Metal-Complexes of Thiocholinate, -SCH2CH2Nme3+. I. Preparation and Crystal-Structure of Pentakis(Thiocholinato)Dilead(II) Hexafluorophosphate

1986 ◽  
Vol 39 (3) ◽  
pp. 383 ◽  
Author(s):  
IG Dance ◽  
PJ Guerney ◽  
AD Rae ◽  
ML Scudder ◽  
AT Baker
Keyword(s):  
Crystal Structure ◽  
Fourier Transform ◽  
Aqueous Solutions ◽  
Electron Pair ◽  
Stacking Faults ◽  
Water Soluble ◽  
Lead Atom ◽  
Crystal Data ◽  
Linear Chains ◽  
Bonding Electron

Aqueous solutions containing lead(II) and deprotonated thiocholine contain water-soluble homoleptic lead thiolates , which crystallize as yellow needles of [Pb2(SCH2CH2NMe3)5] (PF6)4 in the presence of PF6-, but crystallize [ Pb (SCH2CH2NMe3)2](ClO4)2 with 1 : 2 stoichiometry in the presence of ClO4-. Crystalline [Pb2(SCH2CH2NMe3)5](PF6)4 contains almost linear chains composed of end-linked {(SR)2Pb(μ-SR) Pb (SR)2} coordination units, within which the primary Pb -S coordination (mean 2.73 Ǻ, sample e.s.d . 0.10 Ǻ) is orthogonal trigonal (S- Pb -S, mean 88.9°, sample e.s.d .3.7°) at each lead atom. Within the {Pb2(SR)5} unit there is one double bridge with two rimary bonds, and one double bridge involving one secondary Pb --S connection (mean 3.23 Ǻ, sample e.s.d . 0.12 Ǻ). Three double-bridges involving secondary Pb --S coordination link the ends of the dimetallic units, and consequently bis - and tris -double thiolate bridges alternate along the chain. Overall coordination at each lead atom is pseudo-octahedral, with one non-bonding electron pair and two cis secondary Pb --S bonds. The cationic tails of the ligands radiate from the chains into a matrix of PF6- ions, and the chains are approximately hexagonally close-packed with a separation of 14.4 Ǻ. Along the b axis there are homogeneous stacks of the ammonium functions, the anions, and the Pb, S chains, with a pseudo-symmetric repeat of b/3 in each stack, allowing disorder due to stacking faults. This disorder has been adequately modelled in the refinement, which also incorporated back-Fourier-transform techniques to avoid inaccuracies due to spherically disordered PF6- ions. Crystal data: Cc, 25.535(8), b 43.13(1), c 15.123(5)Ǻ, β 100.36(9)°, Z 12 (× Pb2S5C25H65N5P4F24), 3585 observed data, R 0.066.

scholarly journals Einkristallzüchtung und Röntgenstrukturanalyse polymerer 1:1-Komplexe von CuBr2 und CuCl2 mit Pyrazin aus Gelen / Crystal Growth in Gels and X-Ray Characterization of Polymeric 1:1-Complexes of CuBr2 and CuCl2 with Pyrazine

1989 ◽  
Vol 44 (5) ◽  
pp. 553-556 ◽  
Author(s):  
Th. Fetzer ◽  
A. Lentz ◽  
T. Debaerdemaeker
Keyword(s):  
Crystal Structure ◽  
Thermal Decomposition ◽  
Crystal Growth ◽  
Chloro Complex ◽  
Monoclinic Space Group ◽  
Crystal Data ◽  
Space Group ◽  
X Ray ◽  
Linear Chains

Single crystals of Cu(pz)Br2 and Cu(pz)Cl2 were grown by using gel methods with tetramethoxysilane as the gel-forming reagent. Thermal decomposition is interpreted. Crystal data for the bromo complex: monoclinic, space group C2/m with a = 1239.2(3) pm, b = 685.9(2) pm, c = 390.7(3) pm, β = 96,23(5)°. Crystal data for the chloro-complex: monoclinic, space group C2/m with a = 1197.1(3) pm, b = 684.9(3) pm, c = 370.1(3) pm, β = 95.96(5)°. Crystal structure analyses reveal that CuHal2 molecules are bonded by pyrazine to form linear chains. These chains are cross-linked by bridging halogen atoms.

