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.

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.

The first proof of protonated anion tetrahedra in the tsumcorite-type compounds

2004 ◽  
Vol 68 (5) ◽  
pp. 757-767 ◽  
Author(s):  
T. Mihajlović ◽  
H. Effenberger
Keyword(s):  
Crystal Structure ◽  
Hydrothermal Synthesis ◽  
Single Crystal ◽  
Diffraction Data ◽  
Title Compound ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Hydrogen Atoms ◽  
Synthetic Compounds ◽  
X Ray

AbstractHydrothermal synthesis produced the new compound SrCo2(AsO4)(AsO3OH)(OH)(H2O). The compound belongs to the tsumcorite group (natural and synthetic compounds with the general formula M(1)M(2)2(XO4)2(H2O,OH)2; M(1)1+,2+,3+ = Na, K, Rb, Ag, NH4, Ca, Pb, Bi, Tl; M(2)2+,3+ = Al, Mn3+, Fe3+, Co, Ni, Cu, Zn; and X5+,6+ = P, As, V, S, Se, Mo). It represents (1) the first Sr member, (2) the until now unknown [7]-coordination for the M(1) position, (3) the first proof of (partially) protonated arsenate groups in this group of compounds, and (4) a new structure variant.The crystal structure of the title compound was determined using single-crystal X-ray diffraction data. The compound is monoclinic, space group P21/a, with a = 9.139(2), b = 12.829(3), c = 7.522(2) Å, β = 114.33(3)°, V = 803.6(3) Å3, Z = 4 [wR2 = 0.065 for 3530 unique reflections]. The hydrogen atoms were located experimentally.

The Crystal and Molecular Structures of Two Modifications of cis-Dichloro-mer-tris-(dimethylphenylphosphine)hydridoiridium(III)

1988 ◽  
Vol 41 (3) ◽  
pp. 283 ◽  
Author(s):  
GB Robertson ◽  
PA Tucker
Keyword(s):  
Heavy Atom ◽  
Molecular Structures ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths ◽  
Metal Ligand ◽  
Ligand Bond

The structures of two crystalline modifications of mer -(Pme2Ph)3H-cis-Cl2IrIII, (1), have been determined from single-crystal X-ray diffraction data. Modification (A) is monoclinic, space group P21/c with a 12.635(1), b 30.605(3), c 14.992(2)Ǻ, β 110.01(2)° and Z = 8. Modification (B) is orthorhombic, space group Pbca with a 27.646(3), b 11.366(1), c 17.252(2)Ǻ and Z = 8. The structures were solved by conventional heavy atom techniques and refined by full-matrix least- squares analyses to conventional R values of 0.037 [(A), 8845 independent reflections] and 0.028 [(B), 5291 independent reflections]. Important bond lengths [Ǻ] are Ir -P(trans to Cl ) 2.249(1) av. (A) and 2.234(1) (B), Ir -P(trans to PMe2Ph) 2.339(2) av. (A) and 2.344(1), 2.352(1) (B), Ir-Cl (trans to H) 2.492(2), 2.518(2) (A) and 2.503(1) (B) and Ir-Cl (trans to PMe2Ph)2.452(2) av. (A) and 2.449(1)(B). Differences in chemically equivalent metal- ligand bond lengths emphasize the importance of non-bonded contacts in determining those lengths.

Carbacylamidophosphates: Synthethis and Structure of N,N'-Tetramethyl-NM-benzoylphosphoryltriamide and Dimorpholido-N-benzoylphosphorylamide

2000 ◽  
Vol 55 (6) ◽  
pp. 495-498 ◽  
Author(s):  
Katerina E. Gubina ◽  
Vladimir A. Ovchynnikov ◽  
Vladimir M. Amirkhanov ◽  
Viktor V. Skopenkoa ◽  
Oleg V. Shishkinb
Keyword(s):  
Nmr Spectroscopy ◽  
Hydrogen Bonds ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Hydrogen Atoms ◽  
Sodium Salts ◽  
Space Group ◽  
X Ray ◽  
Centrosymmetric Dimers ◽  
Oxygen Atoms

