A refinement of the crystal structures of K2ReCl6, K2ReBr6, and K2PtBr6

1970 ◽  
Vol 48 (7) ◽  
pp. 1151-1154 ◽  
Author(s):  
H. D. Grundy ◽  
I. D. Brown
Keyword(s):  
Single Crystal ◽  
Crystal Structures ◽  
Root Mean Square ◽  
Mean Square ◽  
X Ray ◽  
Bond Lengths ◽  
Using Data

The crystal structures of K2ReCl6, K2ReBr6, and K2PtBr6 have been refined using data collected on a single-crystal X-ray diffractometer to give weighted agreement indices ranging from 0.026 to 0.054 for 75 to 90 nonequivalent reflections. The following bond lengths were obtained: Re—Cl = 235 pm, Re—Br = 248 pm, Pt—Br = 246 pm, K—Cl = 348 pm, and K—Br = 367 and 364 pm in the Re and Pt compounds, respectively. The differences in the root-mean-square angles of libration of the MX62− ions in these and a number of isomorphous crystals are discussed.

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.

Lewis-Base Adducts of Group 11 Metal(I) Compounds. LIX. Crystal Structure Determinations of Tetrakis(trimethylphosphine)copper(I) Halides and Tetrakis(triphenylphosphine)-copper(I) and -silver(I) Hexafluorophosphates

1990 ◽  
Vol 43 (10) ◽  
pp. 1697 ◽  
Author(s):  
GA Bowmaker ◽  
PC Healy ◽  
LM Engelhardt ◽  
JD Kildea ◽  
BW Skelton ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Crystal Structures ◽  
Lewis Base ◽  
X Ray Diffraction ◽  
Coordination Environment ◽  
X Ray ◽  
Bond Lengths ◽  
Cu Complex ◽  
Structure Determinations

The crystal structures of [Cu(Pme3)4]X (X = Cl , Br, I) and of [M(PPh3)4] [PF6] (M = Cu, Ag) have been determined by single-crystal X-ray diffraction methods at 295 K. The former compounds contain nearly tetrahedral [Cu(PMe3)4]+ ions on sites of m symmetry with mean Cu-P bond lengths of 2.270, 2.271 and 2.278 Ǻ for X = Cl , Br and I respectively. The latter compounds contain [M(PPh3)4]+ ions on sites of 3 symmetry. In the M =Ag complex the coordination environment is close to tetrahedral, but in the M =Cu complex the length of the axial Cu-P bond [2.465(2)Ǻ] is significantly shorter than that of the off-axis bonds [2.566(2)Ǻ]. Possible reasons for this are discussed.

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

Derivate des Hydrazins als Liganden in Vanadium(IV)- und -(V)-Komplexen. Darstellung und Struktur dreier dimerer Verbindungen mit Hydrazido- und Hydrazonato-Liganden / D erivatives of H ydrazine as Ligands in V anadium (IV ) and -(V) Complexes. Synthesis and Crystal Structures of Three D im eric C om plexes with H ydrazido and H ydrazonato Ligands

1995 ◽  
Vol 50 (9) ◽  
pp. 1281-1286 ◽  
Author(s):  
Klaus Kopka ◽  
Rainer Mattes
Keyword(s):  
Single Crystal ◽  
Crystal Structures ◽  
Coordination Geometry ◽  
X Ray Diffraction ◽  
X Ray ◽  
Bond Lengths ◽  
Coordination Sites ◽  
Octadentate Ligand ◽  
Back Donation ◽  
Trigonal Prismatic

AbstractThe complexes [(μ-PhCONNCOPh){VOCl(NHNHCOPh)}2 ·5CH3CN, (1), [(μ-PhCONNCOPh){V(dbh)}2]-2CH3CN, (2) and [{VO}2(tbh)], (3) have been prepared by reaction of VCl2(acac)2, acac = acetylaceto n a to (l-), and VCl2(acpn), acpn = propylendiim ino-bis(acetylacetonato(2-)), with benzoylhydrazine. The structures of the centrosymmetric dimeric molecules 1 -3 have been determined by single crystal X-ray diffraction. 1 and 2 contain both doubly deprotonated N,N′-dibenzoylhydrazine as bridging, doubly N,O chelating ligand. In 1 the two remaining coordination sites at the VOCl group are occupied by the hydrazid o(1-) ligand [NHNHCOPh]- . 2 is a non-oxo vanadium(IV) complex. The coordination geometry is approximately trigonal prismatic. The π-back donating effect of the oxo function is substituted by back donation from three negatively charged enolic oxygen atoms. The V - O bond lengths range from 192.0(2) to 193.7(2) pm. 3 contains a unique highly symmetrical octadentate ligand, formed during the synthesis. It is coordinated to two oxovanadin(IV) centers by N,O chelation. The coordination geometry is square pyramidal.

