BINUCLEAR ANTIMONY(V) COMPLEXES WITH BRID GING DIPHENYLPHOSPHATO LIGANDS

The binuclear antimony(V) complexes Cl3Sb(O)[(C6H5O)(2)PO2](2)SbCl3 (1 ), Cl3Sb(O)[(C6H5O)(2)PO2](OCH3)SbCl3 (2), Cl3Sb(O)[(C6H5O)(2)PO2](OH) SbCl3 (3) and Cl4Sb[(C6H5O)(2)PO2](2)SbCl4 (4) are prepared by reactio n of diphenylphosphoric acid with antimony(Ti) chloride, water and met hanol in different molar ratios. The progress of the reactions was con trolled by the P-3l-NMR signals. 1 crystallizes triclinic in the space group P (1) over bar with a = 918.8, b = 1312.9, c = 1395.8 pm, alpha = 91.91, beta = 101.36, gamma = 95.90 degrees and Z = 2. 2 to 4 cryst allize in monoclinic space groups: 2: C2/c, a = 2753.4, b = 1156.1, c = 1476.7 pm, beta = 98.01 degrees and Z = 8; 3: P2(1)/c, a = 1234.8, b = 1471.8, c = 1263.4 pm, beta = 107.15 degrees and Z = 4; 4: P2(1)/n, a = 1943.8, b = 940.8, c = 2015.6 pm, beta = 109.87 degrees and Z = 4 resp. The NMR spectra are discussed and some IR data are communicated .