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Acta Cryst. (2007). E63, m1841-m1842    [ doi:10.1107/S1600536807025834 ]

Poly[ethylenediammonium [cuprate(II)-[mu]4-benzene-1,2,4,5-tetracarboxylato-[kappa]4O:O':O'':O'''] 2.5-hydrate\]

M. Rafizadeh, V. Amani, L. Dehghan, F. Azadbakht and E. Sahlolbei

Abstract top

The asymmetric unit of the title compound, {(C2H10N2)[Cu(C10H2O8)]·2.5H2O}n, contains one cuprate(II)-[mu]4-benzene-1,2,4,5-tetracarboxylate anion, one ethylenediammonium cation and two and a half water molecules. The Cu atom is four-coordinated by four O atoms from four benzene-1,2,4,5-tetracarboxylate anions. Intra- and intermolecular O-H...O and N-H...O hydrogen bonds in the formation of a supramolecular structure. One of the water molecules is disordered equally over two sites.

Comment top

The self-assembly of metal ions with aromatic carboxylates is a rapidly developing research field of modern coordination chemistry, because of the aggregation of metal ions and these carboxylate ligands in versatile binding modes, such as monodentate, chelating bidentate, bridging bidentate and bridging tridentate. Hereby, benzene-1,2,4,5-tetracarboxylic acid (H4BTC) is a good bridging ligand, and numerous complexes with H4BTC anions have been prepared, such as those of cobalt (Hu et al., 2004; Fu et al., 2004; Cheng et al., 2002), nickel (Kim et al., 2003; Cheng et al., 2003), thallium (Day & Luehrs, 1988), copper (Kim et al., 2003; Yuan et al., 2005; Hao et al., 2004), zinc (Hou et al., 2004), iron (Chu et al., 2001) and manganese (Rochon & Massarweh, 2000; Hu et al., 2001). There are also compounds of the rare earth elements reported (Cao et al., 2002; Daiguebonne et al., 2003). The complex of benzene-1,2,4,5-tetracarboxylate containing organic ammonium cations are rare and may have interesting polymeric chemistry. Recently, we have reported the syntheses and crystal structure of a proton transfer system using (H4BTC), with ethylenediamine (en), (BTC)(H2en)2·2H2O, (Rafizadeh et al., 2006). We herein report the synthesis and crystal structure of the title compound, (I), which was synthesized by reaction of Cu(NO3)2·3H2O and (BTC)(H2en)2·2H2O.

The asymmetric unit of (I) contains one [Cu(C10H2O8)] anion, one (N2C2H10) cation and two and a half water molecules. The Cu atom is four-coordinated by four O atoms from four benzene-1,2,4,5-tetracarboxylate (btc) anions (Fig. 1). The Cu—O bond lengths and angles (Table 1) are within normal ranges (Kim et al., 2003; Yuan et al., 2005; Hao et al., 2004).

The intra- and intermolecular O—H—O and N—H···O hydrogen bonds (Table 2) seem to be effective in the stabilization of the crystal structure, resulting in the formation of a supramolecular structure (Fig. 2). Dipol-dipol and van der Waals interactions are also effective in the molecular packing.

Related literature top

For general backgroud, see: Hu et al. (2004, 2001); Fu et al. (2004); Cheng et al. (2002); Hou et al. (2004); Chu et al. (2001); Rochon & Massarweh (2000); Cao et al. (2002); Daiguebonne et al. (2003); Rafizadeh et al. (2006). For related literature, see: Kim et al. (2003); Yuan et al. (2005); Hao et al. (2004).

For related literature, see: Cheng et al. (2003); Day & Luehrs (1988).

Experimental top

For the preparation of the title compound, (I), a solution of (BTC)(H2en)2·2H2O, (0.30 g, 0.73 mmol) in water (100 ml) was added to a solution of Cu(NO3)2·3H2O (0.09 g, 0.365 mmol) in water (10 ml) and the resulting blue solution was stirred for 5 min at room temperature. Then, it was left to evaporate slowly at room temperature. After one week, blue prismatic crystals of (I) were isolated (yield; 0.13 g, 84.6%; decompose <562 K).

