Synthesis and characterization of molybdenum–tin complexes derived from the molybdenum tricarbonyl anion, [MeGapz3]Mo(CO)3−, and organotin chlorides. X-ray crystal structure of [MeGapz3]Mo(CO)3SnPh3 (where pz = pyrazolyl, N2C3H3)

1986 ◽  
Vol 64 (2) ◽  
pp. 321-327 ◽  
Author(s):  
Emmanuel C. Onyiriuka ◽  
Steven J. Rettig ◽  
Alan Storr
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Heavy Atom ◽  
Synthesis And Characterization ◽  
Full Matrix ◽  
X Ray ◽  
Tin Complexes ◽  
Interesting Solution ◽  
Single Bonds

The reaction of the molybdenum tricarbonyl anion, [MeGapz3]Mo(CO)3−, with the organotin chlorides, Ph3SnCl, Me3SnCl, and Me2SnCl2, has yielded a series of complexes in which direct Mo—Sn single bonds are featured. The [MeGapz3]Mo(CO)3SnMe2Cl complex shows an interesting solution behavior in which a transition from a 3:4, or piano stool structure, to a 3:3:1, or capped octahedral arrangement, is thought to occur. The 3:3:1 structure has been demonstrated in the solid state for the [MeGapz3]Mo(CO)3SnPh3 compound by means of a crystal structure determination. Crystals of [methyltris(1-pyrazolyl)gallato-N,N,N](triphenylstannyl)tricarbonylmolybdenum are monoclinic, a = 11.4439(8), b = 19.5116(8), c = 15.2686(12) Å β = 111.370(3)°, Z = 4, space group P21/c. The structure was solved by conventional heavy-atom methods and was refined by full-matrix least-squares procedures to R = 0.025 and Rw = 0.031 for 5259 reflections with I ≥ 3σ(I). Important bond lengths include: Mo—Sn = 2.8579(3), Mo—N = 2.239(2)–2.244(2), Mo—C = 1.967(3)–2.000(3), Sn—C = 2.151(3)–2.166(3), Ga—N = 1.920(3)–1.931(3), and Ga—C = 1.943(4) Å.

Synthesis and characterization of LMo(CO)3M(PPh3)x (where L = tridentate pyrazolyl-gallate or -borate ligand; M = Rh, x = 2; M = Cu, x = 1). X-ray crystal structures of [MeGapz3]Mo(CO)3Rh(PPh3)2 and [MeGapz3]Mo(CO)3Cu(PPh3) (where pz = pyrazolyl, N2C3H3)

1986 ◽  
Vol 64 (2) ◽  
pp. 373-386 ◽  
Author(s):  
Gregory A. Banta ◽  
Brenda M. Louie ◽  
Emmanuel Onyiriuka ◽  
Steven J. Rettig ◽  
Alan Storr
Keyword(s):  
Least Squares ◽  
Crystal Structures ◽  
Heavy Atom ◽  
Synthesis And Characterization ◽  
Octahedral Structure ◽  
Full Matrix ◽  
Space Group ◽  
X Ray

The reactions of the LMo(CO)3− ions (L = MeGapz3, HBpz3, Me2Gapz(OCH2CH2NMe2)) with [Cu(PPh3)Cl]4 and Rh(PPh3)3Cl have yielded complexes with Mo—Cu and Mo—Rh bonds. The X-ray crystal structures of two such complexes have been determined. Crystals of [MeGapz3]Mo(CO)3Cu(PPh3) are monoclinic, a = 17.071(2), b = 16.738(1), c = 23.641(3) Å, β = 104.899(6)°, Z = 8, space group P21/n, and those of [MeGapz3]Mo(CO)3Rh(PPh3)2, are triclinic, a = 12.519(3), b = 17.182(4), c = 12.071(2) Å, α = 105.02(1), β = 109.87(1), γ = 97.10(2)°, Z = 2, space group [Formula: see text]. Both structures were solved by conventional heavy atom methods and were refined by full-matrix least-squares procedures to R = 0.040 and Rw = 0.035 for 6296 reflections with I ≥ 2σ(I) and R = 0.036 and Rw = 0.037 for 5642 reflections with I ≥ 3σ(I), respectively. The former complex provides a rare example of a 3:3:1, or capped octahedral structure, with a short (mean) Mo—Cu distance of 2.513(9) Å. The latter compound displays one terminal and two bridging CO ligands and a Mo—Rh distance of 2.6066(5) Å.

