Structure and Properties of a Dimer Complex: [Co(Hdmg)2(Him)2]·(ClO4)

2012 ◽  
Vol 531-532 ◽  
pp. 280-283
Author(s):  
Xuan Wen Liu ◽  
Shi Hua Yuan ◽  
Ting Ting Lin

A New Complex Crystal [Co(Hdmg)2(Him)2]·(ClO4) (H2dmg = Dimethylglyoxime,Him = Imidazole) Had Been Synthesised in Aqueous Solution and Was Characterized by X-ray Diffraction and IR Spectrum. the Complex Crystallizes in Triclinic Space Group with Cell Constants a= 20.868(7)Å, B=11.408(4)Å, C=15.816(4)Å, α=90.00°, β=116.97(2)°, γ= 90.00°, V= 3355.8(17) Å3, Z=4, F(000)=1732. the Coordination Environment of Cobalt Atom Is a Slightly Distorted Octahedron. the Four Equatorial Donors Are Four Nitrogen Atoms from Two Bidentate Chelate Hdmg Anion Ligands. the Apex Points Are Occupied by Two Nitrogen Atoms from him Ligands. the Co-N(Him) Distance Is 1.930Å, and the Co-N(dmg) Distances Are Varying in the Range from 1.886Å to 1.993Å which Are in Agreement with Corresponding Reported in a Number of other Structurally Related Copper(II) Complexes.

2013 ◽  
Vol 372 ◽  
pp. 80-83
Author(s):  
Xuan Wen Liu ◽  
Bing Wen Zhong ◽  
Yue Hong Zhang ◽  
Rui Guo

A new complex crystal [Co2(Hdmg)2(dien)2](ClO4)24.5(H2O) (H2dmg= dimethylglyoxime, dien = diethylenetriamine) had been synthesised in aqueous solution and was characterized by X-ray diffraction and IR spectrum. The complex crystallizes in monoclinic space groupC2/cwith cell constants =20.868(7)Å, =11.408(4)Å, =15.816(4)Å, =90.00°, =116.97(2)°, =90.00°, =3355.8(17)Å3, =4, (000)=1732. The cobalt atom lies in a distorted octahedron environment and coordinates with one oxygen atom from neighbour Hdmg and five nitrogen atoms from bidentate chelate Hdmg and tridentate chelate dien. The two Hdmgs bridge two cobalt atoms to form a six-number Co2O2N2ring.


2016 ◽  
Vol 71 (1) ◽  
pp. 51-55 ◽  
Author(s):  
Oscar E. Piro ◽  
Gustavo A. Echeverría ◽  
Beatriz S. Parajón-Costa ◽  
Enrique J. Baran

AbstractMagnesium acesulfamate, Mg(C4H4NO4S)2·6H2O, was prepared by the reaction of acesulfamic acid and magnesium carbonate in aqueous solution, and characterized by elemental analysis. Its crystal structure was determined by single crystal X-ray diffraction methods. The substance crystallizes in the triclinic space group P1̅ with one molecule per unit cell. The FTIR spectrum of the compound was also recorded and is briefly discussed. Some comparisons with other simple acesulfamate and saccharinate salts are also made.


1991 ◽  
Vol 46 (1) ◽  
pp. 1-4 ◽  
Author(s):  
Klaus Brodersen ◽  
Jörg Zimmerhackl

1,13-Bis(8-quinolyl)-1,4,7,10,13-pentaoxatridecane-dimercury(I)-diperchlorate is formed by the reaction of 1,13-bis(8-quinolyl)-1,4,7,10,13-pentaoxatridecane in ethanol with an aqueous solution of dimercury(I)-diperchlorate.It crystallizes in the triclinic space group P Ī with a = 1020.6(2), b = 1200.6(8), c = 1441.1(6) pm , α = 69.60(5)°, β = 83.04(13)°, y = 66.53(4)° and Z = 2. The crystal structure was determined by X -ray diffraction and refined to an R-value o f 0.079. The Hg22+ -ion is coordinated to both nitrogen atoms and four oxygen atoms of one molecule of the ligand. By changing four C - O torsional angles from trans to gauche, the ligand adopts a helical, chiral configuration around the Hg22+-ion. The CIO4--ions are not coordinated to the Hg22+-ion.


