Poly[bis­(N,N-dimethyl­formamide-κO)(μ4-naphthalene-1,5-disulfonato)magnesium(II)]

Borkowski, L.A.; Banerjee, D.; Parise, J.B.

doi:10.1107/S1600536810017952

metal-organic compounds

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ISSN: 2056-9890

Volume 66| Part 6| June 2010| Pages m691-m692

https://doi.org/10.1107/S1600536810017952

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Poly[bis(N,N-dimethylformamide-κO)(μ₄-naphthalene-1,5-disulfonato)magnesium(II)]

Lauren A. Borkowski,^a ^* Debasis Banerjee ^b and John B. Parise ^c

^aStony Brook University, Mineral Physics Institute, 255 ESS Building, Stony Brook, NY 11794, USA, ^bDepartment of Chemistry, Stony Brook University, 255 ESS Building, Stony Brook, NY 11794-2100, USA, and ^cDepartment of Geosciences, Department of Chemistry, Stony Brook University, 255 ESS Building, Stony Brook, NY 11794-2100, USA
^*Correspondence e-mail: lauren.borkowski@stonybrook.edu

(Received 19 April 2010; accepted 14 May 2010; online 22 May 2010)

The structure of the title compound, [Mg(C₁₀H₆O₆S₂)(C₃H₇NO)₂]_n, consists of MgO₆ octahedra ( $[\overline{1}]$ symmetry) connected to naphthalene-1,5-disulfonate ligands ( $[\overline{1}]$ symmetry) in the equatoral plane, forming a two-dimensional network propagating parallel to (010). The coordination sphere of the Mg atom is completed by the O atoms of two N,N-dimethylformamide (DMF) molecules in the axial positions. The title compound represents the first time the naphthalene-1,5-disulfonate anion is bound directly to a Mg²⁺ atom. Disorder over two positions was found in the DMF molecule in a 0.518 (8):0.482 (8) ratio.

Related literature

For background to metal-organic coordination polymers (CPs) and frameworks (MOFs), see: Cheetham et al. (2006 ); Kitagawa et al. (2004 ); Rosseinsky (2004 ); Rowsell & Yaghi (2004 ). For structures in which Mg²⁺ is not directly linked to naphthalenedisulfonate ligands but is surrounded by water molecules, see: Cody & Hazel (1977 ); Morris et al. (2003 ); Shakeri & Haussühl (1992 ).

Experimental

Crystal data

[Mg(C₁₀H₆O₆S₂)(C₃H₇NO)₂]
M_r = 456.79
Triclinic, $[P \overline 1]$
a = 5.1328 (2) Å
b = 9.3890 (4) Å
c = 10.4029 (4) Å
α = 85.158 (1)°
β = 75.638 (1)°
γ = 79.501 (1)°
V = 477.13 (3) Å³
Z = 1
Synchrotron radiation
λ = 0.41328 Å
μ = 0.08 mm⁻¹
T = 100 K
0.09 × 0.03 × 0.01 mm

Data collection

Bruker APEXII CCD diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2008 ) T_min = 0.993, T_max = 0.999
8811 measured reflections
1961 independent reflections
1721 reflections with I > 2σ(I)
R_int = 0.054

Refinement

R[F² > 2σ(F²)] = 0.032
wR(F²) = 0.087
S = 1.04
1961 reflections
221 parameters
6 restraints
Only H-atom coordinates refined
Δρ_max = 0.61 e Å⁻³
Δρ_min = −0.51 e Å⁻³

Table 1
Selected bond lengths (Å)

Mg1—O1	2.0193 (11)
Mg1—O2ⁱ	2.0429 (11)
Mg1—O4	2.1562 (11)
Symmetry code: (i) x+1, y, z.

Data collection: APEX2 (Bruker, 2007 ); cell refinement: SAINT-Plus (Bruker, 2007); data reduction: SAINT-Plus; program(s) used to solve structure: SIR2004 (Burla et al., 2005 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ); molecular graphics: CrystalMaker (CrystalMaker, 2009 ); software used to prepare material for publication: enCIFer (Allen et al., 2004 ).

