Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807033685/gg2024sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807033685/gg2024Isup2.hkl |
CCDC reference: 657587
All solvents and chemicals were of analytical grade and were used without further purification. Ligand dttp was prepared via a one-step Mannich reaction as a white powder in 57% yield (Yan et al., 1994). For the synthesis of (I), an ethanol solution (10 ml) of Cd(NO3)2.6H2O (34.4 mg, 0.1 mmol) was added slowly with constant stirring to a solution of dttp (31.2 mg, 0.1 mmol) in ethanol (30 ml) to give a clear solution. The reaction mixture was left to stand at room temperature for one week and colorless crystalline products were obtained (34.2 mg, 79%). Anal. Calcd. for C32H48CdN14O12: C, 43.84; H, 5.52; N, 22.37. Found: C, 41.18; H, 5.18; N, 21.01. Infra-red (KBr, cm-1): 3422(s), 3233(m), 2962(m), 1656(m), 1522(s).
All non-hydrogen atoms were refined anisotropically, whereas the positions of all H atoms were fixed geometrically and treated as riding atoms in the refinement with X—H distances set as follows: C–H 0.93–0.97 Å and O–H 0.82–0.85 Å.
In recent years, organic ligands with azole units have become a new class of supramolecular synthons of intense interest in creating appealing coordination polymers (Hoskins et al., 1997; Li et al., 2005). In our previous studies, we synthesized two kinds of flexible bidentate ligands 1,6-di(imidazole-1-yl-methyl)-4-R-phenol and 1,6-di(triazole-1-yl-methyl)-4-R-phenol (R = Me, t-Bu, or Cl), and demonstrated that they can form different structures and topologies with different metal ions (Ma et al., 2003; Zhu et al., 2004; Zhu et al., 2007). The title compound, (I), is obtained by the reaction of 1,6-di(triazole-1-yl-methyl)-4 - t-Bu-phenol(dttp) with cadmium nitrate in ethanol.
The asymmetric unit of (I) contains half a Cd(II) atom, one dttp ligand, two water molecules and a nitrate ion. The metal atoms are located on the crystallographic inversion center with octahedral geometry, formed equatorially by four N atoms of triazoles from four dttp ligands and axially by two O atoms from two water molecules (Fig. 1). Each dttp adopts a trans conformation in which two triazole groups of a ligand with a dihedral angle of 53.9 (3) ° are on the opposite direction of the central benzene ring. In this way two metal atoms and two dttp ligands form a 24-membered M2L2 macrocycle through Cd—N coordination bonds. In each macrocycle, two phenyl rings are found strictly in a plane and the intermetallic distance between the two CdII atoms is 11.96 (1) Å. Such a metallomacrocyclic unit repeats along the a-axis to generate a double-stranded one-dimensional cationic chain as shown in Fig. 2.
Each phenol O—H moiety is directed at the N atom of a triazole moiety with H···N distances ranging from 1.99 to 2.61 Å, indicative of strong intramolecular hydrogen-bonding interactions. It is noticed that the resulting one-dimensional chains are further linked together to a three-dimensional framework by the uncoordinated water molecules and nitrate anions through O–H···O, O–H···N and C–H···O hydrogen-bonding interactions as shown in Fig. 3.
For related literature, see: Hoskins et al. (1997); Ma et al. (2003); Yan et al. (1994); Zhu et al. (2004, 2007).
For related literature, see: Li et al. (2005).
Data collection: SMART (Bruker, 2000); cell refinement: SAINT (Bruker, 2000); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Bruker, 2000); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.