Über Hexaiodoplatinate(IV) M2PtI6 (M = K, Rb, Cs, NH4, Tl) Darstellungsverfahren, Eigenschaften und Kristallstrukturen / On Hexaiodoplatinates(IV) M2PtI6 (M = K, Rb, Cs, NH4, Tl) -Preparation, Properties and Structural Data

1983 ◽  
Vol 38 (8) ◽  
pp. 905-910 ◽  
Author(s):  
Gerhard Thiele ◽  
Christian Mrozek ◽  
Dieter Kämmerer ◽  
Kurt Wittmann
Keyword(s):  
Aqueous Solutions ◽  
Single Crystal ◽  
Structural Parameters ◽  
Structural Data ◽  
Structure Type ◽  
Water Soluble ◽  
Crystal Data ◽  
Soluble Salts ◽  
Concentrated Aqueous Solutions ◽  
Distorted Version

Crystals of hexaiodoplatinates(IV) M2PtIe (M = K, Rb, Cs, NH4, Tl) have been obtained by heating PtI4 or H2FtCl6 in highly concentrated aqueous solutions of MI in the presence of small amounts of HI and I2 in an ampoule for 24 h at 160 °C. The structural parameters were determined from single crystal data. In water less soluble compounds with M = Rb, Cs, NH4 show the cubic K2PtCl6 structure, whereas the easily water soluble salts with M = K, Tl both crystallize in a tetragonally distorted version of this structure type.

Al2Sb2I12: Vierkern-Einheiten in einem 1:1-Addukt aus AlI3 und SbI3 / Al2Sb2I12: Tetrameric Units in a 1:1 Adduct of AlI3 and SbI3

1983 ◽  
Vol 38 (12) ◽  
pp. 1539-1542 ◽  
Author(s):  
Siegfried Pohl
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Least Squares ◽  
Electron Pair ◽  
Monoclinic Space Group ◽  
X Ray ◽  
Layer Structures ◽  
R Value ◽  
Stereochemical Activity ◽  
Bonding Electron

Al2Sb2I12 (1) was prepared by heating stoichiometric amounts of AlI3 and SbI3 in CS2. The crystal structure of 1 was determined from single crystal X-ray data. The compound crystallizes in the monoclinic space group C2/m with a = 1644.0(3), b = 1318.3(2), c = 728.9(1) pm, β = 119.33(1)°, and Z = 2. The structure was refined by least squares methods to a final unweighted R value of 0.064 for 676 nonequivalent reflections.The structure is built up of Al2Sb2I12 units in which two Sb-I octahedra share four common edges with two Al-I tetrahedra. As a consequence of the stereochemical activity of the non-bonding electron pair of antimony these cations are displaced from the centers of the iodine octahedra so that three different Sb-I bonds with distances of 270.8, 312.3, and 358.9 pm are observed in 1. The structure of Al2Sb2I12 can also be derived from the layer structures of the BiI3 type

Lead thiolates. The formation of water-soluble lead(II) thiolates and the crystal structure of 2-(Morpholin-4-yl)ethanethiolatolead(II) nitrate

1981 ◽  
Vol 34 (1) ◽  
pp. 57 ◽  
Author(s):  
IG Dance ◽  
PJ Guerney
Keyword(s):  
Crystal Structure ◽  
Nitrogen Atom ◽  
Aqueous Media ◽  
Water Soluble ◽  
Crystal Data ◽  
Conjugate Acid ◽  
Thiolate Ligand ◽  
Tertiary Nitrogen Atom ◽  
Thiolate Complexes ◽  
Tertiary Nitrogen

The solubilized thiolate ligand 2-(morpholin-4-yl)ethanethiolate, mes, and its ammonium conjugate acid, Hmes, form crystalline complexes Pb2(Hmes)3(N03)4, Pb(mes)2, Pb(mes)(N03), Pb(mes)- (O2CCH3) and Pb(mes)(O2CCF3). These lead(II) thiolate complexes are soluble in aqueous media. Crystals of Pb(mes)(NO3) contain chains of alternating lead and bridging thiolate sulfur atoms [Pb-S 2.646(4), 2.793(4) �], with the lead coordinated also by the tertiary nitrogen atom [Pb-N 2.61(1) �]. The nitrate ions weakly bridge lead atoms along the chain [Pb-O 2.69(2), 2.88(2), 2.98(2), 3.03(2) �]. Crystal data: Pbca, a l3.396(2), b 21.900(3), c 7.348(1) �, Z 8(x PbSN2O4- C6H12), 1602 observed data, R 0.057.

scholarly journals Molekül- und Kristallstruktur von 1.1-Dimethylsilylentitanocendichlorid, (CH3)2Si(C5H4)2TiCl2 / Molecular and Crystal Structure of l,r-Dimethylsilylene Titanocene Dichloride, (CH3)2Si(C5H4)2TiCl2

1981 ◽  
Vol 36 (10) ◽  
pp. 1208-1210 ◽  
Author(s):  
Hartmut Köpf ◽  
Joachim Pickardt
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Structure Determination ◽  
Titanocene Dichloride ◽  
Molecular And Crystal Structure ◽  
Monoclinic Space Group ◽  
Crystal Data ◽  
Space Group ◽  
X Ray ◽  
Structural Dimensions

