scholarly journals Synthesis and Structural Characterization of ‘Non-VSEPR’ Structures of Oxo-Tungsten Complex

2011 ◽  
Vol 8 (s1) ◽  
pp. S323-S329
Author(s):  
Shahriare Ghammamy ◽  
Hajar Sahebalzamani

The crystal structure of [(CH3)4N]4[WOCl4F][WO3Cl4] was determined by single crystal x-ray diffraction technique. The crystal is monoclinic, space group C 2/m, with a= 28.23(10) Å, b= 11.60(4) Å,c= 13.48(5) Å, β=118.43(7)°, V= 3886(2)Å3, Z=4. The structure was solved by direct methods and refined by least-squares methods to a final R = 0.0512 for 3825 observed reflections with I>2σ(I). In crystal there are two crystallographic distinct anions, both with cis geometry; the O-W-F and O-W-O angles are 97.5(3)° and 103.1(3) ° respectively. All structures are cis configurations that confirm a preference for angles below 90° and 180° between cis and trans σ-donor ligands, respectively.

2019 ◽  
Vol 74 (4) ◽  
pp. 381-387
Author(s):  
Michael Zoller ◽  
Jörn Bruns ◽  
Gunter Heymann ◽  
Klaus Wurst ◽  
Hubert Huppertz

AbstractA potassium tetranitratopalladate(II) with the composition K2[Pd(NO3)4] · 2HNO3 was synthesized by a simple solvothermal process in a glass ampoule. The new compound crystallizes in the monoclinic space group P21/c (no. 14) with the lattice parameters a = 1017.15(4), b = 892.94(3), c = 880.55(3) Å, and β = 98.13(1)° (Z = 2). The crystal structure of K2[Pd(NO3)4] · 2HNO3 reveals isolated complex [Pd(NO3)4]2− anions, which are surrounded by eight potassium cations and four HNO3 molecules. The complex anions and the cations are associated in layers which are separated by HNO3 molecules. K2[Pd(NO3)4] · 2HNO3 can thus be regarded as a HNO3 intercalation variant of β-K2[Pd(NO3)4]. The characterization is based on single-crystal X-ray and powder X-ray diffraction.


1987 ◽  
Vol 65 (12) ◽  
pp. 2830-2833 ◽  
Author(s):  
David M. McKinnon ◽  
Peter D. Clark ◽  
Robert O. Martin ◽  
Louis T. J. Delbaere ◽  
J. Wilson Quail

3,5-Diphenyl-1,2-dithiolium-4-olate (1) reacts with aniline to form 1-phenylimino-2-phenylamino-3-phenylindene (3a). Under suitable conditions, 6-phenylbenzo[b]indeno[1,2-e]-1,2-thiazine is also formed. These structures are confirmed by alternative syntheses. The molecular structure of 3a has been determined by single crystal X-ray diffraction. Compound 3a crystallizes in the monoclinic space group C2/c with unit cell dimensions a = 20.777(3) Å, b = 6.130(3) Å, c = 31.327(3) Å, 3 = 99.59(1)°, and Z = 8. The structure was solved by direct methods and refined by least squares to a final R = 0.055. The molecular structure of 3a shows the three phenyl containing substituents to have the planes of their ring systems tilted between 40° and 60° from the plane of the indene system due to steric repulsions.


Author(s):  
Sandeep Kumar ◽  
Ruchi Khajuria ◽  
Amanpreet Kaur Jassal ◽  
Geeta Hundal ◽  
Maninder S. Hundal ◽  
...  

Donor-stabilized addition complexes of nickel(II) with disubstituted diphenyldithiophosphates, [{(ArO)2PS2}2NiL2] {Ar = 2,4-(CH3)2C6H3[(1), (5)], 2,5-(CH3)2C6H3[(2), (6)], 3,4-(CH3)2C6H3[(3), (7)] and 3,5-(CH3)2C6H3[(4), (8)];L= C5H5N [(1)–(4)] and C7H9N [(5)–(8)]}, were successfully isolated and characterized by elemental analysis, magnetic moment, IR spectroscopy and single-crystal X-ray analysis. Compound (4) crystallizes in the monoclinic space groupP21/nwhereas compounds (7) and (8) crystallize in the triclinic space group P\bar 1. The single-crystal X-ray diffraction analysis of (4), (7) and (8) reveals a six-coordinated octahedral geometry for the NiS4N2chromophore. Two diphenyldithiophosphate ions act as bidentate ligands with their S atoms coordinated to the Ni centre. Each of them forms a four-membered chelate ring in the equatorial plane. The N atoms from two donor ligands are axially coordinated to the Ni atom.


2007 ◽  
Vol 63 (2) ◽  
pp. 270-276 ◽  
Author(s):  
Thomas Reeswinkel ◽  
Sebastian Prinz ◽  
Karine M. Sparta ◽  
Georg Roth

The new spin ½ V4+ barium oxovanadate BaV4O9 was synthesized and studied by means of single-crystal X-ray diffraction. Its room-temperature structure is monoclinic, space group P2/c. We discuss the temperature evolution of the crystal structure and thermal expansion tensor of the material between 293 and 100 K.