Computing details top

Data collection: APEX2 (Bruker, 2005); cell refinement: APEX2; data reduction: APEX2; program(s) used to solve structure: SHELXTL (Sheldrick, 1998); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Figures top
[Figure 1] Fig. 1. The molecular structure of the title molecule, with the atom-numbering scheme. Displacement ellipsoids are drawn at the 50% probability level [symmetry codes: (i) 2 − x, y − 1/2, 2.5 − z, (ii) 2 − x, 1 − y, 2 − z, (iii) 2 − x, y − 1/2, 2.5 − z].
[Figure 2] Fig. 2. A packing diagram for (I). Hydrogen bonds are shown as dashed lines.
Poly[ethylenediammonium [copper(II)-µ4-benzene-1,2,4,5-tetracarboxylato-κ4O:O':O'':O'''] 2.5-hydrate] top
Crystal data top
(C2H10N2)[Cu(C10H2O8)]·2.5H2OF000 = 864
Mr = 420.82Dx = 1.811 Mg m−3
Monoclinic, P21/cMo Kα radiation
λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 5022 reflections
a = 7.3937 (5) Åθ = 2.8–34.7º
b = 18.4414 (11) ŵ = 1.48 mm−1
c = 11.3607 (7) ÅT = 100 (2) K
β = 94.783 (1)ºCube, blue
V = 1543.64 (17) Å30.20 × 0.20 × 0.20 mm
Z = 4
Data collection top
Bruker APEX II CCD area-detector
diffractometer		5364 independent reflections
Radiation source: fine-focus sealed tube4304 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.042
T = 100(2) Kθmax = 32.0º
φ and ω scansθmin = 2.1º
Absorption correction: multi-scan
(APEX2; Bruker, 2005)		h = −11→11
Tmin = 0.744, Tmax = 0.751k = −27→27
22717 measured reflectionsl = −16→16
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: mixed
R[F2 > 2σ(F2)] = 0.037H-atom parameters constrained
wR(F2) = 0.100  w = 1/[σ2(Fo2) + (0.0453P)2 + 1.6005P]
where P = (Fo2 + 2Fc2)/3
S = 1.01(Δ/σ)max = 0.001
5364 reflectionsΔρmax = 0.95 e Å−3
237 parametersΔρmin = −0.70 e Å−3
Primary atom site location: structure-invariant direct methodsExtinction correction: none
Crystal data top
(C2H10N2)[Cu(C10H2O8)]·2.5H2OV = 1543.64 (17) Å3
Mr = 420.82Z = 4
Monoclinic, P21/cMo Kα
a = 7.3937 (5) ŵ = 1.48 mm−1
b = 18.4414 (11) ÅT = 100 (2) K
c = 11.3607 (7) Å0.20 × 0.20 × 0.20 mm
β = 94.783 (1)º
Data collection top
Bruker APEX II CCD area-detector
diffractometer		5364 independent reflections
Absorption correction: multi-scan
(APEX2; Bruker, 2005)		4304 reflections with I > 2σ(I)
Tmin = 0.744, Tmax = 0.751Rint = 0.042
22717 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.037237 parameters
wR(F2) = 0.100H-atom parameters constrained
S = 1.01Δρmax = 0.95 e Å−3
5364 reflectionsΔρmin = −0.70 e Å−3
Special details top

