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Volume 69 
Part 5 
Pages m288-m289  
May 2013  

Received 17 April 2013
Accepted 22 April 2013
Online 27 April 2013

Key indicators
Single-crystal X-ray study
T = 200 K
Mean [sigma](C-C) = 0.007 Å
Disorder in solvent or counterion
R = 0.025
wR = 0.062
Data-to-parameter ratio = 14.6
Details
Open access

cyclo-Tetrakis([mu]2-D-penicillaminato-[kappa]4N,S:O,S)tetrapalladium(II) 9.75-hydrate

aToyonaka, Osaka 560-0043, Department of Chemistry, Graduate School of Science, Osaka University, Japan
Correspondence e-mail: konno@chem.sci.osaka-u.ac.jp

The asymmetric unit of the title compound, [Pd4(C5H9NO2S)4]·9.75H2O, contains two neutral tetranuclear complex molecules with similar conformations and 19.5 solvent water molecules. Of the 21 independent water molecules, three exhibit an occupancy of one-half. In each tetranuclear complex molecule, the four PdII atoms have a square-planar coordination environment and are spanned by four D-penicillaminate ligands in a [kappa]4N,S:S,O coordination mode, forming an eight-membered Pd4S4 metallacycle. In the crystal, two tetranuclear molecules are connected to each other through eight N-H...O hydrogen bonds between amine and carboxylate groups, constructing a cylindrical dimer. The dimers are further hydrogen-bonded with the solvent water molecules, completing a three-dimensional network.

Related literature

For background to this class of compound, see: Igashira-Kamiyama & Konno (2011[Igashira-Kamiyama, A. & Konno, T. (2011). Dalton Trans. 40, 7249-7263.]). For related structures, see: Yoshinari et al. (2009[Yoshinari, N., Hirai, Y., Kawamoto, T., Igasihra-Kamiyama, A., Tsuge, K. & Konno, T. (2009). Chem. Lett. 38, 1056-1057.]).

[Scheme 1]

Experimental

Crystal data
  • [Pd4(C5H9NO2S)4]·9.75H2O

  • Mr = 1190.03

  • Triclinic, P 1

  • a = 12.4517 (3) Å

  • b = 13.2680 (4) Å

  • c = 15.1666 (11) Å

  • [alpha] = 113.527 (8)°

  • [beta] = 98.425 (7)°

  • [gamma] = 108.557 (8)°

  • V = 2067.3 (3) Å3

  • Z = 2

  • Mo K[alpha] radiation

  • [mu] = 1.98 mm-1

  • T = 200 K

  • 0.25 × 0.10 × 0.03 mm

Data collection
  • Rigaku R-AXIS RAPID diffractometer

  • Absorption correction: multi-scan (ABSCOR; Rigaku, 1995[Rigaku (1995). ABSCOR. Rigaku Corporation, Tokyo, Japan.]) Tmin = 0.730, Tmax = 0.916

  • 20447 measured reflections

  • 15410 independent reflections

  • 15064 reflections with I > 2[sigma](I)

  • Rint = 0.027

Refinement
  • R[F2 > 2[sigma](F2)] = 0.025

  • wR(F2) = 0.062

  • S = 1.08

  • 15410 reflections

  • 1052 parameters

  • 67 restraints

  • H atoms treated by a mixture of independent and constrained refinement

  • [Delta][rho]max = 1.52 e Å-3

  • [Delta][rho]min = -0.68 e Å-3

  • Absolute structure: Flack (1983[Flack, H. D. (1983). Acta Cryst. A39, 876-881.]), 6026 Friedel pairs

  • Flack parameter: -0.024 (13)

Table 1
Hydrogen-bond geometry (Å, °)

