scholarly journals Structure and Synthesis of Dihalogenodicyanoaurate Complexes [Ph3PR][Au(CN)2Hal2], Hal = Cl, R = Me, СH2Ph; Hal = Br, R = cyclo-C6H11; Hal = I, R = Ph

2021 ◽  
Vol 13 (1) ◽  
pp. 58-67
Author(s):  
D.P. Shevchenko ◽  
◽  
A.E. Khabina
Keyword(s):  
Structural Organization ◽  
Tetrahedral Coordination ◽  
Analysis Method ◽  
Reaction Products ◽  
X Ray ◽  
Ionic Complexes ◽  
Bond Lengths ◽  
Square Planar ◽  
Average Bond ◽  
Distorted Tetrahedral Coordination

Interaction of organyltriphenylphosphonium halides with potassium dihalogenodicyanoaurates in water followed by recrystallization of reaction products from acetonitrile or DMSO has been used to synthesize gold(III) ionic complexes [Ph3PMe][Au(CN)2Cl2] (1), [Ph3PCH2Ph][Au(CN)2Cl2] (2), [Ph3PC6H11-cyclo][Au(CN)2Br2] (3), and [Ph4P][Au(CN)2I2] (4), which have been structurally characterized by the X-ray analysis method (CIF files CCDC No. 1901681 (1), 1912903 (2), 1912919 (3), 2048146 (4)). According to the X-ray data crystals 1–4 consist of centrosymmetric square-planar [Au(CN)2Hal2]– anions (the Au–Hal average bond lengths are 2.417(3) Å (1), 2.280(2) Å (2), 2.4203(13) Å (3), and 2.6035(10) Å (4); the Au–C average bond lengths are 2.06(2) Å (1), 2.010(7) Å (2), 2.009(7) Å (3,) and 1.998(6) Å (4)); the phosphorus atoms in organyltriphenylphosphonium cations have a slightly distorted tetrahedral coordination (the P–C bond lengths are 1.782(9)-1.806(8) Å (1), 1.788(4)-1.813(5) Å (2), 1.790(5)-1.813(5) Å (3) and 1.793(6)-1.799(5) Å (4)). The structural organization in crystals 2–4 is caused by the interionic С–H∙∙∙N≡C hydrogen bonds (C–HPh∙∙∙N≡C 2.56 Å (2); C–HPh∙∙∙N≡C 2.43–2.59 Å, C–Hcyclohexyl∙∙∙N≡C 2.47 Å (3), C–HPh∙∙∙N≡C 2.63 Å (4)), while in crystals 1 no significant interionic contacts are observed.

Synthese und Struktur von Ni(2,6-iPr2C6H3N = CH – CH =NC6H3-2,6-iPr2)2. Synthesis and Structure of Ni(2,6-iPr2C6H3N=CH–CH = NC6H3-2,6-iPr2)2

1990 ◽  
Vol 45 (12) ◽  
pp. 1647-1650 ◽  
Author(s):  
Werner Bonrath ◽  
Klaus R. Pörschke ◽  
Richard Mynott ◽  
Carl Krüger
Keyword(s):  
Dihedral Angle ◽  
Structure Analysis ◽  
Title Compound ◽  
Tetrahedral Coordination ◽  
X Ray ◽  
Bond Lengths ◽  
Soluble Compound ◽  
Poorly Soluble ◽  
Distorted Tetrahedral Coordination ◽  
C Nmr

Ni(cdt)** reacts with two equivalents of the sterically highly demanding 1,4-diazadiene 2,6-iPr2C6H3N =CH –CH =NC6H3-2,6-iPr, to yield the red-brown, crystalline title compound Ni(2,6-iPr2Ph-dad)2 (3). The existence of this compound was previously uncertain. 1H and 13C NMR, MS, and UV/VIS spectra of 3 are reported. The X-ray structure analysis of 3 revealed a strongly distorted tetrahedral coordination of the nickel center with a dihedral angle of 51 between the planes of the chelate rings and mean bond lengths Ni-Ν 1.965(4) Å and N=CH 1.308(5) Å. The poorly soluble compound appears to be rather unreactive because of the bulk of the ligands.

