (12)	0.0447 (12)	0.0769 (15)	−0.0032 (10)	0.0127 (11)	0.0100 (11)
N1	0.0465 (15)	0.0436 (14)	0.0411 (13)	−0.0027 (11)	0.0062 (11)	0.0033 (10)
O4	0.0420 (13)	0.0704 (16)	0.0692 (15)	−0.0009 (11)	0.0007 (10)	0.0225 (12)
O6	0.0554 (13)	0.0775 (16)	0.0478 (12)	−0.0177 (12)	0.0120 (10)	0.0040 (11)
O5	0.0578 (16)	0.131 (2)	0.0627 (16)	0.0079 (16)	0.0018 (12)	0.0440 (16)
C2	0.0284 (14)	0.0565 (18)	0.0343 (14)	−0.0019 (13)	0.0048 (11)	−0.0107 (14)
C1	0.0268 (13)	0.0393 (14)	0.0353 (13)	−0.0008 (11)	0.0052 (10)	−0.0053 (11)
O3	0.0283 (10)	0.0824 (16)	0.0408 (10)	−0.0016 (10)	0.0083 (8)	−0.0188 (11)

Geometric parameters (Å, º) top

Mg1—O3W	2.021 (2)	O1W—H1W1	0.8499
Mg1—O1W	2.033 (2)	O4W—H4W1	0.8500
Mg1—O2	2.0467 (19)	O4W—H4W2	0.8499
Mg1—O4W	2.052 (2)	O2W—H2W1	0.8499
Mg1—O2W	2.058 (2)	O2W—H2W2	0.8500
Mg1—O1	2.069 (2)	N1—O5	1.223 (3)
O2—C1	1.248 (3)	N1—O6	1.232 (3)
O3W—H3W1	0.8498	N1—O4	1.250 (3)
O3W—H3W2	0.8498	C2—C1	1.509 (4)
O1—C2	1.413 (3)	C2—H1	0.94 (3)
O1—H3	0.88 (3)	C2—H2	0.99 (3)
O1W—H1W2	0.8499	C1—O3	1.247 (3)

O3W—Mg1—O1W	97.25 (8)	Mg1—O1W—H1W2	134.9
O3W—Mg1—O2	168.28 (8)	Mg1—O1W—H1W1	125.8
O1W—Mg1—O2	94.47 (8)	H1W2—O1W—H1W1	98.7
O3W—Mg1—O4W	89.68 (9)	Mg1—O4W—H4W1	129.0
O1W—Mg1—O4W	84.85 (9)	Mg1—O4W—H4W2	128.8
O2—Mg1—O4W	91.19 (8)	H4W1—O4W—H4W2	98.7
O3W—Mg1—O2W	90.83 (9)	Mg1—O2W—H2W1	129.4
O1W—Mg1—O2W	87.06 (9)	Mg1—O2W—H2W2	129.0
O2—Mg1—O2W	89.95 (9)	H2W1—O2W—H2W2	98.7
O4W—Mg1—O2W	171.89 (10)	O5—N1—O6	121.7 (3)
O3W—Mg1—O1	91.56 (8)	O5—N1—O4	117.7 (2)
O1W—Mg1—O1	170.61 (8)	O6—N1—O4	120.6 (2)
O2—Mg1—O1	76.73 (8)	O1—C2—C1	108.6 (2)
O4W—Mg1—O1	92.00 (10)	O1—C2—H1	112 (2)
O2W—Mg1—O1	96.07 (10)	C1—C2—H1	109.3 (19)
C1—O2—Mg1	119.44 (16)	O1—C2—H2	111.1 (19)
Mg1—O3W—H3W1	129.3	C1—C2—H2	111.3 (19)
Mg1—O3W—H3W2	125.7	H1—C2—H2	104 (3)
H3W1—O3W—H3W2	98.8	O3—C1—O2	124.6 (2)
C2—O1—Mg1	117.30 (16)	O3—C1—C2	117.5 (2)
C2—O1—H3	106 (2)	O2—C1—C2	117.8 (2)
Mg1—O1—H3	136 (2)

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O3W—H3W1···O2ⁱ	0.85	1.88	2.719 (3)	167
O3W—H3W2···O6ⁱⁱ	0.85	2.05	2.860 (3)	160
O1—H3···O3ⁱ	0.88 (3)	1.76 (3)	2.638 (3)	172 (3)
O1W—H1W2···O4ⁱⁱⁱ	0.85	1.90	2.747 (3)	173
O1W—H1W1···O6^iv	0.85	2.06	2.905 (3)	174
O4W—H4W1···O3^v	0.85	1.85	2.687 (3)	166
O4W—H4W2···O4^vi	0.85	2.31	3.014 (3)	141
O2W—H2W1···O4	0.85	2.02	2.860 (3)	169
O2W—H2W2···O5^vii	0.85	2.00	2.826 (3)	166

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

Experimental details

Crystal data
Chemical formula	[Mg(C₂H₃O₃)(H₂O)₄]NO₃
M_r	233.43
Crystal system, space group	Monoclinic, P2₁/n
Temperature (K)	298
a, b, c (Å)	5.777 (2), 7.171 (3), 23.045 (8)
β (°)	92.839 (4)
V (Å³)	953.5 (6)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	0.23
Crystal size (mm)	0.20 × 0.18 × 0.18

Data collection
Diffractometer	Bruker SMART CCD area-detector diffractometer
Absorption correction	Multi-scan (SADABS; Bruker, 2001)
T_min, T_max	0.956, 0.960
No. of measured, independent and observed [I > 2σ(I)] reflections	4632, 1713, 1424
R_int	0.027
(sin θ/λ)_max (Å⁻¹)	0.599

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.044, 0.115, 1.06
No. of reflections	1713
No. of parameters	141
H-atom treatment	H atoms treated by a mixture of independent and constrained refinement
Δρ_max, Δρ_min (e Å⁻³)	0.29, −0.18

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

Selected bond lengths (Å) top

Mg1—O3W	2.021 (2)	Mg1—O4W	2.052 (2)
Mg1—O1W	2.033 (2)	Mg1—O2W	2.058 (2)
Mg1—O2	2.0467 (19)	Mg1—O1	2.069 (2)

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O3W—H3W1···O2ⁱ	0.85	1.88	2.719 (3)	167
O3W—H3W2···O6ⁱⁱ	0.85	2.05	2.860 (3)	160
O1—H3···O3ⁱ	0.88 (3)	1.76 (3)	2.638 (3)	172 (3)
O1W—H1W2···O4ⁱⁱⁱ	0.85	1.90	2.747 (3)	173
O1W—H1W1···O6^iv	0.85	2.06	2.905 (3)	174
O4W—H4W1···O3^v	0.85	1.85	2.687 (3)	166
O4W—H4W2···O4^vi	0.85	2.31	3.014 (3)	141
O2W—H2W1···O4	0.85	2.02	2.860 (3)	169
O2W—H2W2···O5^vii	0.85	2.00	2.826 (3)	166

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

Acknowledgements

This work was supported financially by the NSFC (grants 20971047 and U0734005), Guangdong Provincial Science and Technology Bureau (grant 2008B010600009) and the Key Research Program of Guangdong Provincial Universities Science and Technology innovation (grant cxzd1020).

References

Bruker (2001). SMART, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Erxleben, A. & Schumacher, D. (2001). Eur. J. Inorg. Chem. pp. 3039–3046. CrossRef Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar