scholarly journals Synthesis and Structural Study of the Bis(ethylenediamine)CdFe(CO)4 Monomer

2014 ◽  
Vol 2014 ◽  
pp. 1-4
Author(s):  
Marcus Tofanelli ◽  
Atta M. Arif ◽  
Richard D. Ernst

The new (en)2CdFe(CO)4 complex has been isolated from the crystallization of [(en)CdFe(CO)4]x from ethylenediamine (en). The cadmium center bears square-pyramidal coordination, with the iron atom occupying the apical position. The iron coordination may be described either as trigonal bipyramidal, with the cadmium atom being in an axial position, or as monocapped (by cadmium) tetrahedral. The Cd-Fe distance was found to be 2.6250(2) Å. The complex crystallizes in the monoclinic space group P21/a with a=14.4137(3) Å, b=7.65740(10) Å, c=14.5465(2) Å, and β=119.4972(9)° at 150(1) K.

2020 ◽  
Vol 26 (3) ◽  
pp. 212-217
Author(s):  
MODOU SARR ◽  
MOUHAMADOU BIRAME DIOP ◽  
AMINATA DIASSE-SARR ◽  
AI WANG ◽  
ULLRICH ENGLERT

The title polymer [HCO2Sn(C6H5)3]n was isolated by serendipitous from reaction in ethanol 96 % between bis-(monocyclohexyl ammonium) 2-carboxyethyl hydrogen phosphonate, {(CyNH3)2[CO2CH2CH2PO2(OH)]} and triphenyltin chloride, SnPh3Cl. The polymer crystallizes in the monoclinic space group P21/n with Z = 4, a = 14.7091 (18) Å, b = 15.4133 (19) Å, c = 14.7639 (18) Å, β = 94.242 (2)° and V = 3338.0 (7) Å3. The structure consists of an infinite chain propagating along the crystallographic a-axis direction with bidentate formate anions. The O2SnC3 core is organized into a trans-trigonal bipyramidal like-arrangement.


1994 ◽  
Vol 47 (7) ◽  
pp. 1223 ◽  
Author(s):  
JE Cosgriff ◽  
GB Deacon ◽  
BM Gatehouse ◽  
H Hemling ◽  
H Schumann

The complexes Ln (But2pz)3( thf )2 ( Ln = Y, La, Pr, Nd , Sm, Gd, Dy , Er , Yb, Lu; But2pz- = 3,5-di-t-butylpyrazolate; thf = tetrahydrofuran ), and [ Ln (But2pz)3(OPPh3)2].( dme )n ( Ln = La, n = ⅔ ; Ln = Er , n = 1; dme = 1,2-dimethoxyethane) have been prepared by reaction of the lanthanoid metal with bis ( pentafluorophenyl )mercury and the corresponding pyrazole in either thf , or in dme in the presence of triphenylphosphine oxide. The X-ray crystal structure of Er (η2-But2pz)3( thf )2 [monoclinic, space group P21 (No. 4), a 9.738(4), b 19.602(4), c 11.636(4) Ǻ, β 99.42(3)°, R 0.0374 for 3667 observed reflections] shows the complex to be an eight-coordinate monomer with three chelating But2pz ligands . The arrangement of centres ( Cen ) of the N-N bonds of the But2pz ligands [< Er -N> 2.336 Ǻ; Cen-Er-Cen 140.1(4)°, 110.3(4)° and 109.6(4)°] and the thf oxygen atoms [< Er -O> 2.351 Ǻ; O- Er -O 140.1(4)°] is intermediate between trigonal bipyramidal and square pyramidal. The other Ln (But2pz)3( thf )2 complexes and Ln (But2pz)3(OPPh3)2 are considered to have similar structures.


1983 ◽  
Vol 36 (1) ◽  
pp. 183 ◽  
Author(s):  
EJ O'Reilly ◽  
G Smith ◽  
CHL Kennard ◽  
AH White

