Chiral Helices in a 3D Network of Zn2(en)V2O7 (en = Ethylenediamine)

2008 ◽  
Vol 55-57 ◽  
pp. 669-672 ◽  
Author(s):  
S. Krachodnok ◽  
K.J. Haller ◽  
I.D. Williams

An inorganic-organic hybrid vanadate complex, Zn2(en)V2O7 (en = ethylenediamine) has been hydrothermally synthesized and characterized by single-crystal X-ray crystallography, TG analysis, IR spectroscopy, and elemental analysis. The title compound crystallizes in the monoclinic space group P21 with a = 7.0885(7), b = 8.6040(9), c = 8.1869(8) Å, b = 112.224(2)° and V = 462.22(8) Å3, T = 298±2 K and R1[I>2s(I)] = 0.0291 for 2170 observed reflections. The structure consists of undulating sheets constructed from helical chains that share Zn coordination centers with repeating units propagated into a helix by the two-fold screw axes at 0, y, ½ and pillared with alternating VO4 tetrahedra to generate a 3D chiral network. Neighboring helices are interconnected by µ2-O bridges to form the three-dimensional network. The strength of the network is reinforced by hydrogen bonding. TG analysis shows thermal stability of the network up to 283 °C.

2013 ◽  
Vol 2013 ◽  
pp. 1-5 ◽  
Author(s):  
Farzin Marandi ◽  
Ingo Pantenburg ◽  
Gerd Meyer

The new three-dimensional coordination polymer {[Bi(NNO)2(NO3)]·1.5H2O}n(1, NNO−= nicotinateN-oxide) was synthesized and characterized by elemental analysis, IR and1H-NMR spectroscopy, as well as single-crystal X-ray diffraction analysis.1crystallizes in the monoclinic space group C2/c. The crystal structure consists of a rectangular-shaped grid constructed with NNO linkers. Cavities of a diameter of 7.9–8.3 Å2are filled with disordered water molecules. The thermal stability of the compound was evaluated by thermogravimetric analysis.


1992 ◽  
Vol 47 (12) ◽  
pp. 1754-1758 ◽  
Author(s):  
M. A. S. Goher ◽  
M. A. M. Abu-Youssef ◽  
F. A. Mautner ◽  
H. P. Fritzer

The structures of two polymeric complexes of chromium(III) azide with pyridine, KCr(py)4(N3)4 (1), and RbCr(py)3(N3)4 (2), were determined by X-ray crystallography. Crystal data: 1, C20H20N16CrK, monoclinic, space group C2/c, a = 1611.2(5), b = 1050.6(3), c = 1609.0(5) pm, β = 91.69(3)°, Ζ = 4 and Rw = 0.037 for 923 diffractometer data; 2, C15H15N15CrRb, monoclinic, space group P21/n, a = 1311.9(3), b = 1139.0(4), c = 1523.3(4) pm, β = 109.39(2)°, Ζ = 4 and Rw = 0.046 for 2336 data.The crystal structure of 1 contains six-coordinated chromium and potassium cations with two pyridine ligands and four µ(1,3) bridging azido groups forming a three-dimensional network structure. The chromium atoms are trans-coordinated by the pyridine ligands, whereas the potassium cations are cis-coordinated. The polymeric complex 2 features di-µ(l,1,3) azido bridged CrRbN2 rings, distorted octahedral chromium(III) coordination geometry, sevencoordinated rubidium, and di-μ(1,3) azido bridges which link the binuclear RbCr(pyridine)3(N3)2 moieties into infinite chains parallel to the b axis.