Supporting information

Crystal structure: contains datablocks global, I. DOI: https://doi.org/10.1107/S1600536810017952/wm2328sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536810017952/wm2328Isup2.hkl

checkCIF report

Comment top

Interest in metal organic coordination polymers (CPs) and frameworks (MOFs) arises due to the potential applications including size/shape catalysis and gas storage/separation (Cheetham et al., 2006; Kitagawa et al., 2004; Rosseinsky, 2004; Rowsell & Yaghi, 2004). This is owing to the fact that these materials have similar properties to zeolites with the added possiblity of structural design. Three factors need to be considered during the sythesis of CPs and MOFs; the coordination sphere of the metal center, the size, shape and functionality of the organic linker and the synthetic conditions.

Previous studies have looked at the interaction between a variety of metal atoms and 1,5-naphthalenedisulfonic acid. A search of the literature results in examples of direct bonding between this ligand and every alkali and alkali earth metal except Mg²⁺. Due to perodic trends we suspected that Mg²⁺ and naphthalene-1,5-disulfonate should have a direct bonding interaction, which indicates a change in synthetic conditions compared to the previous studies was needed. The previous efforts used water as the solvent resulting in structures where the Mg²⁺ atoms are bound solely to water molecules and interacted with 1,5-naphthalenedisulfonic acid through hydrogen bonds (Cody & Hazel, 1977; Morris et al., 2003; Shakeri & Haussühl, 1992). In our study we used N,N-dimethylformamide (DMF) as the solvent with the thought that DMF is a large solvent molecule and is unlikely to complete for the coordination sphere of the Mg²⁺ atom.

The title compound consists of MgO₆ octahedra linked by 1,5- naphthalenedisulfonate ligands to form a two-dimensional network parallel to (010). The Mg²⁺ atom is bound to four O atoms from four separate naphthalene-1,5-disulfonate ligands in the equitorial plane and two O atoms from two symmetry equivalent N,N-dimethylformamide molecules in the axial positions (Figure 1). The average equitorial Mg—O bond length is 2.031 Å whereas the axial bond length is slightly longer at 2.156 Å (Table 1). The individual MgO₆ octahedra are connected by the naphthalene-1,5-disulfonate linkers in a bridging bidentate fashion to form chains along the [100] direction, which are further connected by the linker molecules to form an overall 2-dimensional structure (Figure 2).

Related literature top

For background to metal-organic coordination polymers (CPs) and frameworks (MOFs), see: Cheetham et al. (2006); Kitagawa et al. (2004); Rosseinsky (2004); Rowsell & Yaghi (2004). For structures in which Mg²⁺ is not directly linked to naphthalenedisulfonate ligands but is surrounded by water molecules, see: Cody & Hazel (1977); Morris et al. (2003); Shakeri & Haussühl (1992).

Experimental top

All of the starting materials are available commercially and were used without any further purification. Magnesium nitrate hexahydrate (Mg(NO₃)₂^.6H₂O, 1.3 grams), 1,5-naphthalenedisulfonic acid tetrahydrate (C₁₀H₈S₂O₆ 4H₂O, 1.87 grams) and ammonium fluoride (NH₄F, 0.021 grams) were dissolved in 15 grams of N,N-dimethylformamide (DMF). The solution was prepared in a 23 mL Teflon lined Parr bomb and stirred for three hours to achieve homogeneity. The resulting solution was heated statically at 373 K for three days. Colorless needle shaped crystals were recovered and were washed with ethanol.

Structure description top

For background to metal-organic coordination polymers (CPs) and frameworks (MOFs), see: Cheetham et al. (2006); Kitagawa et al. (2004); Rosseinsky (2004); Rowsell & Yaghi (2004). For structures in which Mg²⁺ is not directly linked to naphthalenedisulfonate ligands but is surrounded by water molecules, see: Cody & Hazel (1977); Morris et al. (2003); Shakeri & Haussühl (1992).

Computing details top

Data collection: APEX2 (Bruker, 2007); cell refinement: SAINT-Plus (Bruker, 2007); data reduction: SAINT-Plus (Bruker, 2007); program(s) used to solve structure: SIR2004 (Burla et al., 2005); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: CrystalMaker (CrystalMaker, 2009); software used to prepare material for publication: enCIFer (Allen et al., 2004).

Figures top

Fig. 1. Polyhedral representation of a layer of the title compound. The DMF disorder and the H atoms were omitted for clarity. Color codes: blue octahedra Mg, red spheres O, light blue spheres N, and black lines C.

