Poly[(μ(5)-5-carboxylatotetrahydrofuran-2,3,4-tricarboxylic acid)sodium].

The search for the novel metal-organic frameworks (MOFs) materials using tetra-hydro-furan-2,3,4,5-tetra-carboxylic acid (THFTCA) as a versatile multi-carboxyl ligand, lead to the synthesis and the structure determination of the title compound, [Na(H(3)THFTCA)] or [Na(C(8)H(7)O(9))](n), which was obtained by a solution reaction at room temperature. The ligand is mono-deprotonated, coordinating five sodium ions through one furan oxygen atom and six carboxyl oxygen atoms. The sodium ion exhibits a distorted penta-gonal-bipyramidal NaO(7) geometry consisting of seven O atoms derived from five surrounding ligands. Two adjacent pentagonal bipyramids share an O-O edge, forming a dinuclear sodium cluster. Finally, these clusters are effectively linked by the carboxyl groups of THFTCA ligands, forming a firm metal organic framework and O-H⋯O hydrogen bonds contribute to the crystal packing.

Related literature

For potential applications of metal-organic frameworks (MOFs), see: Moulton & Zaworotko (2001 ▶); Bradshaw et al. (2007 ▶). Self-assembly of selected ligands around d-transition metal ions is a widespread method for obtaining novel MOF structures, see: Leininger et al. (2000 ▶). In contrast, the s-elements are more flexible of their coordination behaviour, and maybe present in more various structures, see: Lu et al. (2007 ▶). For related MOF materials constructed from the THFTCA ligand, see: Hanson et al. (2004 ▶); Thuéry et al. (2004 ▶); Ai et al. (2008 ▶); Wang & Sevov (2007 ▶); Wang et al. (2007 ▶); Lü (2008 ▶). For related s-elements and THFTCA ligand compound structures, see: Barnes & Paton (1984 ▶) for Cs+ and Ca2+; Barnes (2002 ▶) for Na+; Paul & Martin (1967 ▶) for Rb+.

Experimental

Crystal data

[Na(C8H7O9)]

M = 270.13

Monoclinic,

a = 8.0663 (16) Å

b = 13.417 (3) Å

c = 9.7358 (19) Å

β = 109.90 (3)°

V = 990.7 (3) Å3

Z = 4

Mo Kα radiation

μ = 0.20 mm−1

T = 296 K

0.41 × 0.28 × 0.10 mm

Data collection

Rigaku R-AXIS RAPID diffractometer

Absorption correction: multi-scan (ABSCOR; Higashi, 1995 ▶) T min = 0.921, T max = 0.980

9567 measured reflections

2263 independent reflections

2095 reflections with I > 2σ(I)

R int = 0.018

Refinement

R[F 2 > 2σ(F 2)] = 0.032

wR(F 2) = 0.090

S = 1.09

2263 reflections

164 parameters

H-atom parameters constrained

Δρmax = 0.39 e Å−3

Δρmin = −0.32 e Å−3

Data collection: PROCESS-AUTO (Rigaku, 1998 ▶); cell refinement: PROCESS-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2004 ▶); 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 datablocks I, global. DOI: 10.1107/S160053680904269X/kp2234sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S160053680904269X/kp2234Isup2.hkl

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

[Na(C8H7O9)]	F(000) = 552
Mr = 270.13	Dx = 1.811 Mg m−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71075 Å
Hall symbol: -P 2ybc	Cell parameters from 8534 reflections
a = 8.0663 (16) Å	θ = 3.0–27.4°
b = 13.417 (3) Å	µ = 0.20 mm−1
c = 9.7358 (19) Å	T = 296 K
β = 109.90 (3)°	Platelet, colorless
V = 990.7 (3) Å3	0.41 × 0.28 × 0.10 mm
Z = 4

Rigaku R-AXIS RAPID diffractometer	2263 independent reflections
Radiation source: fine-focus sealed tube	2095 reflections with I > 2σ(I)
graphite	Rint = 0.018
Detector resolution: 14.6306 pixels mm-1	θmax = 27.4°, θmin = 3.0°
CCD_Profile_fitting scans	h = −10→10
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	k = −17→17
Tmin = 0.921, Tmax = 0.980	l = −12→12
9567 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)] = 0.032	H-atom parameters constrained
wR(F2) = 0.090	w = 1/[σ2(Fo2) + (0.0479P)2 + 0.4297P] where P = (Fo2 + 2Fc2)/3
S = 1.09	(Δ/σ)max < 0.001
2263 reflections	Δρmax = 0.39 e Å−3
164 parameters	Δρmin = −0.31 e Å−3
0 restraints	Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.034 (3)

