Source of materialCrystals of the title compound were unexpectedly formed during an experiment to synthesize amixed-ligand copper complex. In the title crystal structure, the Cu atoms are coordinated by three oxygen atoms of three 4-methoxycinnamate ligands and two ammonia nitrogen atoms (CuO 3N2)i nasquare pyramidal manner. The 4-methoxycinnamate anions display trans conformation and coordinate the Cu atoms in monodentate fashion to generate a dinuclear moiety. As expected the C-Obond lengths of the coordinating Oa toms are 1.293(3) and 1.271(3) Å,r espectively, which is significantly longer than that of the non-coordinating one (1.242(3) and 1.243(3) Å). The Cu1-N1 bond lengths (1.977(2) and 1.985(2) Å)a re comparable with the known Cu carboxylate [6]. The Cu-Obond length range from 1.976(2) to 2.440(2) Å,and are longer than the reported result [8]. The angle ∠O4-Cu1-O1 =177.71(8)°is very close to 180°,and O-Cu-N bond angles are close to 90°also, which implies the pyramide CuO 3N2 is only slightly distorted. The Cu···Cu separation within the dimeric unit is of 3.433 Å,which is larger than the reported results [8]. The presence of CH 3 ···O, C-H···p,C H 3 ···p,a nd N-H···Oh ydrogen bonds between two neighboring dinuclear moieties sets up astrong hydrogen bonding network.
Source of material 0.0396 g (0.30 mmol) glutaric acid and 0.0595 g (0.30 mmol) 1,10-phenanthroline monohydrate were added to a stirred aqueous solution of Dy(NO3)3 · 5H 2 O (0.1316 g, 0.30 mmol) in 10 ml doubly-distilled water. The resulting mixture (pH = 5.0) was loaded into a 23 ml Teflon-lined stainless steel autoclave, which was heated at 170°C for three days, affording colorless crystals. The composition was confirmed by thermogravimetric analyses (weight loss for six moles of H2O molecules per formula unit: calc. 13.13 %, obs. 12.8 % over 25°C 188°C). DiscussionThe title compound was initially reported by Serpaggi and FéreyThe asymmetric unit of the present dysprosium glutarate contains a Dy 3+ cation, one and a half glutarate anions, an aqua ligand and two lattice H2O molecules. The hydrogen atoms of the lattice water molecules were not localized. One glutarate anion (O1, O2, C1 to C3) is located on the twofold rotation axis passing through C3 atom and assumes an anti/anti conformation with non-hydrogen atoms nearly coplanar, while the other dicarboxylate ion (O3 to O6, C4 to C8) adopts an anti/gauche conformation. One lattice H2O molecule (O8) is disordered over four sites with equal occupancies. The large temperature displacement parameters for O9 atom suggest that the water molecules of O9 are disordered ones. The Dy atoms are each coordinated by nine oxygen atoms of one aqua ligand, one anti/anti and four anti/gauche conformational glutarate anions to form distorted mono-capped tetragonal antiprism DyO9 with d(DyO) = 2.344 Å 2.669 Å, ÐODyO = 65.9° 162.3°being comparable with those observed in the literature [3,4]. The anti/anti conformational dicarboxylate bischelate two Dy atoms, and as far as the anti/gauche one is concerned, each terminal carboxylate group chelates one Dy atom with one oxygen atom additionally bonded to second metal atom. Through O3, O6 and their symmetry related partners, the DyO9 polyhedra are edge-shared to generate 1D metal-oxygen chains extending in the [100] direction and the resulting chains are then bridged by the anti/gauche conformational glutarate anions into 2D brick-wall parallel to (001), which are further linked by the bischelating dicarboxylate anions to form 3D framework with the tunnels in the [100] direction filled with the lattice H2O molecules. The glutarate anions exhibit normal bonding values comparable with those reported in the literature [5][6][7].
C 4H13CuNO7,m onoclinic, P12/c1(no. 13), a =8.434(3) Å, b =7.230(3) Å, c =8. Source of materialCrystals of aqua-ammine-(m-succinato)copper(II) dihydrate were unexpectedly formed during an attempt to synthesize the mixed ligand copper complex. Am ixture of copper chloride dihydrate (34.2 mg, 0.2 mmol), NaOH (16 mg, 0.4 mmol), succinic acid (23.6 mg, 0.2 mmol), and 5,7-dimethyl-1,8-naphthyridine-2-amine (35 mg, 0.2 mmol), in ethanol (10 ml) was refluxed for 1h.The resulted light blue precipitate was collected and dissolved in 3mlofconcentrated ammonia. Blue block-like crystals were obtained by slow evaporation of the ammonia solution at ambient temperature. Experimental detailsHydrogen atoms of methylene groups were only placed in corresponding calculated positions [d(C-H) =0.97 Å]. Positions of hydrogen atoms of water and ammonia molecules were located from the difference Fourier syntheses and refined. All U iso values were restrained on U eq values of the parent atoms.
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