Poly[bis(N,N-dimethylformamide-κO)(µ₄- naphthalene-1,5-disulfonato)magnesium(II)] top

Crystal data top

[Mg(C₁₀H₆O₆S₂)(C₃H₇NO)₂]	Z = 1
M_r = 456.79	F(000) = 238
Triclinic, P1	D_x = 1.590 Mg m⁻³
Hall symbol: -P 1	Synchrotron radiation, λ = 0.41328 Å
a = 5.1328 (2) Å	Cell parameters from 4827 reflections
b = 9.3890 (4) Å	θ = 2.4–17.1°
c = 10.4029 (4) Å	µ = 0.08 mm⁻¹
α = 85.158 (1)°	T = 100 K
β = 75.638 (1)°	Needle, colorless
γ = 79.501 (1)°	0.09 × 0.03 × 0.01 mm
V = 477.13 (3) Å³

Data collection top

Bruker APEXII CCD diffractometer	1961 independent reflections
Radiation source: APS Sector 15	1721 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.054
phi scans	θ_max = 15.0°, θ_min = 1.3°
Absorption correction: multi-scan (SADABS; Bruker, 2008)	h = −6→6
T_min = 0.993, T_max = 0.999	k = −11→11
8811 measured reflections	l = −12→12

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)] = 0.032	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.087	Only H-atom coordinates refined
S = 1.04	w = 1/[σ²(F_o²) + (0.0481P)² + 0.2091P] where P = (F_o² + 2F_c²)/3
1961 reflections	(Δ/σ)_max < 0.001
221 parameters	Δρ_max = 0.61 e Å⁻³
6 restraints	Δρ_min = −0.51 e Å⁻³

Crystal data top

[Mg(C₁₀H₆O₆S₂)(C₃H₇NO)₂]	γ = 79.501 (1)°
M_r = 456.79	V = 477.13 (3) Å³
Triclinic, P1	Z = 1
a = 5.1328 (2) Å	Synchrotron radiation, λ = 0.41328 Å
b = 9.3890 (4) Å	µ = 0.08 mm⁻¹
c = 10.4029 (4) Å	T = 100 K
α = 85.158 (1)°	0.09 × 0.03 × 0.01 mm
β = 75.638 (1)°