1981 ◽  
Vol 34 (1) ◽  
pp. 65 ◽  
Author(s):  
GA Williams ◽  
R Robson

The crystal and molecular structure of LCO2 [S2P(OEt)2]2 (where L is a binucleating ligand derived from the macrocycle LH2 formed by condensation of two molecules each of propane-1,3-diamine and 2-hydroxy-5-methylisophthalaldehyde) has been determined by single-crystal X-ray diffraction techniques at 295 K. The compound crystallizes in the triclinic space group Pī with two molecules in a cell of dimensions a 18.644(6), b 11.694(4), c 9.487(4) �, α 84.99(3), β 82.61(3), γ 73.48(2)�. Automatic diffractometry has provided significant Bragg intensities for 2799 independent reflections and the structure has been refined by least-squares methods to R 0.054. The structure is molecular, consisting of discrete binuclear units LCo2[S2P(OEt)2]2. The two centrosymmetric molecules in the unit cell are crystallographically unique but essentially chemically similar. The two cobalt(11) atoms in each molecule are separated by 3.075(2) and 3.072(2) �. Each cobalt atom is in an octahedral environment, with an N2O2 equatorial plane and two sulfur atoms of bridging dithiophosphate ligands in the axial positions. The Co-S bonds are the longest yet observed [2,680(3), 2.652(3), 2.642(3), 2.623(3) �]. The cobalt(11) centres are high spin, with �eff 4.53 BM per cobalt atom. The macrocyclic ligand deviates slightly from planarity. The forces exerted both by the ligand L on associated metal atoms, and by axial ligands on the macrocycle, are discussed.


1983 ◽  
Vol 38 (1) ◽  
pp. 20-29 ◽  
Author(s):  
Bernt Krebs ◽  
Marita Hucke ◽  
Michael Hein ◽  
Andreas Schäffer

Abstract The monomeric SeOCl3- ion, which can be prepared as the tetraphenylarsonium salt from SeOCl2 and As(C6H5)4Cl, was structurally characterized by a low-temperature single crystal X-ray diffraction analysis. [As(C6H5)4]SeOCl3 is monoclinic, space group P21/c, with a = 9,332(3), b = 13,761(4), c = 18,985(6) Å, β = 110,97(3)° (at -135 °C), Z = 4; it contains a novel type of ψ-trigonal bipyramidal oxotrichloroselenate(IV) anion which is not associated to dimers or polymer chains as in known structures. The equatorial positions are occupied by doubly bonded oxygen (Se-O 1,601(3) Å) and by one Cl(Se-Cl 2,234(1) Å), the axial Se-Cl bonds (2,430(1) and 2,475(1) Å) being significantly longer. [N(C2H5)4]SeOCl3, which was obtained as crystals by oxidation of trichloroselenate(II), is triclinic, space group P1̄, with a = 10,607(3), b = 8,950(2), c = 8,862(2) Å, α = 119,79(2)°, β = 101,07(2)°, γ = 96,28(2)°, Z = 2. The X-ray structure analysis shows the anions to be present as centrosymmetric dimers Se2O2Cl62- like in the [P(C6H5)4]+ salt, with two tetragonal SeOCl4 pyramids linked through a Cl···Cl edge and the lone pairs trans to the axial Se-O bonds (1,589(4) Å). Se-Cl bond lengths are 2.270(1) and 2,351(2) Å (terminal); 2,698(1) and 2,920(1) Å (bridging). The results show that the nature of the reaction products of the Lewis acid SeOCl2 with halogenides as bases changes very sensitively with small variations in cations and environment. The vibrational spectra are discussed.


2006 ◽  
Vol 61 (1) ◽  
pp. 33-36 ◽  
Author(s):  
Victor M. Deflon ◽  
Cassia C. de Sousa Lopes ◽  
Karl E. Bessler ◽  
Lincoln L. Romualdo ◽  
Elke Niquet

The so far unknown lead tricyanomethanide, Pb[C(CN)3]2, was obtained from a saturated aqueous solution of PbCl2 and solid AgC(CN)3. Its IR spectrum and thermal behaviour are described. The crystal structure was determined by single-crystal X-ray diffraction (trigonal, P31m, Z = 3, a = 1414.4(5), c = 409.02(6) pm, R1 = 0.0249, wR2 = 0.0527). Two crystallographically independent ninefold coordinated Pb atoms are connected by planar tricyanomethanide ions in two distinct bridging coordination modes. The Pb−N distances range between 254 and 293 pm.


1999 ◽  
Vol 54 (7) ◽  
pp. 904-912 ◽  
Author(s):  
Konstantin V. Domasevitch ◽  
Elena G. Petkova ◽  
Alexander Yu. Nazarenko ◽  
Vera V. Ponomareva ◽  
Joachim Sieler ◽  
...  

