metal-organic compounds
catena-Poly[[aqua(dipyrido[3,2-a:2′,3′-c]phenazine-κ2N4,N5)zinc(II)]-μ-pyrazine-2,3-dicarboxylato-κ3N1,O2:O3]
aJilin Agriculture Engineering Polytechnic College, Siping 136000, People's Republic of China, and bDepartment of Chemistry, Jilin Normal University, Siping 136000, People's Republic of China
*Correspondence e-mail: guangbochejl@yahoo.com
In the title compound, [Zn(C6H2N2O4)(C18H10N4)(H2O)]n or [Zn(PZDC)(DPPZ)(H2O)]n (where DPPZ is dipyrido[3,2-a:2′,3′-c]phenazine and H2PZDC is pyrazine-2,3-dicarboxylic acid), the Zn atom is six-coordinated in a slightly distorted octahedral coordination geometry by three N atoms from one DPPZ ligand and one PZDC2− dianion, three O atoms from two different PZDC2− ligands and one water molecule. Each PZDC2− dianion serves as a spacer, connecting adjacent metal atoms into a polymeric chain structure parallel to the b axis. The chain motif is consolidated into a three-dimensional supramolecular network by O—H⋯O and O—H⋯N hydrogen bonds and π–π aromatic stacking interactions involving adjacent DPPZ ligands and PZDC2− dianions with centroid–centroid separations of 3.522 (6) and 3.732 (8) Å, respectively.
Related literature
For related literature, see: Che et al. (2008); Che, Li et al. (2006); Che, Xu & Liu (2006); Liu et al. (2008); Xu et al. (2008).
Experimental
Crystal data
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Refinement
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Data collection: PROCESS-AUTO (Rigaku, 1998); cell PROCESS-AUTO; data reduction: PROCESS-AUTO; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL-Plus (Sheldrick, 2008); software used to prepare material for publication: SHELXL97.
Supporting information
10.1107/S1600536808022824/rz2235sup1.cif
contains datablocks global, I. DOI:Structure factors: contains datablock I. DOI: 10.1107/S1600536808022824/rz2235Isup2.hkl
The DPPZ ligand was synthesized according to the literature method (Che, Li et al., 2006). The title compound was hydrothermally synthesized under autogenous pressure: a mixture of DPPZ, H2PZDC, ZnNO3 and water in a molar ratio of 1:1:1:5000 was sealed in a Teflon-lined autoclave and heated to 433 K for 3 d. Upon cooling and opening the bomb, yellow blocks of the title compound were obtained (83% yield based on Zn).
All H atoms on C atoms were positioned geometrically (C—H = 0.93 Å) and refined as riding, with Uiso(H)= 1.2Ueq(C). The hydrogen atoms of water molecule were located from a difference Fourier map and refined freely.
Data collection: PROCESS-AUTO (Rigaku, 1998); cell
