Bis(1-ferrocenylmethylidene-4-phenylthiosemicarbazidato-κ2 N 1,S)zinc(II) monohydrate

In the title compound, [Fe2Zn(C5H5)2(C13H11N3S)2]·H2O, the ZnII ion is in a distorted tetrahedral geometry being coordinated by two thiosemicarbazone ligands via N and S atoms. One of the Cp rings is disordered over two positions with occupancies of 0.55 and 0.45. The dihedral angle between the substituted Cp rings is 56.1 (5)° and the two phenyl rings are orientated at a dihedral angle of 41.7 (4)°. In the crystal structure, intermolecular O—H⋯S, N—H⋯O and C—H⋯N hydrogen bonds link the molecules into chains along the b axis. The structure is further consolidated by O—H⋯π interactions.

In the title compound, [Fe 2 Zn(C 5 H 5 ) 2 (C 13 H 11 N 3 S) 2 ]ÁH 2 O, the Zn II ion is in a distorted tetrahedral geometry being coordinated by two thiosemicarbazone ligands via N and S atoms. One of the Cp rings is disordered over two positions with occupancies of 0.55 and 0.45. The dihedral angle between the substituted Cp rings is 56.1 (5) and the two phenyl rings are orientated at a dihedral angle of 41.7 (4) . In the crystal structure, intermolecular O-HÁ Á ÁS, N-HÁ Á ÁO and C-HÁ Á ÁN hydrogen bonds link the molecules into chains along the b axis. The structure is further consolidated by O-HÁ Á Á interactions.

Related literature
For related structures, see: Vikneswaran et al. (2009a,b). For the preparation, see: Casas et al. (2004). For the stability of the temperature controller used for the data collection, see: Cosier & Glazer (1986).
As a continuation of our research related to ferrocenyl thiosemicarbazones and its metal complexes, herein we report the synthesis and crystal structure of a Zn II complex formed with formylferrocene 4-phenyllthiosemicarbazone.
In the crystal structure, intermolecular O-H···S, N-H···O and C-H···N hydrogen bonds (Table 1) link the molecules into chains along the b axis (Fig. 2). The crystal structure is further consolidated by O-H···π interactions involving the C1-C5 ring.

S3. Refinement
One of the Cp rings is disordered over two positions with site occupancies of 0.55 and 0.45. The same U ij parameters is used for the atom pair C14A/C14B, and all disordered atoms were subjected to rigid bond and similarity restraints. All Hatoms were placed in calculated positions, with C-H = 0.93-0.98 Å, N-H = 0.86 and O-H = 0.85 and refined using a riding model, with U iso (H) = 1.2 U eq (C,N) and 1.5U eq (O). The highest residual density peak is located 0.87 Å from atom Zn1 and the deepest hole is located 1.30 Å from atom Zn1.

Figure 1
The molecular structure of the title compound, showing 50% probability displacement ellipsoids and the atom-numbering scheme. All disorder components are shown.  The crystal packing of the title compound, viewed along the c axis, showing chains along b axis. Intermolecular hydrogen bonds are shown as dashed lines. Only the major disorder components are shown.

Bis(1-ferrocenylmethylidene-4-phenylthiosemicarbazidato-κ 2 N 1 ,S)zinc(II) monohydrate
where P = (F o 2 + 2F c 2 )/3 (Δ/σ) max < 0.001 Δρ max = 2.43 e Å −3 Δρ min = −0.71 e Å −3 Absolute structure: Flack (1983), 3458 Friedel pairs Absolute structure parameter: 0.50 (2) Special details Experimental. The crystal was placed in the cold stream of an Oxford Cyrosystems Cobra open-flow nitrogen cryostat (Cosier & Glazer, 1986) operating at 100.0 (1) K. Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. Refinement. Refinement of F 2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F 2 , conventional R-factors R are based on F, with F set to zero for negative F 2 . The threshold expression of F 2 > σ(F 2 ) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F 2 are statistically about twice as large as those based on F, and R-factors based on ALL data will be even larger.