[Cd(C16H20N6O)2(H2O)2](NO3)2·2H2O | F(000) = 964 |
Mr = 933.24 | Dx = 1.543 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 848 reflections |
a = 11.960 (4) Å | θ = 2.3–23.5° |
b = 9.448 (3) Å | µ = 0.62 mm−1 |
c = 18.756 (6) Å | T = 293 K |
β = 108.592 (4)° | Block, colorless |
V = 2008.9 (11) Å3 | 0.35 × 0.30 × 0.20 mm |
Z = 2 |
Bruker SMART CCD area-detector diffractometer | 3897 independent reflections |
Radiation source: fine-focus sealed tube | 2974 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.031 |
φ and ω scans | θmax = 26.0°, θmin = 1.8° |
Absorption correction: multi-scan (SADABS; Bruker, 2000) | h = −12→14 |
Tmin = 0.812, Tmax = 0.886 | k = −7→11 |
8433 measured reflections | l = −22→23 |
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)] = 0.044 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.107 | H-atom parameters constrained |
S = 1.08 | w = 1/[σ2(Fo2) + (0.047P)2] where P = (Fo2 + 2Fc2)/3 |
3897 reflections | (Δ/σ)max < 0.001 |
272 parameters | Δρmax = 0.92 e Å−3 |
0 restraints | Δρmin = −0.46 e Å−3 |
[Cd(C16H20N6O)2(H2O)2](NO3)2·2H2O | V = 2008.9 (11) Å3 |
Mr = 933.24 | Z = 2 |
Monoclinic, P21/c | Mo Kα radiation |
a = 11.960 (4) Å | µ = 0.62 mm−1 |
b = 9.448 (3) Å | T = 293 K |
c = 18.756 (6) Å | 0.35 × 0.30 × 0.20 mm |
β = 108.592 (4)° |
Bruker SMART CCD area-detector diffractometer | 3897 independent reflections |
Absorption correction: multi-scan (SADABS; Bruker, 2000) | 2974 reflections with I > 2σ(I) |
Tmin = 0.812, Tmax = 0.886 | Rint = 0.031 |
8433 measured reflections |
R[F2 > 2σ(F2)] = 0.044 | 0 restraints |
wR(F2) = 0.107 | H-atom parameters constrained |
S = 1.08 | Δρmax = 0.92 e Å−3 |
3897 reflections | Δρmin = −0.46 e Å−3 |
272 parameters |
Experimental. The structure was solved by direct methods (Bruker, 2000) and successive difference Fourier syntheses. |
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 | ||
Cd1 | 1.0000 | 0.5000 | 0.0000 | 0.03931 (14) | |
C1 | 0.4821 (3) | 0.1571 (4) | 0.07099 (17) | 0.0367 (8) | |
C2 | 0.4142 (3) | 0.0348 (3) | 0.05930 (19) | 0.0362 (8) | |
C3 | 0.4560 (3) | −0.0813 (4) | 0.10476 (18) | 0.0389 (8) | |
H3 | 0.4097 | −0.1625 | 0.0971 | 0.047* | |
C4 | 0.5635 (3) | −0.0817 (4) | 0.16110 (18) | 0.0389 (8) | |
C5 | 0.6286 (3) | 0.0425 (4) | 0.17102 (18) | 0.0394 (8) | |
H5 | 0.7015 | 0.0455 | 0.2085 | 0.047* | |
C6 | 0.5898 (3) | 0.1625 (3) | 0.12747 (17) | 0.0359 (7) | |
C7 | 0.6600 (3) | 0.2970 (4) | 0.14719 (19) | 0.0441 (9) | |
H7A | 0.6086 | 0.3715 | 0.1542 | 0.053* | |
H7B | 0.7219 | 0.2835 | 0.1948 | 0.053* | |