PROCESS-AUTO (Rigaku, 1998); data reduction: PROCESS-AUTO (Rigaku, 1998); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL-Plus (Sheldrick, 2008); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).Fig. 1. A view of the title compound. Displacement ellipsoids are drawn at the 30% probability level (arbitrary spheres for the H atoms). [Symmetry code: (i) x, y + 1, z.] | |
Fig. 2. Packing diagram of the three-dimensional supramolecular structure of the title compound formed via π-π interactions. H atoms are omitted for clarity. |
[Zn(C6H2N2O4)(C18H10N4)(H2O)] | Z = 2 |
Mr = 531.78 | F(000) = 540 |
Triclinic, P1 | Dx = 1.744 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 6.7821 (14) Å | Cell parameters from 4412 reflections |
b = 7.4349 (15) Å | θ = 3.0–27.5° |
c = 20.410 (4) Å | µ = 1.27 mm−1 |
α = 91.26 (3)° | T = 292 K |
β = 95.77 (3)° | Block, yellow |
γ = 98.16 (3)° | 0.31 × 0.29 × 0.21 mm |
V = 1012.9 (4) Å3 |
Rigaku R-AXIS RAPID diffractometer | 4412 independent reflections |
Radiation source: fine-focus sealed tube | 3278 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.048 |
Detector resolution: 10.0 pixels mm-1 | θmax = 27.5°, θmin = 3.0° |
ω scans | h = −8→8 |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | k = −9→8 |
Tmin = 0.681, Tmax = 0.765 | l = −26→26 |
9890 measured reflections |
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)] = 0.048 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.148 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.07 | w = 1/[σ2(Fo2) + (0.084P)2 + 0.1727P] where P = (Fo2 + 2Fc2)/3 |
4412 reflections | (Δ/σ)max < 0.001 |
333 parameters | Δρmax = 0.42 e Å−3 |
0 restraints | Δρmin = −0.58 e Å−3 |
[Zn(C6H2N2O4)(C18H10N4)(H2O)] | γ = 98.16 (3)° |
Mr = 531.78 | V = 1012.9 (4) Å3 |
Triclinic, P1 | Z = 2 |
a = 6.7821 (14) Å | Mo Kα radiation |
b = 7.4349 (15) Å | µ = 1.27 mm−1 |
c = 20.410 (4) Å | T = 292 K |
α = 91.26 (3)° | 0.31 × 0.29 × 0.21 mm |
β = 95.77 (3)° |
Rigaku R-AXIS RAPID diffractometer | 4412 independent reflections |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | 3278 reflections with I > 2σ(I) |
Tmin = 0.681, Tmax = 0.765 | Rint = 0.048 |
9890 measured reflections |
R[F2 > 2σ(F2)] = 0.048 | 0 restraints |
wR(F2) = 0.148 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.07 | Δρmax = 0.42 e Å−3 |
4412 reflections | Δρmin = −0.58 e Å−3 |
333 parameters |
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 | ||
C1 | −0.3785 (6) | 0.2965 (5) | 0.7826 (2) | 0.0344 (9) | |
H1 | −0.4426 | 0.3029 | 0.8206 | 0.041* | |
C2 | −0.4723 (6) | 0.1853 (6) | 0.7307 (2) | 0.0375 (10) | |
H2 | −0.5931 | 0.1119 | 0.7349 | 0.045* | |
C3 | −0.3868 (6) | 0.1832 (6) | 0.6728 (2) | 0.0395 (10) | |
H3 | −0.4528 | 0.1144 | 0.6364 | 0.047* | |
