metal-organic compounds
μ-2,5-Dihydroxyterephthalato-bis[triaqua(1,10-phenanthroline)zinc] dihydroxyterephthalate
aDepartment of Information & Technology, Jilin Normal University, Siping 136000, People's Republic of China, and bDepartment of Chemistry, Jilin Normal University, Siping 136000, People's Republic of China
*Correspondence e-mail: chuanbl@gmail.com
In the title compound, [Zn2(C8H4O6)(C12H8N2)2(H2O)6](C8H4O6), the complete ions of both the binuclear dication and the dianion are generated by crystallographic inversion symmetry. The Zn atom is bonded to an N,N′-bidentate phenanthroline ligand, three water moleules and an O-monodenate 2,5-dihydroxyterephthalate dianion. In the resulting distorted octahedral ZnN2O4 coordination polyhedron, the water O atoms are in a mer orientation. Two intramolecular O—H⋯O hydrogen bonds occur in the bridging 2,5-dihydroxyterephthalate dianion within the complex cation and also in the free dianion. An intramolecular Ow—H⋯O (w = water) hydrogen bond also occurs within the dication. In the crystal, O—H⋯O hydrogen bonds link the component ions into a three-dimensional network.
Related literature
For a related structure, see: Sun et al. (2007). For background to the applications of coordination polymers, see: Perry et al. (2009).
Experimental
Crystal data
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Refinement
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Data collection: APEX2 (Bruker, 2002); cell SAINT (Bruker, 2002); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg, 1999); software used to prepare material for publication: SHELXTL.
Supporting information
10.1107/S1600536812045837/hb6960sup1.cif
contains datablocks I, global. DOI:Structure factors: contains datablock I. DOI: 10.1107/S1600536812045837/hb6960Isup2.hkl
A mixture of Zn(CH3COO)2.2H2O (0.2 mmol), phen (0.3 mmol) and dhtp (0.2 mmol) were dissolved in 15 ml water. The resulting solution was stirred for about 0.5 h at room temperature, sealed in a 25-ml Teflon-lined stainless steel autoclave and heated at 443 K for three days under autogenous pressure. Afterward, the reaction system was slowly cooled to room temperature and colourless blocks of the title compound were recovered.
Carbon-bound H-atoms were positioned geometrically (C–H = 0.93 Å) and refined as riding, with Uiso(H) fixed at 1.2Ueq(C). Oxygen-bound for H3A and H6A atoms were positioned geometrically (O–H = 0.82 Å) and refined as riding, with Uiso(H) fixed at 1.5Ueq(O). In the case of coordinated water molecules, H atoms were clearly detected in a difference Fourier map, and refined freely. Final O–H bond length span the range 0.83–0.97 Å. Isotropic displacement parameters for H atoms were calculated as Uiso(H) = 1.2Ueq(C).
Data collection: APEX2 (Bruker, 2002); cell
SAINT (Bruker, 2002); data reduction: SAINT (Bruker, 2002); program(s) used to solve structure: SHELXTL (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg, 1999); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).Fig. 1. A representation of title compound. Displacement ellipsoids are drawn at the 40% probability level. H atoms have been omitted for clarity. Unlabelled atoms are related to the reference atoms by the symmetry operations. [Symmetry codes: (i) - x + 2, - y, - z; (ii) - x + 1, - y, - z + 1]. | |
Fig. 2. The packing diagram of the title compound. All H-atoms except for those involved in hydrogen bonds are omitted for clarity. (hydrogen bonds indicated by dashed lines). |
[Zn2(C8H4O6)(C12H8N2)2(H2O)6](C8H4O6) | Z = 1 |
Mr = 991.46 | F(000) = 508 |
Triclinic, P1 | Dx = 1.662 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 8.765 (5) Å | Cell parameters from 1867 reflections |
b = 10.697 (5) Å | θ = 2.3–24.9° |
c = 11.062 (5) Å | µ = 1.30 mm−1 |
α = 106.994 (5)° | T = 293 K |
β = 92.226 (5)° | Block, colorless |
γ = 90.977 (5)° | 0.25 × 0.18 × 0.15 mm |
V = 990.7 (9) Å3 |
Bruker SMART APEXII CCD diffractometer | 3824 independent reflections |
Radiation source: fine-focus sealed tube | 3205 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.019 |
ω scan | θmax = 26.0°, θmin = 1.9° |
Absorption correction: multi-scan (SADABS; Bruker, 2002) | h = −10→5 |
Tmin = 0.737, Tmax = 0.829 | k = −13→13 |
5446 measured reflections | l = −13→13 |
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)] = 0.036 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.086 | H-atom parameters constrained |
S = 1.04 | w = 1/[σ2(Fo2) + (0.0372P)2 + 0.484P] where P = (Fo2 + 2Fc2)/3 |
3824 reflections | (Δ/σ)max = 0.001 |
289 parameters | Δρmax = 0.33 e Å−3 |
0 restraints | Δρmin = −0.29 e Å−3 |
[Zn2(C8H4O6)(C12H8N2)2(H2O)6](C8H4O6) | γ = 90.977 (5)° |
Mr = 991.46 | V = 990.7 (9) Å3 |
Triclinic, P1 | Z = 1 |
a = 8.765 (5) Å | Mo Kα radiation |
b = 10.697 (5) Å | µ = 1.30 mm−1 |
c = 11.062 (5) Å | T = 293 K |
α = 106.994 (5)° | 0.25 × 0.18 × 0.15 mm |
β = 92.226 (5)° |
Bruker SMART APEXII CCD diffractometer | 3824 independent reflections |
Absorption correction: multi-scan (SADABS; Bruker, 2002) | 3205 reflections with I > 2σ(I) |
Tmin = 0.737, Tmax = 0.829 | Rint = 0.019 |
5446 measured reflections |
R[F2 > 2σ(F2)] = 0.036 | 0 restraints |
wR(F2) = 0.086 | H-atom parameters constrained |
S = 1.04 | Δρmax = 0.33 e Å−3 |
3824 reflections | Δρmin = −0.29 e Å−3 |
289 parameters |
