New adducts of silver(I) halides, AgX (X = Cl, Br), with bidentate phosphine ligands: syntheses and molecular structures of [Ag3(μ3-Cl)2(μ-dppm)3][PF6], [Ag3(μ3-Br)2(μ-dppm)3][AgBr2], {[Et4N][Ag2 (μ-Br)3(μ-dppe)]}n, [Et4N]2[(AgCl2)2(μ-dppe)], and [(AgCl)2(μ-dppp)2]

2017 ◽  
Vol 72 (5) ◽  
pp. 327-334
Author(s):  
Ting-Ting Qian ◽  
Yu-Feng Xie ◽  
Hua-Tian Shi ◽  
Ai-Quan Jia ◽  
Qian-Feng Zhang
Keyword(s):  
Membered Ring ◽  
Phosphine Ligands ◽  
Molecular Structures ◽  
Anionic Complex ◽  
Polymeric Complex ◽  
X Ray Diffraction ◽  
Neutral Complex ◽  
X Ray ◽  
Trigonal Bipyramidal ◽  
Bidentate Phosphine

AbstractInteraction of AgCl with bis(diphenylphosphino)methane (dppm) in THF/MeCN in the presence of K[PF6] or [Et4N]Br afforded typical trinuclear cationic trigonal-bipyramidal complexes [Ag3(μ3-Cl)2(μ-dppm)3][PF6] (1) or [Ag3(μ3-Br)2(μ-dppm)3][AgBr2] (2), respectively. Treatment of AgBr with bis(diphenylphosphino)ethane (dppe) in THF/MeCN in the presence of [Et4N]Br gave a polymeric complex {[Et4N][Ag2(μ-Br)3(μ-dppe)]}n (3) with a dinuclear {Ag2(μ-Br)3} core. The reaction of AgCl with dppe or bis(diphenylphosphino)propane (dppp) in THF/MeCN in the presence of [Et4N]Cl resulted in the isolation of a dinuclear anionic complex [Et4N]2[(AgCl2)2(μ-dppe)] (4) with one μ-dppe bridge or a dinuclear neutral complex [(AgCl)2(μ-dppp)2] (5) with two μ-dppp bridges and a 12-membered ring, respectively. The structures of complexes 1–5 with the bidentate phosphine ligands were determined by single-crystal X-ray diffraction.

scholarly journals Synthesis of Trithia-Borinane Complexes Stabilized in Diruthenium Core: [(Cp*Ru)2(η1-S)(η1-CS){(CH2)2S3BR}] (R = H or SMe)

Inorganics ◽  
2019 ◽  
Vol 7 (2) ◽  
pp. 21 ◽  
Author(s):  
Koushik Saha ◽  
Urminder Kaur ◽  
Rosmita Borthakur ◽  
Sundargopal Ghosh
Keyword(s):  
Mass Spectrometry ◽  
1H Nmr Spectroscopy ◽  
Chair Conformation ◽  
Membered Ring ◽  
Molecular Structures ◽  
Boat Conformation ◽  
X Ray Diffraction ◽  
X Ray ◽  
Butterfly Cluster ◽  
Tellurium Powder

The thermolysis of arachno-1 [(Cp*Ru)2(B3H8)(CS2H)] in the presence of tellurium powder yielded a series of ruthenium trithia-borinane complexes: [(Cp*Ru)2(η1-S)(η1-CS){(CH2)2S3BH}] 2, [(Cp*Ru)2(η1-S)(η1-CS){(CH2)2S3B(SMe)}] 3, and [(Cp*Ru)2(η1-S)(η1-CS){(CH2)2S3BH}] 4. Compounds 2–4 were considered as ruthenium trithia-borinane complexes, where the central six-membered ring {C2BS3} adopted a boat conformation. Compounds 2–4 were similar to our recently reported ruthenium diborinane complex [(Cp*Ru){(η2-SCHS)CH2S2(BH2)2}]. Unlike diborinane, where the central six-membered ring {CB2S3} adopted a chair conformation, compounds 2–4 adopted a boat conformation. In an attempt to convert arachno-1 into a closo or nido cluster, we pyrolyzed it in toluene. Interestingly, the reaction led to the isolation of a capped butterfly cluster, [(Cp*Ru)2(B3H5)(CS2H2)] 5. All the compounds were characterized by 1H, 11B{1H}, and 13C{1H} NMR spectroscopy and mass spectrometry. The molecular structures of complexes 2, 3, and 5 were also determined by single-crystal X-ray diffraction analysis.