C4 | −0.1986 (6) | 0.2861 (5) | 0.6690 (2) | 0.0291 (8) | |
C5 | −0.0963 (6) | 0.2913 (5) | 0.60945 (19) | 0.0283 (8) | |
C6 | −0.0924 (7) | 0.2081 (5) | 0.5015 (2) | 0.0352 (9) | |
C7 | −0.1870 (8) | 0.1180 (6) | 0.4421 (2) | 0.0443 (11) | |
H7 | −0.3185 | 0.0601 | 0.4400 | 0.053* | |
C8 | −0.0836 (8) | 0.1170 (6) | 0.3880 (2) | 0.0493 (12) | |
H8 | −0.1458 | 0.0582 | 0.3491 | 0.059* | |
C9 | 0.1164 (9) | 0.2037 (6) | 0.3903 (2) | 0.0514 (12) | |
H9 | 0.1845 | 0.2003 | 0.3531 | 0.062* | |
C10 | 0.2107 (8) | 0.2921 (7) | 0.4464 (2) | 0.0479 (12) | |
H10 | 0.3420 | 0.3496 | 0.4471 | 0.058* | |
C11 | 0.1095 (7) | 0.2967 (6) | 0.5036 (2) | 0.0379 (10) | |
C12 | 0.1042 (6) | 0.3850 (5) | 0.61078 (19) | 0.0292 (8) | |
C13 | 0.1983 (6) | 0.4856 (5) | 0.67084 (19) | 0.0286 (8) | |
C14 | 0.3909 (6) | 0.5847 (6) | 0.6747 (2) | 0.0345 (9) | |
H14 | 0.4637 | 0.5883 | 0.6384 | 0.041* | |
C15 | 0.4710 (6) | 0.6763 (6) | 0.7322 (2) | 0.0346 (9) | |
H15 | 0.5979 | 0.7444 | 0.7353 | 0.041* | |
C16 | 0.3603 (6) | 0.6662 (5) | 0.7859 (2) | 0.0326 (9) | |
H16 | 0.4165 | 0.7264 | 0.8253 | 0.039* | |
C17 | 0.0958 (5) | 0.4841 (5) | 0.72651 (18) | 0.0242 (7) | |
C18 | −0.1092 (5) | 0.3868 (5) | 0.72530 (18) | 0.0256 (8) | |
C19 | 0.1302 (5) | 0.9551 (5) | 0.89690 (18) | 0.0237 (7) | |
C20 | 0.1992 (5) | 1.1069 (5) | 0.93824 (19) | 0.0247 (8) | |
C21 | 0.2685 (6) | 0.9238 (5) | 1.02315 (19) | 0.0288 (8) | |
H21 | 0.3121 | 0.9090 | 1.0671 | 0.035* | |
C22 | 0.2102 (5) | 0.7712 (5) | 0.98204 (19) | 0.0261 (8) | |
H22 | 0.2235 | 0.6566 | 0.9978 | 0.031* | |
C23 | 0.0378 (6) | 0.9589 (5) | 0.82528 (19) | 0.0271 (8) | |
C24 | 0.2040 (5) | 1.3019 (5) | 0.91602 (18) | 0.0249 (8) | |
N1 | −0.1984 (5) | 0.3963 (4) | 0.78077 (16) | 0.0267 (7) | |
N2 | 0.1761 (5) | 0.5730 (4) | 0.78317 (15) | 0.0271 (7) | |
N3 | −0.1925 (5) | 0.2047 (4) | 0.55512 (17) | 0.0349 (8) | |
N4 | 0.2041 (5) | 0.3872 (5) | 0.55828 (17) | 0.0348 (8) | |
N5 | 0.1356 (4) | 0.7877 (4) | 0.92032 (15) | 0.0234 (6) | |
N6 | 0.2640 (5) | 1.0909 (4) | 1.00185 (16) | 0.0281 (7) | |
O1 | −0.0880 (4) | 0.8227 (4) | 0.80655 (14) | 0.0362 (7) | |
O2 | 0.0974 (5) | 1.0921 (4) | 0.79424 (15) | 0.0410 (7) | |
O1W | −0.2753 (5) | 0.5957 (5) | 0.91335 (17) | 0.0389 (8) | |
O3 | 0.3705 (4) | 1.3872 (4) | 0.91050 (17) | 0.0427 (8) | |
O4 | 0.0381 (4) | 1.3587 (3) | 0.90882 (14) | 0.0305 (6) | |
Zn | −0.03443 (6) | 0.57612 (5) | 0.85620 (2) | 0.02642 (16) | |
HW1A | −0.368 (8) | 0.552 (8) | 0.909 (3) | 0.054 (19)* | |
HW1B | −0.295 (7) | 0.692 (7) | 0.930 (2) | 0.034 (12)* |
U11 | U22 | U33 | U12 | U13 | U23 | |
C1 | 0.034 (2) | 0.031 (2) | 0.037 (2) | −0.0052 (17) | 0.0120 (17) | −0.0021 (17) |