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Cu10.98260 (3)0.743122 (11)0.999045 (17)0.00747 (7)
O11.00080 (18)0.81812 (7)1.12002 (11)0.0109 (2)
O20.72149 (18)0.85964 (7)1.06384 (11)0.0129 (2)
O31.04758 (17)0.66759 (6)1.11446 (11)0.0096 (2)
O40.74826 (18)0.65069 (7)1.11395 (12)0.0137 (3)
O50.96462 (18)0.81928 (7)0.87939 (11)0.0107 (2)
O61.24867 (18)0.85345 (7)0.93744 (11)0.0125 (2)
O70.92059 (17)0.66741 (6)0.88281 (11)0.0092 (2)
O81.22206 (18)0.65801 (7)0.88507 (12)0.0127 (3)
C10.8752 (2)0.86592 (9)1.11718 (14)0.0085 (3)
C20.9277 (2)0.93511 (9)1.18051 (14)0.0075 (3)
C30.8811 (2)1.00135 (9)1.12768 (15)0.0085 (3)
H3A0.80761.00251.05500.010*
C40.9066 (2)0.63317 (9)1.14322 (15)0.0085 (3)
C50.9522 (2)0.56440 (9)1.21098 (14)0.0070 (3)
C60.9048 (2)0.49801 (9)1.15800 (15)0.0080 (3)
H6A0.83070.49681.08560.010*
C71.0580 (2)0.93391 (9)0.81899 (14)0.0078 (3)
C81.0975 (2)0.86364 (9)0.88280 (14)0.0084 (3)
C91.0668 (2)0.63647 (9)0.85520 (14)0.0081 (3)
C101.0338 (2)0.56645 (9)0.78862 (14)0.0076 (3)
N1'1.5660 (2)0.65943 (8)1.32091 (14)0.0127 (3)
H1'C1.66290.64901.37290.019*
H1'D1.57740.63561.25180.019*
H1'E1.46210.64501.35180.019*
N2'1.4052 (2)0.83478 (9)1.17836 (14)0.0137 (3)
H2'C1.31080.84501.12430.021*
H2'D1.51070.85001.15060.021*
H2'E1.38870.85801.24730.021*
C1'1.5587 (3)0.73907 (10)1.29853 (17)0.0134 (3)
H1'A1.67810.75631.27640.016*
H1'B1.53030.76491.37110.016*
C2'1.4139 (3)0.75515 (10)1.19949 (17)0.0138 (3)
H2'A1.44320.72991.12660.017*
H2'B1.29480.73741.22110.017*
O1W0.6201 (2)0.42273 (8)0.89555 (14)0.0216 (3)
H1WA0.56290.41000.95400.032*
H1WB0.72440.40530.88610.032*
O2W0.5892 (2)0.57443 (9)0.87753 (16)0.0262 (4)
H2WA0.57580.52870.88010.039*
H2WB0.69510.59220.89090.039*
O3W1.4335 (4)0.99565 (15)1.1305 (3)0.0217 (6)0.50
H3WA1.32681.00231.15100.033*0.50
H3WB1.47551.01131.06790.033*0.50
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cu10.01489 (11)0.00322 (10)0.00438 (10)0.00031 (7)0.00120 (7)0.00017 (7)
O10.0199 (6)0.0058 (5)0.0068 (5)0.0024 (4)0.0001 (4)−0.0008 (4)
O20.0136 (6)0.0148 (6)0.0103 (6)−0.0050 (5)0.0009 (4)−0.0029 (5)
O30.0151 (6)0.0059 (5)0.0078 (6)−0.0009 (4)0.0014 (4)0.0014 (4)
O40.0139 (6)0.0149 (6)0.0123 (6)0.0060 (5)0.0020 (5)0.0034 (5)
O50.0181 (6)0.0062 (5)0.0077 (6)−0.0025 (4)0.0012 (4)0.0015 (4)
O60.0152 (6)0.0114 (6)0.0107 (6)0.0033 (5)0.0008 (5)0.0023 (5)
O70.0135 (6)0.0069 (5)0.0073 (5)0.0017 (4)0.0015 (4)−0.0014 (4)
O80.0140 (6)0.0120 (6)0.0123 (6)−0.0046 (5)0.0021 (5)−0.0014 (5)
C10.0139 (8)0.0068 (7)0.0053 (7)−0.0017 (5)0.0040 (5)0.0005 (5)
C20.0113 (7)0.0046 (7)0.0067 (7)0.0003 (5)0.0015 (5)−0.0008 (5)
C30.0125 (8)0.0062 (7)0.0067 (7)0.0005 (5)0.0007 (5)−0.0001 (6)
C40.0135 (8)0.0057 (7)0.0065 (7)0.0014 (5)0.0022 (5)−0.0008 (5)
C50.0102 (7)0.0058 (7)0.0052 (7)0.0002 (5)0.0015 (5)0.0007 (5)
C60.0107 (7)0.0069 (7)0.0066 (7)0.0000 (5)0.0012 (5)0.0001 (6)
C70.0131 (7)0.0048 (7)0.0057 (7)0.0004 (5)0.0024 (5)0.0012 (5)
C80.0155 (8)0.0042 (7)0.0060 (7)0.0008 (5)0.0032 (5)−0.0004 (5)
C90.0144 (8)0.0047 (7)0.0054 (7)−0.0005 (5)0.0014 (5)0.0002 (5)
C100.0109 (7)0.0052 (7)0.0067 (7)−0.0005 (5)0.0017 (5)−0.0008 (5)
N1'0.0127 (7)0.0150 (7)0.0105 (7)0.0026 (5)0.0006 (5)0.0012 (5)
N2'0.0142 (7)0.0153 (7)0.0116 (7)0.0032 (5)0.0008 (5)0.0016 (6)
C1'0.0142 (8)0.0122 (8)0.0132 (8)0.0020 (6)−0.0015 (6)0.0016 (6)
C2'0.0130 (8)0.0147 (8)0.0134 (8)0.0016 (6)−0.0013 (6)0.0009 (6)
O1W0.0207 (7)0.0168 (7)0.0282 (8)−0.0001 (5)0.0085 (6)−0.0002 (6)
O2W0.0165 (7)0.0189 (7)0.0429 (10)0.0002 (5)0.0012 (6)0.0094 (7)
O3W0.0218 (15)0.0176 (14)0.0245 (16)−0.0036 (10)−0.0049 (12)0.0016 (12)
Geometric parameters (Å, °) top
Cu1—O31.9456 (12)C7—C81.502 (2)
Cu1—O11.9466 (12)C9—C101.506 (2)
Cu1—O71.9500 (12)C10—C6iii1.393 (2)
Cu1—O51.9514 (12)C10—C2iv1.402 (2)
O1—C11.279 (2)N1'—C1'1.491 (2)
O2—C11.248 (2)N1'—H1'C0.9100
O3—C41.285 (2)N1'—H1'D0.9100
O4—C41.233 (2)N1'—H1'E0.9100
O5—C81.276 (2)N2'—C2'1.489 (2)
O6—C81.247 (2)N2'—H2'C0.9100
O7—C91.284 (2)N2'—H2'D0.9100
O8—C91.235 (2)N2'—H2'E0.9100
C1—C21.500 (2)C1'—C2'1.516 (3)
C2—C31.392 (2)C1'—H1'A0.9900
C2—C10i1.402 (2)C1'—H1'B0.9900
C3—C7ii1.396 (2)C2'—H2'A0.9900
C3—H3A0.9500C2'—H2'B0.9900
C4—C51.507 (2)O1W—H1WA0.8499
C5—C61.396 (2)O1W—H1WB0.8500
C5—C7i1.399 (2)O2W—H2WA0.8501
C6—C10iii1.393 (2)O2W—H2WB0.8500
C6—H6A0.9500O3W—H3WA0.8500
C7—C3ii1.396 (2)O3W—H3WB0.8499
C7—C5iv1.399 (2)
O3—Cu1—O191.96 (5)O8—C9—O7124.89 (16)
O3—Cu1—O788.55 (5)O8—C9—C10121.42 (15)
O1—Cu1—O7170.20 (6)O7—C9—C10113.55 (14)
O3—Cu1—O5169.55 (6)C6iii—C10—C2iv120.14 (15)
O1—Cu1—O588.69 (5)C6iii—C10—C9118.68 (14)
O7—Cu1—O592.59 (5)C2iv—C10—C9120.87 (14)
C1—O1—Cu1117.69 (11)C1'—N1'—H1'C109.5
C4—O3—Cu1111.40 (11)C1'—N1'—H1'D109.5
C8—O5—Cu1115.63 (11)H1'C—N1'—H1'D109.5
C9—O7—Cu1109.17 (11)C1'—N1'—H1'E109.5
O2—C1—O1125.32 (16)H1'C—N1'—H1'E109.5
O2—C1—C2120.03 (15)H1'D—N1'—H1'E109.5
O1—C1—C2114.60 (15)C2'—N2'—H2'C109.5
C3—C2—C10i119.76 (15)C2'—N2'—H2'D109.5
C3—C2—C1119.68 (15)H2'C—N2'—H2'D109.5
C10i—C2—C1120.42 (14)C2'—N2'—H2'E109.5
C2—C3—C7ii120.27 (15)H2'C—N2'—H2'E109.5
C2—C3—H3A119.9H2'D—N2'—H2'E109.5
C7ii—C3—H3A119.9N1'—C1'—C2'109.42 (15)
O4—C4—O3125.01 (16)N1'—C1'—H1'A109.8
O4—C4—C5121.65 (15)C2'—C1'—H1'A109.8
O3—C4—C5113.21 (14)N1'—C1'—H1'B109.8
C6—C5—C7i119.96 (15)C2'—C1'—H1'B109.8
C6—C5—C4118.72 (14)H1'A—C1'—H1'B108.2
C7i—C5—C4120.92 (14)N2'—C2'—C1'109.34 (15)
C10iii—C6—C5119.99 (15)N2'—C2'—H2'A109.8
C10iii—C6—H6A120.0C1'—C2'—H2'A109.8
C5—C6—H6A120.0N2'—C2'—H2'B109.8
C3ii—C7—C5iv119.86 (15)C1'—C2'—H2'B109.8
C3ii—C7—C8119.05 (15)H2'A—C2'—H2'B108.3
C5iv—C7—C8120.96 (14)H1WA—O1W—H1WB120.7