N,N′-Tetramethyl-N"-benzoylphosphoryltriamide (I) and dimorpholido-N-benzoylphosphorylamide (II), and their sodium salts Nal, Nall were synthesized and characterized by means of IR and 1H, 31P NMR spectroscopy. The structures of I, II were determined by X-ray diffraction: I monoclinic, space group P2i/c with a = 10.162(3), b= 11.469(4), c = 12.286(4) Å , β = 94.04°, V = 1428.4(8) A 3, Z = 4, p(calcd) = 1.187 g/cm3; II monoclinic, space group C2/c with a = 15.503(4), b = 10.991(3), c = 22.000(6) Å, β = 106.39°, V = 3596.3(17) Å3, Z = 8, p(calcd.) = 1.253 g/cm3. The refinement of the structures converged at R = 0.0425 for I, and R = 0.068 for II. In both structures the molecules are connected into centrosymmetric dimers via hydrogen bonds formed by the phosphorylic oxygen atoms and hydrogen atoms of amide groups.

The crystal and molecular structure of 1,4-diphenyl-2,2′,3,3′,5,5′,6,6′-octamethylcyclo-1,4-diphospha-2,3,5,6-tetrasilahexane, a phosphorus–silicon heterocycle

1979 ◽  
Vol 57 (2) ◽  
pp. 174-179 ◽  
Author(s):  
A. Wallace Cordes ◽  
Paul F. Schubert ◽  
Richard T. Oakley
Keyword(s):  
Molecular Structure ◽  
Crystal And Molecular Structure ◽  
Direct Methods ◽  
Chair Conformation ◽  
Monoclinic Space Group ◽  
Single Bond ◽  
X Ray Diffraction ◽  
Full Matrix ◽  
X Ray ◽  
Bond Lengths

The crystal structure of 1,4-diphenyl-2,2′,3,3′,5,5′,6,6′-octamethylcyclo-1,4-diphospha-2,3,5,6-tetrasilahexane, (PhPSi2Me4)2, has been determined by single crystal X-ray diffraction. The crystals are monoclinic, space group P21/c, with a = 9.866(1), b = 11.921(1), and c = 11.324(2) Å, β = 104.31(1)°, Z = 2, and ρcalcd = 1.15 g/cm3. The structure was solved by direct methods and was refined by full-matrix least-squares procedures to a final R of 0.060 and Rw of 0.078, for 1173 reflections with intensities greater than 3σ. The (PhPSi2Me4)2 molecule lies on a crystallographic centre of symmetry, and the six-membered P2Si4 ring has a chair conformation with equatorial phenyl groups. The endocyclic angles at P (104.4(1)°) and Si (104.9(2)°) are intermediate between those found in cyclic hexaphosphine and hexasilane molecules, and the Si—Si and P—Si distances of 2.345(3) and 2.252(4) Å, respectively, correspond to single bond lengths, with no appreciable evidence for secondary pπ → dπ bonding between phosphorus and silicon. The Si—C (1.867(8) Å) and P—C (1.828(7) Å) bond lengths are also normal. The variations in the Si—P—C (101.6(2)°, 108.6(2)°), P—Si—C (range 106.2(3)–120.0(3)°), and Si—Si—C (range 105.8(3)–113.7(3)°) angles indicate that the positions of the exocyclic methyl and phenyl groups are influenced by both intra- and intermolecular steric forces.

scholarly journals Accurate Bond Lengths to Hydrogen Atoms from Single-Crystal X-ray Diffraction by Including Estimated Hydrogen ADPs and Comparison to Neutron and QM/MM Benchmarks