C2 | 0.032 (2) | 0.036 (2) | 0.042 (2) | −0.0062 (18) | 0.0058 (18) | −0.0039 (18) |
C3 | 0.038 (2) | 0.037 (2) | 0.038 (2) | −0.0082 (19) | 0.0014 (18) | −0.0108 (18) |
C4 | 0.0326 (19) | 0.0232 (18) | 0.030 (2) | −0.0004 (15) | 0.0040 (16) | −0.0055 (15) |
C5 | 0.0333 (19) | 0.0250 (18) | 0.0254 (19) | 0.0033 (16) | −0.0004 (15) | −0.0022 (15) |
C6 | 0.047 (2) | 0.032 (2) | 0.027 (2) | 0.0109 (19) | −0.0004 (18) | −0.0010 (16) |
C7 | 0.058 (3) | 0.040 (2) | 0.032 (2) | 0.008 (2) | −0.006 (2) | −0.0054 (18) |
C8 | 0.080 (4) | 0.040 (2) | 0.026 (2) | 0.015 (2) | −0.011 (2) | −0.0046 (18) |
C9 | 0.082 (4) | 0.043 (3) | 0.032 (2) | 0.011 (3) | 0.019 (2) | −0.003 (2) |
C10 | 0.065 (3) | 0.048 (3) | 0.033 (2) | 0.011 (2) | 0.013 (2) | −0.001 (2) |
C11 | 0.050 (2) | 0.034 (2) | 0.030 (2) | 0.007 (2) | 0.0097 (19) | −0.0021 (17) |
C12 | 0.0334 (19) | 0.0291 (19) | 0.025 (2) | 0.0046 (16) | 0.0045 (16) | −0.0019 (15) |
C13 | 0.0273 (18) | 0.0256 (19) | 0.031 (2) | −0.0009 (15) | −0.0011 (15) | 0.0024 (15) |
C14 | 0.033 (2) | 0.037 (2) | 0.035 (2) | 0.0046 (17) | 0.0107 (17) | 0.0014 (17) |
C15 | 0.0257 (18) | 0.039 (2) | 0.037 (2) | −0.0023 (17) | 0.0029 (17) | 0.0059 (18) |
C16 | 0.032 (2) | 0.034 (2) | 0.029 (2) | −0.0023 (17) | −0.0001 (16) | −0.0016 (16) |
C17 | 0.0242 (17) | 0.0212 (17) | 0.0275 (19) | 0.0049 (14) | 0.0029 (14) | 0.0012 (14) |
C18 | 0.0274 (18) | 0.0208 (17) | 0.0273 (19) | 0.0009 (14) | −0.0003 (15) | 0.0009 (14) |
C19 | 0.0223 (16) | 0.0213 (17) | 0.0269 (19) | −0.0007 (14) | 0.0061 (14) | −0.0005 (14) |
C20 | 0.0207 (16) | 0.0185 (17) | 0.034 (2) | −0.0023 (14) | 0.0084 (15) | −0.0024 (15) |
C21 | 0.0315 (18) | 0.0289 (19) | 0.0245 (19) | −0.0020 (16) | 0.0060 (15) | −0.0003 (15) |
C22 | 0.0281 (18) | 0.0223 (17) | 0.029 (2) | 0.0052 (15) | 0.0045 (15) | 0.0031 (15) |
C23 | 0.0302 (18) | 0.0231 (18) | 0.028 (2) | 0.0050 (15) | 0.0032 (15) | 0.0015 (15) |
C24 | 0.0307 (18) | 0.0192 (16) | 0.0228 (18) | −0.0046 (15) | 0.0066 (15) | −0.0052 (13) |
N1 | 0.0270 (15) | 0.0228 (15) | 0.0294 (17) | −0.0004 (13) | 0.0050 (13) | −0.0041 (12) |
N2 | 0.0301 (16) | 0.0242 (15) | 0.0240 (16) | −0.0034 (13) | −0.0008 (13) | −0.0030 (12) |
N3 | 0.0423 (19) | 0.0304 (17) | 0.0305 (19) | 0.0023 (15) | 0.0017 (15) | −0.0043 (14) |
N4 | 0.0417 (19) | 0.0354 (18) | 0.0265 (18) | 0.0027 (15) | 0.0038 (15) | −0.0016 (14) |
N5 | 0.0243 (14) | 0.0201 (14) | 0.0260 (16) | 0.0017 (12) | 0.0060 (12) | 0.0013 (12) |
N6 | 0.0277 (15) | 0.0260 (16) | 0.0294 (17) | −0.0008 (13) | 0.0049 (13) | −0.0033 (13) |
O1 | 0.0410 (15) | 0.0258 (14) | 0.0365 (16) | −0.0014 (12) | −0.0119 (13) | 0.0002 (12) |