D-H...A D-H H...A D...A D-H...A
N1-H1...O26i 0.92 2.06 2.963 (5) 169
N1-H1A...O15ii 0.92 2.21 3.109 (4) 166
N2-H2...O27 0.92 2.35 3.139 (5) 143
N2-H2A...O13ii 0.92 2.11 2.928 (5) 148
N3-H3...O35B 0.92 2.01 2.889 (8) 160
N3-H3...O36A 0.92 2.23 3.045 (8) 147
N3-H3A...O11ii 0.92 2.37 3.278 (5) 167
N4-H4...O29iii 0.92 1.98 2.886 (5) 170
N4-H4A...O9ii 0.92 2.04 2.917 (4) 160
N5-H5...O18i 0.92 2.09 3.008 (5) 172
N5-H5A...O7iv 0.92 2.19 3.094 (4) 167
N6-H6...O27v 0.92 2.44 3.183 (5) 138
N6-H6...O28 0.92 2.48 3.326 (5) 153
N6-H6A...O5iv 0.92 2.21 3.041 (5) 151
N7-H7...O23 0.92 2.03 2.938 (5) 170
N7-H7A...O3iv 0.92 2.16 3.066 (5) 169
N8-H8...O28vi 0.92 1.98 2.896 (5) 171
N8-H8A...O1iv 0.92 2.06 2.930 (4) 157
O17-H17F...O26iv 0.85 (2) 1.96 (2) 2.798 (5) 167 (6)
O17-H17G...O16vii 0.86 (2) 1.93 (2) 2.775 (4) 170 (5)
O18-H18F...O17 0.84 (2) 2.00 (3) 2.818 (5) 165 (6)
O18-H18G...O20 0.85 (2) 1.98 (2) 2.814 (5) 165 (5)
O19-H19F...O8vii 0.85 (2) 2.05 (2) 2.892 (5) 168 (5)
O19-H19G...O2viii 0.85 (2) 1.94 (3) 2.760 (5) 160 (6)
O20-H20F...O21 0.85 (2) 1.88 (2) 2.709 (5) 167 (6)
O20-H20G...O8ix 0.86 (2) 1.94 (3) 2.742 (4) 156 (5)
O21-H21F...O22 0.86 (2) 1.97 (3) 2.805 (6) 162 (5)
O21-H21G...O30 0.87 (2) 2.00 (2) 2.857 (6) 169 (6)
O22-H22F...O10vii 0.85 (2) 1.95 (2) 2.802 (5) 174 (6)
O22-H22G...O16viii 0.86 (2) 2.21 (4) 2.915 (5) 139 (6)
O23-H23F...O20 0.85 (2) 1.96 (2) 2.796 (5) 168 (5)
O23-H23G...O25iv 0.85 (2) 1.96 (2) 2.782 (5) 162 (5)
O24-H24F...O19vi 0.85 (2) 1.97 (2) 2.814 (5) 177 (6)
O24-H24G...O32 0.85 (2) 1.90 (2) 2.736 (6) 168 (6)
O25-H25F...O24iii 0.87 (2) 1.91 (2) 2.770 (6) 170 (6)
O25-H25G...O12ii 0.85 (2) 1.97 (3) 2.788 (5) 159 (5)
O26-H26F...O23ii 0.86 (2) 1.95 (2) 2.791 (5) 167 (6)
O26-H26G...O31 0.85 (2) 1.95 (2) 2.788 (6) 169 (6)
O27-H27F...O6vi 0.85 (2) 1.88 (3) 2.687 (5) 158 (5)
O27-H27G...O14ii 0.84 (2) 1.81 (2) 2.650 (5) 175 (5)
O28-H28F...O10 0.82 (2) 2.02 (2) 2.810 (5) 161 (5)
O28-H28G...O27v 0.82 (2) 2.00 (3) 2.797 (5) 164 (5)
O29-H29F...O2 0.87 (2) 1.98 (2) 2.834 (5) 168 (6)
O29-H29G...O27 0.85 (2) 1.98 (2) 2.802 (5) 160 (5)
O30-H30F...O12 0.86 (2) 2.28 (5) 2.911 (7) 130 (6)
O30-H30G...O19iv 0.86 (2) 1.95 (3) 2.791 (5) 165 (6)
O31-H31F...O33ii 0.84 (2) 2.17 (3) 2.946 (8) 154 (7)
O31-H31G...O4 0.86 (2) 2.08 (2) 2.902 (6) 161 (5)
O32-H32F...O34 0.92 (2) 2.07 (2) 2.823 (7) 139 (3)
O32-H32G...O31 0.86 (2) 1.98 (2) 2.837 (7) 178 (9)
O33-H33F...O17 0.88 (2) 2.11 (4) 2.877 (6) 146 (7)
O33-H33G...O30vi 0.87 (2) 1.90 (2) 2.766 (6) 170 (7)
O34-H34F...O18 0.85 (2) 2.12 (4) 2.906 (6) 154 (8)
O34-H34G...O6vi 0.86 (2) 2.02 (3) 2.815 (6) 154 (6)
O35A-H35F...O25 0.85 (2) 2.14 (3) 2.986 (9) 174 (13)
O35A-H35G...O4 0.85 (2) 2.05 (5) 2.848 (9) 157 (12)
O35B-H35H...O4 0.83 (2) 2.45 (8) 3.135 (9) 141 (10)
O35B-H35I...O25 0.84 (2) 2.03 (5) 2.802 (10) 152 (9)
O36A-H36F...O22 0.85 (2) 2.14 (5) 2.949 (9) 159 (12)
O36A-H36G...O35A 0.85 (2) 1.93 (5) 2.746 (12) 158 (12)
Symmetry codes: (i) x, y, z-1; (ii) x, y-1, z; (iii) x+1, y, z; (iv) x, y+1, z; (v) x+1, y+1, z; (vi) x-1, y, z; (vii) x, y, z+1; (viii) x+1, y, z+1; (ix) x, y+1, z+1.

Data collection: PROCESS-AUTO (Rigaku, 2000[Rigaku (2000). PROCESS-AUTO. Rigaku Corporation, Tokyo, Japan.]); cell refinement: PROCESS-AUTO; data reduction: PROCESS-AUTO; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: Yadokari-XG 2009 (Kabuto et al., 2009[Kabuto, C., Akine, S., Nemoto, T. & Kwon, E. (2009). Nihon Kessho Gakkaishi, 51, 218-224.]); software used to prepare material for publication: Yadokari-XG 2009.


Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: IS5266 ).


Acknowledgements

This work was supported by a Grant-in-Aid for Science Research (grant No. 23350026) from the Ministry of Education, Culture, Sports, Science and Technology of Japan, and by the Kurata Memorial Hitachi Science and Technology Foundation.

References

Flack, H. D. (1983). