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In the structure of the title compound, {[Cu
2(C
10H
2O
8)(H
2O)
6]·4H
2O}
n, the benzene-1,2,4,5-tetracarboxylate ligand, (btec)
4-, is located on a crystallographic inversion centre in a
4-coordination mode. The coordination environment of each pentacoordinated Cu
II centre is square pyramidal (SBP), formed by three water molecules and two carboxylate O atoms from two different (btec)
4- ligands. The completely deprotonated (btec)
4- ligand coordinates in a monodentate mode to four Cu
II atoms. The alternation of (btec)
4- ligands and SBP Cu
II centres leads to the formation of a planar two-dimensional covalent network of parallelograms, parallel to the
ab plane. Hydrogen bonds between a basal water molecule and an apical one from an adjacent [Cu(btec)
0.5(H
2O)
3] unit exist in the intralayer space. Hydrogen bonds are also present between the two-dimensional network and the water molecules filling the channels in the structure.
Supporting information
CCDC reference: 963370
Data collection: APEX2 (Bruker, 2001); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT (Bruker, 2001); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Bruker, 2001); software used to prepare material for publication: SHELXTL (Bruker, 2001).
Poly[[hexaaqua(µ
4-benzene-1,2,4,5-tetracarboxylato)dicopper(II)]
tetrahydrate]
top
Crystal data top
[Cu2(C10H2O8)(H2O)6]·4H2O | F(000) = 1136 |
Mr = 278.68 | Dx = 1.901 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 5027 reflections |
a = 12.1571 (3) Å | θ = 3.2–26.1° |
b = 18.1138 (4) Å | µ = 2.27 mm−1 |
c = 9.6370 (4) Å | T = 296 K |
β = 113.405 (1)° | Needle, blue |
V = 1947.56 (10) Å3 | 0.75 × 0.42 × 0.36 mm |
Z = 8 | |
Data collection top
Bruker SMART APEXII area-detector diffractometer | 1911 independent reflections |
Radiation source: fine-focus sealed tube | 1773 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.000 |
φ and ω scans | θmax = 26.0°, θmin = 2.6° |
Absorption correction: empirical (using intensity measurements) (SADABS; Bruker, 2001) | h = −14→14 |
Tmin = 0.281, Tmax = 0.493 | k = 0→22 |
4973 measured reflections | l = 0→11 |
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)] = 0.029 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.083 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.08 | w = 1/[σ2(Fo2) + (0.0333P)2 + 2.2354P] where P = (Fo2 + 2Fc2)/3 |
1911 reflections | (Δ/σ)max = 0.001 |
142 parameters | Δρmax = 0.92 e Å−3 |
6 restraints | Δρmin = −0.48 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. Least-squares planes (x,y,z in crystal coordinates) and
deviations from them (* indicates atom used to define plane) - 8.2615 (0.0049) x + 11.0944 (0.0074) y + 6.1727 (0.0045)