C8 | 0.8256 (3) | 0.3626 (4) | 0.0972 (2) | 0.0463 (9) | |
H8 | 0.8886 | 0.3422 | 0.1401 | 0.056* | |
C9 | 0.7236 (3) | 0.4264 (4) | −0.0096 (2) | 0.0489 (9) | |
H9 | 0.7025 | 0.4610 | −0.0585 | 0.059* | |
C10 | 0.2986 (3) | 0.0280 (4) | −0.0035 (2) | 0.0433 (9) | |
H10A | 0.3098 | 0.0617 | −0.0496 | 0.052* | |
H10B | 0.2725 | −0.0696 | −0.0113 | 0.052* | |
C11 | 0.1637 (3) | 0.2360 (4) | −0.01451 (19) | 0.0452 (9) | |
H11 | 0.1845 | 0.2853 | −0.0513 | 0.054* | |
C12 | 0.0861 (3) | 0.1758 (4) | 0.0643 (2) | 0.0594 (11) | |
H12 | 0.0388 | 0.1771 | 0.0952 | 0.071* | |
C13 | 0.6105 (3) | −0.2113 (4) | 0.21066 (18) | 0.0456 (9) | |
C14 | 0.5190 (4) | −0.3283 (4) | 0.1967 (2) | 0.0707 (13) | |
H14A | 0.5023 | −0.3633 | 0.1464 | 0.106* | |
H14B | 0.4480 | −0.2915 | 0.2032 | 0.106* | |
H14C | 0.5489 | −0.4039 | 0.2318 | 0.106* | |
C15 | 0.6439 (4) | −0.1696 (5) | 0.2937 (2) | 0.0679 (12) | |
H15A | 0.5759 | −0.1321 | 0.3038 | 0.102* | |
H15B | 0.7048 | −0.0990 | 0.3048 | 0.102* | |
H15C | 0.6720 | −0.2514 | 0.3246 | 0.102* | |
C16 | 0.7174 (4) | −0.2704 (5) | 0.1931 (3) | 0.0804 (14) | |
H16A | 0.7468 | −0.3518 | 0.2240 | 0.121* | |
H16B | 0.7779 | −0.1994 | 0.2031 | 0.121* | |
H16C | 0.6948 | −0.2971 | 0.1410 | 0.121* | |
N1 | 0.7139 (2) | 0.3441 (3) | 0.09105 (15) | 0.0391 (7) | |
N2 | 0.6458 (2) | 0.3859 (3) | 0.02182 (16) | 0.0488 (8) | |
N3 | 0.8359 (2) | 0.4139 (3) | 0.03429 (16) | 0.0452 (7) | |
N4 | 0.2073 (2) | 0.1133 (3) | 0.01273 (14) | 0.0390 (7) | |
N5 | 0.1576 (3) | 0.0706 (4) | 0.06402 (18) | 0.0564 (8) | |
N6 | 0.0867 (2) | 0.2805 (3) | 0.01688 (16) | 0.0439 (7) | |
N7 | 0.9577 (4) | 0.0212 (6) | 0.2125 (3) | 0.0825 (13) | |
O1 | 0.43423 (19) | 0.2713 (2) | 0.02633 (14) | 0.0460 (6) | |
H1 | 0.4874 | 0.3215 | 0.0216 | 0.069* | |
O2 | 1.1054 (2) | 0.5603 (3) | 0.12084 (14) | 0.0670 (8) | |
H2A | 1.1197 | 0.6486 | 0.1253 | 0.080* | |
H2B | 1.0652 | 0.5326 | 0.1483 | 0.080* | |
O3 | 0.1714 (3) | 0.8280 (3) | 0.16290 (17) | 0.0990 (11) | |
H3B | 0.2153 | 0.8576 | 0.1383 | 0.149* | |
H3C | 0.1105 | 0.8802 | 0.1535 | 0.149* | |
O4 | 0.9864 (7) | −0.0496 (6) | 0.2614 (3) | 0.239 (4) | |
O5 | 0.9399 (5) | 0.0037 (5) | 0.1480 (3) | 0.164 (3) | |
O6 | 0.9167 (5) | 0.1339 (7) | 0.2248 (4) | 0.178 (2) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Cd1 | 0.0348 (2) | 0.0368 (2) | 0.0502 (2) | 0.00473 (15) | 0.01896 (15) | 0.00747 (17) |
C1 | 0.0419 (18) | 0.032 (2) | 0.0437 (18) | 0.0064 (15) | 0.0250 (15) | 0.0041 (15) |
C2 | 0.0361 (17) | 0.032 (2) | 0.0462 (19) | 0.0023 (13) | 0.0206 (15) | −0.0034 (14) |