1997 ◽  
Vol 53 (2) ◽  
pp. 262-271 ◽  
Author(s):  
Q. Li ◽  
T. C. W. Mak

Air-sensitive selenourea inclusion complexes tetraethylammonium chloride–selenourea (1/2), (C2H5)4N+.C1−.2[(NH2)2CSe] (1), tetra-n-propyl-ammonium chloride–selenourea (1/3), (n-C3H7)4N+.C1−.3[(NH2)2CSe] (2), tetra-n-propylammonium bromide–selenourea (1/3), (n-C3H7)4N+.Br−.3[(NH2)2CSe] (3), and tetra-n-propylammonium iodide–selenourea (1/1), (n-C3H7)4N+.I−.(NH2)2CSe (4), have been prepared and characterized by X-ray crystallography. Crystal data, Mo Kα radiation: (1), space group P21/n, Z = 4, a = 8.768 (5), b = 11.036 (6), c = 19.79 (1) Å, β = 96.92 (1)°, R F = 0.055 for 1468 observed data; (2), space group Cc, Z = 4, a = 18.091 (4), b = 13.719 (3), c = 11.539 (2) Å, β = 111.93 (3)°, R F = 0.051 for 1187 observed data; (3), space group Cc, Z = 4, a = 18.309  (4), b = 13.807 (3), c = 11.577 (2) Å, β = 112.45 (3)°, R F = 0.049 for 1592 observed data; (4), space group P21/n, Z = 4, a = 8.976 (1), b = 14.455 (2), c = 15.377 (3) Å, β = 94.16(1)°, R F = 0.062 for 1984 observed data. In the crystal structure of (1) the parallel alternate arrangement of selenourea–chloride ribbons and selenourea chains generates a puckered layer and the cations are sandwiched between them. In the isomorphous complexes (2) and (3) wide selenourea–halide double ribbons are crosslinked by bridging selenourea molecules via N—H...Se and N—H...X hydrogen bonds [average N...Se = 3.521 (8) and 3.527 (7), N...Cl = 3.354 (8) and N...Br = 3.500 (7) Å in (2) and (3), respectively] to form a channel-like three-dimensional network and the cations are accommodated in a single column within each channel. In the crystal structure of (4) the selenourea molecules are joined in the shoulder-to-shoulder fashion via N—H...Se hydrogen bonds [N...Se = 3.529 (7) and 3.534 (7) Å] to generate a ribbon and each selenourea molecule also forms a pair of chelating N—H...I hydrogen bonds [N...I = 3.567 (7) and 3.652 (7) Å] to an adjacent iodide ion.


2015 ◽  
Vol 70 (4) ◽  
pp. 215-219 ◽  
Author(s):  
Wei Li ◽  
Chang-Hong Li ◽  
Ying-Qun Yang ◽  
Heng-Feng Li

AbstractA new copper(II) coordination polymer [Cu2(C5H4NCOO)2(C7H5N4)2]n (1) has been synthesized with 4-pyridinecarboxylate and 3-(pyridin-2-yl)-1,2,4-triazolyl ligands. The crystal structure shows that two neighboring copper(II) ions are coordinated with two deprotonated (anionic) 3-(pyridin-2-yl)-1,2,4-triazole ligands to form a binuclear structure. Adjacent binuclear units are linked by 4-pyridinecarboxylate anions to form a three-dimensional network structure. The magnetic, fluorescent, and electrochemical properties and thermal stability of 1 were studied. The results show that 1 exhibits antiferromagnetic interaction, and upon excitation at 318 nm, it has an intense fluorescent emission at approximately 430 nm. The electron transfer of 1 is irreversible in electrode reactions. The thermogravimetric analysis shows that 1 is stable below 240 °C.


1992 ◽  
Vol 47 (1) ◽  
pp. 139-143 ◽  
Author(s):  
Mohamed A. S. Goher ◽  
Morsy A. M. Abu-Youssef ◽  
Franz A. Mautner

The structures of mer-Cr(py)3(N3)3 (1) and polymeric NaCr(py)4(N3)4 (2) were determined by X-ray crystallography. Crystal data; 1, C15H15N12Cr, triclinic, space group P1̄, a = 895.3(2), b = 999.1(3), c = 1269.9(5) pm , α = 106.76(3), β = 96.69(3), γ = 116.30(2)°, V = 943.8(6) · 106 pm3, Z = 2 and Rw = 0.038 for 1736 observed MoKα diffractometer data; 2, C20H20N16CrNa, monoclinic, space group C2/c, a = 1561.2(3), b = 1028.8(2), c = 1573.6(4) pm, β = 90.70(2)°, V = 2 527.3(9) · 106 pm3, Z = 4 and = 0.033 for 1272 MoKα diffractometer data.The coordination around the chromium (III) ion in the discrete molecules of 1 is six-coordinate with mean distances Cr-N(py) of 210.2(4) pm and Cr-N(N3) of 200.8(4) pm. The terminal azido ligands are almost linear and asymmetric, the N-N bonds nearer to the metal (118.8(6) to 120.5(7) pm) being significantly longer than the terminal ones (114.7(7) to 115.5(7) pm). In compound 2, each chromium or sodium cation is six-coordinated by four azido groups and two pyridine molecules. The azido groups act as μ(1,3) bridging ligands between chromium and sodium octahedra to form a three-dimensional network structure. The chromium atoms are trans-coordinated by the pyridine ligands whereas the sodium cations are cis-coordinated.


2018 ◽  
Vol 74 (8) ◽  
pp. 981-985
Author(s):  
Flávia H. Silva ◽  
Chris H. J. Franco ◽  
Charlane C. Corrêa ◽  
Renata Diniz

Aromatic polycarboxylate linkers provide structural rigidity and strong interactions among the metal centre and the carboxylate O atoms. A new three-dimensional coordination polymer namely, catena-poly[potassium [tetraaqua(μ-5-sulfobenzene-1,3-dicarboxylato)zinc(II)]], {K[Zn(C8H3O7S)(H2O)4]} n or {K[Zn(SIP)(H2O)4]} n , where SIP is 5-sulfobenzene-1,3-dicarboxylate or 5-sulfoisophthalate, was obtained and characterized by elemental analysis and IR vibrational spectroscopy, and the single-crystal structure was determined by X-ray diffraction analysis. The compound crystallizes in the monoclinic space group P21/n with Z = 4. Topological analysis revealed that K—O interactions form a two-dimensional network, which is uninodal 4-connected and can be described with a point symbol (44.62), and this plane network is classified as sql/Shubnikov. The layers are connected by Zn2+ ions coordinated to the SIP linker, forming a three-dimensional network. This net is a trinodal (3,5,6)-connected system with point symbol (3.44.52.62.73.83).(3.44.52.62.7).(3.72).


