scholarly journals SYNTHESIS AND STRUCTURE OF METHYLTRIPHENYLPHOSPHONIUM DICYANODIBROMOAURATE [Ph3PCH3] [Au(CN)2Br2]

2020 ◽  
Vol 63 (3) ◽  
pp. 10-15
Author(s):  
Andrey N. Efremov ◽  
Vladimir V. Sharutin ◽  
Olga K. Sharutina ◽  
Pavel V. Andreev ◽  
Oleg S. Eltsov
Keyword(s):  
Absorption Band ◽  
Diffraction Analysis ◽  
Ir Spectrum ◽  
Integral Intensity ◽  
Complex Structure ◽  
Crystalline Substance ◽  
X Ray Diffraction ◽  
Tetrahedral Configuration ◽  
X Ray ◽  
Bond Lengths

Methyltriphenylphosphonium dicyanodibromoaurate (1) [Ph3PMe]+[Au(CN)2Br2]– was synthesized by the reaction of potassium dicyanodibromoaurate with methyltriphenylphosphonium bromide in an aqueous solution and was structurally characterized. The complex is a yellow-colored, air-resistant crystalline substance with a clear melting point. The structure of the compound was established by IR spectroscopy, NMR spectroscopy and X-ray diffraction analysis. An intense absorption band was observed in the IR spectrum of compound at 2220 cm−1, corresponding to the stretching vibrations of cyano groups. The absorption band of the deformation vibrations of the P – СPh bonds in the IR spectrum is at 1438 cm−1. In the recorded 1Н, 13С, and 31Р NMR spectra, signals are observed for the number, value of chemical shifts and integral intensity that do not contradict the proposed complex structure. The X-ray diffraction analysis of crystal 1 was carried out on a Bruker D8 QUEST diffractometer (MoKα radiation, λ = 0.71073 Å, graphite monochromator). [C21H18AuBr2N2P, M = 686.13, crystal system triclinic, space group P-1, a = 8.802(5), b = 8.989(5), c = 15.233(11) Å, V = 1143.8(13) Å3, Z = 2, µ = 10.002 mm-1, F(000) = 644, crystal size 0.41×0.30×0.22 mm]. According to the X-ray diffraction analysis (XRDA) data there are two types of centrosymmetric crystallographically independent monomeric dicyanodibromoaurate anions and methyltriphenylphosphonium cations in the crystal of compound MFDDA. The cations have a distorted tetrahedral configuration: the CPC angles equal 108.8(2)°−110.0(2)°, the P−С distances are 1.791(5)−1.800(5) Å. All СAuC and BrAuBr trans-angles are 180.0° in the [Au(CN)2Br2]− anions. The Au−C distances in anions differ from each other and equal 2.040(7), 2.024(1), 1.991(2) Å. These values are close to the sum of the covalent radii of atoms (2.03 Å). The Au-Br bond lengths are equal to 2.4162(14), 2.4591, 2.474(5) Å in dicyanodibromoaurate anions. Formation of the crystal structure occurs due to formation of weak N···Н−С hydrogen bonds between cations and anions (2.68, 2.59, 2.38 Å) and Br···Н−С (3.03, 3.02 Å). Complete tables of coordinates of atoms, bond lengths and valence angles are deposited at the Cambridge Crystallographic Data Centre.

scholarly journals New photochromic salt spiropyrans of indoline series

2019 ◽  
Vol 484 (6) ◽  
pp. 698-702
Author(s):  
A. D. Pugachev ◽  
M. B. Lukyanova ◽  
V. V. Tkachev ◽  
B. S. Lukyanov ◽  
N. I. Makarova ◽  
...  
Keyword(s):  
Absorption Band ◽  
Diffraction Analysis ◽  
Hypsochromic Shift ◽  
X Ray Diffraction ◽  
Photochromic Properties ◽  
Photoinduced Form ◽  
X Ray ◽  
Long Wavelength

The synthesis and study of the structure and photochromic properties of the new salt spiropyrans of the indoline series containing chlorine and bromine atoms as a substituent at the 6' position in 2H-chromene moiety are presented. The structure of the obtained compounds was confirmed by NMR 1H spectroscopy and X-ray diffraction analysis. The compounds are photochromic; the long-wavelength maximum of the absorption band of their open photoinduced form has a significant hypsochromic shift, and the lifetime substantially increases in comparison with the fluorine analog.