C3 | 0.0436 (19) | 0.031 (2) | 0.050 (2) | 0.0004 (15) | 0.0257 (16) | −0.0005 (16) |
C4 | 0.046 (2) | 0.033 (2) | 0.0445 (19) | 0.0035 (16) | 0.0247 (16) | 0.0019 (16) |
C5 | 0.0402 (18) | 0.042 (2) | 0.0401 (18) | 0.0016 (15) | 0.0187 (15) | 0.0037 (15) |
C6 | 0.0406 (18) | 0.034 (2) | 0.0409 (17) | −0.0034 (14) | 0.0241 (15) | −0.0016 (15) |
C7 | 0.050 (2) | 0.041 (2) | 0.049 (2) | −0.0056 (16) | 0.0279 (17) | −0.0027 (17) |
C8 | 0.0394 (19) | 0.049 (2) | 0.050 (2) | −0.0010 (16) | 0.0137 (16) | 0.0048 (18) |
C9 | 0.044 (2) | 0.052 (3) | 0.050 (2) | −0.0069 (17) | 0.0143 (17) | 0.0138 (19) |
C10 | 0.046 (2) | 0.036 (2) | 0.051 (2) | 0.0047 (15) | 0.0189 (16) | −0.0055 (15) |
C11 | 0.049 (2) | 0.038 (2) | 0.052 (2) | 0.0077 (16) | 0.0210 (17) | 0.0092 (17) |
C12 | 0.059 (2) | 0.056 (3) | 0.080 (3) | 0.012 (2) | 0.046 (2) | 0.018 (2) |
C13 | 0.055 (2) | 0.039 (2) | 0.048 (2) | 0.0038 (16) | 0.0224 (17) | 0.0107 (17) |
C14 | 0.087 (3) | 0.046 (3) | 0.073 (3) | −0.006 (2) | 0.016 (2) | 0.019 (2) |
C15 | 0.087 (3) | 0.060 (3) | 0.053 (2) | 0.002 (2) | 0.018 (2) | 0.014 (2) |
C16 | 0.080 (3) | 0.066 (3) | 0.110 (4) | 0.032 (2) | 0.051 (3) | 0.037 (3) |
N1 | 0.0404 (15) | 0.0347 (17) | 0.0460 (16) | −0.0040 (12) | 0.0190 (13) | 0.0022 (13) |
N2 | 0.0390 (16) | 0.051 (2) | 0.0560 (18) | −0.0041 (14) | 0.0148 (14) | 0.0149 (15) |
N3 | 0.0421 (17) | 0.044 (2) | 0.0533 (17) | −0.0008 (13) | 0.0206 (14) | 0.0075 (14) |
N4 | 0.0381 (15) | 0.0352 (18) | 0.0442 (15) | −0.0003 (12) | 0.0138 (12) | −0.0010 (13) |
N5 | 0.0540 (19) | 0.048 (2) | 0.079 (2) | 0.0102 (16) | 0.0372 (17) | 0.0191 (18) |
N6 | 0.0391 (16) | 0.0387 (18) | 0.0575 (18) | 0.0058 (13) | 0.0205 (14) | 0.0071 (14) |
N7 | 0.088 (3) | 0.090 (4) | 0.071 (3) | 0.004 (2) | 0.028 (2) | 0.010 (3) |
O1 | 0.0433 (13) | 0.0332 (15) | 0.0646 (15) | 0.0034 (11) | 0.0215 (12) | 0.0128 (12) |
O2 | 0.086 (2) | 0.0573 (18) | 0.0549 (16) | 0.0001 (16) | 0.0189 (15) | 0.0034 (14) |
O3 | 0.118 (3) | 0.070 (2) | 0.100 (2) | −0.0065 (19) | 0.022 (2) | 0.0237 (19) |
O4 | 0.374 (10) | 0.121 (4) | 0.116 (4) | 0.077 (5) | −0.069 (5) | 0.028 (3) |
O5 | 0.171 (5) | 0.258 (7) | 0.079 (3) | −0.079 (4) | 0.063 (3) | −0.017 (3) |
O6 | 0.169 (5) | 0.143 (5) | 0.242 (7) | 0.026 (4) | 0.093 (5) | 0.025 (5) |
Cd1—O2i | 2.287 (3) | C11—N4 | 1.307 (4) |
Cd1—O2 | 2.287 (3) | C11—N6 | 1.311 (4) |
Cd1—N6ii | 2.295 (3) | C11—H11 | 0.9300 |
Cd1—N6iii | 2.295 (3) | C12—N5 | 1.312 (5) |
Cd1—N3i | 2.395 (3) | C12—N6 | 1.332 (4) |
Cd1—N3 | 2.395 (3) | C12—H12 | 0.9300 |
