Poly[[hexa-μ-aqua-diaqua-bis-(μ₄-dihydrogen benzene-1,2,4,5-tetra-carboxyl-ato)magnesiumdisodium] dihydrate].

The asymmetric unit of the title compound, {[MgNa₂(C₁₀H₄O₈)₂(H₂O)₈]·2H₂O}(n), contains one octa-hedrally coordin-ated Mg(II) atom (site symmetry 2/m), one octahedrally coordinated Na(I) atom (site symmetry 2) and one half of the dihydrogen benzene-1,2,4,5-tetra-carboxyl-ate (btec) ligand, the second half of the ligand being generated by a twofold rotation axis. The basic framework of the title compound features infinite (-Na-Na-Mg-)(n) chains along [10-1] with the metal cations bridged by the coordinating water molecules. The chains are isolated from each other by μ₄-bridging btec ligands, which form inter-molecular O-H⋯O hydrogen bonds to uncoordinated water mol-ecules and the coordinated water mol-ecules of a neighbouring chain. In each btec ligand, there are also intramolecular O-H⋯O hydrogen bonds.

Related literature

For structures based on the H4btec ligand, see: Gong & Zhang (2011 ▶); Liu et al. (2009 ▶, 2010 ▶); Zhang et al. (2007 ▶).

Experimental

Crystal data

[MgNa2(C10H4O8)2(H2O)8]·2H2O

M = 754.71

Monoclinic,

a = 7.3335 (13) Å

b = 20.155 (4) Å

c = 10.4450 (18) Å

β = 103.325 (3)°

V = 1502.3 (5) Å3

Z = 2

Mo Kα radiation

μ = 0.20 mm−1

T = 296 K

0.20 × 0.05 × 0.05 mm

Data collection

Bruker APEXII CCD area-detector diffractometer

Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T min = 0.961, T max = 0.990

4088 measured reflections

1440 independent reflections

1272 reflections with I > 2σ(I)

R int = 0.022

Refinement

R[F 2 > 2σ(F 2)] = 0.030

wR(F 2) = 0.089

S = 1.08

1440 reflections

122 parameters

H-atom parameters constrained

Δρmax = 0.23 e Å−3

Δρmin = −0.21 e Å−3

Data collection: APEX2 (Bruker, 2008 ▶); cell refinement: SAINT (Bruker, 2008 ▶); 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.

Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536812024634/ez2296sup1.cif

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536812024634/ez2296Isup2.hkl

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

[MgNa2(C10H4O8)2(H2O)8]·2H2O	F(000) = 780
Mr = 754.71	Dx = 1.668 Mg m−3
Monoclinic, C2/m	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2y	Cell parameters from 2031 reflections
a = 7.3335 (13) Å	θ = 2.9–27.8°
b = 20.155 (4) Å	µ = 0.20 mm−1
c = 10.4450 (18) Å	T = 296 K
β = 103.325 (3)°	Prism, colourless
V = 1502.3 (5) Å3	0.20 × 0.05 × 0.05 mm
Z = 2

Bruker APEXII CCD area-detector diffractometer	1440 independent reflections
Radiation source: fine-focus sealed tube	1272 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.022
Detector resolution: 83.33 pixels mm-1	θmax = 25.5°, θmin = 2.0°
ω scans	h = −8→8
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	k = −24→22
Tmin = 0.961, Tmax = 0.990	l = −11→12
4088 measured reflections

Refinement on F2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.030	H-atom parameters constrained
wR(F2) = 0.089	w = 1/[σ2(Fo2) + (0.0445P)2 + 0.7471P] where P = (Fo2 + 2Fc2)/3
S = 1.08	(Δ/σ)max < 0.001
1440 reflections	Δρmax = 0.23 e Å−3
122 parameters	Δρmin = −0.21 e Å−3
0 restraints	Extinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0033 (7)

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.

	x	y	z	Uiso*/Ueq
Mg1	0.0000	0.0000	0.0000	0.0220 (2)
Na1	0.31699 (13)	0.0000	0.32732 (8)	0.0356 (3)
O1	0.30603 (18)	0.11183 (5)	0.30357 (11)	0.0464 (3)
C1	0.5000	0.18685 (9)	0.5000	0.0233 (4)
H1	0.5000	0.1407	0.5000	0.028*
O2	0.20225 (19)	0.31210 (6)	0.17351 (10)	0.0487 (4)
C2	0.5000	0.32051 (9)	0.5000	0.0221 (4)
H2	0.5000	0.3667	0.5000	0.027*
O3	0.20002 (18)	0.19389 (6)	0.17286 (10)	0.0481 (4)
H3	0.2132	0.2456	0.1607	0.072*
C3	0.39709 (18)	0.28869 (6)	0.38857 (12)	0.0211 (3)
O4	0.31030 (15)	0.39579 (5)	0.30165 (10)	0.0339 (3)
C4	0.39692 (18)	0.21864 (6)	0.38884 (12)	0.0214 (3)
O5	0.28991 (19)	0.0000	0.08188 (14)	0.0288 (3)
H5	0.3530	0.0340	0.0564	0.043*
C5	0.2960 (2)	0.17086 (7)	0.28270 (14)	0.0283 (3)
O6	0.3317 (3)	0.0000	0.56419 (17)	0.0483 (5)
H6	0.2884	−0.0368	0.5963	0.073*
C6	0.29702 (19)	0.33570 (7)	0.28103 (13)	0.0258 (3)
O7	0.5000	0.09605 (7)	0.0000	0.0311 (3)
H7	0.4367	0.1223	−0.0590	0.047*
O8	0.0000	0.10073 (7)	0.0000	0.0322 (4)
H8	−0.0681	0.1262	−0.0560	0.048*
O9	0.0320 (2)	0.0000	−0.19461 (14)	0.0314 (4)
H9	0.0897	0.0325	−0.2191	0.047*

