Crystal Structures of the ('Maximally') Hydrated Scandium Halides, ScX3.nH2O (X = Cl, Br, I)

2000 ◽  
Vol 53 (10) ◽  
pp. 875 ◽  
Author(s):  
Kevin C. Lim ◽  
Brian W. Skelton ◽  
Allan H. White
Keyword(s):  
Low Temperature ◽  
Water Molecule ◽  
Single Crystal ◽  
Crystal Structures ◽  
Metal Atom ◽  
Coordination Sphere ◽  
Monoclinic Space Group ◽  
Site Symmetry ◽  
X Ray ◽  
Structure Determinations

Low-temperature single-crystal X-ray structure determinations are recorded for the (‘maximally’) hydrated scandium(III) trihalides, ScX3.nH2O (X = Cl, Br, I). The chloride and bromide are isomorphous heptahydrates (n =7), ScX3.7H2O =[Sc(OH2)7]X3, monoclinic, space group P2/n, a ~ 7.6, b ~ 7.7, c ~ 9.6 Å, β ~ 99˚, Z = 2, R 0.051, 0.039 for No 1253, 1339 ‘observed’ (F > 4σ (F)) reflections, respectively, the metal atom disposed in a homoleptic environment of seven water molecule oxygen atoms arranged in an essentially pentagonal-bipyramidal disposition, site symmetry 2, Sc–O(axial) 2.095 Å, Sc–O(eq) 2.157(3)–2.209(4) Å. The iodide is an octahydrate, ScI3.8H2O =[Sc(OH2)7]I3.H2O, monoclinic P21/c, Z = 4, R 0.022 for No 3243; the seven-coordinate metal atom environment here is well distorted from the pentagonal-bipyramidal norm, the largest angle in the coordination sphere being 162.4(1)˚, subtended by Sc–O 2.109(3), 2.128(3) Å, the remaining Sc–O ranging between 2.157(3)–2.219(3) Å.

Crystal-Structures of (Nh4)2(AgI3)∞/ ∞.H2O And (Nme4)(Ag2I3)∞/∞

1986 ◽  
Vol 39 (1) ◽  
pp. 171 ◽  
Author(s):  
JD Kildea ◽  
BW Skelton ◽  
AH White
Keyword(s):  
Water Molecule ◽  
Single Crystal ◽  
Crystal Structures ◽  
X Ray ◽  
Structure Determinations

Single-crystal X-ray structure determinations of the title compounds at 295 K are reported. For (1), (NH4)2(AgI3)∞/∞.H2O, the structure is isomorphous with that reported previously for K2AgI3, being orthorhombic, Pbnm , a 21.20(2), b 10.84(1), c 4.629(3)Ǻ, Z 4, R 0.032 for 1211 'observed' independent reflections. Locations and refinement of an artefact modelled as a water molecule raises the possibility that other members of the isomorphous series may be monohydrates rather than anhydrous. (NMe4)(Ag2I3)∞/∞, (2), is orthorhombic, Pnam , a 17.760(7), b 10.077(4), c 7.431(2)Ǻ, Z 4, R 0.043 for 977 'observed' independent reflections; the structure is a redetermination of better precision confirming the essential features of an earlier study and treating the cation in terms of an ordered rather than a disordered model.

Comparative Structural Studies on Three-Coordinate Copper(I) Halide Complexes With Tertiary Phosphines. Crystal Structures of [(PPh2Mes)CuX]2 and [(PPhMes2)CuX]2 (Mes = Mesityl X = Cl, Br, I)

1992 ◽  
Vol 45 (7) ◽  
pp. 1155 ◽  
Author(s):  
GA Bowmaker ◽  
D Camp ◽  
RD Hart ◽  
PC Healy ◽  
BW Skelton ◽  
...  
Keyword(s):  
Single Crystal ◽  
Crystal Structures ◽  
Copper Atom ◽  
Structural Studies ◽  
Coordination Environment ◽  
X Ray ◽  
Tertiary Phosphines ◽  
Structure Determinations ◽  
Halide Complexes ◽  
The Subject