X-ray diffraction, infrared and TGA/DTG analysis of hydrated nacrite

Clay Minerals ◽  
1997 ◽  
Vol 32 (3) ◽  
pp. 463-470 ◽  
Author(s):  
A. Ben Haj Amara
Keyword(s):  
Weight Loss ◽  
Diffraction Analysis ◽  
Ir Spectrum ◽  
X Ray Diffraction ◽  
Interlayer Water ◽  
X Ray ◽  
Interlamellar Water ◽  
Hydration State ◽  
Coherent Domain

AbstractAn homogenous 8.4 Å hydrate was obtained after washing intercalated KAc- nacrite. X-ray diffraction analysis based on comparison of the experimental and calculated profiles enabled the amount of water (one molecule per Si2Al2O5(OH)4) and the z coordinate along c* (6.5 Å) to be determined. The hydration state was accompanied by a decrease in the coherent domain along c* in the order nacrite > KAc-nacrite > H2O-nacrite. The IR spectrum of the hydrated nacrite showed an evolution of the structure with a shift of ν(OH) from 3702, 3649 and 3630 cm−1 to 3690, 3641 and 3620 cm−1, respectively for the nacrite hydroxyls. The ν(OH) stretching bands of the interlayer water appeared at 3602 and 3545 cm−1 and their bending band at 1655 cm−1. The TGA/DTG analysis of the air-dry hydrated nacrite showed a loss of water at 245°C the weight loss (1 molecule per Si2Al2O5(OH)4) corresponding to the interlamellar water, in agreement with that determined by XRD.

scholarly journals Chloroantimonate(III), IV. Darstellung und Kristallstruktur von 2,2′-Bipyridinium-pentachloroantimonat (C10H8N2H2)SbCl5 und der metastabilen Modifikation von 4,4′ -Bipyridinium-pentachloroantimonat (C10H8N2H2)SbCl5 / Chloroantimonates(III), IV. Preparation and Crystal Structures of 2,2′-Bipyridinium Pentachloroantimonate (C10H8N2H2)SbCl5 and of the Metastable Modification of 4,4′-Bipyridinium Pentachloroantimonate (C10H8N2H2)SbCl5

1983 ◽  
Vol 38 (12) ◽  
pp. 1615-1621 ◽  
Author(s):  
Annegret Lipka
Keyword(s):  
Single Crystal ◽  
Diffraction Analysis ◽  
Crystal Structures ◽  
Bond Order ◽  
X Ray Diffraction ◽  
X Ray ◽  
Bond Lengths ◽  
Distorted Octahedral ◽  
Intermolecular Contacts

2,2′-Bipyridinium pentachloroantimonate (III) and the metastable modification of 4,4′-bipyridinium pentachloroantimonate(III) were synthezised and investigated by single crystal X-ray diffraction analysis. The structures consist of 2,2′-bipyridinium and 4,4′-bipyridinium cations, respectively, and of pentachloroantimonate anions. With regard to bonding and short intermolecular contacts the coordination of the Sb atoms is distorted octahedral in both structures. Bond lengths of equivalent Sb-Cl bonds differ strongly within the structure of the 2,2′-bipyridinium salt (239.9 pm to 312.1 pm) and are not distinguishable from short intermolecular contacts (305.4 pm and 321.8 pm). In the structure of the 4,4′-bipyridinium salt, bond distances vary only from 240.9 pm to 267.8 pm and are clearly below intermolecular contacts at 318.2 pm. In spite of the different distances the total bond order for each Sb atom is 3. In the structure of the 2,2′-bipyridinium salt the anions build tetramers, whereas in the structure of the 4,4′-bipyridinium salt the anions form chains

scholarly journals SYNTHESIS AND STRUCTURE OF POTASSIUM TETRAETHYLAMMONIUM HEXATHIOCYANATOPLATINATE(IV)