Synthesis and characterization of N-silylated, C1-symmetric benzamidinates of lithium, sodium, and tin(II)

2006 ◽  
Vol 84 (2) ◽  
pp. 269-276 ◽  
Author(s):  
Floria Antolini ◽  
Peter B Hitchcock ◽  
Alexei V Khvostov ◽  
Michael F Lappert
Keyword(s):  
Nmr Spectra ◽  
Alkali Metals ◽  
Membered Ring ◽  
Molecular Structures ◽  
Synthesis And Characterization ◽  
Neutral Ligand ◽  
X Ray Diffraction ◽  
X Ray ◽  
Ligand Free

The synthesis and characterization of complexes obtained from the reactions between Li[N-t-Bu(SiMe3)] (A) or the sodium analogue Na[N-t-Bu(SiMe3)] (B) and the cyanoarene RCN (R = Ph or 4-MeOC6H4) are discussed. These are the THF adduct [Li{µ-cis-N(t-Bu)C(Ph)N(SiMe3)}(THF)]2 (1), the TMEDA adduct Li[N(t-Bu)C(Ph)N(SiMe3)](TMEDA) (2), the neutral ligand-free lithium benzamidinate Li[N(t-Bu)C(C6H4OMe-4)N(SiMe3)] (3), and the THF adduct Li[N(t-Bu)C(C6H4OMe-4)N(SiMe3)](THF) (3a). The preparation and structure of the crystalline compound [Na{µ-cis-N(t-Bu)C(Ph)N(SiMe3)}(OEt2)]2 (4) is described. From the lithium benzamidinate 1 and Sn(II) chloride the tin(II) complex [Sn{N(t-Bu)C(Ph)N(SiMe3)}2] (5) was obtained. The molecular structures of the crystalline compounds 1, 4, and 5 were established by X-ray diffraction. In 1 and 4 the benzamidinato ligand is both chelating and bridging, with the Me3Si-substituted nitrogen atom as the bridging site. The central planar (MN)2 four-membered ring is a rhombus in 1, with almost equal Li—N bond lengths, whereas in 4 the bonds to Na(1) are significantly longer than those to Na(2). In 5, the ligand is N,N′-chelating. Key words: alkali metals, tin(II), benzamidinates, NMR spectra, X-ray structures.

The synthesis and structural characterization of linear and macrocyclic bis(dinitrosyliron) complexes supported by bis(phosphine) bridging ligands

2003 ◽  
Vol 81 (6) ◽  
pp. 468-475 ◽  
Author(s):  
Lijuan Li ◽  
Nada Reginato ◽  
Michael Urschey ◽  
Mark Stradiotto ◽  
John D Liarakos
Keyword(s):  
Solid State ◽  
Structural Characterization ◽  
Mononuclear Complex ◽  
Phosphine Ligands ◽  
Molecular Structures ◽  
X Ray Diffraction ◽  
Bridging Ligands ◽  
X Ray ◽  
Phosphine Complexes

Reactions involving Fe(NO)2(CO)2 and the bis(phosphine) ligands bis(diphenylphosphino)methane (DPPM), bis(diphenylphosphino)acetylene (DPPA), 1,6-bis(diphenylphosphino)hexane (DPPH), and 1,4-bis(diphenyl phosphino)benzene (DPPB) have been examined. From these reactions, the mononuclear complex, Fe(κ1-DPPM)(NO)2(CO) 3, linear dinuclear species of the type Fe2(µ-L)(NO)4(CO)2 (L = Ph2PCH2PPh2 4, Ph2PC[Formula: see text]CPPh2 5, Ph2PCH2(CH3)4CH2PPh2 6, and Ph2P(p-C6H4)PPh2 7), and macrocyclic dinuclear species of the type Fe2(µ-L)2(NO)4 (L = Ph2PCH2PPh2 8 and Ph2PC[Formula: see text]CPPh2 9) were isolated and spectroscopically characterized. For 4, 5, 8, and 9, the solid-state molecular structures of the products were determined by use of single-crystal X-ray diffraction techniques. Key words: dinitrosyliron, iron nitrosyls, dinuclear macrocycles, bis(phosphine) complexes.

Preparation of Hybrid Bidentate Phosphine-Ligands by Reduction of Their Benzylphosphonium or Phenylphosphonium Salts - X-Ray Crystal-Structure of 2-Aminophenyltriphenylphosphonium Tetrachloronickelate(II)

1992 ◽  
Vol 45 (3) ◽  
pp. 595 ◽  
Author(s):  
MK Cooper ◽  
JM Downes ◽  
PA Duckworth ◽  
ERT Tiekink
Keyword(s):  
Aryl Halide ◽  
Phosphine Ligands ◽  
Monoclinic Space Group ◽  
Phosphonium Salts ◽  
X Ray Diffraction ◽  
X Ray ◽  
Mercury Cathode ◽  
Bidentate Phosphine ◽  
Hybrid Ligands ◽  
Sodium Naphthalenide