	U11	U22	U33	U12	U13	U23
Mg1	0.0265 (5)	0.0161 (4)	0.0222 (5)	0.000	0.0032 (4)	0.000
Na1	0.0521 (6)	0.0188 (4)	0.0328 (5)	0.000	0.0034 (4)	0.000
O1	0.0678 (8)	0.0176 (6)	0.0428 (7)	−0.0038 (5)	−0.0098 (6)	−0.0044 (5)
C1	0.0259 (10)	0.0152 (9)	0.0275 (10)	0.000	0.0037 (8)	0.000
O2	0.0697 (8)	0.0256 (6)	0.0343 (6)	0.0023 (5)	−0.0222 (6)	0.0038 (5)
C2	0.0262 (9)	0.0136 (9)	0.0258 (10)	0.000	0.0046 (8)	0.000
O3	0.0683 (8)	0.0244 (6)	0.0350 (6)	−0.0028 (5)	−0.0224 (6)	−0.0032 (5)
C3	0.0216 (7)	0.0186 (7)	0.0225 (7)	0.0007 (5)	0.0038 (5)	0.0014 (5)
O4	0.0478 (7)	0.0177 (5)	0.0335 (6)	0.0032 (4)	0.0040 (5)	0.0050 (4)
C4	0.0215 (6)	0.0185 (7)	0.0231 (7)	−0.0010 (5)	0.0031 (5)	−0.0012 (5)
O5	0.0280 (7)	0.0221 (7)	0.0363 (8)	0.000	0.0070 (6)	0.000
C5	0.0318 (8)	0.0214 (7)	0.0282 (7)	−0.0012 (6)	0.0000 (6)	−0.0036 (6)
O6	0.0713 (12)	0.0291 (8)	0.0533 (11)	0.000	0.0321 (9)	0.000
C6	0.0282 (7)	0.0211 (7)	0.0263 (7)	0.0011 (5)	0.0028 (6)	0.0028 (6)
O7	0.0357 (8)	0.0214 (7)	0.0304 (8)	0.000	−0.0046 (6)	0.000
O8	0.0419 (9)	0.0162 (7)	0.0299 (8)	0.000	−0.0094 (6)	0.000
O9	0.0469 (9)	0.0185 (7)	0.0324 (8)	0.000	0.0166 (7)	0.000