2017 ◽  
Vol 23 (19) ◽  
pp. 4605-4614 ◽  
Author(s):  
Birger Dittrich ◽  
Jens Lübben ◽  
Stefan Mebs ◽  
Armin Wagner ◽  
Peter Luger ◽  
...  
Keyword(s):  
Single Crystal ◽  
X Ray Diffraction ◽  
Hydrogen Atoms ◽  
X Ray ◽  
Bond Lengths

scholarly journals Darstellung und Kristallstruktur von [(NH3)5Rh(H7O4)Rh(NH3)5](S2O6)2,5 · H2O (1). Ein gemischtes Aquopentamminrhodium(III)-hydroxopentamminrhodium(III)- dithionat mit einer neuartigen μ-H7O4-Struktureinheit / Preparation and Crystal Structure of [(NH3)5Rh(H7O4)Rh(NH3)5](S2O6)2,5 · H2O (1). A Mixed Aquopentaamminerhodium(III)-hydroxopentaamminerhodium(III) Dithionate with a Novel μ-H7O4 Structural Unit

1988 ◽  
Vol 43 (2) ◽  
pp. 189-195 ◽  
Author(s):  
Walter Frank ◽  
Thomas Stetzer ◽  
Ludwig Heck
Keyword(s):  
Crystal Structure ◽  
Structural Unit ◽  
Small Difference ◽  
Point Group ◽  
Group Symmetry ◽  
Monoclinic Space Group ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Hydrogen Atoms ◽  
X Ray

The title compound 1 can be obtained from an aqueous solution of aquopentaammine rhodium(III) dithionate and hydroxopentaammine rhodium(III) dithionate. The crystal structure has been determined from single crystal X-ray diffraction data and refined to R = 0.035 for 4390 unique reflections. Crystal data: monoclinic, space group P21/c, a = 1300.9(5) pm. b = 1472.3(6) pm. c = 1478.8(9) pm, β = 106.20(4)°, Z = 4.In the crystal dinuclear rhodium cations with point group symmetry 1 (C1) are found. A central μ-H3O2-bridge is formed by strong hydrogen bonding between aquo and hydroxo ligands; this bridge is additionally coordinated by two molecules of water. The entire bridging system is therefore H7O4-(H3O2- · 2 H2O). O-O distances characterizing the strength of the three hydrogen bonds within this new kind of structural unit are O(H2O-Rh 1)-O(HO-Rh2): 248 pm. O(H2O-Rh 1)-O(H2Oa): 273 pm, O(HO-Rh2)-O(H2Ob): 287 pm. The hydrogen atoms involved in these bridges have been located. The small difference in the Rh 1-O(H2O) - (205.4(3) pm) and Rh2-O(OH)- (204.3(3) pm) distances indicates that the entire H7O4-- moiety serves as a μ-bridging unit between Rh 1 and Rh 2

Solvent-assisted planar structure of a stilbene-based salicylhydrazone compound: crystal structure, solvent- and aggregation-induced emission, and switchable luminescence colouration

2020 ◽  
Vol 76 (8) ◽  
pp. 734-740
Author(s):  
Zong-Bin Fang ◽  
Bin Zhang ◽  
Qi-Zheng Yang ◽  
Wenxu Zheng ◽  
Xiao-Lin Hu ◽  
...  
Keyword(s):  
Dimethyl Sulfoxide ◽  
Single Molecule ◽  
Solvent Molecule ◽  
Geometry Optimization ◽  
Planar Structure ◽  
Luminescence Spectroscopy ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Aggregation Induced Emission ◽  
X Ray

