The synthesis and structural characterization of a series of triphenyltin(IV) esters of N-arylidene-ω-amino acids

1992 ◽  
Vol 70 (10) ◽  
pp. 2683-2687 ◽  
Author(s):  
Y. C. Toong ◽  
S. P. Tai ◽  
M. C. Pun ◽  
Rosemary C. Hynes ◽  
L. E. Khoo ◽  
...  

Methods of synthesis, elemental analyses, and IR and NMR spectroscopic data are reported for a series of triphenyltin esters of N-salicylidene-ω amino acids of the general formula: Ph3SnOCO(CH2)nN=CHAr (Ar = 2-HOC6H4− and 2-HOC10H6−; n = 1, 2, 3, and 5). The crystal structure of triphenyltin N-salicylidene-6-aminohexanoate was determined. The crystals are monoclinic, space group P21/a, with a = 16.3493(8) Å, b = 9.0675(7) Å, c = 18.8562(14) Å, β = 100.493(5)°, V = 2748.6(3) Å3, Z = 4, and Dcalc = 1.427 Mg m−3. The final discrepancy factors are RF = 0.033, and RW = 0.036 for 2339 significant reflections. This compound, believed typical of the series described, adopts a polymeric trans-O2SnC3 trigonal bipyramidal geometry with the axial positions occupied by a carboxylate oxygen and the phenolic oxygen of an adjacent molecule. These compounds appear to be the first reported triphenyltin(IV) carboxylates with phenolic oxygen bridges.

Author(s):  
Roberto Santos Barbiéri ◽  
Vilma Reis Terra ◽  
Allan Kardec Carlos Dias ◽  
Walclée De Carvalho Melo ◽  
Daniel Rodrigues Silva

This paper describes the preparation and description of four new complexes [Bu2Sn(AA)Cl] (AA = glycine, DL-valine and L-leucine) and [Bu2SnPhen2] (Phen = DL-phenylalanine) They were characterized by elemental analyses of carbon, hydrogen, nitrogen, chlorine and tin; and by infrared, 119mSn-Mössbauer and 119mSn-RMN spectroscopies, and by the applications of TG and DSC techniques in dynamic helium atmosphere. For the [Bu2Sn(AA)Cl], trigonal bipyramidal tin species, AA were coordinated bidentatedly by the carboxylic oxygen and by the NH2 group. The [Bu2SnPhen2)], with tin atoms in trans-octahedral sites, had the Phen-coordinated by both carboxylic oxygen atoms.


1989 ◽  
Vol 44 (4) ◽  
pp. 502-504 ◽  
Author(s):  
Jung Su Han ◽  
Werner Wolfsberger

Some unsymmetrical chlorophosphines RR′PCI were prepared by the reaction of RPCl2 (R = CH3, C2H5, i-C3H7, C6H5) with Grignard reagents R′MgCl (R′ = c-C5H9, c-C6H11, i-C3H7) and characterized by elemental analyses and spectroscopic data (IR, 31P and 13C NMR).


1990 ◽  
Vol 45 (4) ◽  
pp. 508-514 ◽  
Author(s):  
B. Nuber ◽  
W. Schatz ◽  
M. L. Ziegler

[CpMo(CO)3]2 (1) (Cp = cyclopentadienyl) reacts with InCl3 in diglyme to yield the oxo-cluster [Cp3Mo3(CO)4(μ-Cl)(μ3-O)] (2) and the cationic oxo-cluster [Cp3Mo3(μ-CO)3(CO)3(μ3-O)]+ as the salt [Cp3Mo3(μ-CO)3(CO)3(μ3-O)][CpMo(CO)3InCl3] (3). The compounds were characterized by elemental analysis, spectroscopic data and X-ray structure analysis. Compound 2 crystallizes in the orthorhombic space group P212121 with a = 1006.0(3), b = 1244.6(4) and c = 1600.8(5) pm, V = 2004.3 x 106 pm3, Z = 4. Compound 3 crystallizes in the monoclinic space group P 21/m with a = 874.4(8), b = 1407(1) and c = 1500(1) pm, β = 92.95(6) , V = 1843 × 106 pm3, Z = 2.