Data collection top

Bruker APEXII CCD diffractometer	1961 independent reflections
Absorption correction: multi-scan (SADABS; Bruker, 2008)	1721 reflections with I > 2σ(I)
T_min = 0.993, T_max = 0.999	R_int = 0.054
8811 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.032	6 restraints
wR(F²) = 0.087	Only H-atom coordinates refined
S = 1.04	Δρ_max = 0.61 e Å⁻³
1961 reflections	Δρ_min = −0.51 e Å⁻³
221 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 > 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) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
S1	0.07457 (7)	0.11525 (4)	0.80723 (4)	0.00723 (15)
Mg1	0.5000	0.0000	1.0000	0.00731 (19)
O1	0.2916 (2)	0.11924 (12)	0.87562 (11)	0.0100 (3)
O2	−0.1359 (2)	0.04071 (13)	0.88296 (11)	0.0117 (3)
O3	−0.0320 (2)	0.25885 (12)	0.76873 (12)	0.0123 (3)
O4	0.5528 (2)	−0.18505 (12)	0.88102 (12)	0.0115 (3)
C1	0.4500 (3)	0.04297 (17)	0.56082 (16)	0.0084 (3)
C2	0.2241 (3)	0.00625 (17)	0.65774 (15)	0.0088 (3)
C3	0.1051 (3)	−0.10819 (18)	0.63682 (17)	0.0113 (3)
H3	−0.048 (4)	−0.127 (2)	0.698 (2)	0.014*
C4	0.4211 (3)	−0.16097 (18)	0.42018 (17)	0.0103 (3)
H4	0.474 (4)	−0.216 (2)	0.343 (2)	0.012*
C5	0.2054 (4)	−0.19167 (19)	0.51598 (17)	0.0135 (4)
H5	0.112 (4)	−0.269 (2)	0.503 (2)	0.016*
C6	0.3941 (13)	−0.2695 (7)	0.8776 (6)	0.0152 (12)	0.518 (8)
H6	0.213 (9)	−0.258 (4)	0.935 (4)	0.018*	0.518 (8)
N1	0.4566 (15)	−0.3857 (7)	0.7960 (6)	0.0128 (13)	0.518 (8)
C7	0.2600 (9)	−0.4804 (5)	0.7982 (5)	0.0269 (13)	0.518 (8)
H7A	0.355 (14)	−0.580 (7)	0.827 (7)	0.040*	0.518 (8)
H7B	0.089 (11)	−0.435 (6)	0.866 (5)	0.040*	0.518 (8)
H7C	0.224 (10)	−0.489 (6)	0.713 (6)	0.040*	0.518 (8)
C8	0.7147 (16)	−0.4185 (7)	0.6958 (6)	0.0182 (13)	0.518 (8)
H8A	0.809 (13)	−0.505 (9)	0.686 (7)	0.027*	0.518 (8)
H8B	0.683 (11)	−0.383 (6)	0.620 (5)	0.027*	0.518 (8)
H8C	0.839 (10)	−0.384 (5)	0.721 (5)	0.027*	0.518 (8)
C6'	0.4544 (12)	−0.2955 (6)	0.9149 (6)	0.0098 (11)	0.482 (8)
H6'	0.362 (9)	−0.313 (5)	1.007 (5)	0.012*	0.482 (8)
N1'	0.4704 (16)	−0.4086 (8)	0.8350 (7)	0.0108 (13)	0.482 (8)
C7'	0.3529 (8)	−0.5363 (4)	0.8827 (4)	0.0154 (13)	0.482 (8)
H7A'	0.228 (11)	−0.544 (8)	0.839 (6)	0.023*	0.482 (8)
H7B'	0.500 (10)	−0.625 (5)	0.860 (5)	0.023*	0.482 (8)
H7C'	0.279 (9)	−0.520 (5)	0.977 (5)	0.023*	0.482 (8)
C8'	0.6042 (17)	−0.4110 (8)	0.6929 (6)	0.0157 (14)	0.482 (8)
H8A'	0.751 (13)	−0.511 (9)	0.678 (7)	0.024*	0.482 (8)
H8B'	0.674 (10)	−0.320 (6)	0.674 (5)	0.024*	0.482 (8)
H8C'	0.469 (11)	−0.418 (5)	0.651 (5)	0.024*	0.482 (8)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
S1	0.0075 (2)	0.0079 (2)	0.0062 (2)	−0.00348 (15)	−0.00026 (15)	0.00097 (15)
Mg1	0.0080 (4)	0.0073 (4)	0.0069 (4)	−0.0044 (3)	−0.0006 (3)	0.0014 (3)
O1	0.0109 (5)	0.0108 (6)	0.0091 (6)	−0.0057 (4)	−0.0027 (4)	0.0039 (5)
O2	0.0097 (5)	0.0156 (6)	0.0103 (6)	−0.0080 (5)	0.0006 (4)	0.0010 (5)
O3	0.0140 (6)	0.0089 (6)	0.0134 (6)	−0.0014 (5)	−0.0038 (5)	0.0028 (5)
O4	0.0138 (6)	0.0098 (6)	0.0116 (6)	−0.0058 (5)	−0.0016 (5)	0.0002 (5)
C1	0.0093 (7)	0.0077 (8)	0.0085 (8)	−0.0017 (6)	−0.0031 (6)	0.0018 (6)
C2	0.0099 (7)	0.0090 (8)	0.0072 (8)	−0.0012 (6)	−0.0022 (6)	0.0009 (6)
C3	0.0116 (8)	0.0126 (8)	0.0098 (8)	−0.0062 (6)	−0.0005 (6)	0.0025 (6)
C4	0.0138 (8)	0.0093 (8)	0.0083 (8)	−0.0051 (6)	−0.0013 (6)	−0.0007 (6)
C5	0.0173 (8)	0.0120 (8)	0.0134 (8)	−0.0104 (7)	−0.0019 (7)	−0.0004 (7)
C6	0.016 (3)	0.020 (3)	0.012 (3)	−0.0077 (19)	−0.0046 (19)	−0.001 (2)
N1	0.020 (2)	0.010 (2)	0.011 (3)	−0.0105 (18)	−0.004 (2)	0.002 (2)
C7	0.032 (2)	0.022 (2)	0.031 (3)	−0.0188 (19)	−0.0045 (19)	−0.0054 (19)
C8	0.020 (3)	0.015 (3)	0.017 (2)	−0.001 (3)	−0.002 (3)	−0.0009 (16)
C6'	0.010 (2)	0.011 (2)	0.010 (3)	−0.0038 (18)	−0.0023 (18)	−0.004 (2)
N1'	0.012 (2)	0.008 (2)	0.010 (3)	−0.0034 (17)	0.000 (2)	0.002 (2)
C7'	0.0156 (19)	0.008 (2)	0.022 (3)	−0.0054 (14)	−0.0012 (16)	−0.0012 (16)
C8'	0.018 (3)	0.016 (2)	0.014 (3)	−0.004 (3)	−0.003 (3)	−0.0018 (16)