Geometry. All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'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 > 2σ(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 | ||
Zn1 | 0.50422 (4) | 0.32879 (3) | 0.16460 (3) | 0.03368 (11) | |
C1 | 0.4116 (3) | 0.0549 (3) | 0.1904 (3) | 0.0410 (7) | |
H1 | 0.5020 | 0.0258 | 0.1515 | 0.049* | |
C2 | 0.3222 (4) | −0.0322 (3) | 0.2306 (3) | 0.0490 (8) | |
H2 | 0.3518 | −0.1180 | 0.2177 | 0.059* | |
C3 | 0.1916 (4) | 0.0092 (3) | 0.2888 (3) | 0.0534 (9) | |
H3 | 0.1321 | −0.0478 | 0.3178 | 0.064* | |
C4 | 0.1455 (3) | 0.1379 (3) | 0.3054 (3) | 0.0468 (8) | |
C5 | 0.0065 (4) | 0.1877 (4) | 0.3598 (3) | 0.0634 (10) | |
H5 | −0.0560 | 0.1351 | 0.3920 | 0.076* | |
C6 | −0.0360 (4) | 0.3089 (4) | 0.3656 (3) | 0.0643 (11) | |
H6 | −0.1282 | 0.3382 | 0.4008 | 0.077* | |
C7 | 0.0574 (3) | 0.3950 (3) | 0.3186 (3) | 0.0518 (8) | |
C8 | 0.0161 (4) | 0.5197 (4) | 0.3177 (3) | 0.0677 (11) | |
H8 | −0.0762 | 0.5528 | 0.3500 | 0.081* | |
C9 | 0.1111 (5) | 0.5934 (4) | 0.2692 (4) | 0.0735 (12) | |
H9 | 0.0833 | 0.6761 | 0.2667 | 0.088* | |
C10 | 0.2505 (4) | 0.5432 (3) | 0.2235 (3) | 0.0600 (9) | |
H10 | 0.3157 | 0.5949 | 0.1925 | 0.072* | |
C11 | 0.1974 (3) | 0.3504 (3) | 0.2684 (3) | 0.0386 (6) | |
C12 | 0.2414 (3) | 0.2194 (3) | 0.2602 (2) | 0.0357 (6) | |
C13 | 0.7999 (3) | 0.2201 (3) | 0.0587 (2) | 0.0319 (6) | |
C14 | 0.9054 (3) | 0.1076 (2) | 0.0300 (2) | 0.0274 (5) | |
C15 | 0.8650 (3) | −0.0063 (2) | 0.0586 (2) | 0.0300 (6) | |
H15 | 0.7743 | −0.0104 | 0.0985 | 0.036* | |
C16 | 0.9569 (3) | −0.1134 (2) | 0.0290 (2) | 0.0296 (5) | |
C17 | 0.4052 (3) | 0.2683 (3) | 0.5940 (3) | 0.0377 (6) | |
C18 | 0.4543 (3) | 0.1290 (2) | 0.5460 (2) | 0.0307 (6) | |
C19 | 0.5797 (3) | 0.0989 (2) | 0.4716 (2) | 0.0338 (6) | |
H19 | 0.6340 | 0.1660 | 0.4531 | 0.041* | |
C20 | 0.6264 (3) | −0.0285 (2) | 0.4243 (2) | 0.0334 (6) | |
N1 | 0.3740 (2) | 0.1776 (2) | 0.2049 (2) | 0.0346 (5) | |
N2 | 0.2937 (3) | 0.4250 (2) | 0.2225 (2) | 0.0419 (6) | |
O1 | 0.6766 (2) | 0.20561 (17) | 0.10775 (18) | 0.0382 (4) | |
O2 | 0.8398 (2) | 0.32217 (18) | 0.0314 (2) | 0.0447 (5) | |
O3 | 0.9102 (2) | −0.22265 (18) | 0.0592 (2) | 0.0461 (5) | |
H3A | 0.9735 | −0.2795 | 0.0370 | 0.069* | |
O4 | 0.4677 (3) | 0.35176 (18) | 0.5525 (2) | 0.0592 (7) | |
O5 | 0.3055 (3) | 0.29470 (18) | 0.6758 (2) | 0.0500 (5) | |
O6 | 0.7485 (3) | −0.05155 (19) | 0.3502 (2) | 0.0563 (6) | |
H6A | 0.7647 | −0.1301 | 0.3282 | 0.084* | |
O1W | 0.4148 (2) | 0.28676 (19) | −0.03067 (18) | 0.0434 (5) | |
H1WA | 0.3083 | 0.2617 | −0.0317 | 0.052* | |
H1WB | 0.4161 | 0.3598 | −0.0582 | 0.052* | |
O2W | 0.6253 (2) | 0.49092 (17) | 0.12905 (17) | 0.0371 (4) | |
H2WA | 0.7050 | 0.4415 | 0.0879 | 0.045* | |