2021 ◽  
pp. 255-260 ◽  
Author(s):  
Shaban A. A. Abdel-Raheem ◽  
Adel M. Kamal El-Dean ◽  
Reda Hassanien ◽  
Mohamed E. A. El-Sayed ◽  
Mostafa Sayed ◽  
...  

Starting from 3-cyano-4,6-distyrylpyridin-2(1H)-thione (1), the compound N-(4-chlorophenyl)-2-((3-cyano-4,6-distyrylpyridin-2-yl)thio)acetamide (2) was prepared. Compound (2) underwent cyclization upon heating in ethanolic sodium ethoxide solution to give the corresponding cyclized form 3-amino-N-(4-chlorophenyl)-4,6-distyrylthieno[2,3-b]pyridine-2-carboxamide (3). The elemental analyses and spectroscopic data of compounds (2) and (3) are in agreement with their proposed structures. Their insecticidal activity against cowpea aphid, Aphis craccivora Koch, was studied. The results of insecticidal activity for compounds (2) and (3) against the nymphs and the adults of the tested insects exhibited that compounds (2) and (3) have a higher insecticidal activity than that of acetamiprid, a reference insecticide, after 24 h of treatment.


2007 ◽  
Vol 62 (11) ◽  
pp. 1353-1357 ◽  
Author(s):  
Aytaç Gürhan Gökçe ◽  
Rafet Kılınçarslan ◽  
Muhittin Aygün ◽  
Bekir Çetinkaya ◽  
Santiago García-Granda

A Pd(II) complex of a new N-heterocyclic carbene (NHC) ligand with bulky substituents and functionalized methoxy-donor side arms has been synthesized and characterized by elemental analyses, 1H and 13C NMR, and IR spectroscopy. Molecular and crystal structures of the title complex have been determined by single crystal X-ray diffraction. The compound crystallizes in the monoclinic space group P21/c, with a = 15.927(2), b = 8.489(2), c = 20.309(5) Å, β = 99.213(2)°, Z = 2, Dx = 1.253 g cm−3. The palladium atom is situated on an inversion center. There are several weak intramolecular C-H ··· N/O interactions.


1991 ◽  
Vol 46 (11) ◽  
pp. 1578-1580 ◽  
Author(s):  
Werner Wolfsberger

Some (cyanomethyl)alkylphenyl phosphines R(C6H5)PCH2CN (R = CH3, C2H5, C3H7, C4H9, i-C4H9, C5H11,) were prepared by the reaction of the corresponding (trimethylsilyl)alkylphenyl phosphines with chloroacetonitrile and characterized by elemental analyses and spectroscopic data (IR; 1H, 31P and 13C NMR).


1973 ◽  
Vol 51 (4) ◽  
pp. 618-623 ◽  
Author(s):  
K. R. Dixon ◽  
A. D. Rattray

Reactions of 1,10-phenanthroline with halogen bridged dinuclear species, [M2X2(PPh2O)2(PPh2OH)2] and [M2X2(PR3)4][BF4]2, give the new five co-ordinate complexes, [MX(PPh2O)(PPh2OH)(Phen)] and [MX(PR3)2(Phen)][BF4], where M = Pd or Pt, X = Cl or Br, Ph = phenyl, and R = ethyl (or phenyl when M = Pd). Decomposition of the [MX(PR3)2(Phen)][BF4] complexes in hot solvents gives the four co-ordinate species, [MX(PR3)(Phen)][BF4]. The complexes are characterized by elemental analyses, molecular weight, and conductance measurements and infrared and nuclear magnetic resonance spectroscopy. The spectroscopic data show that [PtCl(PEt3)2(Phen)][BF4] has a trigonal bipyramidal structure with the phenanthroline and one triethylphosphine in the equatorial plane and a chlorine and a triethylphosphine in the axial positions.