A novel stilbene-based salicylhydrazone compound {systematic name: (E)-4,4′-(ethene-1,2-diyl)bis[(N′E)-N′-(2-hydroxybenzylidene)benzohydrazide] dimethyl sulfoxide disolvate, C30H24N4O4·2C2H6OS or L·2DMSO} was synthesized and characterized by single-crystal X-ray diffraction, powder X-ray diffraction and luminescence spectroscopy. The title compound crystallizes in the monoclinic space group P21/c, with half a symmetry-independent L molecule and one dimethyl sulfoxide (DMSO) solvent molecule in the asymmetric unit. The L molecule adopts an almost planar structure, with a small dihedral angle between the planes of the stilbene and salicylhydrazone groups. There are multiple π–π stacking interactions between adjacent L molecules. The DMSO solvent molecules act as proton donors and acceptors, forming hydrogen bonds of various strengths with the L molecules. In addition, the geometry optimization of a single molecule of L and its luminescence properties either in solution, as a solvated solid or as a desolvated solid were studied. The compound shows an aggregation-induced emission (AIE) effect and exhibits switchable luminescence colouration in the solid state by the simple removal or re-addition of the DMSO solvent.

The Crystal Structure of (2,2′-Bipyridine)(pyrazine)(2,2′:6′,2″-terpyridine)ruthenium(II) Hexafluorophosphate

1996 ◽  
Vol 49 (4) ◽  
pp. 527 ◽  
Author(s):  
PT Gulyas ◽  
TW Hambley ◽  
PA Lay
Keyword(s):  
Crystal Structure ◽  
Monoclinic Space Group ◽  
Coordination Geometry ◽  
X Ray Diffraction ◽  
Steric Strain ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths ◽  
Distorted Octahedral ◽  
Back Bonding

The crystal structure of [ Ru ( terpy )( bpy )( pz )] (PF6)2 has been determined by X-ray diffraction methods and refined to a residual of 0.046 for 1855 independent observed reflections. The crystals are monoclinic, space group P 21/a, a 16.836(7), b 10.778(5), c l9.342(5) Ǻ, β 115.11(3)°. The coordination geometry around the ruthenium(II) ion is distorted octahedral, with the various Ru -N bond lengths indicative of considerable interligand steric strain. The Ru -N pyrazine bond is the longest within the structure, consistent with other evidence that n back-bonding to pyrazine is weak in the complex.

Steric Modification of Metal-Phosphorus Bond Lengths: the Preparation, Characterization and CrystalStructures of mer-trans-(PPri3)2(Pme2Ph)-Cl-cis-H2IrIII(1) and mer-trans-(PPri3)2(PMe2Ph)H3IrIII

1995 ◽  
Vol 48 (6) ◽  
pp. 1183 ◽  
Author(s):  
EJ Ditzel ◽  
GB Robertson
Keyword(s):  
Chloride Content ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths ◽  
Steric Crowding ◽  
Unit Increase

The syntheses and subsequent characterization of the complexes mer -trans-(PPri3)2(Pme2Ph)-Cl-cis-H2IrIII(1) and mer-trans-(PPri3)2(PMe2Ph)H3IrIII (2) by n.m.r. and by low temperature (153�5 K) X-ray diffraction analyses are reported. Crystals of (1) are monoclinic, space group P21/c with a 19.277(2), b 9.020(1), c 17.657(2) Ǻ, β 101.40(1)° and Z 4. Crystals of (2) are orthorhombic, space group P212121, with a 19.373(3), b 18.724(2), c 8.113(1) Ǻ and Z 4. Full-matrix least-squares analyses converged with R = 0.027 and wR = 0.031 for (1) (3243 reflections), and R = 0.030 and wR = 0.038 for (2) (2892 reflections). Consistent with previous observation, the unit increase in chloride content (in place of hydride) in (1) is accompanied by a global lengthening of 0.036 Ǻ (av.) in the Ir -P bond lengths cf. those in (2). Also, because of increased steric crowding (two PPri3 ligands in place of two Pme2Ph), the Ir-PMe2Ph bond in (1) is 0.019(2) Ǻ longer than the chemically equivalent bond in mer-(PMe2Ph)3Cl-cis-H2IrIII. In previously reported complexes in this series metrically similar increases in Ir-PMe2Ph distances result from the replacement of just one Pme2Ph ligand by PPri3.

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