Silver(I) cyanoximate complexes Ag{ONC(CN)-R} (R = COPh, {L1}; COC(CH3)3, {L2}; benzothiazol-2-yl, {L3}) with triphenylphosphine and -stibine of compositions Ag(PPh3)n{L} (n = 2, 4) and Ag(SbPh3)n{L} (n = 3 for {L1} and {L2}, n = 2 for {L3}) were synthesized by the reaction of the components in acetonitrile solution and characterized by elemental analyses and IR spectroscopy. The crystal structures of Ag(SbPh3)3{L} (L = {L1} (1), {L2} (2), Ag(SbPh3)2{L3} ∙ CH3CN (3) and Ag(PPh3)2{L1} ∙ CH3CN (4), have been determined by X-ray diffraction. For all the compounds examined the coordination environment of the silver atom has the geometry of a distorted terahedron ([AgP2NO] (4); [AgSb3N] (1), (2); [AgSb2N2] (3)). The bis adducts Ag(EPh3)n{L} adopt molecular structures, in which the organic anions are coordinated in bidentate chelate fashion via the nitroso nitrogen atom and the oxygen (nitrogen for {L3}) atom of the substituent R. In the tris-stibino complexes (Ag-Sb 2.670(4) - 2.7748(8) Å; Sb-Ag-Sb 108.87(4) - 115.00(2)°) the cyanoximates are unidentate ligands and coordinated via the nitroso nitrogen atoms (Ag-N ca. 2.35(1) Å). The different behaviour of N ,O and N,N chelating cyanoximes under the same conditions suggests, that the Sb donor triphenylstibine is able to substitute the oxygen atoms in the silver(I) coordination sphere, but not the nitrogen ones. This causes the formation of 1:3 adducts of Ag{L} with SbPh3 for N ,O donors {L1} and {L2}, and only 1:2 for N,N donor anionic {L3}.


1986 ◽  
Vol 41 (1) ◽  
pp. 48-52 ◽  
Author(s):  
Elke Conradi ◽  
Heribert Wadle ◽  
Ulrich Müller ◽  
Kurt Dehnicke

Violet crystals of AsPh4[W(O)Cl3(HN3S2)] were obtained by partial hydrolysis of AsPh4[WCl4(N3S2)] in a saturated solution in CH2Cl2/CCl4. Its IR spectrum is reported. The crystal structure was determined by X-ray diffraction (2284 independent observed reflexions, R = 0.041). Crystal data: triclinic, space group P1̄, Z = 2, a = 812.2, b = 1268.4, c = 1343.9 pm, α = 88.58, β = 82.04 and γ = 88.26°. The compound consists of AsPh4⊕ cations and [W(O)Cl3(HN3S2)⊖ anions in which the tungsten atoms have a distorted octahedral coordination with one oxo-ligand (171 pm), three chlorine atoms and two nitrogen atoms of the planar (HN3S7)2⊖ ligand. The WN bond lengths are 183 and 226 pm; the longer WN bond is due to the hydrogen atom attached to its N atom and to the trans influence of the oxo group. The crystal packing corresponds to one of the types frequently found among tetraphenylphosphonium compounds with cations stacked to parallel columns.


Author(s):  
Monsumi Gogoi ◽  
Birinchi Kumar Das

A nickel(II) terephthalate complex, viz. [Ni(C6H4N2)2(H2O)4](O2CC6H4CO2)·4H2O, has been synthesized and studied by single-crystal X-ray diffraction. It crystallizes in the triclinic space group P\overline{1}. The crystal structure shows an approximately octahedral coordination environment of the complex with the [Ni(H2O)4(3-NCpy)2]2+ (3-NCpy is pyridine-3-carbonitrile) cation associated with four free water molecules and hydrogen bonded to a terephthalate dianion [graph set R 2 2(8)]. The supramolecular structure of the compound is stabilized by a three-dimensional array of O—H...O and O—H...N hydrogen bonds, along with π–π stacked pyridine-3-carbonitrile rings and C—H...O interactions.


1998 ◽  
Vol 53 (11) ◽  
pp. 1338-1342 ◽  
Author(s):  
A. Strueß ◽  
W. Preetz

The treatment of K2[OsO2(OH)4] with oxamide in aqueous solution yields [OsO2(N2H2C2O2)2]2-. The crystal structure of trans-(Ph4P)2[ OsO2(N2H2C2O2)2]·CH2Cl2 (triclinic, space group P1̅, a = 10.447(1), b = 14.102(4), c = 16.962(2) Å, a = 90.037(1), β = 90.633(7), γ = 98.812(2)°, Z = 2) has been determined by single crystal X-ray diffraction analysis. The IR and Raman spectra were measured at room temperature. Based on the molecular parameters of the X-ray determination a normal coordinate analysis has been performed and the vibrations are assigned. The valence force constants are fd(Os=O) = 6.7, fd(Os-N) = 2.4, fd(C-N) = 4.9, fd(C=0) = 11.15 and fd(C-C) = 4.7 mdyn/Å.


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