Cluster chemistry. V. Reactions between [Ru3(CO)11(CNBut)] and [Pt(η-C2H4)(PPh3)2] and related chemistry : Crystal and molecular structures of Di-μ-carbonyl-[μ-carbonyl-bis {(triphenylphosphine)platinum}]dicarbonyl(triphenylphosphine)ruthenium(2Ru-Pt)(Pt-Pt), [RuPt2(CO)5(PPh3)3], and its benzene solvate

1982 ◽  
Vol 35 (4) ◽  
pp. 687 ◽  
Author(s):  
MI Bruce ◽  
JG Matisons ◽  
BW Skelton ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Room Temperature ◽  
Molecular Structures ◽  
X Ray Diffraction ◽  
Cluster Chemistry ◽  
X Ray ◽  
Crystal And Molecular Structures ◽  
Analogous Compound ◽  
Benzene Solvate ◽  
Unstable Intermediate

The reaction between [Ru3(CO)11(CNBut)] and [Pt(η-C2H4)(PPh3)2] at -30° affords a thermally unstable intermediate complex (A), which decomposes at room temperature affording, inter alia, [Ru2Pt(CO)7(PPhd3)3 (1), [RuPt2(CO)5(PPh3)3] (2), [RuPt2(CO)6(CNBut)(PPh3)] (5) and [Ru2Pt2- (CO)9(CNBut)(PPh3)] (6). The hexanuclear complexes [Ru2Pt4(CO)5-n(CNBut)(PPh3)4+n] [n = 0 (17) and 1 (18)] are obtained, with [Ru2Pt(CO)5(CNBut)(PPh3)4] (16), from reactions at 80°. Related Ru2Pt and RuPt, complexes are obtained from reactions between complex (A) and CO, CNBut, Pme3, P(C6H4Me-p)3, or P(OMe)3; related reactions between [Ru3(CO)11(CNBut)] and [Pt{P(C6H4Me-p)3}4], and between [Ru3(CO)10(CNBut)2] and [Pt(η-C2H4)(PPh3)2, are also described. The crystal structure of [RuPt2(CO)5(PPh3)3] has been determined by single-crystal X-ray diffraction methods at 295(1) K and refined by least squares to a residual of 0.035 for 6774 'observed' reflections. Crystals are triclinic, P 1, a 15.893(5), b 15.400(5), c 12.651(4) Ǻ, α 57.04(2), β 77.09(3), γ 84.10(3)°, Z 2. Crystals of the dibenzene solvate of the complex are monoclinic, P 21/c, a 11.868(4), b 18.647(8), c 29.24(1) A, β 98.35(3)°, Z 4, the structure being refined to a residual of 0.057 for 4530 'observed' reflections. Ligand dispositions are compared in detail with those observed in the analogous compound previously described with the methyldiphenylphosphine Iigand.

scholarly journals Synthesis and crystal structures of 2-(ferrocenylcarbonyl)benzoic acid and 3-ferrocenylphthalide

2020 ◽  
Vol 76 (7) ◽  
pp. 1163-1167
Author(s):  
Uttam R. Pokharel ◽  
Jonathan T. Bergeron ◽  
Frank R. Fronczek
Keyword(s):  
Crystal Structure ◽  
Benzoic Acid ◽  
Sandwich Structure ◽  
Room Temperature ◽  
Crystal Packing ◽  
Molecular Structures ◽  
X Ray Diffraction ◽  
Centrosymmetric Dimer ◽  
X Ray ◽  
Graph Set

The title compounds, 2-(ferrocenylcarbonyl)benzoic acid, [Fe(C5H5)(C13H9O3)], 1, and 3-ferrocenylphthalide [systematic name: 3-ferrocenyl-2-benzofuran-1(3H)-one], [Fe(C5H5)(C13H9O2)], 2, have been synthesized and structurally characterized by single-crystal X-ray diffraction. The crystal structure of compound 1 was solved recently at room temperature [Qin, Y. (2019). CSD Communication (CCDC deposition number 1912662). CCDC, Cambridge, England]. Here we report a redetermination of its crystal structure at 90 K with improved precision by a factor of about three. The molecular structures of both compounds exhibit a typical sandwich structure. In the crystal packing of compound 1, each molecule engages in intermolecular hydrogen bonding, forming a centrosymmetric dimer with graph-set notation R 2 2 (8) and an O...O distance of 2.6073 (15) Å. There are weak C—H...O and C—H...π interactions in the crystal packing of compound 2. The phthalide moiety in 2 is oriented roughly perpendicular to the ferrocene backbone, with a dihedral angle of 77.4 (2)°.