Tetrahalogenotellurate(II): Synthese und Kristallstrukturen von Verbindungen mit den Ionen TeX42- (X = Cl, Br, I)/Tetrahalotellurates(II): Syntheses and Crystal Structures of Compounds with TeX42- Ions (X = Cl, Br, I)

1985 ◽  
Vol 40 (2) ◽  
pp. 251-257 ◽  
Author(s):  
Siegfried Pohl ◽  
Wolfgang Saak ◽  
Bernt Krebs
Keyword(s):  
Single Crystal ◽  
Crystal Structures ◽  
Acetonitrile Solution ◽  
Monoclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths ◽  
Square Planar

Abstract The compounds [(C6H5)4As]2 TeCl4 (1), [(C2H5)4 N]2 TeBr4 · CH3CN (2), and [(C2H5)4N]2TeI4 (3) were prepared by the reaction of Te, X2 , and excess (C2H5)4NX (X = Br, I) in acetonitrile solution or by heating of [(C6H5)4 As]2TeCl6 , Te, and (C6H5)4 ASCl for several hours in the same solvent.The structures of 1-3 were determined from single crystal X-ray data.1 crystallizes in the monoclinic space group P21/n with a = 1061.8(2), b = 1614.2(3), c = 1341.7(3) pm, β = 94.21° and Z = 2; 2: tetragonal, P4/mmm, a = 1039.7(2), c = 690.5(1), Z = 1; 3: tetragonal, I4/mmm, a = 1061.7(2), c = 1342.8(4), Z = 2. In 1-3 Te(II) exhibits a square planar coordination. The Te -CI, Te -Br, and Te-I bond lengths were found to be 260.7 (mean), 275.3, and 298.5 pm, respectively.

Four (2,2′-bipyridyl)(ferrocenyl)boronium derivatives

2015 ◽  
Vol 71 (1) ◽  
pp. 26-31 ◽  
Author(s):  
Jan W. Bats ◽  
Kuangbiao Ma ◽  
Hans-Wolfram Lerner
Keyword(s):  
Hydrogen Bonding ◽  
Crystal Structures ◽  
Tetrahedral Coordination ◽  
Asymmetric Unit ◽  
Bond Lengths ◽  
Distorted Tetrahedral Coordination

Crystal structures are reported for four (2,2′-bipyridyl)(ferrocenyl)boronium derivatives, namely (2,2′-bipyridyl)(ethenyl)(ferrocenyl)boronium hexafluoridophosphate, [Fe(C5H5)(C17H15BN2)]PF6, (Ib), (2,2′-bipyridyl)(tert-butylamino)(ferrocenyl)boronium bromide, [Fe(C5H5)(C19H22BN3)]Br, (IIa), (2,2′-bipyridyl)(ferrocenyl)(4-methoxyphenylamino)boronium hexafluoridophosphate acetonitrile hemisolvate, [Fe(C5H5)(C22H20BN3O)]PF6·0.5CH3CN, (IIIb), and 1,1′-bis[(2,2′-bipyridyl)(cyanomethyl)boronium]ferrocene bis(hexafluoridophosphate), [Fe(C17H14BN3)2](PF6)2, (IVb). The asymmetric unit of (IIIb) contains two independent cations with very similar conformations. The B atom has a distorted tetrahedral coordination in all four structures. The cyclopentadienyl rings of (Ib), (IIa) and (IIIb) are approximately eclipsed, while a bisecting conformation is found for (IVb). The N—H groups of (IIa) and (IIIb) are shielded by the ferrocenyl andtert-butyl or phenyl groups and are therefore not involved in hydrogen bonding. The B—N(amine) bond lengths are shortened by delocalization of π-electrons. In the cations with an amine substituent at boron, the B—N(bipyridyl) bonds are 0.035 (3) Å longer than in the cations with a methylene C atom bonded to boron. A similar lengthening of the B—N(bipyridyl) bonds is found in a survey of related cations with an oxy group attached to the B atom.

The Crystal and Molecular Structure of Dinitrato(triphenylphosphine)mercury(II)

1974 ◽  
Vol 52 (2) ◽  
pp. 198-202 ◽  
Author(s):  
Simon H. Whitlow
Keyword(s):  
Molecular Structure ◽  
Single Crystal ◽  
Crystal And Molecular Structure ◽  
Bond Distance ◽  
The Other ◽  
Tetrahedral Coordination ◽  
X Ray ◽  
R Factor ◽  
Computer Controlled ◽  
Distorted Tetrahedral Coordination