2018 ◽  
Vol 61 (12) ◽  
pp. 63-67
Author(s):  
Vladimir V. Sharutin ◽  
Olga K. Sharutina ◽  
Alena R. Tkacheva
Keyword(s):  
Crystal Size ◽  
Three Dimensional ◽  
Monoclinic Space Group ◽  
Slow Evaporation ◽  
X Ray Diffraction ◽  
Tetraethylammonium Chloride ◽  
Tetrahedral Configuration ◽  
X Ray ◽  
Bond Lengths ◽  
Graphite Monochromator

Potassium tetraethylammonium hexathiocyanatoplatinate(IV) (Et4N)(K)[Pt(SCN)6] (I) was synthesized by the reaction of potassium hexathiocyanatoplatinate(IV) with tetraethylammonium chloride in acetonitrile aqueous solution. Slow evaporation of the solvent led to the formation of large red-brown crystals. The product structure was determined by XRDA. The X-ray diffraction pattern of crystal I was carried out on a Bruker D8 QUEST diffractometer (MoKα radiation, λ = 0.71073 Å, graphite monochromator). [С14H20N7KPtS6, M = 712.92, Crystal system monoclinic, space group C 2/c, a = 10.432(8), b = 14.767(13), c = 16.300(13) Å, V = 2510(4) Å3, Z = 4, µ = 6.272 mm-1, F(000) = 1384, crystal size 0.86×0.66×0.50 mm]. The tetrahedral configuration of the tetraethylammonium cation is slightly distorted (CNC angles are 105.5(5)º-111.8(4)º, bond lengths N-С are 1.503(5)-1.519(5) Å). Platinum ions in anions have octahedral coordination (trans-angles SPtS are 180º, cis-angles SPtS are (88.47(4)º-91.53(4)º). The bond lengths Pt-S are equal to 2.373 (2)-2.37(2) Å. Potassium cations are coordinated by six nitrogen atoms of thiocyanate groups (distances N K (2.828(4)-2.896 (4) Å). Trans-angles NKN (128.44 (15)º-146.9 (2)º) are far from ideal values for the octahedron. Bridged thiocyanate ligands are bonded cations of the platinum and potassium. Ambidentate thiocyanate ligands are simultaneously coordinated to the K+ cation by nitrogen atoms. By means of the bridged thiocyanate ligands a three-dimensional coordination polymer is formed. The resulting structure is a three-dimensional grid, in the cells of which the cations of tetraethylammonium (Et4N)+ are located.

scholarly journals SYNTHESIS AND STRUCTURE OF (METHOXYMETHYL)TRIPHENYLPHOSPHONIIUM TRICHLORO(DIMETHYLSULFOXIDO)PLATINATE

2020 ◽  
Vol 63 (5) ◽  
pp. 33-37
Author(s):  
Alena R. Tkacheva ◽  
Olga K. Sharutina ◽  
Vladimir V. Sharutin
Keyword(s):  
Dimethyl Sulfoxide ◽  
Direct Method ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Compound I ◽  
Hydrogen Atoms ◽  
Chlorine Atoms ◽  
Tetrahedral Configuration ◽  
X Ray ◽  
Bond Lengths