The 1 : 1 complexes of the substituted triphenylphosphine ligands mesityldiphenylphosphine and dimesitylphenylphosphine with copper(1) chloride, bromide and iodide have been the subject of single-crystal X-ray structure determinations at 295 K. All six complexes crystallize as air-stable dimeric molecules, [(PPh2Mes)CuX]2 and [ (PPhMes2)CUX]2 with each copper atom in a distorted trigonal PCuX2. coordination environment. Crystals of [(PPh2Mes)CuCl]2 (1) are monoclinic, P21/n, a 9.961(3), b 18.687(6), c 11.009(7) Ǻ, β 114.63(4)°; R was 0.049 for 2450 'observed' reflections. [(PPh2Mes)CuBrI2 (2) is monoclinic, P21/n, a 9.939(2), b 18.832(6), c 11.238(6) Ǻ, β 115.36(3)°; R was 0.046 for 1803 'observed' reflections. [(PPh2Mes)CuI]2.4/3 C6H6 (3) is rhornbohedral, R3, a 36.877(8), c 9.047(5) A; R was 0.039 for 2537 'observed' reflections. Crystals of [(PPhMes2)CuCl]2.2MeCN (4) are triclinic, Pi, a 15.783(7), b 9.570(4), c 8.914(4) Ǻ, α 72.43(3), β 76.37(3), γ 74.03(3)°; R was 0.045 for 3341 'observed' reflections. [(PPhMes2)CuBr]2.3C6H6 (5) is monoclinic, C2/c, a 9.694(6), b 30.15(2), c 20.66(2) Ǻ, β 98.00(7)°; R was 0.047 for 2117 'observed' reflections. [(PPhMes2)CuI]2.2MeCN (6) is orthorhombic, PP1nb, a 11.694(8), b 14.77(1), c 29.76(3) Ǻ; R was 0.049 for 3447 'observed' reflections. Cu-P bond lengths are: 2.196(2) A (1); 2.198(3) Ǻ (2); 2.222(5) and 2.226(5) Ǻ (3); 2.202(1) Ǻ (4); 2.197(3) A (5); 2.201(4) and 2.264(5) Ǻ (6). The geometries of the LCuX2 and CuX2Cu units are compared with data reported for other monomeric and dimeric compounds for both phosphorus- and nitrogen-based ligands L.

Crystal structures of some eriostyl/nitrobenzoate derivatives

1980 ◽  
Vol 33 (2) ◽  
pp. 313 ◽  
Author(s):  
PR Jefferies ◽  
BW Skelton ◽  
B Walter ◽  
AH White
Keyword(s):  
Charge Transfer ◽  
Solid State ◽  
Single Crystal ◽  
Crystal Structures ◽  
X Ray Diffraction ◽  
X Ray ◽  
Structure Determinations

Following the suggestion made earlier, on the basis of solution spectroscopy, that a number of eriostyl/nitrobenzoate compounds form charge-transfer self-complexes, a number of these have been investigated structurally by single-crystal X-ray diffraction methods in order to ascertain the presence or otherwise of such interactions in the solid state. The substances thus studied were eriostyl 3,5-dinitrobenzoate (1), eriostyl p-nitrobenzoate (2), tetrahydroeriostyl 3,5-dinitrobenzoate (3), and eriostemyl 3,5-dinitrobenzoate (4);* structure determinations in all cases, although displaying the presence of strong charge-transfer interactions from the two moieties of each molecule, show that the interactions in the solid state are intermolecular in nature.

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.

Crystal-Structures of 2 3-Substituted 10,11-Dimethoxy-1,2,3,4,5,6-Hexahydro-7,9-etheno-3-benzazecine Derivatives

1989 ◽  
Vol 42 (2) ◽  
pp. 321
Author(s):  
XY Jia ◽  
JB Bremner ◽  
BW Skelton ◽  
AH White ◽  
KN Winzenberg
Keyword(s):  
Hydrogen Atom ◽  
Chemical Shift ◽  
Single Crystal ◽  
Crystal Structures ◽  
Naphthalene Ring ◽  
Methyl Derivative ◽  
X Ray ◽  
Structure Determinations

The title compounds are 3-aza[6](1,7)-naphthalenophanes with 3-Me and 3-CO2Me substituents, C18H23NO2 and C19H23NO4; in the former the chemical shift of the naphthalene hydrogen enclosed by the medium nitrogen-containing ring is the highest yet observed in a derivative of this type ( σ 9.33). In order to examine the environment of this hydrogen atom and the expected associated naphthalene ring distortions in both compounds, single-crystal X-ray structure determinations have been carried out at 295 K showing the transannular H…N distance in the methyl derivative to be remarkably short at 2.08(2) � . Crystals are triclinic, P1, a 11.683(3), b 10.846(3), c 6.729(2) �, α 90.08(2), β 93.33(2), γ 112.88 Z 2; R was 0.041 for 1378 'observed' reflections. Crystals of the 3-CO2Me derivative are also triclinic, P1, a 12.587(9), b 10.650(4), c 6.758(3) � , a 91.91(3), β 100.51(4), γ 104.74(5)° Z 2; R 0.067 for 1267 'observed' reflections.