The structure of dinitrato(triphenylphosphine)mercury(II), Hg(N03)2.P(C6H5)3, has been determined from single–crystal X-ray data measured on a computer–controlled diffractometer. The crystals are monoclinic, have a unit cell of dimensions a = 10.39(1), b = 9.56(1), c = 19.44(2) Å, β = 94.3(1)°, which contains 4 molecules, and they belong to the space group, P21/c. The structure has been refined by least–squares methods from 2470 independent observed reflections to a conventional R-factor of 0.061. The Hg atom has a distorted tetrahedral coordination with Hg—O bond lengths of 2.190(8), 2.428(8), and 2.560(9) Å and an Hg—P bond distance of 2.359(3) Å. There are 2 distinct types of NO3 groups bonded to Hg. One is an unshared, unidentate ligand and the other acts as a bridging group joining 2 Hg atoms. Chains of—Hg—NO3—Hg—atoms are formed which follow crystallographic two-fold screw axes in the b-direction.

scholarly journals Reactions of Pentaphenylantimony and Penta-Para-Tolylanimony with Calixarene [4-t-BuC6H2OH(S-2)]4

2021 ◽  
Vol 13 (1) ◽  
pp. 47-57
Author(s):  
A.N. Efremov ◽  
◽  
V.V. Sharutin
Keyword(s):  
Hydrogen Bonds ◽  
Antimony Atom ◽  
Tetrahedral Coordination ◽  
X Ray Diffraction ◽  
Deprotonated Form ◽  
X Ray ◽  
Bond Lengths ◽  
Tert Butyl ◽  
Average Value ◽  
Intramolecular Hydrogen

Pentaphenylantimony and penta-para-tolylantimony react with calixarene [4-t-BuC6H2OH(S-2)]4 (СArH) by way of arene elimination and formation of the [Ph4Sb]+[СAr]- × TolH (1), [p-Tol4Sb]+[CAr]- × H2O (2) ionic products with a yield up to 96%. The compound has been identified by IR spectroscopy and X-ray diffraction analysis. According to the X-ray diffraction data, compounds 1 and 2 are ionic complexes with solvate molecules of toluene (1) and water (2). The cation has a tetrahedral coordination of the antimony atom with aryl ligands at the polyhedron vertices; the anion is represented by the deprotonated form of p-tert-butylthiacalix[4]arene. The three tert-butyl groups, the phenyl ring and solvated toluene in the structure of compound 1, and two tert-butyl fragments in the structure of compound 2 are disordered over two positions. The tetrahedral coordination of antimony atoms in the cations of compounds 1 and 2 is slightly distorted. The CSbC angles deviate from the theoretical value and vary within 106.0(4)−117.7(4)° (1), 105.75(15)−112.84(15)° (2). The average Sb–C bond lengths are 2.101(3) and 2.106(4) Å in structures 1 and 2, respectively. The [СAr]- anion is in the cone conformation, the upper rim of which is represented by the tert-butyl groups in the para-position, while the lower one is represented by hydroxy groups, one of which is deprotonated. The СAr–O– bond length (1.318(4) (1) and 1.326(4) (2) Å) is less than the average value of the СAr–OH bond lengths (1.338(4) (1) and 1.343(4) (2) Å), which indicates increasing multiplicity of the bond and localization of a negative charge on the oxygen atom. Intramolecular hydrogen bonds with the neiboring O atom are observed. The H∙∙∙O distances are 2.16, 1.69, 1.77 Å in 1 and 1.92, 1.79, 1.76 Å in 2. Dihedral angles between opposite phenoxide rings are 60.64° and 87.07° (1) and 83.85° and 80.42° (2), which indicates somewhat less symmetric anion in structure 1 than in structure 2. The formation of the crystal spatial structure is due to the formation of hydrogen bonds between ions with participation of oxygen and sulfur atoms, as well as СН∙∙∙π–interactions, while the ions form chains in the crystal of compound 1, and layers in the crystal of compound 2. Complete tables of atom coordinates, bond lengths and valence angles are deposited at the Cambridge Crystallographic Data Center (No. 1850118 (1); No. 2013220 (2); [email protected] or http://www.ccdc.cam.ac.uk/data_request/cif).

scholarly journals Synthesis and Characterisation of Zinc(II) Complex With 2-Amino-5-bromopyridine Ligand

2017 ◽  
Author(s):  
Fitriani
Keyword(s):  
Ir Spectroscopy ◽  
Elemental Analysis ◽  
Coordination Geometry ◽  
Tetrahedral Coordination ◽  
Visible Absorption ◽  
X Ray ◽  
X Ray Crystallography ◽  
Uv Visible ◽  
Cl Atoms ◽  
Distorted Tetrahedral Coordination

The synthesis and characterisation of zinc(II) complex with 2-amino-5-bromopyridine (C5H5BrN2) ligand have been described. The complex was structurally characterised via X-ray crystallography, in the title compound, (2-amino-5-bromopyridinium) [ZnCl¬3(2-amino-5-bromopyridine)] or which is also called (C5H6BrN2) [ZnCl3(C5H5BrN2)]¬. The Zn(II) atom is four-coordinated by three Cl atoms and one imine N-atom of 2-amino-5-bromopyridine ligand, forming a distorted tetrahedral coordination geometry. The complex was also investigated by elemental analysis, 1H NMR, IR spectroscopy and UV-Visible absorption. The protonation behaviour upon coordination is discussed.