The crystal structures of two copper(II) complexes of the herbicide Picloram (4-amino-3,5,6-trichloro- pyridine-2-carboxylic acid) have been determined by single-crystal X-ray diffractometry. Bis(4-amino- 3,5,6-trichloropyridine-2-carboxylato)aquacopper(II) dihydrate (1) is monoclinic, space group C2/c, with Z 4 in a cell of dimensions a 15.593(6), b 7.940(6), c 16.983(6) �, β 107.58(3)�. The structure was refined to a residual R 0.046 for 905 'observed' reflections. Complex (1) is trigonal bipyramidal with the trigonal plane consisting of oxygens from two picolinate ligands [Cu-O 1.995(5) �] and a water molecule [Cu-O 2.080(5) �]. The apical positions are occupied by pyridine ring nitrogens from the Picloram ligands [Cu-N 2.021(5) �]. Bis(4-amino-3,5,6-trichloropyridine- 2-carboxylato)bis(pyrimidin-2-amine)copper(II) (2) is monoclinic, space group P2,/c, with Z 4 in a cell of dimensions a 12.3 11(5), b 15.435(5), c 15.320(6) �, β 115.95(3)�, and gave a final R 0.059 for 2429 'observed' reflections. In complex (2), the copper(II) atom has a tetragonally distorted octahedral stereochemistry with the Picloram ring nitrogens once again occupying the two axial positions [Cu-N 2.586(7) and 2.611(7) �]. The square plane consists of two carboxylato oxygens [Cu-O 1.941(6) and 1.960(7) �] and two hetero-nitrogens from pyrimidin-2-amine ligands [Cu-N 2.048(6) and 2.054(6) �].


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.


1997 ◽  
Vol 50 (2) ◽  
pp. 123
Author(s):  
Margaret A. Brimble ◽  
Andrew Johnston ◽  
Trevor W. Hambley ◽  
Peter Turner

The structures of (3S*,4S*,5S*,6S*)-3,4-epoxy-1,7-dioxaspiro[5.5]undecan-5-ol (2), (3R*,5S*,6S*)-1,7- dioxaspiro[5.5]undecane-3,5-diyl diacetate (4) and (4S*,5S*,6S*)-1,7-dioxaspiro[5.5]undecane-4,5-diol (5) have been determined by X-ray crystallography. The unsubstituted tetrahydropyran ring in (2) adopts an axial position with respect to the epoxy-substituted ring and the hydroxy group at C5 is syn to the epoxide group. Intermolecular hydrogen bonding is observed between the C5 hydroxy group and O1. The two six-membered rings in (4) adopt chair conformations and the two acetate groups adopt 1,3-diaxial positions. The C5 hydroxy group in (5) assumes an axial position anti to the C-O bond of the neighbouring ring whilst 4-OH occupies an equatorial position. Intermolecular hydrogen bonding is also observed between 4-OH and 5-OH. Compound (2), C9H14O4, M 186·21, crystallized in the monoclinic space group P 21/c with a 7·867(1), b 12·2060(9), c 9·3676(8) Å, b 102·744(8), V 877·4(1) Å 3 and No 1163 [I > 2·5s (I)], R 0·031, Rw 0·035. Compound (4), C13H20O6, M 272·30, crystallized in the triclinic space group P 1 with a 9·902(1), b 11·0024(9), c 6·9183(5)Å, a 104·078(8), b 96·769(9), g 101·980(8), V 703·8(1) Å 3 , No 1657 [I > 2·5s(I)], R 0·047, Rw 0·044. Compound (5), C9H16O4, M 188·22, crystallized in the orthorhombic space group Pbca with a 25·504(3), b 8·909(2), c 8·038(2) Å, V 1826·4(5) QA 3 , No 1096 [I > 2·5s(I)], R 0·030, Rw 0·030.


1980 ◽  
Vol 35 (7) ◽  
pp. 855-859 ◽  
Author(s):  
Ulf Thewalt

The adduct α-FeCl3 · S4N4 has been prepared from FeCl3 and S4N4 in CCl4. The new compound crystallizes in the monoclinic space group P 21/c with Z = 4 and lattice parameters a = 6.360(2), b = 13.066(4), c = 12.686(5) Å, and β = 99.43(3)°. An X-ray analysis shows that the S4N4 ring is bonded via one of its nitrogen atoms to the iron atom of the FeCl3 group and that the four ligand atoms around the iron atom form a tetrahedron. The structure of the complex is similar to the known structure of BF3 · S4N4


2014 ◽  
Vol 2014 ◽  
pp. 1-5
Author(s):  
Torsten Kolb ◽  
Atta M. Arif ◽  
Richard D. Ernst

The new [(teeda)CdFe(CO)4]2 complex has been isolated from the reaction of [(NH3)2CdFe(CO)4]n with tetraethylethylenediamine. Unlike previous structural reports of ligand adducts of [L2CdFe(CO)4]x complexes, which have all been trimeric species composed of six-membered Cd3Fe3 rings, the teeda complex crystallized as a dimer, analogous to [(2,2-bpy)ZnFe(CO)4]2. As in the zinc dimer, significant distortion arises from steric interactions between the axial carbonyl ligands on opposing iron centers. The complex sits on an inversion center, leading to two independent Cd–Fe distances, 2.7244(6) and 2.7433(6) Å, and crystallizes in the monoclinic space group P21/a with a = 14.8546(2) Å, b = 15.1647(3) Å, c = 15.5252(3) Å, β = 90.9517(12)°, and Dcalc = 1.719 g/cm3 at 150(1) K.