O6—C8—O5125.05 (16)H2WA—O2W—H2WB118.9
O6—C8—C7120.04 (15)H3WA—O3W—H3WB126.4
O5—C8—C7114.85 (15)
O3—Cu1—O1—C1−135.64 (12)Cu1—O3—C4—C5167.38 (10)
O7—Cu1—O1—C1−42.8 (4)O4—C4—C5—C663.2 (2)
O5—Cu1—O1—C154.80 (12)O3—C4—C5—C6−112.90 (17)
O1—Cu1—O3—C4100.44 (11)O4—C4—C5—C7i−124.12 (19)
O7—Cu1—O3—C4−69.76 (11)O3—C4—C5—C7i59.8 (2)
O5—Cu1—O3—C4−166.2 (3)C7i—C5—C6—C10iii−1.4 (3)
O3—Cu1—O5—C8−35.5 (3)C4—C5—C6—C10iii171.39 (15)
O1—Cu1—O5—C858.23 (12)Cu1—O5—C8—O615.9 (2)
O7—Cu1—O5—C8−131.50 (12)Cu1—O5—C8—C7−161.28 (11)
O3—Cu1—O7—C9−70.78 (11)C3ii—C7—C8—O6−40.7 (2)
O1—Cu1—O7—C9−163.9 (3)C5iv—C7—C8—O6143.24 (17)
O5—Cu1—O7—C998.82 (11)C3ii—C7—C8—O5136.63 (17)
Cu1—O1—C1—O218.8 (2)C5iv—C7—C8—O5−39.4 (2)
Cu1—O1—C1—C2−158.60 (11)Cu1—O7—C9—O8−9.2 (2)
O2—C1—C2—C3−42.1 (2)Cu1—O7—C9—C10166.48 (11)
O1—C1—C2—C3135.45 (17)O8—C9—C10—C6iii61.5 (2)
O2—C1—C2—C10i142.31 (17)O7—C9—C10—C6iii−114.33 (17)
O1—C1—C2—C10i−40.1 (2)O8—C9—C10—C2iv−124.93 (19)
C10i—C2—C3—C7ii1.0 (3)O7—C9—C10—C2iv59.2 (2)
C1—C2—C3—C7ii−174.62 (15)N1'—C1'—C2'—N2'179.25 (14)
Cu1—O3—C4—O4−8.5 (2)
Symmetry codes: (i) x, −y+3/2, z+1/2; (ii) −x+2, −y+2, −z+2; (iii) −x+2, −y+1, −z+2; (iv) x, −y+3/2, z−1/2.
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
N1'—H1'C···O2v0.912.182.921 (2)138
N1'—H1'C···O5v0.912.302.993 (2)132
N1'—H1'D···O4vi0.912.112.810 (2)133
N1'—H1'E···O6i0.911.922.799 (2)161
N2'—H2'C···O60.912.142.902 (2)141
N2'—H2'D···O2vi0.911.922.807 (2)164
N2'—H2'E···O8i0.912.092.810 (2)135
O1W—H1WA···O2Wvii0.852.323.116 (2)157
O1W—H1WB···O3iii0.852.162.9784 (19)162
O2W—H2WA···O1W0.851.992.813 (2)164
O2W—H2WB···O70.852.182.987 (2)159
Symmetry codes: (v) x+1, −y+3/2, z+1/2; (vi) x+1, y, z; (i) x, −y+3/2, z+1/2; (vii) −x+1, −y+1, −z+2; (iii) −x+2, −y+1, −z+2.
Table 1
Selected geometric parameters (Å, °) top
Cu1—O31.9456 (12)Cu1—O71.9500 (12)
Cu1—O11.9466 (12)Cu1—O51.9514 (12)
O3—Cu1—O191.96 (5)O3—Cu1—O5169.55 (6)
O3—Cu1—O788.55 (5)O1—Cu1—O588.69 (5)
O1—Cu1—O7170.20 (6)O7—Cu1—O592.59 (5)
Table 2
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
N1'—H1'C···O2i0.912.182.921 (2)138
N1'—H1'C···O5i0.912.302.993 (2)132
N1'—H1'D···O4ii0.912.112.810 (2)133
N1'—H1'E···O6iii0.911.922.799 (2)161
N2'—H2'C···O60.912.142.902 (2)141
N2'—H2'D···O2ii0.911.922.807 (2)164
N2'—H2'E···O8iii0.912.092.810 (2)135
O1W—H1WA···O2Wiv0.852.323.116 (2)157
O1W—H1WB···O3v0.852.162.9784 (19)162
O2W—H2WA···O1W0.851.992.813 (2)164
O2W—H2WB···O70.852.182.987 (2)159
Symmetry codes: (i) x+1, −y+3/2, z+1/2; (ii) x+1, y, z; (iii) x, −y+3/2, z+1/2; (iv) −x+1, −y+1, −z+2; (v) −x+2, −y+1, −z+2.
Acknowledgements top

We are grateful to the Teacher Training University and the Academy of Scientific Studies in Education for financial support.

references
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