Synthesis and X-ray crystal structure of the novel Mo—Cu complex, (Ph2PCH2CH2PPh2)2Cu+[(HBpz″3)Mo(CO)3]2Cu−(where pz″ = 3,5-dimethylpyrazolyl, N2C5H7)

1988 ◽  
Vol 66 (9) ◽  
pp. 2194-2199 ◽  
Author(s):  
Steven J. Rettig ◽  
Alan Storr ◽  
James Trotter
Keyword(s):  
Crystal Structure ◽  
Heavy Atom ◽  
Coordination Geometry ◽  
The Novel ◽  
Tetrahedral Coordination ◽  
X Ray ◽  
Carbonyl Ligands ◽  
Cu Complex ◽  
Anionic Ligand ◽  
Average Bond

The novel complex, (Ph2PCH2CH2PPh2)2Cu+[(HBpz″3)Mo(CO)3]2Cu− (where pz″ = 3,5-dimethylpyrazolyl), has been synthesized by reacting the (HBpz″3)Mo(CO)3− anionic ligand with CuI in the presence of a stoichiometric amount of Ph2PCH2CH2PPh2. Crystals of (Ph2PCH2CH2PPh2)2Cu+[(HBpz″3)Mo(CO)3]2Cu−•3.5C6H6•CH2Cl2 are triclinic, a = 13.421(1), b = 14.931(3), c = 28.523(5) Å, α = 90.41(2), β = 90.19(1), γ = 104.65(1)°, Z = 2, space group [Formula: see text] The structure was solved by heavy atom methods and was refined by full-matrix least-squares procedures to R = 0.047 and Rw = 0.049 for 8779 reflections with I ≥ 3σ(I). The crystal structure consists of (Ph2PCH2CH2PPh2)2Cu+ cations having irregular tetrahedral coordination geometry about the copper atom (Cu—P = 2.263(2)–2.304(2) Å and P—Cu—P = 88.30(7)–134.62(8)°) and novel [(HBpz″3)Mo(CO)3]2Cu− anions having exact Ci and approximate D3d symmetry. The central Cu atom of the anion is bonded to two Mo atoms in a linear fashion and also interacts with six semi-bridging carbonyl ligands, three from each (HBpz″3)Mo(CO)3− ligand. Average bond lengths and angles for the anion are Mo–Cu = 2.565, Mo—C = 1.955, Mo—N = 2.256, Cu—C = 2.309, C—O = 1.174 Å, Mo—C—O = 171.7° and Cu—C—O = 114.7°.

Coordination compounds containing a novel tridentate pyrazolylgallate ligand. X-ray structures of Me2Ga(μ-OH)(μ-Me2pz)GaMe2•HOCH2Me2pz and [Me2Ga(pz)(OCH2pz)]2Ni (pz = N2C3H3)

1988 ◽  
Vol 66 (1) ◽  
pp. 101-108 ◽  
Author(s):  
Arthur Mar ◽  
Steven J. Rettig ◽  
Alan Storr ◽  
James Trotter
Keyword(s):  
Transition Metal Complexes ◽  
Heavy Atom ◽  
Direct Reaction ◽  
Coordination Geometry ◽  
The Novel ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths ◽  
Normal Bond ◽  
Cis Isomer

The syntheses of the novel anionic tridentate dimethyl(pyrazol-1-yl)(1-oxymethylpyrazolyl)gallate ligand and representative transition metal complexes thereof are reported. The direct reaction of Me3Ga with 1-hydroxymethyl-3,5-dimethylpyrazole leads to the isolation of Me2Ga(μ-OH)(μ-Me2pz)GaMe2•HOCH2Me2pz. Crystals of (μ-hydroxy)(μ-3,5-dimethylpyrazolyl)bis(dimethylgallium) 1-hydroxymethyl-3,5-dimethylpyrazole solvate are monoclinic, a = 33.105(2), b = 7.3048(7), c = 8.8336(6) Å, β = 97.474(7)°, Z = 4, space group P21/n, and those of bis[dimethyl(pyrazol-1-yl)(1-oxymethylpyrazolyl)gallato-N2,N2′,O]nickel(II) are monoclinic, a = 9.6345(3), b = 14.2731(6), c = 18.6356(7) Å, β = 99,660(3)°, Z = 4, space group P21/c. Both structures were solved by conventional heavy atom methods and were refined by full-matrix least-squares procedures to R = 0.044 and 0.037 for 2660 and 3904 reflections with I ≥ 3σ(I), respectively. Mean bond lengths in Me2Ga(μ-OH)(μ-Me2pz)GaMe2•HOCH2Me2pz are Ga—O = 1.918(11), Ga—N = 2.001(5), and Ga—C = 1.955(5) Å. Fac-[Me2Ga(pz)(OCH2pz)]2Ni crystallizes as an all-cis isomer with normal bond lengths and angles at Ga and Ni—O = 1.918(3) and 1.927(3), Ni—N = 2.030(4)–2.111(4) Å. The coordination geometry about Ni is irregular pseudo-octahedral with evidence of both steric and structural trans effects.

scholarly journals Synthesis and structural characterization of glycinatodimethylgallium, (C2H4NO2)Ga(CH3)2

1987 ◽  
Vol 65 (6) ◽  
pp. 1349-1352 ◽  
Author(s):  
Steven J. Rettig ◽  
Alan Storr ◽  
James Trotter
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Structural Characterization ◽  
Title Compound ◽  
Heavy Atom ◽  
Coordination Geometry ◽  
Tetrahedral Coordination ◽  
Full Matrix ◽  
Independent Molecules