 (Methoxymethyl)triphenylphosphonium trichloro(dimethylsulfoxido)platinate [Ph3PCH2OCH3][PtCl3(dmso-S)] was synthesized by the reaction of hexachloroplatinic acid with (methoxymethyl)triphenylphosphonium chloride in dimethyl sulfoxide. During the reaction, Pt (IV) was reduced to Pt (II). The reactions are accompanied by the ligand exchange in anions with substitution of the S-coordinated dimethyl sulfoxide molecule for one of chlorine atoms. Slow evaporation of the solvent led to the formation of large orange crystals. The product structure was determined by XRDA. The structures were interpreted by the direct method. Positions and temperature parameters of non-hydrogen atoms were refined in isotropic and then in anisotropic approximations by the full-matrix LSM. The X-ray diffraction pattern of crystal I was carried out on a Bruker D8 QUEST diffractometer. According to the data of X-ray analysis the unit cell crystallographic parameters of compound I are [crystal system monoclinic, space group P21/c, M 686.90, a 14.48(2), b 14.48(2), c 19.99(3) Å]. The tetrahedral configuration of the (methoxymethyl)triphenylphosphonium cation approaches the ideal values (CPC angles are 108.5(2)°-110.3(2)°, bond lengths Р-С are slightly differ from each other). Platinum atoms in anions have square coordination (trans-arranged angles ClPtCl are 177.65(5)°, SPtCl are 178.88(6)°, cis-angles approach 90°). The bond lengths Pt–Cl are equal to 2.290(3)–2.314(3) Å, Pt–S are equal to 2.205(3) Å. The platinum atoms are coordinated by three chlorine atoms and dimethyl sulfoxide molecule in the anion. Dimethyl sulfoxide molecule is coordinated to the platinum atoms by sulfur atoms. The geometry of the coordinated dimethyl sulfoxide ligand [OSC and СSC angles, S−O bond] differs from the geometry of a free dimethyl sulfoxide molecule.

The solid-state molecular structure of W(NO)3Cl3 and the nature of its W—NO bonding

2004 ◽  
Vol 82 (2) ◽  
pp. 285-292 ◽  
Author(s):  
Trevor W Hayton ◽  
Brian O Patrick ◽  
Peter Legzdins ◽  
W Stephen McNeil
Keyword(s):  
Molecular Structure ◽  
Solid State ◽  
Dft Calculations ◽  
Diffraction Analysis ◽  
Mirror Plane ◽  
Ambient Conditions ◽  
X Ray Diffraction ◽  
X Ray ◽  
Bond Lengths ◽  
Complex Solutions

The monomeric trinitrosyl complex, W(NO)3Cl3, can be prepared by the treatment of WCl6 in CH2Cl2 with NO gas, and its identity has been unambiguously confirmed by a single-crystal X-ray diffraction analysis. The complex crystallizes in the space group Pmn21 as a three-component twin (a = 10.4280(4) Å, b = 6.3289(2) Å, c = 5.6854(2) Å, Z = 2, R1 = 0.065, wR2 = 0.176). Its solid-state molecular structure consists of a tungsten centre bound to three chloride ligands and three linear nitrosyl ligands in a fac-octahedral stereochemistry. In addition, the structure contains a crystallographically imposed mirror plane. The two independent W—N linkages are 1.88(2) and 1.92(1) Å long, while the two corresponding N—O bond lengths are 1.13(2) and 1.16(2) Å. DFT calculations on fac-W(NO)3Cl3 at the B3LYP/LANL2DZ level of theory afford optimized intramolecular metrical parameters that match the X-ray crystallographically determined bond lengths and bond angles quite well. In addition, they provide a rationale for the nearly linear W-N-O linkages extant in the complex. Solutions of fac-W(NO)3Cl3 in CH2Cl2 lose ClNO under ambient conditions and deposit the well-known [W(NO)2Cl2]n polymer, and this conversion is fully reversible.Key words: nitrosyl, tungsten, structure, bonding.

scholarly journals Synthesis and Structure Features of Tetraphenylantimony 2,3-Difluoro- and 2,3,4,5,6-Pentafluorobenzoate