H2WB | 0.6629 | 0.5567 | 0.1971 | 0.045* | |
O3W | 0.5968 (2) | 0.39846 (17) | 0.35216 (17) | 0.0380 (4) | |
H3WA | 0.5567 | 0.3612 | 0.4060 | 0.046* | |
H3WB | 0.5806 | 0.4777 | 0.3793 | 0.046* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Zn1 | 0.03234 (18) | 0.02944 (18) | 0.04078 (19) | 0.00700 (12) | 0.01051 (13) | 0.01119 (13) |
C1 | 0.0402 (16) | 0.0353 (15) | 0.0467 (17) | −0.0007 (13) | −0.0064 (13) | 0.0120 (13) |
C2 | 0.058 (2) | 0.0409 (17) | 0.0477 (18) | −0.0125 (15) | −0.0175 (16) | 0.0160 (14) |
C3 | 0.061 (2) | 0.057 (2) | 0.0446 (18) | −0.0277 (18) | −0.0106 (16) | 0.0206 (16) |
C4 | 0.0400 (17) | 0.063 (2) | 0.0343 (16) | −0.0155 (15) | −0.0036 (13) | 0.0107 (14) |
C5 | 0.044 (2) | 0.091 (3) | 0.050 (2) | −0.018 (2) | 0.0094 (16) | 0.011 (2) |
C6 | 0.0291 (17) | 0.102 (3) | 0.048 (2) | −0.0024 (19) | 0.0123 (15) | 0.000 (2) |
C7 | 0.0350 (16) | 0.069 (2) | 0.0410 (17) | 0.0148 (16) | −0.0012 (13) | −0.0009 (15) |
C8 | 0.047 (2) | 0.085 (3) | 0.057 (2) | 0.029 (2) | 0.0002 (17) | −0.002 (2) |
C9 | 0.081 (3) | 0.058 (2) | 0.074 (3) | 0.040 (2) | −0.002 (2) | 0.007 (2) |
C10 | 0.068 (2) | 0.050 (2) | 0.065 (2) | 0.0224 (17) | 0.0092 (18) | 0.0192 (17) |
C11 | 0.0307 (14) | 0.0508 (17) | 0.0319 (14) | 0.0062 (13) | 0.0012 (12) | 0.0081 (13) |
C12 | 0.0293 (14) | 0.0456 (16) | 0.0305 (14) | −0.0035 (12) | −0.0027 (11) | 0.0093 (12) |
C13 | 0.0296 (14) | 0.0303 (14) | 0.0331 (14) | 0.0045 (11) | 0.0008 (11) | 0.0048 (11) |
C14 | 0.0230 (12) | 0.0291 (13) | 0.0270 (12) | 0.0053 (10) | 0.0003 (10) | 0.0033 (10) |
C15 | 0.0215 (13) | 0.0336 (14) | 0.0340 (14) | 0.0037 (10) | 0.0072 (10) | 0.0076 (11) |
C16 | 0.0285 (13) | 0.0277 (13) | 0.0316 (13) | −0.0013 (11) | 0.0006 (11) | 0.0074 (11) |
C17 | 0.0541 (18) | 0.0248 (14) | 0.0333 (14) | 0.0011 (12) | 0.0027 (13) | 0.0068 (11) |
C18 | 0.0399 (15) | 0.0221 (12) | 0.0296 (13) | 0.0005 (11) | −0.0001 (11) | 0.0071 (10) |
C19 | 0.0412 (15) | 0.0210 (12) | 0.0387 (15) | −0.0053 (11) | 0.0038 (12) | 0.0081 (11) |
C20 | 0.0379 (15) | 0.0276 (13) | 0.0349 (14) | 0.0012 (11) | 0.0051 (12) | 0.0091 (11) |
N1 | 0.0306 (12) | 0.0355 (13) | 0.0381 (12) | 0.0005 (10) | 0.0001 (10) | 0.0115 (10) |
N2 | 0.0410 (14) | 0.0395 (13) | 0.0450 (14) | 0.0138 (11) | 0.0050 (11) | 0.0111 (11) |
O1 | 0.0308 (10) | 0.0313 (10) | 0.0540 (12) | 0.0106 (8) | 0.0151 (9) | 0.0124 (9) |
O2 | 0.0440 (12) | 0.0337 (11) | 0.0599 (13) | 0.0102 (9) | 0.0169 (10) | 0.0167 (10) |
O3 | 0.0384 (11) | 0.0346 (11) | 0.0705 (14) | 0.0081 (9) | 0.0190 (10) | 0.0211 (10) |
O4 | 0.1041 (19) | 0.0225 (10) | 0.0548 (13) | 0.0075 (11) | 0.0337 (13) | 0.0132 (9) |
O5 | 0.0615 (14) | 0.0293 (10) | 0.0564 (13) | 0.0071 (10) | 0.0205 (11) | 0.0058 (9) |