O2 | 0.0549 (19) | 0.0329 (15) | 0.0347 (17) | 0.0005 (14) | 0.0095 (14) | 0.0072 (12) |
O1W | 0.0271 (16) | 0.0357 (18) | 0.052 (2) | −0.0066 (14) | 0.0164 (14) | −0.0192 (15) |
O3 | 0.0335 (15) | 0.0341 (16) | 0.057 (2) | −0.0112 (13) | 0.0087 (14) | 0.0051 (14) |
O4 | 0.0342 (14) | 0.0237 (13) | 0.0367 (16) | 0.0096 (11) | 0.0091 (12) | 0.0088 (11) |
Zn | 0.0313 (3) | 0.0203 (2) | 0.0259 (3) | −0.00162 (17) | 0.00328 (17) | −0.00223 (16) |
C1—N1 | 1.341 (5) | C15—H15 | 0.9300 |
C1—C2 | 1.374 (6) | C16—N2 | 1.335 (5) |
C1—H1 | 0.9300 | C16—H16 | 0.9300 |
C2—C3 | 1.369 (6) | C17—N2 | 1.345 (5) |
C2—H2 | 0.9300 | C17—C18 | 1.471 (5) |
C3—C4 | 1.402 (5) | C18—N1 | 1.341 (5) |
C3—H3 | 0.9300 | C19—N5 | 1.347 (4) |
C4—C18 | 1.393 (5) | C19—C20 | 1.390 (5) |
C4—C5 | 1.457 (5) | C19—C23 | 1.534 (5) |
C5—N3 | 1.332 (5) | C20—N6 | 1.342 (5) |
C5—C12 | 1.435 (5) | C20—C24 | 1.525 (5) |
C6—N3 | 1.344 (5) | C21—N6 | 1.328 (5) |
C6—C7 | 1.420 (6) | C21—C22 | 1.383 (5) |
C6—C11 | 1.429 (6) | C21—H21 | 0.9300 |
C7—C8 | 1.367 (7) | C22—N5 | 1.325 (5) |
C7—H7 | 0.9300 | C22—H22 | 0.9300 |
C8—C9 | 1.412 (7) | C23—O2 | 1.229 (4) |
C8—H8 | 0.9300 | C23—O1 | 1.253 (5) |
C9—C10 | 1.360 (7) | C24—O3 | 1.231 (4) |
C9—H9 | 0.9300 | C24—O4 | 1.254 (5) |
C10—C11 | 1.414 (6) | N1—Zn | 2.130 (3) |
C10—H10 | 0.9300 | N2—Zn | 2.167 (3) |
C11—N4 | 1.346 (5) | N5—Zn | 2.147 (3) |
C12—N4 | 1.324 (5) | O1—Zn | 2.172 (3) |
C12—C13 | 1.462 (5) | O1W—Zn | 2.120 (3) |
C13—C17 | 1.390 (5) | O1W—HW1A | 0.66 (5) |
C13—C14 | 1.399 (5) | O1W—HW1B | 0.82 (5) |
C14—C15 | 1.367 (6) | O4—Zni | 2.051 (3) |
C14—H14 | 0.9300 | Zn—O4ii | 2.051 (3) |
C15—C16 | 1.387 (6) | ||
N1—C1—C2 | 122.7 (4) | N1—C18—C17 | 116.8 (3) |
N1—C1—H1 | 118.6 | C4—C18—C17 | 119.9 (3) |
C2—C1—H1 | 118.6 | N5—C19—C20 | 119.5 (3) |
C3—C2—C1 | 119.5 (4) | N5—C19—C23 | 115.0 (3) |
C3—C2—H2 | 120.2 | C20—C19—C23 | 125.5 (3) |
C1—C2—H2 | 120.2 | N6—C20—C19 | 121.5 (3) |
C2—C3—C4 | 119.2 (4) | N6—C20—C24 | 115.0 (3) |
C2—C3—H3 | 120.4 | C19—C20—C24 | 123.5 (3) |
C4—C3—H3 | 120.4 | N6—C21—C22 | 122.1 (4) |
C18—C4—C3 | 117.3 (4) | N6—C21—H21 | 119.0 |
C18—C4—C5 | 119.9 (3) | C22—C21—H21 | 119.0 |
C3—C4—C5 | 122.9 (4) | N5—C22—C21 | 120.2 (3) |
N3—C5—C12 | 121.8 (4) | N5—C22—H22 | 119.9 |
N3—C5—C4 | 118.3 (3) | C21—C22—H22 | 119.9 |
C12—C5—C4 | 120.0 (3) | O2—C23—O1 | 129.1 (4) |
N3—C6—C7 | 119.4 (4) | O2—C23—C19 | 116.4 (3) |
N3—C6—C11 | 121.2 (4) | O1—C23—C19 | 114.5 (3) |
C7—C6—C11 | 119.3 (4) | O3—C24—O4 | 127.8 (3) |
C8—C7—C6 | 119.6 (5) | O3—C24—C20 | 116.4 (3) |
C8—C7—H7 | 120.2 | O4—C24—C20 | 115.7 (3) |
C6—C7—H7 | 120.2 | C1—N1—C18 | 117.8 (3) |
C7—C8—C9 | 121.0 (4) | C1—N1—Zn | 127.4 (3) |
C7—C8—H8 | 119.5 | C18—N1—Zn | 114.9 (2) |