2020 ◽  
Vol 12 (4) ◽  
pp. 51-62
Author(s):  
A. Efremov ◽  
Keyword(s):  
Diffraction Analysis ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths ◽  
Trigonal Bipyramidal ◽  
Cambridge Crystallographic Data Center ◽  
Redistribution Reaction ◽  
Distorted Trigonal Bipyramidal Coordination ◽  
Distorted Trigonal Bipyramidal

Tetraphenylantimony 2,3-difluorobenzoate (1) and tetraphenylantimony 2,3,4,5,6-pentafluorobenzoate (2) was obtained by the interaction of pentaphenylantimony with 2,3-difluorobenzoic and 2,3,4,5,6-pentafluorobenzoic acids in benzene with a yield of up to 98 %. The compounds were also synthesized by the ligand redistribution reaction between pentaphenylantimony and triphenylantimony dicarboxylates. The compounds have been identified by IR spectroscopy and X-ray diffraction analysis. According to the X-ray diffraction data, the antimony atoms in compounds 1 and 2 have a distorted trigonal-bipyramidal coordination with the oxygen atom in axial positions. X-ray diffraction analysis was performed on a D8 QUEST diffractometer (Bruker). The crystallographic parameters of the unit cell of the compounds: 1 space group Р1 ̅, а = 9.857(5), b = 10.154(7), c = 14.362(11) Å, α = 83.74(4)°, β = 82.59(3), γ = 68.34(2)°, V = 1321.9(16) Å3, ρcalc = 1.475 g/cm3, Z = 2; 2 space group Р21/с, а = 16.186(9), b = 8.771(6), c = 20.413(13) Å, α = 90.00°, β = 113.073(17), γ = 90.00°, V = 2666(3) Å3, ρcalc = 1.597 g/cm3, Z = 4. The OSbO axial angles are slightly different and amount to 177.90(5)º in 1 and 179.00(5)º in 2. The sums of the CSbC equatorial angles are 356.89(9)º (1), 355.85(7)º (2). The Sb–Ceq distances in compounds 1 and 2 are 2.116(2), 2.119(2), 2.118(2) and 2.1073(17), 2.1158(18), 2.1152(19) Å respectively, which are significantly shorter than the Sb–Сax bond lengths (2.169(2) and 2.1617(19) Å). The organization of molecules in the crystals of compounds is due to hydrogen bonds and CHπ-interactions of the aryl and carboxyl ligands. The main difference between structures 1 and 2 is the different Sb–O bond lengths (2.2864(18) and 2.3168(18) Å), which is due to an increase in the electronegativity of the carboxyl ligand in 2, caused by the presence of five electronegative fluorine atoms in the benzoate substituent. Complete tables of atom coordinates, bond lengths and valence angles are deposited at the Cambridge Crystallographic Data Center (No. 1980908 (1); 1977189 (2); [email protected]; http://www.ccdc.cam.ac.uk/data_request/cif).

Molecular and Crystal Structure of Chlorido[2-(N,N,N',N'- tetramethylamidinio)ethynido]silver

2013 ◽  
Vol 68 (5-6) ◽  
pp. 687-692
Author(s):  
Werner Weingärtner ◽  
Gerhard Maas
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Diffraction Analysis ◽  
Quantum Chemical Calculations ◽  
Quantum Chemical ◽  
Silver Complex ◽  
State Structure ◽  
X Ray Diffraction ◽  
X Ray ◽  
Bond Lengths

The solid-state structure of chlorido[2-(N,N,N',N'-tetramethylamidinio)ethynido]silver (3), obtained by C(sp)-metalation of N,N,N',N'-tetramethyl-propiolamidinium chloride with silver(I) oxide, has been determined by X-ray diffraction analysis. A comparison of bond lengths in the propiolamidinium moiety with those of the two genuine propiolamidinium salts 4 and 5, as well as with data for the isolated N,N,N',N'-tetramethyl-propiolamidinium cation obtained by quantum-chemical calculations, has been made. It can be concluded that complex 3 is better described as a (tetramethylamidinio) ethynyl than as a 3,3-bis(dimethylamino)allenylidene silver complex

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