TY - JOUR
T1 - Structural Studies of Bis-Catecholate, Bis-Dithiocatecholate, and Tetraalkoxy Diborane(4) Compounds
AU - Clegg, William
AU - Elsegood, Mark R.J.
AU - Lawlor, Fiona J.
AU - Norman, Nicholas C.
AU - Pickett, Nigel L.
AU - Robins, Edward G.
AU - Scott, Andrew J.
AU - Nguyen, Paul
AU - Taylor, Nicholas J.
AU - Marder, Todd B.
PY - 1998
Y1 - 1998
N2 - X-ray structures are described for the bis-catecholate, bis-dithiocatecholate, and tetraalkoxy diborane(4) compounds B2(1,2-O2C6H4)2 (1), B2(1,2-O2-4-ButC6H3) 2 (2), B2(1,2-O2-3,5-But2C 6H2)2 (3), B2(1,2-S2C6H4)2 (4), B2(1,2-S2-4-MeC6H3)2 (5), and B2(OCH2CMe2CH2O)2 (6). All the compounds adopt structures in the solid-state in which the B2O4 or B2S4 units are planar or very nearly so. In compounds 2 and 3, the dihedral angles between the two BO2C2 planes are 17.3 and 31.8° respectively whereas in 1, 4 and 5 these angles are exactly 0°. In 6, a 3-fold disorder precluded our obtaining accurate positions for the two boron atoms, yet a dihedral angle of 0° is required by the 3̄ site symmetry. The structure of the bis(Lewis base) adduct of B2Cl4 [B2Cl4(NHMe2)2] (7), is also described and structures of the salt [NH2Me2][B(1,2-O2C6H 4)2] (8)and the NMe2-bridged dimer [{BCl2(μ-NMe2}2] (9) are available in the Supporting Information. Compound 1 crystallized in the monoclinic space group P2√c with a = 4.746(1) Å, b = 16.427(3) Å, c = 7.053(2) Å, β= 98.59(2)°, and Z = 2. Crystals of 2 were monoclinic, space group P2√c with a = 6.847(1) Å, b = 18.871(5) Å, c = 15.270(2) Å, β = 93.16(2)°, and Z = 4. Crystals of 3 were triclinic, space group P1̄ with a = 9,478(4) Å, b = 10,355(4) Å, c = 15.082(7) Å, α = 105.71(3)°, β = 100.31(4)°. γ = 94.58(3)°, and Z = 2. Crystals of 4 were monoclinic, space group P2√c with a = 15.364(3) Å, b = 4.0502(4) Å, c = 21.532(3) Å, β= 99.320(7)°, and Z = 4. Crystals of 5 were monoclinic, space group P2√c with a = 6.0458(9) Å, b = 7.5319(11) Å, c = 16.552(2) Å, β= 96.291(3)° and Z = 2. Compound 6 crystallized in the rhombohedral space group R3̄m with a = 8.876(2) Å, c = 13.821(3) Å and Z = 3. Crystals of 7 were monoclinic, space group P2√c with a = 11.831(3) Å, b = 19.458(5) Å, c = 14.823(5) Å, β= 96.63-(4)°, and Z = 12.
AB - X-ray structures are described for the bis-catecholate, bis-dithiocatecholate, and tetraalkoxy diborane(4) compounds B2(1,2-O2C6H4)2 (1), B2(1,2-O2-4-ButC6H3) 2 (2), B2(1,2-O2-3,5-But2C 6H2)2 (3), B2(1,2-S2C6H4)2 (4), B2(1,2-S2-4-MeC6H3)2 (5), and B2(OCH2CMe2CH2O)2 (6). All the compounds adopt structures in the solid-state in which the B2O4 or B2S4 units are planar or very nearly so. In compounds 2 and 3, the dihedral angles between the two BO2C2 planes are 17.3 and 31.8° respectively whereas in 1, 4 and 5 these angles are exactly 0°. In 6, a 3-fold disorder precluded our obtaining accurate positions for the two boron atoms, yet a dihedral angle of 0° is required by the 3̄ site symmetry. The structure of the bis(Lewis base) adduct of B2Cl4 [B2Cl4(NHMe2)2] (7), is also described and structures of the salt [NH2Me2][B(1,2-O2C6H 4)2] (8)and the NMe2-bridged dimer [{BCl2(μ-NMe2}2] (9) are available in the Supporting Information. Compound 1 crystallized in the monoclinic space group P2√c with a = 4.746(1) Å, b = 16.427(3) Å, c = 7.053(2) Å, β= 98.59(2)°, and Z = 2. Crystals of 2 were monoclinic, space group P2√c with a = 6.847(1) Å, b = 18.871(5) Å, c = 15.270(2) Å, β = 93.16(2)°, and Z = 4. Crystals of 3 were triclinic, space group P1̄ with a = 9,478(4) Å, b = 10,355(4) Å, c = 15.082(7) Å, α = 105.71(3)°, β = 100.31(4)°. γ = 94.58(3)°, and Z = 2. Crystals of 4 were monoclinic, space group P2√c with a = 15.364(3) Å, b = 4.0502(4) Å, c = 21.532(3) Å, β= 99.320(7)°, and Z = 4. Crystals of 5 were monoclinic, space group P2√c with a = 6.0458(9) Å, b = 7.5319(11) Å, c = 16.552(2) Å, β= 96.291(3)° and Z = 2. Compound 6 crystallized in the rhombohedral space group R3̄m with a = 8.876(2) Å, c = 13.821(3) Å and Z = 3. Crystals of 7 were monoclinic, space group P2√c with a = 11.831(3) Å, b = 19.458(5) Å, c = 14.823(5) Å, β= 96.63-(4)°, and Z = 12.
UR - http://www.scopus.com/inward/record.url?scp=0001549903&partnerID=8YFLogxK
U2 - 10.1021/ic9804317
DO - 10.1021/ic9804317
M3 - Article
AN - SCOPUS:0001549903
SN - 0020-1669
VL - 37
SP - 5289
EP - 5293
JO - Inorganic Chemistry
JF - Inorganic Chemistry
IS - 20
ER -