C9—C8—H8 | 119.5 | C16—N2—C17 | 118.8 (3) |
C10—C9—C8 | 120.8 (5) | C16—N2—Zn | 127.2 (3) |
C10—C9—H9 | 119.6 | C17—N2—Zn | 113.4 (2) |
C8—C9—H9 | 119.6 | C5—N3—C6 | 116.8 (4) |
C9—C10—C11 | 120.1 (5) | C12—N4—C11 | 117.0 (4) |
C9—C10—H10 | 119.9 | C22—N5—C19 | 119.2 (3) |
C11—C10—H10 | 119.9 | C22—N5—Zn | 126.6 (2) |
N4—C11—C10 | 119.3 (4) | C19—N5—Zn | 113.1 (2) |
N4—C11—C6 | 121.5 (4) | C21—N6—C20 | 117.3 (3) |
C10—C11—C6 | 119.2 (4) | C23—O1—Zn | 113.8 (2) |
N4—C12—C5 | 121.6 (4) | Zn—O1W—HW1A | 129 (5) |
N4—C12—C13 | 119.0 (3) | Zn—O1W—HW1B | 123 (3) |
C5—C12—C13 | 119.3 (3) | HW1A—O1W—HW1B | 100 (6) |
C17—C13—C14 | 118.0 (4) | C24—O4—Zni | 127.6 (2) |
C17—C13—C12 | 119.8 (3) | O4ii—Zn—O1W | 90.19 (13) |
C14—C13—C12 | 122.2 (4) | O4ii—Zn—N1 | 90.37 (12) |
C15—C14—C13 | 119.5 (4) | O1W—Zn—N1 | 96.93 (13) |
C15—C14—H14 | 120.2 | O4ii—Zn—N5 | 97.78 (12) |
C13—C14—H14 | 120.2 | O1W—Zn—N5 | 86.87 (13) |
C14—C15—C16 | 119.0 (4) | N1—Zn—N5 | 171.02 (11) |
C14—C15—H15 | 120.5 | O4ii—Zn—N2 | 98.61 (11) |
C16—C15—H15 | 120.5 | O1W—Zn—N2 | 169.43 (13) |
N2—C16—C15 | 122.4 (4) | N1—Zn—N2 | 77.29 (11) |
N2—C16—H16 | 118.8 | N5—Zn—N2 | 97.65 (12) |
C15—C16—H16 | 118.8 | O4ii—Zn—O1 | 174.40 (11) |
N2—C17—C13 | 122.3 (3) | O1W—Zn—O1 | 90.70 (13) |
N2—C17—C18 | 116.9 (3) | N1—Zn—O1 | 95.01 (11) |
C13—C17—C18 | 120.8 (3) | N5—Zn—O1 | 76.76 (11) |
N1—C18—C4 | 123.3 (3) | N2—Zn—O1 | 81.10 (12) |
Symmetry codes: (i) x, y+1, z; (ii) x, y−1, z. |
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—HW1A···O3iii | 0.66 (5) | 2.01 (5) | 2.662 (4) | 169 (7) |
O1W—HW1B···N6iv | 0.82 (5) | 2.07 (5) | 2.859 (5) | 159 (4) |
Symmetry codes: (iii) x−1, y−1, z; (iv) −x, −y+2, −z+2. |
Experimental details
Crystal data | |
Chemical formula | [Zn(C6H2N2O4)(C18H10N4)(H2O)] |
Mr | 531.78 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 292 |
a, b, c (Å) | 6.7821 (14), 7.4349 (15), 20.410 (4) |
α, β, γ (°) | 91.26 (3), 95.77 (3), 98.16 (3) |
V (Å3) | 1012.9 (4) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 1.27 |
Crystal size (mm) | 0.31 × 0.29 × 0.21 |
Data collection | |
Diffractometer | Rigaku R-AXIS RAPID diffractometer |
Absorption correction | Multi-scan (ABSCOR; Higashi, 1995) |
Tmin, Tmax | 0.681, 0.765 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 9890, 4412, 3278 |
Rint | 0.048 |
(sin θ/λ)max (Å−1) | 0.649 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.048, 0.148, 1.07 |
No. of reflections | 4412 |
No. of parameters | 333 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 0.42, −0.58 |
Computer programs: PROCESS-AUTO (Rigaku, 1998), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL-Plus (Sheldrick, 2008).