The 2-substituted phenylphosphine bidentate hybrid ligands, 2-aminophenyl-, 2-methylamino- phenyl-, 2-hydroxphenyl- and (2-amino-3-methylpheny1)- diphenylphosphine , (1a-d), respectively, and 2-aminophenylmethylphenylphosphine, (le), were synthesized by reduction of their phenylphosphoniurn halides, (2a-e)X (X = Cl or Br), with sodium naphthalenide in tetrahydrofuran at -68�, or electrochemically at a mercury cathode. The phosphonium salts were prepared by reaction of triphenylphosphine with aryl halide and anhydrous nickel halide at 200�. X-Ray diffraction of (2a)2 [NiCl4] showed it to have monoclinic space group P21/n, a 10.657(4), b 20.966(3), c 20.422(6) � , β101.33(2) and Z4. The structure was refined by a full-matrix least-squares procedure to a final R 0.050 for 3534 reflections with I

Crystal structure determination of the conformation of two bicyclo[3.3.1]nonan-ones

1985 ◽  
Vol 63 (6) ◽  
pp. 1166-1169 ◽  
Author(s):  
John F. Richardson ◽  
Ted S. Sorensen
Keyword(s):  
Crystal Structure ◽  
Direct Methods ◽  
Chair Conformation ◽  
Molecular Structures ◽  
Boat Conformation ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Final Agreement

The molecular structures of exo-7-methylbicyclo[3.3.1]nonan-3-one, 3, and the endo-7-methyl isomer, 4, have been determined using X-ray-diffraction techniques. Compound 3 crystallizes in the space group [Formula: see text] with a = 15.115(1), c = 7.677(2) Å, and Z = 8 while 4 crystallizes in the space group P21 with a = 6.446(1), b = 7.831(1), c = 8.414(2) Å, β = 94.42(2)°, and Z = 2. The structures were solved by direct methods and refined to final agreement factors of R = 0.041 and R = 0.034 for 3 and 4 respectively. Compound 3 exists in a chair–chair conformation and there is no significant flattening of the chair rings. However, in 4, the non-ketone ring is forced into a boat conformation. These results are significant in interpreting what conformations may be present in the related sp2-hybridized carbocations.

Synthesis, structural characterization and catalytic activity of chlororuthenium(II) complexes with substituted Schiff base/phosphine ancillary ligands

2020 ◽  
Vol 75 (9-10) ◽  
pp. 851-857
Author(s):  
Chong Chen ◽  
Fule Wu ◽  
Jiao Ji ◽  
Ai-Quan Jia ◽  
Qian-Feng Zhang
Keyword(s):  
Schiff Base ◽  
Catalytic Activity ◽  
Structural Characterization ◽  
Room Temperature ◽  
Molecular Structures ◽  
Cationic Complex ◽  
Neutral Complex ◽  
Ancillary Ligands ◽  
X Ray ◽  
X Ray Crystallography

AbstractTreatment of [(η6-p-cymene)RuCl2]2 with one equivalent of chlorodiphenylphosphine in tetrahydrofuran at reflux afforded a neutral complex [(η6-p-cymene)RuCl2(κ1-P-PPh2OH)] (1). Similarly, the reaction of [Ru(bpy)2Cl2·2H2O] (bpy = 2,2′-bipyridine) and chlorodiphenylphosphine in methanol gave a cationic complex [Ru(bpy)2Cl(κ1-P-PPh2OCH3)](PF6) (2), while treatment of [RuCl2(PPh3)3] with [2-(C5H4N)CH=N(CH2)2N(CH3)2] (L1) in tetrahydrofuran at room temperature afforded a ruthenium(II) complex [Ru(PPh3)Cl2(κ3-N,N,N-L1)] (3). Interaction of the chloro-bridged complex [Ru(CO)2Cl2]n with one equivalent of [Ph2P(o-C6H4)CH=N(CH2)2N(CH3)2] (L2) led to the isolation of [Ru(CO)Cl2(κ3-P,N,N-L2)] (4). The molecular structures of the ruthenium(II) complexes 1–4 have been determined by single-crystal X-ray crystallography. The properties of the ruthenium(II) complex 4 as a hydrogenation catalyst for acetophenone were also tested.