Synthesis and characterization of [Me2Ga(3,5-Me2pz)2]Rh(CO)PPh3 and the X-ray structure of its toluene solvate

1985 ◽  
Vol 63 (2) ◽  
pp. 503-508 ◽  
Author(s):  
Brenda M. Louie ◽  
Steven J. Rettig ◽  
Alan Storr ◽  
James Trotter
Keyword(s):  
Physical Properties ◽  
Least Squares ◽  
Heavy Atom ◽  
Synthesis And Characterization ◽  
Boat Conformation ◽  
Full Matrix ◽  
Space Group ◽  
X Ray ◽  
Square Planar

Details of the synthesis and physical properties of [Me2Ga(3,5-Me2pz)2]Rh(CO)PPh3 are given. Crystals of [dimethylbis(3,5-dimethyl-1-pyrazolyl)gallato-N,N′](triphenylphosphine)carbonylrhodium(I) – toluene (1:1) are triclinic, a = 10.690(2), b = 12.928(2), c = 13.998(2) Å, α = 77.44(1), β = 83.50(1), γ = 72.70(1)°, Z = 2, space group [Formula: see text]. The structure was solved by conventional heavy-atom methods and was refined by full-matrix least-squares procedures to R = 0.039 and Rw = 0.048 for 5987 reflections with I ≥ 3σ(I). The Rh(I) is in a distorted square planar environment with Rh—N = 2.090(3) and 2.097(2), Rh—CO = 1.815(4), and Rh—P = 2.2700(8) Å. The central six-membered RhGaN4 ring has a steep boat conformation with a [Formula: see text] separation of 3.3819(4) Å.

Structural Systematics of Rare Earth Complexes. VII. Crystal Structure of Bis(2,2'/6',2␛-Terpyridinium) Octaaquaterbium(III) Heptachloride Hydrate

1994 ◽  
Vol 47 (2) ◽  
pp. 391 ◽  
Author(s):  
CJ Kepert ◽  
BW Skeleton ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Rare Earth ◽  
Single Crystal ◽  
Structural Characterization ◽  
Title Compound ◽  
Room Temperature ◽  
Chloride Ions ◽  
Full Matrix ◽  
X Ray

The room-temperature single-crystal X-ray structural characterization of the title compound (tpyH2)2[Tb(OH2)8]Cl7.~2⅓H2O is recorded. Crystals are triclinic, Pī , a 17.063(5), b 16.243(3), c 7.878(3) Ǻ, α 84.78(2), β 84.39(3), γ 87.81(2)°, Z = 2 formula units; 3167 'observed' diffractometer reflections were refined by full-matrix least-squares procedures to a residual of 0.057. Notable features of interest of the compound are the 'chelation' of chloride ions by the terpyridinium cations , and the existence of a free [Tb(OH2)8]2+ cation in the presence of an abundance of chloride ions.

