Key indicatorsSingle-crystal X-ray study T = 120 K Mean (C-C) = 0.003 Å R factor = 0.045 wR factor = 0.102 Data-to-parameter ratio = 13.9For details of how these key indicators were automatically derived from the article, see
Recently, we reported the synthesis and crystal structure of [La(µ-DMP)2(µ3-NO3)(DMSO)]n, 1 [UO2(µ-DEP)4(DMSO)]n, 2 [UO2(µ-DMP)4(DMSO)]n, 3 and [Cu2(µ-DMP)4(DMSO]n, 4 (DMP = dimethyl phosphate and DMSO = dimethyl sulfoxide). In these complexes, DMP and DEP act as an O-atom donor ligand, forming coordination polymers in the solid state. Also, we reported the synthesis and crystal structures of [Ni(H2O)6](DMP)2 as an ionic complex. 5 In this complex, DMP is not bonded to the metal, and acts as a counter-ion. We now report on the synthesis and crystal structure of the title compound.Preparation: The title compound was obtained from a reaction between triethyl phosphate with CeCl3·7H2O in tetrahydroforan in a 4:1 molar ratio. Notably, the DEP ligand was obtained by eliminating one C2H5 molecule from the TEP ligand in the reaction mixture. Slow evaporation of this solution resulted an prismatic colorless crystals after two months.The X-ray data were collected on a diffractometer (Mo Kα radiation, graphite monochromator) at 120(2)K. The crystal data and experimental parameters are given in Table 1. As can be seen in Table 1, the highest peak, 4.838 eÅ -3 , is found close to the Ce atom. The non-hydrogen atoms were refined anisotropically, and all hydrogen atoms were located from sequent difference Fourier maps and refined with the riding model to final R indices of R1(0.0614) and WR2(0.1280).The X-ray structural analysis in Fig. 1 consists of a Ce2(µ-DEP)6(TEP) fragment and a repeation unit in this polymer. As is clear from an ORTEP view of the compound, Fig. 2, the repeation unit of this linear polymer consists of two 6 and 7-coordinated cerium atoms, which are linked together via six O-P-O bridges from phosphate esters. The seventh site of one of the cerium atoms is occupied by TEP as a monodentede ligand. Selected bond lengths and angles are given in The crystal structure of [Ce2(µ-DEP)6(TEP)]n, (DEP = diethyl phosphate), (TEP = triethyl phosphate) was determined by the X-ray diffraction method. This polymeric complex crystallizes in the monoclinic system, with space group P21/c, and the following unit-cell dimension: a = 19.517 (4)
Treatment of a solution of CuCl 2 in dimethyl phosphate (DMP) in an inert solvent under nitrogen atmosphere resulted in a light blue fluorescence powder. Slow evaporation of H 2 O-DMSO solution of this powder led to the formation of blue-sky crystals of a new polymeric Cu(II) complex, with a unit cell composed of Cu 2 (DMP) 4 (DMSO), (1). The crystal and molecular structure of the complex was established crystallographically. Compound (1) crystallizes in the monoclinic space group P2 1 /n with a = 12.8920(11)Å, b = 13.1966(11)Å, c = 14.7926(13)Å, α = 90°, β = 98.943(2)°, γ = 90° and Z = 4. A square pyramidal environment for the metal center is established by coordination of oxygen atoms of four bridging DMP ligands in the basal positions and a tri-centered oxygen atom of DMSO in the apical disposition. The sixth position is also affected by a weak interaction with the sulfur atom of DMSO. The phosphorous atom in the bridging DMP is arranged in a deformed tetrahedron with gg conformation for methyl esters with C 2v symmetry. Accordingly, the angles of methoxy substituents are unexpectedly smaller than the bridging oxygens, and synchronous z-in and z-out distortions are suggested for DMP anion. The oxygen atom of SOCuCu´ fragment derived from DMSO, functions as a tri-centered nuclei lie almost in a trigonal triangle environment. This study helps provide further insights into the binding nature of phosphate esters to the active sites of enzymes, which catalyze phosphoryl transfer reactions.
Key indicatorsSingle-crystal X-ray study T = 115 K Mean '(C±C) = 0.004 A Ê R factor = 0.028 wR factor = 0.059 Data-to-parameter ratio = 19.3For details of how these key indicators were automatically derived from the article, see http://journals.iucr.org/e.
The reaction of an ethanolic solution 2,6‐pyridinedicarboxylic acid (1, LH2) with TlNO3 in the presence of triethylamine led to the coordination polymer [Tl(LH)]n (2). The complex was characterized by elemental analysis, IR spectroscopy and single‐crystal X‐ray diffraction. Crystal data for 2 at –80 °C: monoclinic, space group I2/a, a = 696.1(1), b = 1190.6(2), c = 931.0(2) pm, β = 103.28(1)°, Z = 4, R1 = 0.0256.
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