The crystal structure of ammonium bis-mu-oxalato-tinanate(III) dihydra
te, NH4[Ti(C2O4)(2)].2H(2)O, is reinvestigated by careful single-cryst
al X-ray diffraction using Mo K alpha (room temperature and 130 K) and
Ag K alpha radiation (room temperature). It crystallized in noncentro
symmetric hexagonal space group P6(4)22, with cell parameters a = 8.94
7 (2), c = 10.898 (1) Angstrom, Z = 3, F(000) = 423, M(r) = 278.1, D-x
= 1.833, R = 0.035, wR = 0.030 for 2296 observed relections with I gr
eater than or equal to 2 sigma(I), on Ag K alpha data. Accurate data m
easurement was applied using two wavelengths (0.7107 Angstrom for Mo K
alpha and 0.5609 Angstrom for Ag K alpha) in order to study the charg
e density distribution and also to investigate the wavelength effect i
n such investigations. A total of 22 650 and 20 298 reflections were m
easured using Mo K alpha radiation. The Ti atom is coordinated by four
oxalate dianions with coordination number 8 in an approximate symmetr
y of D-4 geometry. Each oxalato ligand is bridged between two Ti atoms
and forms and infinite polymeric spiral column along the c axis. The
deformation density maps, Delta rho, obtained from all three data sets
are consistent and agree well. Although the formal charge of Ti in th
is complex is 3+, with only one electron on the 3d orbitals expected,
the net atomic charge on Ti from this study is similar to 2+. Charge a
sphericity around the Ti atom caused by the spitting of 3d orbitals is
clearly observed in the deformation density. The d-orbital population
are evaluated from multipole refinement. The expected d(1) electron i
s mainly located in the d(z2) orbital.