Synthesis and characterization of the binuclear diamido titanium chalcogenides [(Ar)NCH2CH2CH2N(Ar)]2Ti(µ-E)2 (E = Se, Te)

2002 ◽  
Vol 80 (11) ◽  
pp. 1524-1529 ◽  
Author(s):  
Tianle Zhang ◽  
Warren E Piers ◽  
Masood Parvez
Keyword(s):  
Solid State ◽  
Key Words ◽  
Synthesis And Characterization ◽  
Catalyst Precursor ◽  
Tellurium Atom ◽  
Titanium Complex ◽  
X Ray ◽  
X Ray Crystallography ◽  
Atom Source

Reaction of McConville's chelating amido titanium complex [(Ar)NCH2CH2CH2N(Ar)]Ti(CH3)2 (Ar = 2,6-i-Pr2C6H3) with either elemental Se or the tellurium atom source Te=PBu3 resulted in the formation of bis-µ-chalcogenido dimers [(Ar)NCH2CH2CH2N(Ar)]2Ti(µ-E)2 (E = Se, 2; Te, 3) with concommitant loss of EMe2. The dimers 2 and 3 were characterized spectroscopically and via X-ray crystallography. The two compounds are isostructural in the solid state. The tellurido dimer 3 may also be synthesized by reduction of the diamido dichloride [(Ar)NCH2CH2CH2N(Ar)]2TiCl2 with Na–Hg amalgam followed by treatment with Te=PBu3. This dimer is unreactive toward further Te=PBu3 or stannanes such as HSnBu3. Unlike decamethyltitanocene derivatives, the diamido complex is not an effective catalyst precursor for the heterohydrodecoupling of Te=PBu3 and HSnBu3.Key words: diamido titanium complexes, selenides, tellurides.

Synthesis and characterization of antimony complexes of meso-tetraphenylporphyrin (tpp) and meso-tetra(4-methoxyphenyl)porphyrin (tmpp), and the x-ray crystal structure of [Sb(tmpp)Cl2]+OH

Polyhedron ◽  
1996 ◽  
Vol 15 (22) ◽  
pp. 3947-3954 ◽  
Author(s):  
I-Chih Liu ◽  
Jyh-Horung Chen ◽  
Shin-Shin Wang ◽  
Ju-Chun Wang
Keyword(s):  
Crystal Structure ◽  
Synthesis And Characterization ◽  
X Ray ◽  
Antimony Complexes

Synthesis and characterization of tantalum(V) complexes containing bis-sulfamide ligands: X-ray crystal structure of Ta[N(Me)2]3[SO2(NCMe3)2]

Polyhedron ◽  
2002 ◽  
Vol 21 (11) ◽  
pp. 1051-1055 ◽  
Author(s):  
R.C. Mills ◽  
P. Doufou ◽  
K.A. Abboud ◽  
James M. Boncella
Keyword(s):  
Crystal Structure ◽  
Synthesis And Characterization ◽  
X Ray

Darstellung und Charakterisierung von Rubidiumhydrogencyanamid/Synthesis and Characterization of Rubidium Hydrogen Cyanamide

1999 ◽  
Vol 54 (11) ◽  
pp. 1375-1378 ◽  
Author(s):  
Michael Becker ◽  
Martin Jansen
Keyword(s):  
Crystal Structure ◽  
Liquid Ammonia ◽  
Synthesis And Characterization ◽  
Hydrogen Cyanamide ◽  
X Ray ◽  
Bond Lengths

The synthesis of RbHCN2 was carried out by reaction of cyanamide with rubidium amide in liquid ammonia. The crystal structure has been determinedo by x-ray powder methods (orthorhombic, P21,21,21, a = 7.299(1), b = 9.435(1), c = 9.420(1) Å; Z = 8). The anion is slightly bent (174°) and exhibits two different bond lengths (C-N: 1.17, HN-C: 1.31 Å).

Synthesis and characterization of a new potentially ditopic receptor, 1,4,7,10-tetraoxa-13,16,19,22-tetraazacyclotetracosane, and the x-ray crystal structure of its mononuclear copper(II) complex

1989 ◽  
Vol 28 (7) ◽  
pp. 1417-1419 ◽  
Author(s):  
Jonathan L. Sessler ◽  
John W. Sibert ◽  
Jeffrey D. Hugdahl ◽  
Vincent Lynch
Keyword(s):  
Crystal Structure ◽  
Synthesis And Characterization ◽  
X Ray ◽  
Ditopic Receptor
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