Details of the preparation and crystal structure of the title compound are given. Crystals of glycinatodimethylgallium are monoclinic, a = 12.502(1), b = 12.023(1), c = 10.732(1) Å, β = 110.05(1)°, Z = 8, space group P21/c. The structure was solved by conventional heavy atom methods and was refined by full-matrix least-squares procedures to R = 0.033 and Rw = 0.039 for 1172 reflections with I ≥ 3σ(I). The structure consists of monomeric (C2H4NO2)GaMe2 molecules which are linked together by an extensive network of [Formula: see text] hydrogen bonds. The Ga atoms have tetrahedral coordination geometry with bond lengths averaged over the two crystallographically independent molecules: Ga—O = 1.958(18), Ga—N = 2.031(5), and Ga—C = 1.937(7) Å.

scholarly journals Some Novel Cobalt Diphenylphosphine Complexes: Synthesis, Characterization, and Behavior in the Polymerization of 1,3-Butadiene

Molecules ◽  
2021 ◽  
Vol 26 (13) ◽  
pp. 4067
Author(s):  
Giovanni Ricci ◽  
Giuseppe Leone ◽  
Giorgia Zanchin ◽  
Benedetta Palucci ◽  
Alessandra Forni ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Single Crystals ◽  
The Novel ◽  
X Ray Diffraction ◽  
X Ray ◽  
And Behavior

Some novel cobalt diphenylphosphine complexes were synthesized by reacting cobalt(II) chloride with (2-methoxyethyl)diphenylphosphine, (2-methoxyphenyl)diphenylphosphine, and 2-(1,1-dimethylpropyl)-6-(diphenylphosphino)pyridine. Single crystals suitable for X-ray diffraction studies were obtained for the first two complexes, and their crystal structure was determined. The novel compounds were then used in association with methylaluminoxane (MAO) for the polymerization of 1,3-butadiene, and their behavior was compared with that exhibited in the polymerization of the same monomer by the systems CoCl2(PnPrPh2)2/MAO and CoCl2(PPh3)2/MAO. Some significant differences were observed depending on the MAO/Co ratio used, and a plausible interpretation for such a different behavior is proposed.

Crystal Structure of (NH4)2[Mo3S(S2)6] Containing the Novel Isolated Cluster [MO3S13]2-

1979 ◽  
Vol 34 (3) ◽  
pp. 434-436 ◽  
Author(s):  
A. Müller ◽  
S. Pohl ◽  
M. Dartmann ◽  
J. P. Cohen ◽  
J. M. Bennett ◽  
...  
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Aqueous Solutions ◽  
Single Crystal ◽  
Ammonium Salt ◽  
Crystal And Molecular Structure ◽  
Monoclinic Space Group ◽  
The Novel ◽  
Mean Values ◽  
X Ray

Abstract The novel tri-nuclear metal-sulfur cluster [Mo3S(S2)6]2- can be obtained as its ammonium salt by the reaction of a Moiv containing aqueous solutions with polysulfide. Its crystal and molecular structure has been determined by a single crystal X-ray study. The crystals are monoclinic (space group Cm, with a = 11.577(6) Å, b = 16.448(7) Å, c = 5.716(2) Å, β = 117.30(3)°, V = 967.2 Å3 , Z = 2, dexptl. = 2.54(2) g/cm3 , dcal = 2.54 g/cm3). The structure consists of isolated [Mo3S(S2)6]2- units, with three Mo atoms at the vertices of a triangle. There are bridging as well as terminal S22--ligands lying above and below the Mo3-plane (bond distances: Mo-Mo = 2.722 Å, Mo-S(terminal) = 2.435, Mo-S(bridging) = 2.452, Mo3-S = 2.353(4) Å and S-S = 2.04 Å (mean values)).

A first Mn member in the struvite morphotropic series, CsMn(H2O)6(PO4): hydrothermal synthesis, crystal structure and interconnections within the family of related phosphates

2018 ◽  
Vol 74 (8) ◽  
pp. 936-943
Author(s):  
Galina V. Kiriukhina ◽  
Olga V. Yakubovich ◽  
Ekaterina M. Kochetkova ◽  
Olga V. Dimitrova ◽  
Anatoliy S. Volkov
Keyword(s):  
Crystal Structure ◽  
Ionic Radius ◽  
The Novel ◽  
X Ray Diffraction ◽  
Unit Cell Parameters ◽  
Hydrothermal Conditions ◽  
X Ray ◽  
Cell Parameters ◽  
Structural Relationships ◽  
The Family

Caesium manganese hexahydrate phosphate, CsMn(H2O)6(PO4), was synthesized under hydrothermal conditions. Its crystal structure was determined from single-crystal X-ray diffraction data. The novel phase crystallizes in the hexagonal space group P63 mc and represents the first manganese member in the struvite morphotropic series, AM(H2O)6(TO4). Its crystal structure is built from Mn(H2O)6 octahedra and PO4 tetrahedra linked into a framework via hydrogen bonding. The large Cs atoms are encapsulated in the framework cuboctahedral cavities. It is shown that the size of the A + ionic radius within the morphotropic series AM(H2O)6(XO4) results is certain types of crystal structures and affects the values of the unit-cell parameters. Structural relationships with Na(H2O)Mg(H2O)6(PO4) and the mineral hazenite, KNa(H2O)2Mg2(H2O)12(PO4)2, are discussed.

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