O6 | 0.0590 (14) | 0.0323 (11) | 0.0774 (16) | 0.0039 (10) | 0.0363 (12) | 0.0113 (11) |
O1W | 0.0437 (12) | 0.0450 (11) | 0.0452 (11) | 0.0008 (9) | 0.0007 (9) | 0.0191 (9) |
O2W | 0.0425 (11) | 0.0287 (10) | 0.0407 (11) | 0.0044 (8) | 0.0081 (9) | 0.0097 (8) |
O3W | 0.0471 (11) | 0.0270 (9) | 0.0401 (11) | 0.0057 (8) | 0.0097 (9) | 0.0090 (8) |
Zn1—O1 | 2.0181 (19) | C11—C12 | 1.437 (4) |
Zn1—O1W | 2.184 (2) | C12—N1 | 1.356 (3) |
Zn1—O2W | 2.1581 (19) | C13—O1 | 1.255 (3) |
Zn1—O3W | 2.113 (2) | C13—O2 | 1.263 (3) |
Zn1—N1 | 2.124 (2) | C13—C14 | 1.497 (3) |
Zn1—N2 | 2.156 (2) | C14—C15 | 1.389 (4) |
C1—N1 | 1.324 (3) | C14—C16i | 1.402 (3) |
C1—C2 | 1.388 (4) | C15—C16 | 1.380 (3) |
C1—H1 | 0.9300 | C15—H15 | 0.9300 |
C2—C3 | 1.353 (5) | C16—O3 | 1.367 (3) |
C2—H2 | 0.9300 | C16—C14i | 1.402 (3) |
C3—C4 | 1.403 (5) | C17—O4 | 1.244 (3) |
C3—H3 | 0.9300 | C17—O5 | 1.258 (3) |
C4—C12 | 1.407 (4) | C17—C18 | 1.505 (4) |
C4—C5 | 1.422 (5) | C18—C19 | 1.384 (4) |
C5—C6 | 1.339 (5) | C18—C20ii | 1.401 (3) |
C5—H5 | 0.9300 | C19—C20 | 1.385 (4) |
C6—C7 | 1.441 (5) | C19—H19 | 0.9300 |
C6—H6 | 0.9300 | C20—O6 | 1.356 (3) |
C7—C8 | 1.391 (5) | C20—C18ii | 1.401 (3) |
C7—C11 | 1.400 (4) | O3—H3A | 0.8200 |
C8—C9 | 1.364 (6) | O6—H6A | 0.8200 |
C8—H8 | 0.9300 | O1W—H1WA | 0.9650 |
C9—C10 | 1.397 (5) | O1W—H1WB | 0.9182 |
C9—H9 | 0.9300 | O2W—H2WA | 0.9333 |
C10—N2 | 1.322 (4) | O2W—H2WB | 0.9127 |
C10—H10 | 0.9300 | O3W—H3WA | 0.8873 |
C11—N2 | 1.362 (4) | O3W—H3WB | 0.8287 |
O1—Zn1—O3W | 93.06 (8) | C7—C11—C12 | 119.7 (3) |
O1—Zn1—N1 | 90.52 (9) | N1—C12—C4 | 122.2 (3) |
O3W—Zn1—N1 | 92.67 (8) | N1—C12—C11 | 117.9 (2) |
O1—Zn1—N2 | 168.50 (8) | C4—C12—C11 | 119.9 (3) |
O3W—Zn1—N2 | 90.35 (8) | O1—C13—O2 | 124.5 (2) |
N1—Zn1—N2 | 78.34 (9) | O1—C13—C14 | 117.3 (2) |
O1—Zn1—O2W | 93.13 (8) | O2—C13—C14 | 118.2 (2) |
O3W—Zn1—O2W | 86.71 (7) | C15—C14—C16i | 119.1 (2) |
N1—Zn1—O2W | 176.32 (8) | C15—C14—C13 | 119.7 (2) |
N2—Zn1—O2W | 98.03 (9) | C16i—C14—C13 | 121.2 (2) |
O1—Zn1—O1W | 90.61 (8) | C16—C15—C14 | 121.1 (2) |
O3W—Zn1—O1W | 171.35 (7) | C16—C15—H15 | 119.4 |
N1—Zn1—O1W | 95.13 (8) | C14—C15—H15 | 119.4 |
N2—Zn1—O1W | 87.58 (9) | O3—C16—C15 | 118.2 (2) |
O2W—Zn1—O1W | 85.27 (7) | O3—C16—C14i | 122.0 (2) |
N1—C1—C2 | 122.9 (3) | C15—C16—C14i | 119.8 (2) |
N1—C1—H1 | 118.6 | O4—C17—O5 | 123.5 (3) |
C2—C1—H1 | 118.6 | O4—C17—C18 | 118.2 (3) |
C3—C2—C1 | 119.2 (3) | O5—C17—C18 | 118.3 (2) |
C3—C2—H2 | 120.4 | C19—C18—C20ii | 119.3 (2) |
C1—C2—H2 | 120.4 | C19—C18—C17 | 120.2 (2) |
C2—C3—C4 | 120.3 (3) | C20ii—C18—C17 | 120.5 (2) |
C2—C3—H3 | 119.9 | C18—C19—C20 | 121.6 (2) |
C4—C3—H3 | 119.9 | C18—C19—H19 | 119.2 |