Backbone Phosphonamide-Functionalized Imidazol-2-ylidene Complexes

2016 ◽  
Vol 69 (10) ◽  
pp. 1186
Author(s):  
Paresh Kumar Majhi ◽  
Gregor Schnakenburg ◽  
Anthony J. Arduengo ◽  
Rainer Streubel
Keyword(s):  
Low Temperature ◽  
Single Crystal ◽  
X Ray ◽  
Structure Determinations

The synthesis of M(CO)5 complexes bearing 4-phosphonamide and 4,5-bis(phosphonamide)-imidazol-2-ylidene ligands (NHCP = phosphonamide-based N-heterocyclic carbene) is reported. Deprotonation of respective imidazolium hydrogensulfate salts with potassium tert-butoxide (KOtBu) in the presence of [M(CO)5(CH3CN)] afforded complexes with the formula [M(CO)5(NHCP)]. In a similar fashion, reaction of in situ generated NHCP with [Rh(cod)Cl]2 (cod = 1,5-cyclooctadiene) afforded a complex with the formula [Rh(cod)Cl(NHCP)]. Low-temperature deprotonation of the imidazolium NHCP·H2SO4 with potassium hexamethyldisilazide (KHMDS) in the presence of [AuCl(SMe2)] furnished the corresponding AuI NHC complex. All complexes were characterized by various spectroscopic and spectrometric methods. In addition, further structural confirmation is provided by key single-crystal X-ray structure determinations for three of the new complexes.

One-dimensional ribbons of solvated Ag sulfonates

1999 ◽  
Vol 77 (3) ◽  
pp. 313-318 ◽  
Author(s):  
George KH Shimizu ◽  
Gary D Enright ◽  
Gabriela S Rego ◽  
John A Ripmeester
Keyword(s):  
Coordination Polymer ◽  
Single Crystal ◽  
The Other ◽  
Monoclinic Space Group ◽  
Triclinic Space Group ◽  
Space Group ◽  
One Dimensional ◽  
X Ray ◽  
Structure Determinations

Single crystal X-ray structure determinations of two solvated silver sulfonates have been obtained and these compounds have been shown to adopt infinite one-dimensional motifs. {AgOTs(MeCN)}[Formula: see text] (OTs = p-toluenesulfonate) crystallizes in the monoclinic space group, P21, a = 8.4278(5) Å, b = 5.7413(3) Å, c = 12.1057(7) Å, β = 109.24(1)°. {Ag(NDSA)(MeCN)2(H3O)(H2O)2}[Formula: see text] (NDSA = 1,5-naphthalenedisulfonate) crystallizes in the triclinic space group, P[Formula: see text], a = 8.3407(4) Å, b = 10.4374(5) Å, c = 12.3399(6) Å, α = 101.941(8)°, β = 109.24(1)°, γ = 102.190(8)°. Despite one compound containing a monosulfonate and the other a disulfonate, both complexes form infinite one-dimensional arrays.Key words: silver, sulfonates, coordination polymer.

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.

On racemic and L-malates: a comparison of their crystal structures

2004 ◽  
Vol 219 (2) ◽  
Author(s):  
Michel Fleck ◽  
Ekkehart Tillmanns ◽  
Ladislav Bohatý ◽  
Peter Held
Keyword(s):  
Single Crystal ◽  
Crystal Structures ◽  
Powder Diffraction ◽  
Diffraction Data ◽  
Monoclinic Space Group ◽  
Powder Diffraction Data ◽  
X Ray Diffraction ◽  
Powder Diffraction File ◽  
Space Group ◽  
X Ray

AbstractThe crystal structures of eight different L-malates have been determined and refined from single-crystal X-ray diffraction data. The compounds are the monoclinic (space groupIn addition, for all the compounds, powder diffraction data were collected, analysed and submitted to the powder diffraction file (PDF).

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