Geometric parameters (Å, º) top

S1—O3	1.4234 (12)	C5—H5	0.98 (2)
S1—O2	1.4276 (12)	C6—N1	1.381 (8)
S1—O1	1.4701 (11)	C6—H6	0.97 (4)
S1—C2	1.8560 (16)	N1—C7	1.456 (7)
Mg1—O1	2.0193 (11)	N1—C8	1.469 (9)
Mg1—O1ⁱ	2.0193 (11)	C7—H7A	1.03 (7)
Mg1—O2ⁱⁱ	2.0429 (11)	C7—H7B	1.03 (6)
Mg1—O2ⁱⁱⁱ	2.0429 (11)	C7—H7C	0.97 (6)
Mg1—O4ⁱ	2.1562 (11)	C8—H8A	0.87 (9)
Mg1—O4	2.1562 (11)	C8—H8B	0.87 (5)
O2—Mg1^iv	2.0429 (11)	C8—H8C	0.87 (5)
O4—C6'	1.223 (6)	C6'—N1'	1.382 (8)
O4—C6	1.244 (6)	C6'—H6'	0.97 (5)
C1—C2	1.409 (2)	N1'—C7'	1.436 (7)
C1—C4^v	1.440 (2)	N1'—C8'	1.468 (8)
C1—C1^v	1.488 (3)	C7'—H7A'	0.89 (6)
C2—C3	1.386 (2)	C7'—H7B'	1.02 (5)
C3—C5	1.469 (2)	C7'—H7C'	0.97 (5)
C3—H3	0.92 (2)	C8'—H8A'	1.09 (9)
C4—C5	1.350 (2)	C8'—H8B'	0.98 (5)
C4—C1^v	1.440 (2)	C8'—H8C'	0.92 (5)
C4—H4	0.95 (2)