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
Na1	0.16477 (7)	0.01271 (4)	0.39826 (6)	0.02678 (17)
O1	0.19961 (11)	0.20181 (7)	0.39121 (9)	0.0179 (2)
O2	−0.03876 (14)	0.10910 (7)	0.48915 (13)	0.0313 (3)
O3	−0.17693 (14)	0.25311 (8)	0.49566 (13)	0.0333 (3)
H3	−0.2454	0.2189	0.5252	0.033*
O4	0.02774 (14)	0.47842 (9)	0.33101 (13)	0.0362 (3)
O5	0.31727 (15)	0.46326 (10)	0.42755 (16)	0.0506 (4)
H5	0.3204	0.5163	0.3827	0.051*
O6	0.60941 (12)	0.37079 (7)	0.68721 (11)	0.0251 (2)
O7	0.39834 (13)	0.43913 (7)	0.75861 (11)	0.0281 (2)
H7	0.4778	0.4798	0.8028	0.028*
O8	0.39053 (12)	0.07324 (7)	0.60685 (11)	0.0234 (2)
O9	0.63546 (12)	0.13823 (7)	0.58976 (12)	0.0272 (2)
C11	0.05765 (15)	0.26035 (9)	0.40594 (13)	0.0167 (2)
H11	−0.0167	0.2819	0.3091	0.017*
C22	0.14282 (15)	0.34871 (9)	0.50496 (13)	0.0159 (2)
H22	0.0684	0.3706	0.5593	0.016*
C33	0.31740 (15)	0.30122 (8)	0.60199 (12)	0.0147 (2)
H33	0.2877	0.2598	0.6734	0.015*
C44	0.36719 (15)	0.23349 (8)	0.49541 (12)	0.0149 (2)
H44	0.4337	0.2705	0.4470	0.015*
C55	−0.05776 (16)	0.19811 (10)	0.46899 (14)	0.0202 (3)
C66	0.15670 (16)	0.43746 (9)	0.41175 (14)	0.0197 (3)
C77	0.45783 (16)	0.37456 (9)	0.68641 (13)	0.0178 (2)
C88	0.47422 (15)	0.14121 (9)	0.56952 (13)	0.0163 (2)

	U11	U22	U33	U12	U13	U23
Na1	0.0233 (3)	0.0215 (3)	0.0317 (3)	−0.0036 (2)	0.0044 (2)	−0.0026 (2)
O1	0.0145 (4)	0.0192 (4)	0.0191 (4)	0.0008 (3)	0.0043 (3)	−0.0038 (3)
O2	0.0268 (5)	0.0179 (5)	0.0538 (7)	0.0001 (4)	0.0195 (5)	0.0058 (4)
O3	0.0272 (5)	0.0212 (5)	0.0619 (7)	−0.0005 (4)	0.0286 (5)	0.0012 (5)
O4	0.0261 (5)	0.0321 (6)	0.0424 (6)	0.0028 (4)	0.0012 (5)	0.0170 (5)
O5	0.0222 (6)	0.0509 (7)	0.0725 (9)	−0.0036 (5)	0.0078 (6)	0.0436 (7)
O6	0.0173 (5)	0.0233 (5)	0.0327 (5)	−0.0026 (4)	0.0059 (4)	0.0003 (4)
O7	0.0258 (5)	0.0243 (5)	0.0355 (5)	−0.0092 (4)	0.0123 (4)	−0.0145 (4)
O8	0.0186 (4)	0.0189 (4)	0.0319 (5)	0.0009 (4)	0.0077 (4)	0.0092 (4)
O9	0.0158 (4)	0.0232 (5)	0.0433 (6)	0.0031 (4)	0.0112 (4)	0.0073 (4)
C11	0.0146 (5)	0.0151 (5)	0.0195 (5)	0.0006 (4)	0.0047 (4)	0.0002 (4)
C22	0.0140 (5)	0.0138 (5)	0.0199 (5)	−0.0006 (4)	0.0056 (4)	0.0000 (4)
C33	0.0154 (5)	0.0128 (5)	0.0161 (5)	−0.0004 (4)	0.0058 (4)	0.0007 (4)
C44	0.0142 (5)	0.0142 (5)	0.0164 (5)	−0.0006 (4)	0.0052 (4)	0.0012 (4)
C55	0.0152 (5)	0.0188 (6)	0.0256 (6)	−0.0023 (5)	0.0057 (5)	−0.0010 (5)
C66	0.0190 (6)	0.0151 (5)	0.0238 (6)	0.0001 (4)	0.0057 (5)	0.0014 (4)
C77	0.0197 (6)	0.0149 (5)	0.0171 (5)	−0.0017 (4)	0.0042 (4)	0.0021 (4)
C88	0.0158 (5)	0.0149 (5)	0.0182 (5)	0.0009 (4)	0.0058 (4)	−0.0008 (4)