Formamidinium Salts of Low Valent Metal Halide Anions MX3 – (M = Ge, Sn) and M2X62– (M = Ga, In)

2004 ◽  
Vol 59 (11-12) ◽  
pp. 1524-1531 ◽  
Author(s):  
Xin Tian ◽  
Tania Pape ◽  
Norbert W. Mitzel
Keyword(s):  
Hydrogen Bonds ◽  
Single Crystal ◽  
Crystal Structures ◽  
Raman Spectra ◽  
X Ray Diffraction ◽  
X Ray ◽  
Bond Lengths ◽  
Metal Metal ◽  
Weak Hydrogen Bonds ◽  
Low Valent

Tetramethylformamidinium trichlorogermanite, [CH(NMe2)2][GeCl3], tetramethylformamidinium trichlorostannite, [CH(NMe2)2][SnCl3], bis-(tetramethylformamidinium hexaiododigallate, [CH(NMe2)2]2[Ga2I6] and bis-(tetramethylformamidinium hexachlorodiindate, [CH(NMe2)2]2[In2Cl6] have been prepared by the reactions between tetramethylformamidinium chloride, [CH(NMe2)2]Cl, and the corresponding low valent halides GeCl2 (as dioxane adduct), SnCl2, “GaI” and InCl. Their crystal structures have been determined by single crystal X-ray diffraction. [CH(NMe2)2][GeCl3] aggregates in a centrosymmetric dimeric structure, in which two trigonal pyramidal GeCl3 units are connected together by two weak Ge···Cl bonds and each Ge atom is bonded to one cation by a weak Ge···N contact. Two sets of weak hydrogen bonds C-H···Cl are observed with bond lengths of 2.87(2) Å and 2.85(2) Å . In [CH(NMe2)2][SnCl3], the SnCl3 − units adopts a (3+3) coordination with three normal Sn-Cl bonds and three weak Sn···Cl contacts. [CH(NMe2)2]2[Ga2I6] and [CH(NMe2)2]2[In2Cl6] contain metal-metal bonded anions with distorted staggered ethane-like conformations. The metal-metal bond lengths are 2.423(1) Å (Ga-Ga) and 2.719(1) Å (In-In). Their Raman spectra contain intense bands at 118.7 cm−1(Ga-Ga) and 174.7 cm−1(In-In) associated with metal-metal stretching modes.

Darstellung und Kristallstrukturen von LiGaCl4 und LiGaI4/ Preparation and Crystal Structure of LiGaCL4 and LiGaI4

1987 ◽  
Vol 42 (2) ◽  
pp. 248-250 ◽  
Author(s):  
Wolfgang Hönle ◽  
Bernhard Hettich ◽  
Arndt Simon
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Crystal Structures ◽  
X Ray ◽  
Common Features ◽  
Bond Lengths ◽  
Ray Methods

Abstract The crystal structures of LiGaCl4 and LiGaI4 have been determined by single crystal X-ray methods. Both compounds are isotypic with LiAlCl4 and characterized by LiX6 octahedra and GaX4 tetrahedra. Mean bond lengths are: d̄(Ga-X) = 217.4 pm (Cl) and 255.9 pm (I); d̄(Li-X) = 263.9 pm (Cl) and 305.3 pm (I), respectively. Common features of the isotypic compounds LiGaX4 (X = Cl, Br. I) are discussed.

Syntheses and Structures of Two Arene-Ruthenium(II) Complexes with Cyclometalating 2-Pyridyl-m-tolyl Ligands

2007 ◽  
Vol 62 (5) ◽  
pp. 675-678
Author(s):  
Xiu-Zhen Zhang ◽  
Wen-Rui Yao ◽  
Qian-Feng Zhang ◽  
Wa-Hung Leung
Keyword(s):  
Single Crystal ◽  
Crystal Structures ◽  
X Ray Diffraction ◽  
X Ray ◽  
Bond Lengths ◽  
Ruthenium Atom ◽  
Octahedral Configuration

Abstract Reactions of [(η6-C6Me6)RuCl2]2 and [(η6-p-cymene)RuCl2]2 with [Hg(ptpy)2] (Hptpy = 2-pyridyl-m-toluene) in THF afforded [{(η6-C6Me6)Ru(ptpy)}2(μ-Hg2Cl6)] 1 and [(η6-pcymene) Ru(ptpy)(HgCl3)] 2, respectively. The crystal structures of complexes 1 and 2 have been determined by single-crystal X-ray diffraction. The ruthenium atom in both molecules 1 and 2 adopts a pseudo octahedral configuration containing a cyclometalated ptpy ligand. The Ru−C(ptpy) and Ru−N bond lengths in 1 are 2.049(3) and 2.089(2) Å, respectively. The corresponding bond lengths for 2 are 2.025(9) and 2.089(7) Å .