O3—S1—O2	111.65 (7)	C3—C5—H5	119.7 (12)
O3—S1—O1	109.59 (7)	O4—C6—N1	124.7 (6)
O2—S1—O1	113.33 (7)	O4—C6—H6	120 (2)
O3—S1—C2	109.78 (7)	N1—C6—H6	115 (2)
O2—S1—C2	104.07 (7)	O4—C6—H6'	94.7 (18)
O1—S1—C2	108.22 (7)	N1—C6—H6'	111.8 (18)
O1—Mg1—O1ⁱ	180.00 (4)	H6—C6—H6'	61 (3)
O1—Mg1—O2ⁱⁱ	91.70 (5)	C6—N1—C7	121.5 (6)
O1ⁱ—Mg1—O2ⁱⁱ	88.30 (5)	C6—N1—C8	123.5 (6)
O1—Mg1—O2ⁱⁱⁱ	88.30 (5)	C7—N1—C8	114.9 (6)
O1ⁱ—Mg1—O2ⁱⁱⁱ	91.70 (5)	N1—C7—H7A	103 (4)
O2ⁱⁱ—Mg1—O2ⁱⁱⁱ	180.0	N1—C7—H7B	104 (3)
O1—Mg1—O4ⁱ	90.98 (5)	H7A—C7—H7B	115 (5)
O1ⁱ—Mg1—O4ⁱ	89.02 (5)	N1—C7—H7C	114 (3)
O2ⁱⁱ—Mg1—O4ⁱ	93.38 (5)	H7A—C7—H7C	108 (5)
O2ⁱⁱⁱ—Mg1—O4ⁱ	86.62 (4)	H7B—C7—H7C	112 (4)
O1—Mg1—O4	89.02 (5)	N1—C8—H8A	123 (5)
O1ⁱ—Mg1—O4	90.98 (5)	N1—C8—H8B	107 (4)
O2ⁱⁱ—Mg1—O4	86.62 (4)	H8A—C8—H8B	110 (6)
O2ⁱⁱⁱ—Mg1—O4	93.38 (5)	N1—C8—H8C	108 (3)
O4ⁱ—Mg1—O4	180.0	H8A—C8—H8C	94 (5)
S1—O1—Mg1	141.82 (7)	H8B—C8—H8C	115 (5)
S1—O2—Mg1^iv	161.80 (8)	N1'—C6'—H6'	113 (2)
C6'—O4—Mg1	126.6 (3)	C6'—N1'—C7'	123.1 (5)
C6—O4—Mg1	130.9 (3)	C6'—N1'—C8'	124.2 (6)
C2—C1—C4^v	120.44 (15)	C7'—N1'—C8'	112.7 (6)
C2—C1—C1^v	118.31 (17)	N1'—C7'—H7A'	109 (5)
C4^v—C1—C1^v	121.26 (18)	N1'—C7'—H7B'	109 (3)
C3—C2—C1	119.08 (15)	H7A'—C7'—H7B'	106 (5)
C3—C2—S1	120.03 (12)	N1'—C7'—H7C'	103 (3)
C1—C2—S1	120.80 (12)	H7A'—C7'—H7C'	114 (5)
C2—C3—C5	122.01 (15)	H7B'—C7'—H7C'	116 (4)
C2—C3—H3	117.9 (12)	N1'—C8'—H8A'	107 (4)
C5—C3—H3	119.9 (12)	N1'—C8'—H8B'	104 (3)
C5—C4—C1^v	118.10 (15)	H8A'—C8'—H8B'	118 (5)
C5—C4—H4	118.1 (12)	N1'—C8'—H8C'	105 (3)
C1^v—C4—H4	123.7 (12)	H8A'—C8'—H8C'	107 (4)
C4—C5—C3	121.24 (15)	H8B'—C8'—H8C'	115 (4)
C4—C5—H5	119.0 (12)

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

Experimental details

Crystal data
Chemical formula	[Mg(C₁₀H₆O₆S₂)(C₃H₇NO)₂]
M_r	456.79
Crystal system, space group	Triclinic, P1
Temperature (K)	100
a, b, c (Å)	5.1328 (2), 9.3890 (4), 10.4029 (4)
α, β, γ (°)	85.158 (1), 75.638 (1), 79.501 (1)
V (Å³)	477.13 (3)
Z	1
Radiation type	Synchrotron, λ = 0.41328 Å
µ (mm⁻¹)	0.08
Crystal size (mm)	0.09 × 0.03 × 0.01

Data collection
Diffractometer	Bruker APEXII CCD
Absorption correction	Multi-scan (SADABS; Bruker, 2008)
T_min, T_max	0.993, 0.999
No. of measured, independent and observed [I > 2σ(I)] reflections	8811, 1961, 1721
R_int	0.054
(sin θ/λ)_max (Å⁻¹)	0.625

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.032, 0.087, 1.04
No. of reflections	1961
No. of parameters	221
No. of restraints	6
H-atom treatment	Only H-atom coordinates refined
Δρ_max, Δρ_min (e Å⁻³)	0.61, −0.51

Computer programs: APEX2 (Bruker, 2007), SAINT-Plus (Bruker, 2007), SIR2004 (Burla et al., 2005), SHELXL97 (Sheldrick, 2008), CrystalMaker (CrystalMaker, 2009), enCIFer (Allen et al., 2004).

Selected bond lengths (Å) top

Mg1—O1	2.0193 (11)	Mg1—O4	2.1562 (11)
Mg1—O2ⁱ	2.0429 (11)

Symmetry code: (i) x+1, y, z.

Acknowledgements

This work was supported by the National Science Foundation (DMR-0800415). The authors would like to thank Yu-Sheng Chen at ChemMatCARS, APS, for his assistance during the data collection. ChemMatCARS (APS, Sector 15) is principally supported by the National Science Foundation/Department of Energy under grant No. CHE-0535644. Use of the Advance Photon Source was supported by the US Department of Energy, Office of Science, Office of Basic Energy Sciences, under Contract No. DE—AC02-06CH11357.

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