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C4H10N2O2, monoclinic, Cc(no. 9), a= 9.5726(8) Å, b= 9.2271(9) Å, c= 7.4577(7) Å, β= 115.295(3)°, V= 595.56(9) Å3, Z= 4, Rgt(F) = 0.0520, wRref(F2) = 0.1436, T = 298 K .

C18H17NO3S, monoclinic, Cc(no. 9), a= 32.036(3) Å, b= 7.2154(7) Å, c= 7.4283(8) Å, β= 99.943(2)∘, V= 1691.3(3) Å3, Z= 4, Rgt(F) = 0.0343, wRref(F2) = 0.0821, T = 298 K.

C10H5N5O5, monoclinic, P21/c(no. 14), a= 10.9546(11) Å, b= 7.3433(8) Å, c= 13.2567(15) Å, β= 102.972(5)∘$102.972{(5)}^{\circ }$ , V= 1039.19(19) Å3, Z= 4, Rgt${R}_{gt}$ (F) = 0.0630, wRref$w{R}_{ref}$ (F2) = 0.1622, T = 298 K.

Four new zinc(II) complexes Zn2(μ‐dmpz)2(Hdmpz)2(L1)2(1) (Hdmpz = 3,5‐dimethylpyrazole, HL1 = 2‐methyl‐2‐phenoxypropanoic acid), Zn(Hdmpz)2(L2)2(2) [HL2 = 2‐hydroxy‐5‐(phenyldiazenyl)benzoic acid], Zn2(μ‐dmpz)2(Hdmpz)2(L3)2(3) [HL3 = 3,4‐(methylenedioxy)benzoic acid], and Zn2(μ‐dmpz)2(Hdmpz)2(L4)2(4) [HL4 = 3‐(4‐methoxyphenyl)acrylic acid] were prepared and structurally characterized by different techniques including elemental analysis, IR spectroscopy, and single‐crystal X‐ray diffraction analysis. The X‐ray studies suggested that all these complexes except compound 2are centrosymmetric dinuclear complexes with a tetrahedral arrangement around each zinc ion, whereas compound 2is a mononuclear complex. The pyrazole ligand is coordinated in both terminal as well as a bridging fashion in the dinuclear moiety, whereas the pyrazole ligand in compound 2is coordinated only in monodentate terminal fashion with its neutral nitrogen group. In all four complexes the carboxylate functions behave as monodentate ligands. All complexes show intramolecular hydrogen bonding of N–H···O between N–H of pyrazole and nonbonded oxygen atom of carboxylate. Furthermore, rich intermolecular weak interactions such as classical hydrogen bonds, C–H···O, C–H···N, C–H···π, and CH3–π interactions exist and complexes 1–4display a set of 3D superamolecular frameworks. In addition, the four compounds are thermally stable below 150 °C.

Five novel coordination polymers, [(Cu(L1)2OH)·Cl·3H2O] (1) [L1= bis(N‐imidazolyl)methane], [Cd(L1)2(NCS)2] (2), [Zn(L1)2(NCS)2] (3), [Cu(L1)2(NO3)2] (4), and [Cu(L2)1.5(NCS)2] (5) [L2= 1,4‐bis(N‐imidazolyl)butane] were obtained from self‐assembly of the corresponding metal salts with flexible ligands and their structures were fully characterized by X‐ray diffraction (XRD) analysis, Fourier Transform Infrared (FT‐IR) spectroscopy, elemental analysis and thermogravimetric (TGA) measurements. X‐ray diffraction analyses revealed that complexes 1, 2, 3, and 4exhibit 1D double‐stranded chain structures, which result from doubly bridged [CuOH], [M(NCS)2] (M= Cd, Zn), and [Cu(NO3)2] units, respectively. The polymeric copper complex 5displays 1D ladder structure., These complexes, with the exception of complex 1, are stable up to 300 °C.