1993 ◽  
Vol 71 (9) ◽  
pp. 1437-1442 ◽  
Author(s):  
Heinz-Bernhard Kraatz ◽  
P. Michael Boorman ◽  
Masood Parvez

The reaction of NaSeMes (Mes = mesityl, 2,4,6-(CH3)3C6H2) with WCl4(PPh2Me)2 in THF leads to the formation of W(SeMes)4•THF (1), a possible mononuclear tetrakis(selenolato) complex of tungsten. The identity of the red crystalline material has been confirmed by elemental analysis and NMR spectroscopic methods (1H, 13C, and 77Se NMR). The reaction of W(SeMes)4•THF with tert-butyl isocyanide results in the formation of (tBuNC)(MesSe)2W(µ-Se)2W(SeMes)2(CNtBu) (2). Compound 2 crystallized in the monoclinic space group C2/c (no. 15) with a = 23.933(2) Å,b = 16.776(2) Å, c = 15.595(2) Å, β = 122.98(2)°, and four formula units per unit cell. Refinement by full-matrix least squares gave final residuals of R = 0.038 and Rw = 0.028. The two metal centres in 2 are in a trigonal bipyramidal (tbp) coordination environment. The two tbps are connected via a common edge (axial–equatorial). The W—W bond length of 2.732(1) Å and the diamagnetism of 2 indicate the presence of a metal–metal bonding interaction.


2018 ◽  
Vol 74 (11) ◽  
pp. 1658-1664
Author(s):  
Sida Wang ◽  
Phil Liebing ◽  
Felix Engelhardt ◽  
Liane Hilfert ◽  
Sabine Busse ◽  
...  

Deliberate hydrolysis of lithium cyclopropylalkynylamidinates, Li[c-C3H5—C[triple-bond]C(NR′)2] [R′ = i Pr, Cy = cyclohexyl)], afforded the hitherto unknown neutral cyclopropylalkynylamidine derivatives c-C3H5—C[triple-bond]C—C(NR′)(NHR′) [R′ = i Pr (1), Cy (2)]. Subsequent reactions of 1 or 2 with metal(II) chlorides, MCl2 (M = Mn, Fe, Co), provided the title complexes dichloridobis(3-cyclopropyl-N,N′-diisopropylprop-2-ynamidine)manganese(II), [MnCl2(C12H20N2)2], (3), dichloridobis(3-cyclopropyl-N,N′-diisopropylprop-2-ynamidine)iron(II), [FeCl2(C12H20N2)2], (4), dichloridobis(N,N′-dicyclohexyl-3-cyclopropylprop-2-ynamidine)iron(II), [FeCl2(C18H28N2)2], (5), and dichloridobis(N,N′-dicyclohexyl-3-cyclopropylprop-2-ynamidine)cobalt(II), [CoCl2(C18H28N2)2], (6), or more generally MCl2[c-C3H5—C[triple-bond]C—C(NR′)(NHR′)]2 [R′ = i Pr, M = Mn (3), Fe (4); R′ = Cy, M = Fe (5), Co (6)] in moderate yields (30–39%). Besides their spectroscopic data (IR and MS) and elemental analyses, all complexes 3–6 were structurally characterized. The two isopropyl-substituted complexes 3 and 4 are isotypic, and so are the cyclohexyl-substituted complexes 5 and 6. In all cases, the central metal atom is coordinated by two Cl atoms and two N atoms in a distorted-tetrahedral fashion, and the structure is supported by intramolecular N—H...Cl hydrogen bonds.


2012 ◽  
Vol 466-467 ◽  
pp. 463-468
Author(s):  
Hong Tao Gao

Reactions of (R3Sn)2O (R=Ph, 2-ClC6H4CH2, 2-FC6H4CH2, 4-CNC6H4CH2) with 5-chloro-6-hydroxynicotinic acid in 1/2 stoichiometry yielded eight triorganotin compounds. These compounds have been characterized by elemental analysis, IR and NMR spectroscopy. The crystal structures of triphenyltin esters of 5-chloro-6-hydroxynicotinic acid were determined by single crystal X-ray diffraction. In the compound, the tin atoms are rendered five-coordinated in a trigonal bipyramidal structure by coordinating though the three phenyl carbon atoms and two oxygen atoms one from carboxylate and other from the phenolic hydroxide. The resulting structure is one-dimensional linear polymers through an interaction between the O atoms of phenolic hydroxide and tin atoms of an adjacent molecule.


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