2000 ◽  
Vol 53 (3) ◽  
pp. 237 ◽  
Author(s):  
Andrew B. Hughes ◽  
Maureen F. Mackay ◽  
Luigi Aurelio

The solid-state conformation of racemic N-methylglutamic acid has been defined by single-crystal X-ray crystallography. Orthorhombic crystals belong to the space group Pbca with a 15.219(2), b 10.583(1), c 9.595(1) Å and Z 8. The structure was refined to a final R value of 0.049 for the 1285 measured data. In the crystal the molecules adopt a zwitterionic form with protonation having occurred at the amino nitrogen atom. The a-carboxyl is unprotonated with the d-carboxy group retaining a proton. The i.r. spectrum shows absorptions which also are indicative of the amino acid being in the zwitterionic form. Intermolecular H-bonds involving the carboxylate proton and the two protons on the N-atom link the molecules into a three-dimensional network in the crystal.


2000 ◽  
Vol 15 (9) ◽  
pp. 1955-1961 ◽  
Author(s):  
T. S. Kang ◽  
Y. S. Kim ◽  
Jung Ho Je

The thermal stability of RuO2/Si(100) films in air was studied using ex situ synchrotron x-ray scattering. The (110) textured RuO2 film showed good thermal stability due to the low surface and strain energies. However, the RuO2 films of high strain and surface energies were transformed to three-dimensional islands during annealing up to 800 °C. We also studied, during the post annealing process, the interface roughness of BaxSr1−xTiO3 (BST)/RuO2/Si(100) and BST/Pt/Ti/SiO2/Si(100) structures comparatively, using in situ synchrotron x-ray scattering. The interfaces of the BST/RuO2/Si were thermally stable up to 500 °C, and the deterioration of the interfaces above 500 °C was attributed to the crystallization of amorphous BST film. Meanwhile, the interfaces of the BST/Pt/Ti/SiO2/Si were significantly degraded even at the low temperature of 350 °C, mainly due to the formation of the Pt–Ti alloy and the Ti oxidation.


2008 ◽  
Vol 587-588 ◽  
pp. 568-571 ◽  
Author(s):  
S. Martínez-Gallegos ◽  
Maria Herrero ◽  
Vicente Rives

A polyethylenterephthalate-hydrotalcite (PET-HT) composite was prepared by in situ polymerisation, using polyethylenterephthalate (PET) and different amounts of a hydrotalcite with dodecylsulphate in the interlayer space (DS-HT). The resulting material has been characterised by powder X-ray diffraction (PXRD) and thermogravimetric (TG) analysis. The thermal stability of PET is not greatly enhanced upon incorporation of the inorganic component, despite PXRD shows that the HT is exfoliated in the composite. Thus with 2-10% shows a complete dispersion of the layered component in the polymeric matrix, while if the inorganic loading is between 20-50 % (larger loadings were not tested) no complete dispersion is achieved and PXRD-detectable agglomerates are formed.


2007 ◽  
Vol 2007 ◽  
pp. 1-7 ◽  
Author(s):  
Labrini Drakopoulou ◽  
Constantina Papatriantafyllopoulou ◽  
Aris Terzis ◽  
Spyros P. Perlepes ◽  
Evy Manessi-Zoupa ◽  
...  

The 12: 1 reaction of urea (U) with CoI2in EtOH yielded the “clathrate-coordination” compound[CoU6]I2·4U (1). The complex crystallizes in the monoclinic space group P21/c. The lattice constants area= 9.844(4),b= 7.268(3),c= 24.12(1) Å, andβ=98.12(1)∘. The crystal structure determination demonstrates the existence of octahedral[CoU6]2+cations,I-counterions, and two different types (twoU1and twoU2) of hydrogen-bonded, lattice urea molecules. The[CoU6]2+cations and theU1lattice molecules form two-dimensional hydrogen-bonded layers which are parallel to theabplane. TheI-anions are placed above and below each layer, and are hydrogen bonded both toU1molecules and[CoU6]2+cations. EachU2molecule is connected to a[CoU6]2+cation through anN–H⋯Ohydrogen bond resulting in a three-dimensional network. Room temperature magnetic susceptibility and spectroscopic (solid-state UV/Vis, IR, Raman) data of1are discussed in terms of the nature of bonding and the known structure.


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