Crystal structures of rac- and meso-o-Phenylenebis(iodomethylarsine), the latter as its lattice complex with the methiodide of 1,3-Dimethyl-1,3-dihydro-2,1,3-benzoxadiarsole

1977 ◽  
Vol 30 (11) ◽  
pp. 2417 ◽  
Author(s):  
K Henrick ◽  
CL Raston ◽  
AH White ◽  
SB Wild
Keyword(s):  
Charge Transfer ◽  
Single Crystal ◽  
Least Squares ◽  
Crystal Structures ◽  
X Ray Diffraction ◽  
X Ray ◽  
Bond Lengths ◽  
Iodine Species ◽  
Iodide Anion ◽  
The Mean

The crystal structures of the title compounds, o-C6H4(AsMeI)2 (1), and o- C6H4(AsMeI)2- [o-C6H4(AsMe)(As+Me2)O] I- (2), have been determined at 295 K by single-crystal X-ray diffraction and refined by least squares to residuals of 0.037 and 0.067 for 2095 and 2913 reflections respectively. Crystals of (1) are triclinic, Pī, a 9.865(5), b 9.837(7), c 7.765(4) Ǻ, α 98.89(5), β 96.71(4), γ 60.72(4)�, Z 2. <As- I> is 2.585 Ǻ and <As-C> 1.97 Ǻ. The angles about the arsenic differ only trivially, the mean being 98.4�. Crystals of (2) are monoclinic, P21/n, a 15.315(4), b 21.511(8), c 7.952(2) Ǻ, β 98.19(2)�, Z 4. In the cation As-O distances are unequal [1.75(1) (quaternary As), 1.86(2) Ǻ]; As-O-As is very small being 115.8(8)�. Charge-transfer interactions between iodine species are present in both derivatives; in (2), there is an interaction between the tertiary arsenics of the meso molecule and the iodide anion, As...I being 3.307(3), 3.551(3) Ǻ, with the geometry of the arsenics approaching that of a tetrahedral disposition. Within the cation, the geometry about the quaternary arsenic is typical of arsenic(v), the bond lengths being shorter than those about the ternary arsenic.

scholarly journals Ni(II) complexes with thioether-functionalized silylamide ligands. Synthesis and crystal structures of [Ni{Me2Si(N-C6H4-2-S-t-Bu)2}], [Ni{Ph2Si(N-C6H4-2-SMe)2}] and [Ni{Ph2Si(N-C6H4-2-SPh)2}]

2019 ◽  
Vol 74 (2) ◽  
pp. 233-240 ◽  
Author(s):  
Ralf Albrecht ◽  
Phil Liebing ◽  
Uwe Morgenstern ◽  
Christoph Wagner ◽  
Kurt Merzweiler
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Crystal Structures ◽  
Nickel Complexes ◽  
Subsequent Reaction ◽  
X Ray ◽  
Bond Lengths ◽  
Tetradentate Ligands ◽  
Square Planar ◽  
Structure Determinations

AbstractThioether-functionalized aminosilanes R2Si(NH-C6H4-2-SR′)2 with R=Me, Ph and R′=t-Bu, Me, Ph were synthesized from the corresponding dichlorosilanes R2SiCl2 and lithiated aniline derivatives LiNH-C6H4-2-SR′. Treatment of the functionalized aminosilanes R2Si(NH-C6H4-2-SR′)2 with two eq. of n-BuLi and subsequent reaction with nickel(II) halides NiX2 (X=Cl, Br) or [Ni(acac)2(TMEDA)] led to the formation of the Ni(II) complexes [Ni{R2Si(N-C6H4-2-SR′)2}]. The X-ray single-crystal structure determinations of the nickel complexes revealed that the thioether-functionalized silylamides R2Si(NC6H4-2-SR′)22− act as tetradentate ligands. The nickel atoms exhibit a distorted square-planar coordination with Ni–N and Ni–S bond lengths in the range of 186.4(3)–186.9(2) pm and 217.5(1)–221.5(1) pm, respectively.

scholarly journals M + M 3+ 2As(HAsO4)6 (M + M 3+ = TlGa, CsGa, CsAl): three new metal arsenates containing AsO6 octahedra

2018 ◽  
Vol 74 (8) ◽  
pp. 1163-1167 ◽  
Author(s):  
Karolina Schwendtner ◽  
Uwe Kolitsch
Keyword(s):  
Single Crystal ◽  
Crystal Structures ◽  
Structure Type ◽  
X Ray Diffraction ◽  
X Ray ◽  
Bond Lengths ◽  
New Compounds ◽  
Metal Arsenates

The crystal structures of hydrothermally synthesized (T = 493 K, 7 d) thallium(I) digallium arsenic(V) hexakis[hydrogenarsenate(V)], TlGa2As(HAsO4)6, caesium digallium arsenic(V) hexakis[hydrogenarsenate(V)], CsGa2As(HAsO4)6, and caesium dialuminium arsenic(V) hexakis[hydrogenarsenate(V)], CsAl2As(HAsO4)6, were solved by single-crystal X-ray diffraction. The three compounds are isotypic and adopt the structure type of RbAl2As(HAsO4)6 (R\overline{3}c), which itself represents a modification of the RbFe(HPO4)2 structure type and consists of a tetrahedral–octahedral framework in which the slightly disordered M + cations are located in channels. The three new compounds contain AsO6 octahedra assuming the topological role of M 3+O6 octahedra. The As—O bond lengths are among the shortest As—O bond lengths known so far in AsO6 octahedra.

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