Strukturuntersuchungen an Diaryldichalkogeniden: Die Molekülstrukturen von [2,4,6-(CF3)3C6H2S]2,[2,4,6-Me3C6H2Te]2 und [2-Me2N-4,6-(CF3)2C6H2Te]2 / Structural Investigations of Diaryl Dichalcogenides: The Molecular Structures of [2,4,6-(CF3)3C6H2S]2, [2,4,6-Me3C6H2Te]2 and [2-Me2N-4,6-(CF3)2C6H2Te]2

1992 ◽  
Vol 47 (3) ◽  
pp. 305-309 ◽  
Author(s):  
Anja Edelmann ◽  
Sally Brooker ◽  
Norbert Bertel ◽  
Mathias Noltemeyer ◽  
Herbert W. Roesky ◽  
...  
Keyword(s):  
Molecular Structures ◽  
Monoclinic Space Group ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Structural Investigations ◽  
Space Group ◽  
X Ray

Abstract The Molecular Structures of [2,4,6-(CF3)3C6H2S]2 (1) [2,4,6-Me3C6H2Te]2 and [2-Me2N-4,6-(CF3)2C6H2Te]2 (3) have been determined by X-ray diffraction. Crystal data: 1: orthorhombic, space group P212121, Z = 4, a = 822.3(2), b = 1029.2(2), c = 2526.6(5) pm (2343 observed independent reflexions, R = 0.042); 2: orthorhombic, space group Iba 2, Z = 8, a = 1546.5(2), b = 1578.4(2), c = 1483.9(1) pm (2051 observed independent reflexions, R = 0.030); 3: monoclinic, space group P 21/c, Z = 4, a = 1118.7(1), b = 1536.5(2), c = 1492.6(2) pm, β = 98.97(1)° (3033 observed independent reflexions, R = 0.025).

Crystal and molecular structure of diorganoammonium oxalatotrimethylstannate, [R2NH2][Me3Sn(C2O4)] (R=i-Bu, cyclohexyl)

2011 ◽  
Vol 34 (5-6) ◽  
pp. 127-130 ◽  
Author(s):  
Yaya Sow ◽  
Libasse Diop ◽  
Kieran C. Molloy ◽  
Gabrielle Kociok-Köhn
Keyword(s):  
Molecular Structure ◽  
Hydrogen Bonds ◽  
Diffraction Study ◽  
Crystal And Molecular Structure ◽  
X Ray Diffraction ◽  
X Ray ◽  
Trigonal Bipyramidal ◽  
Trans Complex ◽  
A Chain ◽  
Distorted Trigonal Bipyramidal

Abstract The title compounds [R2NH2][C2O4SnMe3](R=i-Bu, Cy), in which tin atoms adopt a distorted trigonal bipyramidal configuration, have been prepared and submitted to an X-ray diffraction study. These compounds have been obtained from the reaction of (Cy2NH2)2C2O4·H2O or (i-Bu2NH2)2C2O4 with SnMe3Cl. In both [R2NH2][C2O4SnMe3] compounds, the trans complex has an almost regular trigonal bipyramidal geometry around the tin atom. The SnMe3 residues are connected as a chain with bridging oxalate anions in a trans-SnC3O2 framework, the oxygen atoms being in axial positions. The cations connect linear adjacent chains through NH…O hydrogen bonds giving layered structures.

scholarly journals Relation between photochromic properties and molecular structures in salicylideneaniline crystals

2012 ◽  
Vol 68 (3) ◽  
pp. 297-304 ◽  
Author(s):  
Kohei Johmoto ◽  
Takashi Ishida ◽  
Akiko Sekine ◽  
Hidehiro Uekusa ◽  
Yuji Ohashi
Keyword(s):  
Dihedral Angle ◽  
Steric Hindrance ◽  
Molecular Structures ◽  
Dihedral Angles ◽  
Clear Correlation ◽  
X Ray Diffraction ◽  
Photochromic Properties ◽  
X Ray ◽  
Benzene Rings ◽  
The Relationship

The crystal structures of the salicylideneaniline derivatives N-salicylidene-4-tert-butyl-aniline (1), N-3,5-di-tert-butyl-salicylidene-3-methoxyaniline (2), N-3,5-di-tert-butyl-salicylidene-3-bromoaniline (3), N-3,5-di-tert-butyl-salicylidene-3-chloroaniline (4), N-3,5-di-tert-butyl-salicylidene-4-bromoaniline (5), N-3,5-di-tert-butyl-salicylidene-aniline (6), N-3,5-di-tert-butyl-salicylidene-4-carboxyaniline (7) and N-salicylidene-2-chloroaniline (8) were analyzed by X-ray diffraction analysis at ambient temperature to investigate the relationship between their photochromic properties and molecular structures. A clear correlation between photochromism and the dihedral angle of the two benzene rings in the salicylideneaniline derivatives was observed. Crystals with dihedral angles less than 20° were non-photochromic, whereas those with dihedral angles greater than 30° were photochromic. Crystals with dihedral angles between 20 and 30° could be either photochromic or non-photochromic. Inhibition of the pedal motion by intra- or intermolecular steric hindrance, however, can result in non-photochromic behaviour even if the dihedral angle is larger than 30°.

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