C1—O1 | 1.374 (4) | C13—C14 | 1.518 (5) |
C1—C6 | 1.383 (4) | C13—C16 | 1.524 (5) |
C1—C2 | 1.389 (4) | C13—C15 | 1.531 (5) |
C2—C3 | 1.382 (5) | C14—H14A | 0.9600 |
C2—C10 | 1.505 (5) | C14—H14B | 0.9600 |
C3—C4 | 1.380 (4) | C14—H14C | 0.9600 |
C3—H3 | 0.9300 | C15—H15A | 0.9600 |
C4—C5 | 1.387 (5) | C15—H15B | 0.9600 |
C4—C13 | 1.532 (5) | C15—H15C | 0.9600 |
C5—C6 | 1.388 (4) | C16—H16A | 0.9600 |
C5—H5 | 0.9300 | C16—H16B | 0.9600 |
C6—C7 | 1.502 (4) | C16—H16C | 0.9600 |
C7—N1 | 1.469 (4) | N1—N2 | 1.353 (4) |
C7—H7A | 0.9700 | N4—N5 | 1.343 (4) |
C7—H7B | 0.9700 | N6—Cd1iv | 2.295 (3) |
C8—N1 | 1.315 (4) | N7—O4 | 1.099 (6) |
C8—N3 | 1.318 (4) | N7—O5 | 1.170 (6) |
C8—H8 | 0.9300 | N7—O6 | 1.225 (6) |
C9—N2 | 1.307 (4) | O1—H1 | 0.8200 |
C9—N3 | 1.338 (4) | O2—H2A | 0.8500 |
C9—H9 | 0.9300 | O2—H2B | 0.8500 |
C10—N4 | 1.465 (4) | O3—H3B | 0.8500 |
C10—H10A | 0.9700 | O3—H3C | 0.8499 |
C10—H10B | 0.9700 | ||
O2i—Cd1—O2 | 180.00 (8) | N4—C11—H11 | 124.5 |
O2i—Cd1—N6ii | 90.38 (10) | N6—C11—H11 | 124.5 |
O2—Cd1—N6ii | 89.62 (10) | N5—C12—N6 | 114.7 (3) |
O2i—Cd1—N6iii | 89.62 (10) | N5—C12—H12 | 122.7 |
O2—Cd1—N6iii | 90.38 (10) | N6—C12—H12 | 122.7 |
N6ii—Cd1—N6iii | 180.0 | C14—C13—C16 | 107.7 (3) |
O2i—Cd1—N3i | 93.35 (10) | C14—C13—C15 | 107.6 (3) |
O2—Cd1—N3i | 86.65 (10) | C16—C13—C15 | 110.5 (3) |
N6ii—Cd1—N3i | 91.65 (10) | C14—C13—C4 | 111.9 (3) |
N6iii—Cd1—N3i | 88.35 (10) | C16—C13—C4 | 109.4 (3) |
O2i—Cd1—N3 | 86.65 (10) | C15—C13—C4 | 109.7 (3) |
O2—Cd1—N3 | 93.35 (10) | C13—C14—H14A | 109.5 |
N6ii—Cd1—N3 | 88.35 (10) | C13—C14—H14B | 109.5 |
N6iii—Cd1—N3 | 91.65 (10) | H14A—C14—H14B | 109.5 |
N3i—Cd1—N3 | 180.00 (12) | C13—C14—H14C | 109.5 |
O1—C1—C6 | 122.9 (3) | H14A—C14—H14C | 109.5 |
O1—C1—C2 | 116.6 (3) | H14B—C14—H14C | 109.5 |
C6—C1—C2 | 120.4 (3) | C13—C15—H15A | 109.5 |
C3—C2—C1 | 119.0 (3) | C13—C15—H15B | 109.5 |
C3—C2—C10 | 120.7 (3) | H15A—C15—H15B | 109.5 |
C1—C2—C10 | 120.3 (3) | C13—C15—H15C | 109.5 |
C4—C3—C2 | 122.7 (3) | H15A—C15—H15C | 109.5 |
C4—C3—H3 | 118.7 | H15B—C15—H15C | 109.5 |
C2—C3—H3 | 118.7 | C13—C16—H16A | 109.5 |
C3—C4—C5 | 116.5 (3) | C13—C16—H16B | 109.5 |
C3—C4—C13 | 122.6 (3) | H16A—C16—H16B | 109.5 |
C5—C4—C13 | 120.9 (3) | C13—C16—H16C | 109.5 |
C4—C5—C6 | 123.0 (3) | H16A—C16—H16C | 109.5 |
C4—C5—H5 | 118.5 | H16B—C16—H16C | 109.5 |
C6—C5—H5 | 118.5 | C8—N1—N2 | 109.3 (3) |
C1—C6—C5 | 118.4 (3) | C8—N1—C7 | 130.0 (3) |
C1—C6—C7 | 122.0 (3) | N2—N1—C7 | 120.6 (3) |
C5—C6—C7 | 119.4 (3) | C9—N2—N1 | 102.7 (3) |