z = 6.7576 (0.0042) * -0.0345 (0.0006) Cu * -0.0458 (0.0007) O1 * 0.0630 (0.0008) O6 * 0.0670
(0.0008) O5 * -0.0497 (0.0008) O3_$8 Rms deviation of fitted atoms = 0.0533 5.5927 (0.0102) x - 7.4133 (0.0147) y + 5.2077 (0.0074) z
= 1.5270 (0.0108) Angle to previous plane (with approximate e.s.d.) = 75.81 (0.06) * -0.0041 (0.0005) O1 * 0.0115 (0.0014) C1 * -0.0033 (0.0004) C2 * -0.0041
(0.0005) O2 Rms deviation of fitted atoms = 0.0066 the 7.3951 (0.0096) x - 7.9113
(0.0178) y + 3.5326 (0.0095) z = 0.8877 (0.0105) Angle to previous plane (with approximate e.s.d.) = 65.59 (0.06) * 0.0021 (0.0006) O3_$8 * -0.0058 (0.0016) C5_$8 * 0.0016 (0.0004) C4_$8 *
0.0022 (0.0006) O4_$8 Rms deviation of fitted atoms = 0.0034 |
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 | Uiso*/Ueq | |
Cu1 | 0.27996 (2) | 0.441393 (15) | 0.67052 (3) | 0.01200 (13) | |
O1 | 0.37365 (16) | 0.52682 (9) | 0.64069 (19) | 0.0148 (4) | |
C1 | 0.3665 (2) | 0.57872 (13) | 0.7256 (3) | 0.0111 (5) | |
O2 | 0.29745 (17) | 0.57583 (10) | 0.7923 (2) | 0.0195 (4) | |
C2 | 0.4398 (2) | 0.64728 (13) | 0.7414 (3) | 0.0102 (5) | |
C3 | 0.3825 (2) | 0.71442 (13) | 0.7360 (3) | 0.0132 (5) | |
H5A | 0.3036 | 0.7145 | 0.7276 | 0.016* | |
C4 | 0.4407 (2) | 0.78137 (13) | 0.7429 (3) | 0.0125 (5) | |
C5 | 0.3723 (2) | 0.85229 (13) | 0.7288 (3) | 0.0148 (5) | |
O3 | 0.32031 (17) | 0.85931 (10) | 0.8187 (2) | 0.0207 (4) | |
O4 | 0.3696 (2) | 0.89728 (12) | 0.6308 (3) | 0.0337 (5) | |
O5 | 0.15185 (18) | 0.46427 (11) | 0.4747 (2) | 0.0250 (4) | |
H1W | 0.157 (4) | 0.5056 (15) | 0.431 (5) | 0.073 (15)* | |
H2W | 0.082 (2) | 0.445 (3) | 0.454 (6) | 0.082 (19)* | |
O6 | 0.39550 (18) | 0.42212 (13) | 0.8757 (2) | 0.0251 (4) | |
H3W | 0.392 (5) | 0.450 (2) | 0.948 (4) | 0.076 (17)* | |
H4W | 0.4656 (19) | 0.402 (2) | 0.900 (5) | 0.062 (14)* | |
O7 | 0.38393 (17) | 0.37018 (11) | 0.5742 (2) | 0.0201 (4) | |
H5W | 0.346 (4) | 0.370 (3) | 0.4764 (7) | 0.080 (17)* | |
H6W | 0.383 (3) | 0.3226 (3) | 0.586 (4) | 0.031 (9)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Cu1 | 0.01281 (19) | 0.00741 (18) | 0.01753 (19) | −0.00314 (10) | 0.00786 (13) | 0.00076 (10) |
O1 | 0.0199 (9) | 0.0082 (8) | 0.0188 (9) | −0.0044 (7) | 0.0103 (7) | −0.0026 (7) |
C1 | 0.0095 (11) | 0.0085 (11) | 0.0146 (11) | 0.0005 (9) | 0.0041 (9) | 0.0022 (9) |
O2 | 0.0205 (9) | 0.0157 (9) | 0.0294 (10) | −0.0050 (7) | 0.0175 (8) | −0.0030 (8) |
C2 | 0.0122 (11) | 0.0058 (11) | 0.0142 (11) | −0.0008 (9) | 0.0069 (9) | −0.0001 (8) |
C3 | 0.0109 (10) | 0.0093 (12) | 0.0211 (12) | 0.0007 (9) | 0.0083 (10) | 0.0021 (9) |
C4 | 0.0155 (12) | 0.0077 (11) | 0.0183 (11) | 0.0019 (9) | 0.0110 (10) | 0.0008 (9) |
C5 | 0.0142 (11) | 0.0072 (11) | 0.0237 (12) | 0.0000 (9) | 0.0081 (10) | −0.0006 (9) |
O3 | 0.0261 (10) | 0.0142 (9) | 0.0281 (10) | 0.0096 (8) | 0.0174 (8) | 0.0020 (8) |