C3—C4—C12 | 117.0 (3) | C20—C19—H19 | 119.2 |
C3—C4—C5 | 124.0 (3) | O6—C20—C19 | 118.7 (2) |
C12—C4—C5 | 119.0 (3) | O6—C20—C18ii | 122.3 (2) |
C6—C5—C4 | 121.2 (3) | C19—C20—C18ii | 119.1 (2) |
C6—C5—H5 | 119.4 | C1—N1—C12 | 118.5 (2) |
C4—C5—H5 | 119.4 | C1—N1—Zn1 | 128.2 (2) |
C5—C6—C7 | 121.7 (3) | C12—N1—Zn1 | 113.14 (18) |
C5—C6—H6 | 119.1 | C10—N2—C11 | 118.1 (3) |
C7—C6—H6 | 119.1 | C10—N2—Zn1 | 129.8 (2) |
C8—C7—C11 | 117.5 (3) | C11—N2—Zn1 | 112.08 (18) |
C8—C7—C6 | 124.1 (3) | C13—O1—Zn1 | 131.20 (17) |
C11—C7—C6 | 118.4 (3) | C16—O3—H3A | 109.5 |
C9—C8—C7 | 119.9 (3) | C20—O6—H6A | 109.5 |
C9—C8—H8 | 120.1 | Zn1—O1W—H1WA | 107.0 |
C7—C8—H8 | 120.1 | Zn1—O1W—H1WB | 112.0 |
C8—C9—C10 | 119.3 (3) | H1WA—O1W—H1WB | 105.5 |
C8—C9—H9 | 120.4 | Zn1—O2W—H2WA | 95.5 |
C10—C9—H9 | 120.4 | Zn1—O2W—H2WB | 118.0 |
N2—C10—C9 | 122.6 (4) | H2WA—O2W—H2WB | 110.3 |
N2—C10—H10 | 118.7 | Zn1—O3W—H3WA | 114.7 |
C9—C10—H10 | 118.7 | Zn1—O3W—H3WB | 108.4 |
N2—C11—C7 | 122.6 (3) | H3WA—O3W—H3WB | 106.6 |
N2—C11—C12 | 117.6 (2) |
Symmetry codes: (i) −x+2, −y, −z; (ii) −x+1, −y, −z+1. |
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1WA···O3iii | 0.97 | 1.95 | 2.902 (3) | 170 |
O1W—H1WB···O2Wiv | 0.92 | 2.01 | 2.911 (3) | 168 |
O2W—H2WA···O2 | 0.93 | 1.75 | 2.663 (3) | 166 |
O3—H3A···O2i | 0.82 | 1.84 | 2.562 (3) | 147 |
O2W—H2WB···O5v | 0.91 | 1.80 | 2.692 (3) | 166 |
O3W—H3WA···O4 | 0.89 | 1.85 | 2.695 (3) | 158 |
O3W—H3WB···O4v | 0.83 | 1.82 | 2.650 (3) | 175 |
O6—H6A···O5ii | 0.82 | 1.84 | 2.566 (3) | 146 |
Symmetry codes: (i) −x+2, −y, −z; (ii) −x+1, −y, −z+1; (iii) −x+1, −y, −z; (iv) −x+1, −y+1, −z; (v) −x+1, −y+1, −z+1. |
Experimental details
Crystal data | |
Chemical formula | [Zn2(C8H4O6)(C12H8N2)2(H2O)6](C8H4O6) |
Mr | 991.46 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 293 |
a, b, c (Å) | 8.765 (5), 10.697 (5), 11.062 (5) |
α, β, γ (°) | 106.994 (5), 92.226 (5), 90.977 (5) |
V (Å3) | 990.7 (9) |
Z | 1 |
Radiation type | Mo Kα |
µ (mm−1) | 1.30 |
Crystal size (mm) | 0.25 × 0.18 × 0.15 |
Data collection | |
Diffractometer | Bruker SMART APEXII CCD diffractometer |
Absorption correction | Multi-scan (SADABS; Bruker, 2002) |
Tmin, Tmax | 0.737, 0.829 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 5446, 3824, 3205 |
Rint | 0.019 |
(sin θ/λ)max (Å−1) | 0.616 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.036, 0.086, 1.04 |
No. of reflections | 3824 |
No. of parameters | 289 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.33, −0.29 |
Computer programs: APEX2 (Bruker, 2002), SAINT (Bruker, 2002), SHELXTL (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), DIAMOND (Brandenburg, 1999).
