Complexes containing heteronuclear and homonuclear quadruple bonds. Preparation and characterization of MoWCl[sub 4](dmpm)[sub 2] and Mo[sub 2]X[sub 4](dmpm)[sub 2] (X = Br, I)
- Texas A M Univ., College Station, TX (United States)
- Michigan State Univ., East Lansing, MI (United States)
- Los Alamos National Lab., NM (United States)
The quadruply bonded heterobimetallic complex MoWCl[sub 4](dmpm)[sub 2] (1) and the homobimetallic complexes Mo[sub 2]X[sub 4](dmpm)[sub 2] (X = Br, I,) were synthesized and their structures determined. The crystals of compound 1 exhibit the typical disorder for heteronuclear systems, namely, the random orientation of the M-M[prime] vector, with each metal atom appearing as 50% Mo and 50% W. The structural refinement in the space group P4 resulted in lower residuals, with R = 0.048 and R[sub W] = 0.067, than in the space group P4/m. For complexes 2 and 3, crystals obtained from THF solutions are monoclinic, with space groups P2[sub 1]/c and P2[sub 1]/n for 2 and 3, respectively. The quadruple bond distances are 2.193(2), 2.1271(8), and 2.132(2) [angstrom] for 1, 2, and 3, respectively. In addition, each complex has been characterized using UV-visible, [sup 31]P[[sup 1]H] NMR, and [sup 1]H NMR spectroscopies. The average magnetic anisotropy of the Mo-Mo quadruple bond in complexes 2 and 3 has been calculated from [sup 1]H NMR data as [minus]4450 [times] 10[sup [minus]36] m[sup 3] molecule[sup [minus]1]. The crystal structures of complexes 1-3 are fully described, and their crystallographic data are as follows: (1) space group P4 with a = b = 9.083(2) [angstrom], c = 8.092(2) [angstrom], V = 667.5(5) [angstrom][sup 3], and Z = 2; (2) space group P2[sub 1]/n with a = 8.694(1) [angstrom], b = 8.695(2) [angstrom], c = 15.369(2) [angstrom], [beta] = 100.70(1)[degrees], V = 1141.6(6) [angstrom][sup 3], and Z = 2; (3) space group P2[sub 1]/c with a = 9.076(2) [angstrom], b = 16.813(7) [angstrom], c = 16.654(5) [angstrom], [beta] = 102.4(1)[degrees], V = 2481(4) [angstrom][sup 3], and Z = 4.
- OSTI ID:
- 5110165
- Journal Information:
- Inorganic Chemistry; (United States), Journal Name: Inorganic Chemistry; (United States) Vol. 32:23; ISSN 0020-1669; ISSN INOCAJ
- Country of Publication:
- United States
- Language:
- English
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Related Subjects
400201* -- Chemical & Physicochemical Properties
ABSORPTION SPECTROSCOPY
BROMIDES
BROMINE COMPOUNDS
CHELATES
CHEMICAL PREPARATION
CHLORIDES
CHLORINE COMPOUNDS
COHERENT SCATTERING
COMPLEXES
CRYSTAL LATTICES
CRYSTAL STRUCTURE
DIFFRACTION
HALIDES
HALOGEN COMPOUNDS
IODIDES
IODINE COMPOUNDS
ISOTOPES
LATTICE PARAMETERS
LIGHT NUCLEI
MAGNETIC RESONANCE
MOLECULAR STRUCTURE
MOLYBDENUM COMPLEXES
MONOCLINIC LATTICES
NUCLEAR MAGNETIC RESONANCE
NUCLEI
ODD-EVEN NUCLEI
PHOSPHINES
PHOSPHORUS 31
PHOSPHORUS COMPOUNDS
PHOSPHORUS ISOTOPES
RESONANCE
SCATTERING
SPECTROSCOPY
STABLE ISOTOPES
SYNTHESIS
TRANSITION ELEMENT COMPLEXES
TUNGSTEN COMPLEXES
X-RAY DIFFRACTION