1999 ◽  
Vol 77 (12) ◽  
pp. 2088-2094 ◽  
Author(s):  
Sudeep Bhattacharyya ◽  
Raymond J Batchelor ◽  
Frederick WB Einstein ◽  
Alan S Tracey

Reaction of β-mercaptoethanol with vanadate under slightly alkaline conditions provided a crystalline complex that was characterized by X-ray diffraction and FTIR spectroscopy. The complex was dimeric in structure with a central [VO]2 core and a pentacoordinate, crudely trigonal bipyramidal arrangement about each vanadium atom with a sulphur occupying a pseudo-axial position. A single 51V NMR signal was observed for this complex when dissolved in water, chloroform or acetonitrile. A large influence of acetonitrile on the vanadium chemical shift suggested the possibility of reaction with acetonitrile. FTIR showed the presence of two complexes in acetonitrile solution but only one in chloroform or water. Mixed solvent studies were carried out in an effort to further characterize the solution complexes. Crystal structure of [{VO2(OC2H4S)}2][NEt4]2: monoclinic, space group P21/n,. a = 8.3451(17), b = 16.954(4), c = 10. 2064(25) Å; β = 101. 271(18)°; V = 1416.2 Å3; Z = 2; RF = 0.048 for 1355 data (Io 2..5σ (Io) and 147 variables.Key words: mercaptoethanol, vanadate, vanadium NMR, X-ray diffraction, FTIR, thiolate.


2000 ◽  
Vol 78 (11) ◽  
pp. 1484-1490 ◽  
Author(s):  
Xiaoping Cai ◽  
Barbara Gehrhus ◽  
Peter B Hitchcock ◽  
Michael F Lappert

Treatment of the thermally stable aminosilylene Si[{N(CH2tBu)}2C6H4-1,2] [= Si(NN)] with a tris(cyclopentadienyl)- group 3 or -lanthanide metal compound LnCp3 (Cp = η5-C5H5 and Ln = Y or Yb) in toluene at ambient temperature afforded the first earliest transition or f-block metal-silylene complexes [LnCp3{Si(NN)}]·C7H8 (Ln = Y (1) or Yb (2)), characterized by NMR spectroscopy and X-ray crystallography: complex 1 (monoclinic, space group P21/c (no. 14), a = 15.641(5), b = 15.895(7), c = 14.876(5) Å, β = 112.93(3), Z = 4, R1 = 0.067 for 6194 observed data), and2 (monoclinic, space group P21/c (no. 14), a = 15.635(3), b = 15.795(2), c = 14.842(2) Å, β = 112.87(2), Z = 4, R1 = 0.044 for 9829 observed data). The Ln atom in each of the isoleptic complexes 1 and 2 has distorted trigonal monopyramidal geometry, with the approximately trigonal silicon atom in the apical position. The Ln-Si bond length is 3.038(2) (1) or 2.984(2) Å (2). Variable temperature 29Si{1H} NMR spectra in toluene-d8 show that each complex readily dissociates (Y > Yb) into its factors; at 188 K, the 29Si{1H} signal for (1) was a doublet centred at δ 119.5, 1J(29Si-89Y) = 59 Hz.Key words: crystallography, NMR, silylene, yttrium, ytterbium, organometallic complexes.


1991 ◽  
Vol 44 (2) ◽  
pp. 219 ◽  
Author(s):  
D Onggo ◽  
DC Craig ◽  
AD Rae ◽  
HA Goodwin

Bis ( ligand ) complexes of 6-methyl-2,2′-bipyridine (L) with copper(II) and palladium(II) have been prepared, and their structures have been determined by single-crystal X-ray diffractometry . In the formation of the complex fromcopper(II) tetrafluoroborate and L, partial hydrolysis of a coordinated fluoroborate ion to the hydroxytrifluoroborate ion occurs. The stereochemistry about copper in [CuL2OHBF3][BF4] is essentially trigonal bipyramidal with an axial compression. The nitrogens of the methyl-substituted pyridine rings coordinate in the axial sites. In [PdL2Cl][BF4] the coordination environment about palladium is square planar and one of the 6-methylbipyridine molecules functions as a unidentate group, the nitrogen of the methyl-substituted pyridine ring being uncoordinated. The average metal-nitrogen distance is 2.032 Ǻ in the copper complex and 2.042 Ǻ in the palladium complex. [CuL2OHBF3][BF4] is monoclinic, space group P21/c, Z = 4, a 9.005(2), b 17.868(2), c 15.298(3) Ǻ, β 104.13(1)°. [PdL2Cl][BF4] is monoclinic, space group P21/c, Z = 4, a 9.606(5), b 14.748(2), c 16.311(8)Ǻ, β 96.13(2)°.


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