N1—Zn | 2.130 (3) | O1—Zn | 2.172 (3) |
N2—Zn | 2.167 (3) | O1W—Zn | 2.120 (3) |
N5—Zn | 2.147 (3) | O4—Zni | 2.051 (3) |
O4ii—Zn—O1W | 90.19 (13) | O1W—Zn—N5 | 86.87 (13) |
O4ii—Zn—N1 | 90.37 (12) | N1—Zn—N5 | 171.02 (11) |
O1W—Zn—N1 | 96.93 (13) | O4ii—Zn—N2 | 98.61 (11) |
O4ii—Zn—N5 | 97.78 (12) | O1W—Zn—N2 | 169.43 (13) |
Symmetry codes: (i) x, y+1, z; (ii) x, y−1, z. |
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—HW1A···O3iii | 0.66 (5) | 2.01 (5) | 2.662 (4) | 169 (7) |
O1W—HW1B···N6iv | 0.82 (5) | 2.07 (5) | 2.859 (5) | 159 (4) |
Symmetry codes: (iii) x−1, y−1, z; (iv) −x, −y+2, −z+2. |
Acknowledgements
The authors thank the Doctoral Foundation of Jilin Normal University (grant Nos. 2006006 and 2007009) and the Subject and Base Construction Foundation of Jilin Normal University (grant No. 2006041).
References
Che, G.-B., Li, W.-L., Kong, Z.-G., Su, Z.-S., Chu, B., Li, B., Zhang, Z.-Q., Hu, Z.-Z. & Chi, H.-J. (2006). Synth. Commun. 36, 2519–2524. Web of Science CrossRef CAS Google Scholar
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A successful strategy for preparing metal-organic supramolecular architectures is the assembly reaction between a transition d10 metal ion and two types of ligands with one acting as a bridging ligand and the other as a chelating ligand (Liu et al., 2008; Che et al., 2008). Pyrazine-2,3-dicarboxylic acid (H2PZDC) possesses the ability to bridge and chelate metal atoms using the carboxylate oxygen atoms and nitrogen atoms (Xu et al., 2008). 1,10-Phenanthroline (phen) and its derivatives are important chelating ligands for the construction of metal-organic complexes (Che, Xu & Liu, 2006). Dipyrido[3,2-a:2',3'-c]-phenazine (DPPZ) as a phen derivative possesses potential supramolecular recognition sites for π-π aromatic stacking interactions. The present attempt at synthesizing a new zinc polymer with DPPZ and H2PZDC gave the title complex, [Zn(DPPZ)(PZDC)(H2O)]n, whose structure is reported here.
The Zn atom is six-coordinated by three N atoms from one DPPZ ligand and one PZDC2- ligand, and three O atoms from two different PZDC2- ligands and one water molecule in a slightly distorted octahedral coordination geometry (Fig. 1). The Zn—O distances range from 2.051 (3) Å to 2.172 (3) Å and the Zn—N lengths from 2.130 (3) Å to 2.167 (3) Å (Table 1). Each PZDC2- dianion serves as a spacer to connect adjacent metal centres into a one-dimensional chain structure parallel to the b axis. Neighbouring chains interact through π-π contacts, leading to a three-dimensional supramolecular structure (Fig. 2). There are two types of π-π interactions, occurring between adjacent DPPZ ligands (centroid-to-centroid separation = 3.732 (8) Å) and PZDC2- anions (centroid-to-centroid separation = 3.522 (6) Å). Hydrogen bonds involving the O1W atom as donor and the N6 and O3 atoms of the PZDC2- dianion as acceptors further stabilize the structure (Table 2).