Abstract The molecular structure of the bridged [1]-titanocenophane 1,1'-dimethylsilylene titanocene dichloride, (CH3)2Si(C5H4)2TiCl2, has been investigated by an X-ray structure determination. Crystal data: monoclinic, space group C2/c, Z = 4, a = 1332.9(3), 6 = 988.7(3), c = 1068.9(3) pm, β = 113.43(2)°. The results are compared with the structural dimensions of similar compounds: 1,1'-methylene titanocene dichloride, CH2(C5H4)TiCl2, with the unbridged titanocene dichloride, (C5H5)2TiCl2 and the ethylene-bridged compound (CH2)2(C5H4)2TiCl2

Effect of solution acidity on the crystallization of polychromates in uranyl-bearing systems: synthesis and crystal structures of Rb2[(UO2)(Cr2O7)(NO3)2] and two new polymorphs of Rb2Cr3O10

2021 ◽  
Vol 236 (1-2) ◽  
pp. 11-21
Author(s):  
Evgeny V. Nazarchuk ◽  
Oleg I. Siidra ◽  
Dmitry O. Charkin ◽  
Stepan N. Kalmykov ◽  
Elena L. Kotova
Keyword(s):  
Crystal Structure ◽  
Aqueous Solutions ◽  
Crystal Structures ◽  
Hydrothermal Treatment ◽  
Ambient Conditions ◽  
Screw Axis ◽  
3D Framework ◽  
Solution Acidity

Abstract Three new rubidium polychromates, Rb2[(UO2)(Cr2O7)(NO3)2] (1), γ-Rb2Cr3O10 (2) and δ-Rb2Cr3O10 (3) were prepared by combination of hydrothermal treatment at 220 °C and evaporation of aqueous solutions under ambient conditions. Compound 1 is monoclinic, P 2 1 / c $P{2}_{1}/c$ , a = 13.6542(19), b = 19.698(3), c = 11.6984(17) Å, β = 114.326(2)°, V = 2867.0(7) Å3, R 1 = 0.040; 2 is hexagonal, P 6 3 / m $P{6}_{3}/m$ , a = 11.991(2), c = 12.828(3) Å, γ = 120°, V = 1597.3(5) Å3, R 1 = 0.031; 3 is monoclinic, P 2 1 / n $P{2}_{1}/n$ , a = 7.446(3), b = 18.194(6), c = 7.848(3) Å, β = 99.953(9)°, V = 1047.3(7) Å3, R 1 = 0.037. In the crystal structure of 1, UO8 bipyramids and NO3 groups share edges to form [(UO2)(NO3)2] species which share common corners with dichromate Cr2O7 groups producing novel type of uranyl dichromate chains [(UO2)(Cr2O7)(NO3)2]2−. In the structures of new Rb2Cr3O10 polymorphs, CrO4 tetrahedra share vertices to form Cr3O10 2− species. The trichromate groups are aligned along the 63 screw axis forming channels running in the ab plane in the structure of 2. The Rb cations reside between the channels and in their centers completing the structure. The trichromate anions are linked by the Rb+ cations into a 3D framework in the structure of 3. Effect of solution acidity on the crystallization of polychromates in uranyl-bearing systems is discussed.

THE SOLUBLE PROTEINS OF THE MUSCLE TISSUE OF THE HADDOCK

1931 ◽  
Vol 6 (1) ◽  
pp. 1-11 ◽  
Author(s):  
J. F. LOGAN
Keyword(s):  
Sodium Chloride ◽  
Aqueous Solutions ◽  
Muscle Tissue ◽  
Soluble Protein ◽  
Potassium Phosphate ◽  
Extraction Methods ◽  
Water Soluble ◽  
Tabular Form ◽  
Water Soluble Protein ◽  
Isoelectric Points

As a contribution to the chemistry of muscle tissue, the solubility of the protein of haddock muscle in aqueous solutions of sodium chloride and neutral potassium phosphate, respectively, was determined. The results are expressed in tabular form and graphically in the form of solubility curves. A water-soluble protein and also a salt-soluble protein were isolated from dialyzed haddock muscle by extraction methods. These proteins were obtained in a comparatively pure condition by precipitation from solution in the region of their isoelectric points.

Application of a synthetic water-soluble poly( N -maleyl glycine- co -acrylamide) as polychelatogen for inorganic ions in aqueous solutions

1998 ◽  
Vol 41 (6) ◽  
pp. 687-694 ◽  
Author(s):  
G. del C. Pizarro ◽  
O. G. Marambio ◽  
B. L. Rivas ◽  
K. E. Geckeler
Keyword(s):  
Aqueous Solutions ◽  
Inorganic Ions ◽  
Water Soluble ◽  
Soluble Poly ◽  
Synthetic Water
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