N1—C7—C6 | 114.7 (3) | C8—N3—C9 | 102.8 (3) |
N1—C7—H7A | 108.6 | C8—N3—Cd1 | 133.2 (2) |
C6—C7—H7A | 108.6 | C9—N3—Cd1 | 123.6 (2) |
N1—C7—H7B | 108.6 | C11—N4—N5 | 109.5 (3) |
C6—C7—H7B | 108.6 | C11—N4—C10 | 129.6 (3) |
H7A—C7—H7B | 107.6 | N5—N4—C10 | 120.8 (3) |
N1—C8—N3 | 110.6 (3) | C12—N5—N4 | 102.3 (3) |
N1—C8—H8 | 124.7 | C11—N6—C12 | 102.4 (3) |
N3—C8—H8 | 124.7 | C11—N6—Cd1iv | 125.4 (2) |
N2—C9—N3 | 114.6 (3) | C12—N6—Cd1iv | 131.7 (2) |
N2—C9—H9 | 122.7 | O4—N7—O5 | 133.1 (7) |
N3—C9—H9 | 122.7 | O4—N7—O6 | 114.0 (7) |
N4—C10—C2 | 111.9 (3) | O5—N7—O6 | 111.5 (6) |
N4—C10—H10A | 109.2 | C1—O1—H1 | 109.5 |
C2—C10—H10A | 109.2 | Cd1—O2—H2A | 111.9 |
N4—C10—H10B | 109.2 | Cd1—O2—H2B | 106.5 |
C2—C10—H10B | 109.2 | H2A—O2—H2B | 112.2 |
H10A—C10—H10B | 107.9 | H3B—O3—H3C | 109.5 |
N4—C11—N6 | 111.0 (3) |
Symmetry codes: (i) −x+2, −y+1, −z; (ii) −x+1, −y+1, −z; (iii) x+1, y, z; (iv) x−1, y, z. |
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1···N1 | 0.82 | 2.61 | 3.247 (4) | 135 |
O1—H1···N2 | 0.82 | 1.99 | 2.777 (4) | 161 |
C8—H8···O6 | 0.93 | 2.48 | 3.150 (8) | 129 |
O2—H2A···O3iii | 0.85 | 1.86 | 2.692 (4) | 164 |
O2—H2B···O4v | 0.85 | 2.13 | 2.951 (7) | 164 |
O2—H2B···O6v | 0.85 | 2.51 | 3.070 (7) | 124 |
O3—H3B···N5vi | 0.85 | 2.42 | 2.920 (5) | 118 |
O3—H3C···O5vii | 0.85 | 2.32 | 3.163 (7) | 169 |
C7—H7B···O3viii | 0.97 | 2.60 | 3.501 (5) | 155 |
C8—H8···O4v | 0.93 | 2.22 | 2.996 (7) | 140 |
C12—H12···O5iv | 0.93 | 2.41 | 3.149 (7) | 136 |
Symmetry codes: (iii) x+1, y, z; (iv) x−1, y, z; (v) −x+2, y+1/2, −z+1/2; (vi) x, y+1, z; (vii) x−1, y+1, z; (viii) −x+1, y−1/2, −z+1/2. |
Experimental details
Crystal data | |
Chemical formula | [Cd(C16H20N6O)2(H2O)2](NO3)2·2H2O |
Mr | 933.24 |
Crystal system, space group | Monoclinic, P21/c |
Temperature (K) | 293 |
a, b, c (Å) | 11.960 (4), 9.448 (3), 18.756 (6) |
β (°) | 108.592 (4) |
V (Å3) | 2008.9 (11) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 0.62 |
Crystal size (mm) | 0.35 × 0.30 × 0.20 |
Data collection | |
Diffractometer | Bruker SMART CCD area-detector |
Absorption correction | Multi-scan (SADABS; Bruker, 2000) |
Tmin, Tmax | 0.812, 0.886 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 8433, 3897, 2974 |
Rint | 0.031 |
(sin θ/λ)max (Å−1) | 0.617 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.044, 0.107, 1.08 |
No. of reflections | 3897 |
No. of parameters | 272 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.92, −0.46 |
Computer programs: SMART (Bruker, 2000), SAINT (Bruker, 2000), SAINT, SHELXTL (Bruker, 2000), SHELXTL.