O4 | 0.0447 (13) | 0.0188 (11) | 0.0524 (14) | 0.0142 (9) | 0.0350 (12) | 0.0191 (10) |
O5 | 0.0183 (10) | 0.0176 (10) | 0.0314 (11) | −0.0040 (8) | 0.0019 (8) | 0.0087 (9) |
O6 | 0.0225 (10) | 0.0347 (12) | 0.0196 (10) | 0.0081 (9) | 0.0100 (8) | 0.0022 (9) |
O7 | 0.0232 (10) | 0.0158 (10) | 0.0233 (10) | 0.0000 (8) | 0.0113 (8) | −0.0013 (8) |
Geometric parameters (Å, º) top
Cu1—O6 | 1.949 (2) | C3—C4 | 1.392 (3) |
Cu1—O3i | 1.9513 (18) | C3—H5A | 0.9300 |
Cu1—O5 | 1.956 (2) | C4—C4iii | 1.393 (5) |
Cu1—O1 | 2.0087 (17) | C4—C5 | 1.507 (3) |
Cu1—O7 | 2.248 (2) | C5—O4 | 1.238 (3) |
O3—Cu1ii | 1.9513 (18) | C5—O3 | 1.266 (3) |
Cu1—Cu1i | 9.2625 (5) | O5—H1W | 0.8700 |
O1—C1 | 1.272 (3) | O5—H2W | 0.8700 |
C1—O2 | 1.244 (3) | O6—H3W | 0.8700 |
C1—C2 | 1.501 (3) | O6—H4W | 0.8700 |
C2—C3 | 1.392 (3) | O7—H5W | 0.8700 |
C2—C2iii | 1.406 (5) | O7—H6W | 0.8700 |
| | | |
O6—Cu1—O3i | 91.34 (9) | C2—C3—H5A | 119.3 |
O6—Cu1—O5 | 173.67 (9) | C4—C3—H5A | 119.3 |
O3i—Cu1—O5 | 86.44 (8) | C3—C4—C4iii | 119.42 (14) |
O6—Cu1—O1 | 93.56 (9) | C3—C4—C5 | 119.1 (2) |
O3i—Cu1—O1 | 175.08 (8) | C4iii—C4—C5 | 121.43 (13) |
O5—Cu1—O1 | 88.74 (8) | O4—C5—O3 | 126.0 (2) |
O6—Cu1—O7 | 91.10 (8) | O4—C5—C4 | 118.4 (2) |
O3i—Cu1—O7 | 92.88 (8) | O3—C5—C4 | 115.5 (2) |
O5—Cu1—O7 | 94.93 (8) | C5—O3—Cu1ii | 127.24 (17) |
O1—Cu1—O7 | 86.52 (7) | Cu1—O5—H1W | 118 |
C1—O1—Cu1 | 106.82 (15) | Cu1—O5—H2W | 118 |
O2—C1—O1 | 122.3 (2) | H1W—O5—H2W | 119 |
O2—C1—C2 | 118.6 (2) | Cu1—O6—H3W | 118 |
O1—C1—C2 | 119.1 (2) | Cu1—O6—H4W | 125 |
C3—C2—C2iii | 119.11 (14) | H3W—O6—H4W | 112 |
C3—C2—C1 | 116.8 (2) | Cu1—O7—H5W | 108 |
C2iii—C2—C1 | 124.10 (13) | Cu1—O7—H6W | 118 |
C2—C3—C4 | 121.4 (2) | H5W—O7—H6W | 97 |
| | | |
O6—Cu1—O1—C1 | −69.63 (16) | C2iii—C2—C3—C4 | 1.9 (4) |
O3i—Cu1—O1—C1 | 116.5 (9) | C1—C2—C3—C4 | −177.2 (2) |
O5—Cu1—O1—C1 | 104.47 (16) | C2—C3—C4—C4iii | −0.6 (4) |
O7—Cu1—O1—C1 | −160.52 (16) | C2—C3—C4—C5 | 176.9 (2) |
Cu1—O1—C1—O2 | −9.6 (3) | C3—C4—C5—O4 | −125.5 (3) |
Cu1—O1—C1—C2 | 173.00 (16) | C4iii—C4—C5—O4 | 52.0 (4) |
O2—C1—C2—C3 | −41.2 (3) | C3—C4—C5—O3 | 53.2 (3) |
O1—C1—C2—C3 | 136.3 (2) | C4iii—C4—C5—O3 | −129.2 (3) |
O2—C1—C2—C2iii | 139.7 (3) | O4—C5—O3—Cu1ii | 0.7 (4) |
O1—C1—C2—C2iii | −42.8 (4) | C4—C5—O3—Cu1ii | −177.94 (16) |
Symmetry codes: (i) −x+1/2, y−1/2, −z+3/2; (ii) −x+1/2, y+1/2, −z+3/2; (iii) −x+1, y, −z+3/2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O6—H4W···O7iii | 0.87 | 1.84 | 2.698 (3) | 170 |
O5—H1W···O4iv | 0.87 | 1.85 | 2.679 (3) | 160 |
O7—H5W···O2v | 0.87 | 1.90 | 2.679 (3) | 148 |
O6—H3W···O1vi | 0.87 | 2.00 | 2.826 (3) | 157 |
Symmetry codes: (iii) −x+1, y, −z+3/2; (iv) −x+1/2, −y+3/2, −z+1; (v) x, −y+1, z−1/2; (vi) x, −y+1, z+1/2. |
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