N,N′-methylenedipyridinium Pt(II) and Pt(IV) hybrid salts: synthesis, crystal and molecular structures of [(C5H5N)2CH2] · [PtCl4] and [(C5H5N)2CH2] · [PtCl6]

2012 ◽  
Vol 66 (11) ◽  
Author(s):  
Mahmoud Al-Ktaifani ◽  
Mwaffak Rukiah
Keyword(s):  
Crystal Structure ◽  
Molecular Structures ◽  
Planar Geometry ◽  
X Ray Diffraction ◽  
Inorganic Hybrid ◽  
X Ray ◽  
Crystal And Molecular Structures ◽  
Square Planar ◽  
Ionic Compounds ◽  
Methylene Group

AbstractThe highly insoluble organic-inorganic hybrid ionic compounds N,N′-methylenedipyridinium tetrachloroplatinate(II) [(C5H5N)2CH2] · [PtCl4] and N,N′-methylenedipyridinium hexachloroplatinate(IV) [(C5H5N)2CH2] · [PtCl6] were obtained by the treatment of N,N′-methylenedipyridinium dichloride monohydrate [(C5H5N)2CH2]Cl2 · H2O with K2[PtCl4] or (NH4)2[PtCl6], respectively, in an aqueous solution. Both complexes were isolated, purified, characterised by elemental analysis, and their molecular structures were confirmed by powder X-ray diffraction. The crystal structure of both compounds consists of separated discrete dications [(C5H5N)2CH2]2+ and anions [PtCln]2− (n = 4 or 6). As anticipated, the dications formed a butterfly shape consisting of two pyridine rings bound to the methylene group via their N atoms, while the Pt centre had a square planar geometry in [(C5H5N)2CH2] · [PtCl4] and an octahedral coordination in [(C5H5N)2CH2] · [PtCl6]. Interestingly, both crystal structures are stabilised by intermolecular C-H…Cl non-standard hydrogen bonds, π-π ring interactions between two pyridine rings of adjacent dications, and also by Cl-π interactions.

Single-crystal X-ray structure determinations of vardenafil, vardenafil dihydrate, vardenafil monohydrochloride trihydrate and vardenafil dihydrochloride hexahydrate

2020 ◽  
Vol 0 (0) ◽  
Author(s):  
Dedong Wu ◽  
Faraj Atassi
Keyword(s):  
Crystal Structure ◽  
Synchrotron Radiation ◽  
Single Crystal ◽  
Molecular Structures ◽  
Free Base ◽  
X Ray Diffraction ◽  
X Ray ◽  
Crystal And Molecular Structures ◽  
Structure Determinations ◽  
Good Agreement

AbstractThe crystal and molecular structures of vardenafil (free, unprotonated base), vardenafil dihydrate and the hydrochloride salts, vardenafil monohydrochloride trihydrate and vardenafil dihydrochloride hexahydrate, were determined by single-crystal X-ray diffraction. The crystal structure of vardenafil monohydrochloride trihydrate is in good agreement with the published crystal structure obtained by powder diffraction using synchrotron radiation. This work shows that the crystal structure of anhydrous vardenafil free base is very similar to the crystal structure of sildenafil free base.

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.

scholarly journals Exploring the Structural Chemistry of Pyrophosphoramides: N,N′,N″,N‴-Tetraisopropylpyrophosphoramide

Chemistry ◽  
2021 ◽  
Vol 3 (1) ◽  
pp. 149-163
Author(s):  
Duncan Micallef ◽  
Liana Vella-Zarb ◽  
Ulrich Baisch
Keyword(s):  
Crystal Structure ◽  
Mass Spectrometry ◽  
Nuclear Magnetic Resonance ◽  
Hydrogen Bonding ◽  
Nmr Spectroscopy ◽  
Ir Spectroscopy ◽  
Room Temperature ◽  
Intermolecular Hydrogen Bonding ◽  
X Ray Diffraction ◽  
X Ray

N,N′,N″,N‴-Tetraisopropylpyrophosphoramide 1 is a pyrophosphoramide with documented butyrylcholinesterase inhibition, a property shared with the more widely studied octamethylphosphoramide (Schradan). Unlike Schradan, 1 is a solid at room temperature making it one of a few known pyrophosphoramide solids. The crystal structure of 1 was determined by single-crystal X-ray diffraction and compared with that of other previously described solid pyrophosphoramides. The pyrophosphoramide discussed in this study was synthesised by reacting iso-propyl amine with pyrophosphoryl tetrachloride under anhydrous conditions. A unique supramolecular motif was observed when compared with previously published pyrophosphoramide structures having two different intermolecular hydrogen bonding synthons. Furthermore, the potential of a wider variety of supramolecular structures in which similar pyrophosphoramides can crystallise was recognised. Proton (1H) and Phosphorus 31 (31P) Nuclear Magnetic Resonance (NMR) spectroscopy, infrared (IR) spectroscopy, mass spectrometry (MS) were carried out to complete the analysis of the compound.