Na1—O4i	2.2903 (14)	O7—C77	1.3056 (16)
Na1—O8	2.3626 (14)	O7—Na1vi	2.7495 (13)
Na1—O2ii	2.3800 (12)	O7—H7	0.8400
Na1—O2	2.4778 (13)	O8—C88	1.2595 (15)
Na1—O1	2.5561 (12)	O9—C88	1.2480 (15)
Na1—O9iii	2.5658 (12)	O9—Na1iii	2.5658 (12)
Na1—O7iv	2.7495 (13)	C11—C55	1.5264 (17)
O1—C11	1.4354 (14)	C11—C22	1.5349 (16)
O1—C44	1.4502 (14)	C11—H11	0.9734
O2—C55	1.2114 (16)	C22—C66	1.5242 (17)
O2—Na1ii	2.3800 (12)	C22—C33	1.5413 (16)
O3—C55	1.3061 (16)	C22—H22	0.9710
O3—H3	0.8400	C33—C77	1.5143 (16)
O4—C66	1.2021 (17)	C33—C44	1.5322 (16)
O4—Na1v	2.2903 (14)	C33—H33	0.9811
O5—C66	1.2982 (17)	C44—C88	1.5410 (16)
O5—H5	0.8402	C44—H44	0.9638
O6—C77	1.2210 (16)
O4i—Na1—O8	167.22 (5)	O1—C11—C22	106.48 (9)
O4i—Na1—O2ii	93.25 (5)	C55—C11—C22	111.95 (10)
O8—Na1—O2ii	99.51 (4)	O1—C11—H11	108.4
O4i—Na1—O2	98.11 (5)	C55—C11—H11	107.0
O8—Na1—O2	85.65 (4)	C22—C11—H11	112.0
O2ii—Na1—O2	75.83 (4)	C66—C22—C11	109.71 (10)
O4i—Na1—O1	102.56 (4)	C66—C22—C33	116.80 (10)
O8—Na1—O1	67.81 (3)	C11—C22—C33	100.71 (9)
O2ii—Na1—O1	139.65 (4)	C66—C22—H22	105.8
O2—Na1—O1	65.41 (3)	C11—C22—H22	110.4
O4i—Na1—O9iii	95.32 (5)	C33—C22—H22	113.4
O8—Na1—O9iii	86.78 (4)	C77—C33—C44	115.65 (10)
O2ii—Na1—O9iii	78.30 (4)	C77—C33—C22	114.99 (10)
O2—Na1—O9iii	151.39 (4)	C44—C33—C22	103.04 (9)
O1—Na1—O9iii	135.36 (4)	C77—C33—H33	107.5
O4i—Na1—O7iv	85.22 (5)	C44—C33—H33	109.1
O8—Na1—O7iv	83.50 (4)	C22—C33—H33	106.0
O2ii—Na1—O7iv	149.44 (4)	O1—C44—C33	104.52 (9)
O2—Na1—O7iv	134.65 (4)	O1—C44—C88	109.41 (9)
O1—Na1—O7iv	69.72 (3)	C33—C44—C88	113.18 (9)
O9iii—Na1—O7iv	71.49 (4)	O1—C44—H44	110.5
C11—O1—C44	110.80 (9)	C33—C44—H44	110.1
C11—O1—Na1	116.21 (7)	C88—C44—H44	109.1
C44—O1—Na1	110.91 (6)	O2—C55—O3	125.86 (12)
C55—O2—Na1ii	134.52 (9)	O2—C55—C11	122.93 (12)
C55—O2—Na1	121.28 (9)	O3—C55—C11	111.21 (11)
Na1ii—O2—Na1	104.17 (4)	O4—C66—O5	124.19 (13)
C55—O3—H3	111.9	O4—C66—C22	121.59 (12)
C66—O4—Na1v	151.37 (11)	O5—C66—C22	114.22 (11)
C66—O5—H5	111.7	O6—C77—O7	125.09 (12)
C77—O7—Na1vi	149.49 (8)	O6—C77—C33	122.61 (11)
C77—O7—H7	110.5	O7—C77—C33	112.29 (11)
Na1vi—O7—H7	97.2	O9—C88—O8	124.29 (11)
C88—O8—Na1	109.44 (8)	O9—C88—C44	119.16 (11)
C88—O9—Na1iii	129.58 (8)	O8—C88—C44	116.55 (10)
O1—C11—C55	110.94 (10)
O4i—Na1—O1—C11	77.60 (8)	C11—C22—C33—C77	164.09 (10)
O8—Na1—O1—C11	−111.21 (8)	C66—C22—C33—C44	−81.34 (12)
O2ii—Na1—O1—C11	−33.01 (10)	C11—C22—C33—C44	37.35 (11)