2018 ◽  
Vol 96 (6) ◽  
pp. 570-577 ◽  
Author(s):  
Alina M. Secara ◽  
Justin F. Binder ◽  
Ala’aeddeen Swidan ◽  
Charles L.B. Macdonald

A series of germanium(II) and tin(II) bromide polyether complexes have been synthesized. Specifically, [GeBr([15]crown-5)][GeBr3], [GeBr([18]crown-6)][GeBr3], [GeBr(triglyme)][GeBr3], [GeBr(tetraglyme)][GeBr3], [SnBr([18]crown-6)][SnBr3], [Sn([15]crown-5)2][SnBr3]2, [SnBr(triglyme)][SnBr3], and [SnBr(tetraglyme)][SnBr3] have been fully characterized including by single crystal X-ray diffraction. The synthesis of [GeBr(dibenzo[24]crown-8)][GeBr3] and [GeCl(dibenzo[24]crown-8)][GeCl3] are also reported, along with the crystal structure of the latter’s water adduct, which features a water molecule adjacent to the GeCl+ ion within the cavity of the crown ether.


2019 ◽  
Vol 74 (11-12) ◽  
pp. 857-860
Author(s):  
Hai-Wei Kuai ◽  
Xiao-Hong Zhu ◽  
Ding-Yun Jiang ◽  
Xiao-Chun Cheng ◽  
Deng-Hao Li

Abstract1,3,5-Tri(1H-imidazol-4-yl)benzene (H3L) reacts with Ni(ClO4)2 · 6H2O under hydrothermal conditions at T = 100°C to yield a new complex: [Ni(H2L)2] · 5.5H2O (1). The product is characterized by single crystal and powder X-ray diffraction, infrared spectroscopy, and elemental and thermogravimetric analyses. Complex 1 crystallizes in the monoclinic space group C2/c and exhibits a binodal (3,6)-connected 2D kgd network structure with (43)2(46.66.83) topology.


1985 ◽  
Vol 38 (5) ◽  
pp. 669 ◽  
Author(s):  
PC Healy ◽  
C Pakawatchai ◽  
AH White

The crystal structure of [C13H10N] [CuCl3(C13H9N)].H2O(C13H9N ≡ acridine ) has been determined by single-crystal X-ray diffraction methods at 295 K, being refined by least squares to a residual of 0.037 for 1942 independent 'observed' reflections. Crystals are triclinic, Pī , a 16.27(2), b 10.080(8), c 7.236(5) Ǻ, α 88.85(6), β 82.68(8), γ 81.12(9)°, Z 2. The metal atom stereochemistry is unusual, being of pseudo-m symmetry; one of the chlorine atoms is coplanar with the copper and the acridine [Cu- Cl 2.237(2) Ǻ, N-Cu- Cl 143.5(1)°], with the other two disposed to either side of that plane [Cu- Cl 2.252(3), 2.243(2) Ǻ; Cl-Cu-Cl 145.62(7)°]. Cu-N is 2.018(5) Ǻ.


1989 ◽  
Vol 42 (6) ◽  
pp. 907 ◽  
Author(s):  
LM Engelhardt ◽  
PC Healy ◽  
JD Kildea ◽  
AH White

The mononuclear adducts chloro - and bromo-pyridinebis (triphenylphosphine)silver have been synthesized and structurally characterized by single-crystal X-ray diffraction methods. The two complexes are isomorphous, monoclinic, space group P21 or P21/m, a ≈ 9.8, b ≈ 20.0, c ≈ 9.1 � , β ≈ 97.5�, Z 2; in space group P21/m, they were refined to residuals of 0.038, 0.036 for 2392, 2157 'observed' reflections respectively. No comparable iodide adduct has been isolated. In both structures the silver atom is four-coordinate; Ag-Cl,Br are 2.511(2), 2.629(1) �; Ag-P, 2.472(1), 2.476(1) �, and Ag-N, 2.585(5), 2.570(5) � respectively, the Ag-N distance being longer than Ag-P, indicating very weak coordination of the pyridine.


2004 ◽  
Vol 68 (5) ◽  
pp. 757-767 ◽  
Author(s):  
T. Mihajlović ◽  
H. Effenberger

AbstractHydrothermal synthesis produced the new compound SrCo2(AsO4)(AsO3OH)(OH)(H2O). The compound belongs to the tsumcorite group (natural and synthetic compounds with the general formula M(1)M(2)2(XO4)2(H2O,OH)2; M(1)1+,2+,3+ = Na, K, Rb, Ag, NH4, Ca, Pb, Bi, Tl; M(2)2+,3+ = Al, Mn3+, Fe3+, Co, Ni, Cu, Zn; and X5+,6+ = P, As, V, S, Se, Mo). It represents (1) the first Sr member, (2) the until now unknown [7]-coordination for the M(1) position, (3) the first proof of (partially) protonated arsenate groups in this group of compounds, and (4) a new structure variant.The crystal structure of the title compound was determined using single-crystal X-ray diffraction data. The compound is monoclinic, space group P21/a, with a = 9.139(2), b = 12.829(3), c = 7.522(2) Å, β = 114.33(3)°, V = 803.6(3) Å3, Z = 4 [wR2 = 0.065 for 3530 unique reflections]. The hydrogen atoms were located experimentally.


1994 ◽  
Vol 47 (2) ◽  
pp. 391 ◽  
Author(s):  
CJ Kepert ◽  
BW Skeleton ◽  
AH White

The room-temperature single-crystal X-ray structural characterization of the title compound (tpyH2)2[Tb(OH2)8]Cl7.~2⅓H2O is recorded. Crystals are triclinic, Pī , a 17.063(5), b 16.243(3), c 7.878(3) Ǻ, α 84.78(2), β 84.39(3), γ 87.81(2)°, Z = 2 formula units; 3167 'observed' diffractometer reflections were refined by full-matrix least-squares procedures to a residual of 0.057. Notable features of interest of the compound are the 'chelation' of chloride ions by the terpyridinium cations , and the existence of a free [Tb(OH2)8]2+ cation in the presence of an abundance of chloride ions.


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