X-ray absorption spectroscopy studies on the carbothermal reduction reaction products of 3 mol% yttria-stabilized zirconia

2014 ◽  
Vol 47 (5) ◽  
pp. 1512-1519
Author(s):  
A. Sondhi ◽  
O. Okobiah ◽  
S. Chattopadhyay ◽  
T. Shibata ◽  
T. W. Scharf ◽  
...  
Keyword(s):  
Bond Length ◽  
Absorption Spectroscopy ◽  
Carbothermal Reduction ◽  
Yttria Stabilized Zirconia ◽  
Sintered Pellet ◽  
Reaction Products ◽  
Stabilized Zirconia ◽  
X Ray ◽  
Bond Lengths ◽  
X Ray Absorption

Extended X-ray absorption spectroscopy (EXAFS) at the ZrKedge has been used to determine changes in various bond lengths in 3 mol% yttria-stabilized zirconia (YSZ) during zirconium carbide (ZrC) formation. The principal objective of this study was to determine if ZrC formation at the YSZ/carbon interface alters the zirconia structure. A mixed-phase sample (YSZ and graphite) was carbothermally reduced to form ZrC. X-ray diffraction phase quantification by Rietveld analysis confirmed the formation of ∼50% ZrC in the analyzed sample volume. EXAFS data of ZrC and YSZ powders and a sintered YSZ pellet (∼96.7% density) were used as standards to compare with the carbothermally reduced sample.Ab initocalculations using these spectra quantified various Zr—O, Zr—C and Zr—Zr bond distances in the system. Best fit results revealed Zr—OI(tetragonal), Zr—O (monoclinic), Zr—Zr (tetragonal) and Zr—Zr (monoclinic) bond length values of 2.10, 2.25, 3.65 and 3.52 Å, respectively, in the YSZ powder, Zr—OI(tetragonal) and Zr—Zr (tetragonal) bond length values of 2.12 and 3.62 Å, respectively, in the sintered pellet, and Zr—C and Zr—Zr bond lengths of 2.32 and 3.33 Å, respectively, in the ZrC powder. Similar fitting procedures were carried out on the carbothermally reduced pellet, with measured Zr—O, Zr—Zr (of YSZ), Zr—C and Zr—Zr (of ZrC) bond lengths of 2.13, 3.62, 2.36 and 3.33 Å, respectively. These bond lengths indicate that the formation of ZrC in the YSZ matrix does not influence the local structure when compared to pure standards. Therefore, carbothermal reduction does not induce any apparent strain or thermally induced effects on the first and second coordination shells of Zr as measured by the X-ray absorption spectra of the carbothermally reduced sample. Interestingly, the results indicated that sintering of the YSZ powder into pellets did not result in any significant change in the Zr—O and Zr—Zr distances for tetragonal YSZ.

Synthesis, characterization, and X-ray structural analysis of the Cu(I) derivative, [Me2Ga(OCH2CH2NMe2)N2C5H7]Cu• PPh3

1981 ◽  
Vol 59 (3) ◽  
pp. 518-523 ◽  
Author(s):  
Kenneth S. Chong ◽  
Steven J. Rettig ◽  
Alan Storr ◽  
James Trotter
Keyword(s):  
Structural Analysis ◽  
Copper Atom ◽  
Direct Methods ◽  
Carbonyl Complex ◽  
Coordination Geometry ◽  
Tetrahedral Coordination ◽  
Full Matrix ◽  
X Ray ◽  
Complex Crystals ◽  
Distorted Tetrahedral Coordination