O2—Na1—O1—C11	−15.66 (7)	C11—O1—C44—C33	12.61 (12)
O9iii—Na1—O1—C11	−171.25 (7)	Na1—O1—C44—C33	−117.99 (7)
O7iv—Na1—O1—C11	157.62 (8)	C11—O1—C44—C88	134.10 (10)
O4i—Na1—O1—C44	−154.68 (7)	Na1—O1—C44—C88	3.50 (10)
O8—Na1—O1—C44	16.50 (7)	C77—C33—C44—O1	−157.88 (9)
O2ii—Na1—O1—C44	94.70 (9)	C22—C33—C44—O1	−31.56 (11)
O2—Na1—O1—C44	112.05 (8)	C77—C33—C44—C88	83.16 (12)
O9iii—Na1—O1—C44	−43.54 (9)	C22—C33—C44—C88	−150.52 (10)
O7iv—Na1—O1—C44	−74.67 (7)	Na1ii—O2—C55—O3	−7.4 (2)
O4i—Na1—O2—C55	−87.32 (12)	Na1—O2—C55—O3	170.75 (11)
O8—Na1—O2—C55	80.39 (11)	Na1ii—O2—C55—C11	173.27 (9)
O2ii—Na1—O2—C55	−178.65 (14)	Na1—O2—C55—C11	−8.56 (18)
O1—Na1—O2—C55	12.84 (10)	O1—C11—C55—O2	−6.66 (17)
O9iii—Na1—O2—C55	155.50 (10)	C22—C11—C55—O2	−125.45 (14)
O7iv—Na1—O2—C55	3.96 (14)	O1—C11—C55—O3	173.94 (10)
O4i—Na1—O2—Na1ii	91.33 (5)	C22—C11—C55—O3	55.15 (14)
O8—Na1—O2—Na1ii	−100.96 (5)	Na1v—O4—C66—O5	73.4 (3)
O2ii—Na1—O2—Na1ii	0.0	Na1v—O4—C66—C22	−106.3 (2)
O1—Na1—O2—Na1ii	−168.51 (6)	C11—C22—C66—O4	65.15 (16)
O9iii—Na1—O2—Na1ii	−25.85 (10)	C33—C22—C66—O4	178.86 (12)
O7iv—Na1—O2—Na1ii	−177.39 (5)	C11—C22—C66—O5	−114.57 (14)
O4i—Na1—O8—C88	3.2 (2)	C33—C22—C66—O5	−0.86 (17)
O2ii—Na1—O8—C88	−179.35 (8)	Na1vi—O7—C77—O6	−151.33 (12)
O2—Na1—O8—C88	−104.52 (9)	Na1vi—O7—C77—C33	27.3 (2)
O1—Na1—O8—C88	−39.34 (8)	C44—C33—C77—O6	−10.65 (16)
O9iii—Na1—O8—C88	103.09 (9)	C22—C33—C77—O6	−130.65 (12)
O7iv—Na1—O8—C88	31.37 (8)	C44—C33—C77—O7	170.70 (10)
C44—O1—C11—C55	−110.30 (11)	C22—C33—C77—O7	50.70 (14)
Na1—O1—C11—C55	17.46 (12)	Na1iii—O9—C88—O8	29.64 (19)
C44—O1—C11—C22	11.74 (12)	Na1iii—O9—C88—C44	−150.88 (8)
Na1—O1—C11—C22	139.51 (7)	Na1—O8—C88—O9	−120.38 (12)
O1—C11—C22—C66	93.14 (11)	Na1—O8—C88—C44	60.13 (12)
C55—C11—C22—C66	−145.46 (10)	O1—C44—C88—O9	138.01 (11)
O1—C11—C22—C33	−30.58 (11)	C33—C44—C88—O9	−105.88 (13)
C55—C11—C22—C33	90.82 (11)	O1—C44—C88—O8	−42.47 (14)
C66—C22—C33—C77	45.40 (14)	C33—C44—C88—O8	73.63 (13)

D—H···A	D—H	H···A	D···A	D—H···A
O3—H3···O9vii	0.84	1.70	2.5395 (15)	173
O5—H5···O6viii	0.84	1.83	2.6468 (16)	165
O7—H7···O8ix	0.84	1.68	2.5169 (14)	171

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O3—H3⋯O9i	0.84	1.70	2.5395 (15)	173
O5—H5⋯O6ii	0.84	1.83	2.6468 (16)	165
O7—H7⋯O8iii	0.84	1.68	2.5169 (14)	171

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