Cd1—O2 | 2.287 (3) | Cd1—N3 | 2.395 (3) |
Cd1—N6i | 2.295 (3) | ||
O2—Cd1—N6ii | 89.62 (10) | O2—Cd1—N3 | 93.35 (10) |
O2—Cd1—N6i | 90.38 (10) | N6ii—Cd1—N3 | 88.35 (10) |
O2—Cd1—N3iii | 86.65 (10) | N6i—Cd1—N3 | 91.65 (10) |
Symmetry codes: (i) x+1, y, z; (ii) −x+1, −y+1, −z; (iii) −x+2, −y+1, −z. |
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1···N1 | 0.82 | 2.61 | 3.247 (4) | 135.0 |
O1—H1···N2 | 0.82 | 1.99 | 2.777 (4) | 161.0 |
C8—H8···O6 | 0.93 | 2.48 | 3.150 (8) | 129.0 |
O2—H2A···O3i | 0.85 | 1.86 | 2.692 (4) | 164.0 |
O2—H2B···O4iv | 0.85 | 2.13 | 2.951 (7) | 164.0 |
O2—H2B···O6iv | 0.85 | 2.51 | 3.070 (7) | 124.0 |
O3—H3B···N5v | 0.85 | 2.42 | 2.920 (5) | 118.0 |
O3—H3C···O5vi | 0.85 | 2.32 | 3.163 (7) | 169.0 |
C7—H7B···O3vii | 0.97 | 2.60 | 3.501 (5) | 155.0 |
C8—H8···O4iv | 0.93 | 2.22 | 2.996 (7) | 140.0 |
C12—H12···O5viii | 0.93 | 2.41 | 3.149 (7) | 136.0 |
Symmetry codes: (i) x+1, y, z; (iv) −x+2, y+1/2, −z+1/2; (v) x, y+1, z; (vi) x−1, y+1, z; (vii) −x+1, y−1/2, −z+1/2; (viii) x−1, y, z. |
In recent years, organic ligands with azole units have become a new class of supramolecular synthons of intense interest in creating appealing coordination polymers (Hoskins et al., 1997; Li et al., 2005). In our previous studies, we synthesized two kinds of flexible bidentate ligands 1,6-di(imidazole-1-yl-methyl)-4-R-phenol and 1,6-di(triazole-1-yl-methyl)-4-R-phenol (R = Me, t-Bu, or Cl), and demonstrated that they can form different structures and topologies with different metal ions (Ma et al., 2003; Zhu et al., 2004; Zhu et al., 2007). The title compound, (I), is obtained by the reaction of 1,6-di(triazole-1-yl-methyl)-4 - t-Bu-phenol(dttp) with cadmium nitrate in ethanol.
The asymmetric unit of (I) contains half a Cd(II) atom, one dttp ligand, two water molecules and a nitrate ion. The metal atoms are located on the crystallographic inversion center with octahedral geometry, formed equatorially by four N atoms of triazoles from four dttp ligands and axially by two O atoms from two water molecules (Fig. 1). Each dttp adopts a trans conformation in which two triazole groups of a ligand with a dihedral angle of 53.9 (3) ° are on the opposite direction of the central benzene ring. In this way two metal atoms and two dttp ligands form a 24-membered M2L2 macrocycle through Cd—N coordination bonds. In each macrocycle, two phenyl rings are found strictly in a plane and the intermetallic distance between the two CdII atoms is 11.96 (1) Å. Such a metallomacrocyclic unit repeats along the a-axis to generate a double-stranded one-dimensional cationic chain as shown in Fig. 2.
Each phenol O—H moiety is directed at the N atom of a triazole moiety with H···N distances ranging from 1.99 to 2.61 Å, indicative of strong intramolecular hydrogen-bonding interactions. It is noticed that the resulting one-dimensional chains are further linked together to a three-dimensional framework by the uncoordinated water molecules and nitrate anions through O–H···O, O–H···N and C–H···O hydrogen-bonding interactions as shown in Fig. 3.