Evolution of crystal structure of dual layered molecular conductor (ET)4ZnBr4(C6H4Cl2) with temperature

CrystEngComm ◽  
2021 ◽  
Author(s):  
Gennady V. Shilov ◽  
Elena I. Zhilyaeva ◽  
Sergey M. Aldoshin ◽  
Alexandra M Flakina ◽  
Rustem B. Lyubovskii ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Electrical Resistivity ◽  
Single Crystal ◽  
Room Temperature ◽  
Organic Conductor ◽  
X Ray Diffraction ◽  
X Ray ◽  
Resistivity Measurements ◽  
Molecular Conductor ◽  
Abrupt Changes

Electrical resistivity measurements of a dual layered organic conductor (ET)4ZnBr4(1,2-C6H4Cl2) above room temperature show abrupt changes in resistivity at 320 K. Single-crystal X-ray diffraction studies in the 100-350 K range...

CRYSTAL STRUCTURE OF ZIRCONIUM TRICHLORIDE

1964 ◽  
Vol 42 (10) ◽  
pp. 1886-1889 ◽  
Author(s):  
B. Swaroop ◽  
S. N. Flengas
Keyword(s):  
Crystal Structure ◽  
Room Temperature ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Main Cell ◽  
Diffraction Patterns

The crystal structure of zirconium trichloride was determined from X-ray diffraction patterns. Zirconium trichloride belongs to the [Formula: see text]space group. The dimensions of the main cell at room temperature are: a = 5.961 ± 0.005 Å and c = 9.669 ± 0.005 Å.The density of zirconium trichloride was measured and gave the value of 2.281 ± 0.075 g/cm3 while, from the X-ray calculations, the value was found to be 2.205 g/cm3.

Lewis-Base Adducts of Group 1B Metal(I) Compounds. XXI The Crystal and Molecular Structures of the Unsolvated Forms of Dibromotris(triphenylphosphine)dicopper(I) and 'step' Tetrabromotetrakis(triphenyl-phosphine)tetracopper(I)

1985 ◽  
Vol 38 (8) ◽  
pp. 1243 ◽  
Author(s):  
JC Dyason ◽  
LM Engelhardt ◽  
C Pakawatchai ◽  
PC Healy ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Crystal Structures ◽  
Molecular Structures ◽  
Lewis Base ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Triphenyl Phosphine ◽  
X Ray ◽  
Crystal And Molecular Structures

The crystal structures of the title compounds have been determined by single-crystal X-ray diffraction methods at 295 K. Crystal data for (PPh3)2CuBr2Cu(PPh3) (1) show that the crystals are iso-morphous with the previously studied chloro analogue, being monoclinic, P21/c, a 19.390(8), b 9.912(5), c 26.979(9) Ǻ, β 112,33(3)°; R 0.043 for No 3444. Cu( trigonal )- P;Br respectively are 2.191(3); 2.409(2), 2.364(2) Ǻ. Cu(tetrahedral)- P;Br respectively are 2.241(3), 2.249(3); 2.550(2), 2.571(2) Ǻ. Crystals of 'step' [PPh3CuBr]4 (2) are isomorphous with the solvated bromo and unsolvated iodo analogues, being monoclinic, C2/c, a 25.687(10), b 16.084(7), c 17.815(9) Ǻ, β 110.92(3)°; R 0.072 for No 3055. Cu( trigonal )- P;Br respectively are 2.206(5); 2.371(3), 2.427(2) Ǻ. Cu(tetrahedral)- P;Br are 2.207(4); 2.446(2), 2.676(3), 2.515(3) Ǻ.

Study of thermal properties of Ga0.5In1.5Se3 by differential scanning calorimetry

2021 ◽  
pp. 2150407
Author(s):  
S. I. Ibrahimova
Keyword(s):  
Crystal Structure ◽  
Differential Scanning Calorimetry ◽  
Thermal Properties ◽  
Thermal Effects ◽  
Room Temperature ◽  
Structural Studies ◽  
X Ray Diffraction ◽  
Hexagonal Symmetry ◽  
Scanning Calorimetry ◽  
X Ray

The crystal structure and thermal properties of the [Formula: see text] compound have been investigated. Structural studies were performed by X-ray diffraction at room temperature. The crystal structure of this compound was found to correspond to the hexagonal symmetry of the space group P61. Thermal properties were studied using a differential scanning calorimetry (DSC). It was found in the temperature range [Formula: see text] that thermal effects occur at temperatures [Formula: see text] and [Formula: see text]. The thermodynamic parameters of these effects are calculated.

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