The Cu(I) complex [Me2Ga(OCH2CH2NMe2)N2C5H7]Cu•PPh3 has been synthesized and its fluxional behavior in solution probed. Attempts have been made to isolate the analogous Cu(I) carbonyl complex. Crystals of [dimethyl(3,5-dimethyl-1-pyrazolyl)(N,N-dimethylethanolamino)gallato (N(2),O,N(3))](triphenylphosphine)copper(I) are monoclinic, a = 18.871(2), b = 9.464(1), c = 18.374(2) Ā, β = 109.62(1)°, Z = 4, space group P21/c. The structure was solved by direct methods and was refined by full-matrix least-squares procedures to R = 0.028 and Rw = 0.035 for 2729 reflections with I ≥ 3σ(I). The copper atom is bonded to the phosphine and to the tridentate Me2Ga(OCH2CH2NMe2)N2C5H7− ligand resulting in a distorted tetrahedral coordination geometry. The Cu—P distance of 2.156(1) Å is unusually short. Other important bond distances (corrected for libration) are: Cu—O, 2.163(2), Cu—N(pyrazolyl), 2.025(3), Cu—N(amino), 2.144(3), Ga—O, 1.896(3), Ga—N, 2.005(3), and Ga—C, 1.972(5) and 1.987(5) Å.

Crystal structure of low-cristobalite-type Al0.5Ga0.5PO4: A combined Rietveld refinement of neutron and X-ray diffraction data

2005 ◽  
Vol 20 (3) ◽  
pp. 207-211 ◽  
Author(s):  
S. N. Achary ◽  
A. K. Tyagi ◽  
S. K. Kulshreshtha ◽  
O. D. Jayakumar ◽  
P. S. R. Krishna ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Diffraction Data ◽  
Three Dimensional ◽  
Crystal Structure Analysis ◽  
Tetrahedral Coordination ◽  
X Ray Diffraction ◽  
Rietveld Refinements ◽  
X Ray ◽  
Cell Parameters ◽  
Bond Lengths

The low-cristobalite-type modification of Al0.5Ga0.5PO4 is prepared by annealing the amorphous precipitate of stoichiometric phosphate at 1300 °C. The phase purity of the sample is ascertained by powder X-ray diffraction. The crystal structure is refined by Rietveld refinements of the neutron and X-ray diffraction data of the polycrystalline powder. This compound crystallizes in an orthorhombic lattice with unit cell parameters, a=7.0295(8), b=7.0132(8), and c=6.9187(4) Å, V=341.08(6) Å3, Z=4 (Space group C 2221, No. 20). The crystal structure analysis reveals the random distribution of the Al3+ and Ga3+ having tetrahedral coordination with typical M–O (M=Al3+:Ga3+) bond lengths as 1.74 Å. Similarly, the P5+ have tetrahedral coordination with typical P–O bond lengths 1.52–1.54 Å. The Mo4 and PO4 tetraheda are linked by common corners forming a three-dimensional framework lattice. The details of the crystal structure are presented in this paper.

scholarly journals New platinum(II) complexes with benzothiazole ligands

2016 ◽  
Vol 72 (3) ◽  
pp. 412-416 ◽  
Author(s):  
José A. Carmona-Negrón ◽  
Mayra E. Cádiz ◽  
Curtis E. Moore ◽  
Arnold L. Rheingold ◽  
Enrique Meléndez
Keyword(s):  
Single Crystal ◽  
Metal Atom ◽  
Cancer Chemotherapy ◽  
Potential Application ◽  
Dihedral Angles ◽  
Coordination Geometry ◽  
X Ray Diffraction ◽  
X Ray ◽  
Bond Lengths ◽  
Square Planar

Four new platinum(II) complexes, namely tetraethylammonium tribromido(2-methyl-1,3-benzothiazole-κN)platinate(II), [NEt4][PtBr3(C8H7NS)] (1), tetraethylammonium tribromido(6-methoxy-2-methyl-1,3-benzothiazole-κN)platinate(II), [NEt4][PtBr3(C9H9NOS)] (2), tetraethylammonium tribromido(2,5,6-trimethyl-1,3-benzothiazole-κN)platinate(II), [NEt4][PtBr3(C10H11NS)] (3), and tetraethylammonium tribromido(2-methyl-5-nitro-1,3-benzothiazole-κN)platinate(II), [NEt4][PtBr3(C8H6N2O2S)] (4), have been synthesized and structurally characterized by single-crystal X-ray diffraction techniques. These species are precursors of compounds with potential application in cancer chemotherapy. All four platinum(II) complexes adopt the expected square-planar coordination geometry, and the benzothiazole ligand is engaged in bonding to the metal atom through the imine N atom (Pt—N). The Pt—N bond lengths are normal: 2.035 (5), 2.025 (4), 2.027 (5) and 2.041 (4) Å for complexes1,2,3and4, respectively. The benzothiazole ligands are positioned out of the square plane, with dihedral angles ranging from 76.4 (4) to 88.1 (4)°. The NEt4cation in3is disordered with 0.57/0.43 occupancies.

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