Mg1—O8	2.0301 (14)	O2—C6	1.2691 (17)
Mg1—O8i	2.0302 (14)	O2—H3	1.3505
Mg1—O9	2.0992 (14)	C2—C3	1.3895 (15)
Mg1—O9i	2.0992 (14)	C2—C3iv	1.3895 (15)
Mg1—O5i	2.1008 (14)	C2—H2	0.9300
Mg1—O5	2.1008 (14)	O3—C5	1.2865 (17)
Mg1—Na1i	3.6645 (10)	O3—H3	1.0579
Mg1—Na1	3.6646 (10)	C3—C4	1.4119 (18)
Na1—O1	2.2669 (12)	C3—C6	1.5225 (18)
Na1—O1ii	2.2669 (12)	O4—C6	1.2301 (17)
Na1—O6	2.4515 (19)	C4—C5	1.5250 (18)
Na1—O5	2.5252 (16)	O5—H5	0.9007
Na1—O6iii	2.564 (2)	O6—Na1iii	2.564 (2)
Na1—O9i	2.6146 (18)	O6—H6	0.9011
Na1—Na1iii	3.9692 (17)	O7—H7	0.8628
O1—C5	1.2088 (18)	O8—H8	0.8481
C1—C4	1.3876 (15)	O9—Na1i	2.6146 (17)
C1—C4iv	1.3876 (15)	O9—H9	0.8510
C1—H1	0.9300
O8—Mg1—O8i	180.0	O1ii—Na1—Mg1	84.21 (4)
O8—Mg1—O9	90.0	O6—Na1—Mg1	144.34 (6)
O8i—Mg1—O9	90.0	O5—Na1—Mg1	33.73 (3)
O8—Mg1—O9i	90.0	O6iii—Na1—Mg1	140.26 (5)
O8i—Mg1—O9i	90.0	O9i—Na1—Mg1	34.15 (3)
O9—Mg1—O9i	180.00 (8)	O1—Na1—Na1iii	95.68 (4)
O8—Mg1—O5i	90.0	O1ii—Na1—Na1iii	95.68 (4)
O8i—Mg1—O5i	90.0	O6—Na1—Na1iii	38.69 (5)
O9—Mg1—O5i	86.23 (6)	O5—Na1—Na1iii	143.24 (5)
O9i—Mg1—O5i	93.77 (6)	O6iii—Na1—Na1iii	36.70 (4)
O8—Mg1—O5	90.0	O9i—Na1—Na1iii	148.88 (5)
O8i—Mg1—O5	90.0	Mg1—Na1—Na1iii	176.97 (4)
O9—Mg1—O5	93.77 (6)	C5—O1—Na1	175.97 (11)
O9i—Mg1—O5	86.23 (6)	C4—C1—C4iv	125.01 (18)
O5i—Mg1—O5	180.0	C4—C1—H1	117.5
O8—Mg1—Na1i	90.0	C4iv—C1—H1	117.5
O8i—Mg1—Na1i	90.0	C6—O2—H3	115.2
O9—Mg1—Na1i	44.36 (4)	C3—C2—C3iv	125.01 (17)
O9i—Mg1—Na1i	135.64 (4)	C3—C2—H2	117.5
O5i—Mg1—Na1i	41.87 (4)	C3iv—C2—H2	117.5
O5—Mg1—Na1i	138.13 (4)	C5—O3—H3	114.6
O8—Mg1—Na1	90.0	C2—C3—C4	117.42 (12)
O8i—Mg1—Na1	90.0	C2—C3—C6	114.02 (12)
O9—Mg1—Na1	135.64 (4)	C4—C3—C6	128.56 (11)
O9i—Mg1—Na1	44.36 (4)	C1—C4—C3	117.57 (12)
O5i—Mg1—Na1	138.13 (4)	C1—C4—C5	113.34 (13)
O5—Mg1—Na1	41.87 (4)	C3—C4—C5	129.09 (11)
Na1i—Mg1—Na1	180.0	Mg1—O5—Na1	104.40 (6)
O1—Na1—O1ii	167.72 (7)	Mg1—O5—H5	114.8
O1—Na1—O6	95.89 (4)	Na1—O5—H5	112.0
O1ii—Na1—O6	95.89 (4)	O1—C5—O3	120.93 (13)
O1—Na1—O5	84.05 (4)	O1—C5—C4	119.43 (13)
O1ii—Na1—O5	84.05 (4)	O3—C5—C4	119.64 (12)
O6—Na1—O5	178.07 (7)	Na1—O6—Na1iii	104.61 (6)
O1—Na1—O6iii	93.16 (4)	Na1—O6—H6	116.0
O1ii—Na1—O6iii	93.16 (4)	Na1iii—O6—H6	103.9
O6—Na1—O6iii	75.39 (6)	O4—C6—O2	121.94 (13)
O5—Na1—O6iii	106.54 (6)	O4—C6—C3	118.58 (12)
O1—Na1—O9i	86.35 (4)	O2—C6—C3	119.48 (12)
O1ii—Na1—O9i	86.35 (4)	Mg1—O8—H8	127.2
O6—Na1—O9i	110.19 (6)	Mg1—O9—Na1i	101.49 (6)
O5—Na1—O9i	67.88 (5)	Mg1—O9—H9	117.8
O6iii—Na1—O9i	174.41 (6)	Na1i—O9—H9	109.5
O1—Na1—Mg1	84.21 (4)

D—H···A	D—H	H···A	D···A	D—H···A
O3—H3···O2	1.06	1.35	2.3827 (17)	163
O5—H5···O7	0.90	1.83	2.7313 (14)	173
O6—H6···O4v	0.90	1.97	2.8519 (15)	167
O7—H7···O2vi	0.86	1.91	2.7699 (14)	173
O8—H8···O3vii	0.85	1.94	2.7779 (14)	172
O9—H9···O4vi	0.85	1.91	2.7559 (14)	171

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O3—H3⋯O2	1.06	1.35	2.3827 (17)	163
O5—H5⋯O7	0.90	1.83	2.7313 (14)	173
O6—H6⋯O4i	0.90	1.97	2.8519 (15)	167
O7—H7⋯O2ii	0.86	1.91	2.7699 (14)	173
O8—H8⋯O3iii	0.85	1.94	2.7779 (14)	172
O9—H9⋯O4ii	0.85	1.91	2.7559 (14)	171

Symmetry codes: (i) ; (ii) ; (iii) .