Zn1—O1 | 2.0181 (19) | Zn1—O3W | 2.113 (2) |
Zn1—O1W | 2.184 (2) | Zn1—N1 | 2.124 (2) |
Zn1—O2W | 2.1581 (19) | Zn1—N2 | 2.156 (2) |
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1WA···O3i | 0.97 | 1.95 | 2.902 (3) | 170 |
O1W—H1WB···O2Wii | 0.92 | 2.01 | 2.911 (3) | 168 |
O2W—H2WA···O2 | 0.93 | 1.75 | 2.663 (3) | 166 |
O3—H3A···O2iii | 0.82 | 1.84 | 2.562 (3) | 147 |
O2W—H2WB···O5iv | 0.91 | 1.80 | 2.692 (3) | 166 |
O3W—H3WA···O4 | 0.89 | 1.85 | 2.695 (3) | 158 |
O3W—H3WB···O4iv | 0.83 | 1.82 | 2.650 (3) | 175 |
O6—H6A···O5v | 0.82 | 1.84 | 2.566 (3) | 146 |
Symmetry codes: (i) −x+1, −y, −z; (ii) −x+1, −y+1, −z; (iii) −x+2, −y, −z; (iv) −x+1, −y+1, −z+1; (v) −x+1, −y, −z+1. |
Acknowledgements
The authors thank Jilin Normal University for supporting this study.
References
Brandenburg, K. (1999). DIAMOND. Crystal Impact BbR, Bonn, Germany. Google Scholar
Bruker (2002). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Perry, J. J. IV, Perman, J. A. & Zaworotko, M. J. (2009). Chem. Soc. Rev. 38, 1400–1417. Web of Science PubMed CAS Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Sun, Y. G., Gao, E. J. & Wei, D. Z. (2007). Inorg. Chem. Commun. 10, 467–470. Web of Science CSD CrossRef CAS Google Scholar
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The design and synthesis of coordination compounds have attracted much interest in the fields of supramolecular chemistry and crystal engineering because of their intriguing structural diversities and potential applications (Sun et al., 2007; Perry IV, et al., 2009). To extend the previous work, we obtained the title compound, (I), by using ZnII, phenanthroline (phen) and 2,5-dihydroxyterephthalic acid (dhtp) as the starting materials.
The title compound, (I), is composed of a ZnII canion, a phen molecule, half a coordinated dhtp anion, half a free dhtp anion and three coordinated water molecules in the asymmetric unit as shown in Fig. 1. ZnII canion exhibits a distorted octahedral geometry, being coordinated by two N atoms of a phen molecule, one O atom from dhtp anion and three water O atoms. The Zn–O and Zn–N distances are normal. ZnII canions are connected by dhtp anion to form a [Zn2(phen)2(dhtp)(H2O)6]II cation unit. In additon, the free dhtp anion as the counter-ion presents in the sturcture. By way of O–H···O hydrogen bonding between the cation units and counter-anions, a three-dimensional network is formed (Fig. 2). The detailed hydrogen-bonding parameters are summarized in Table 1.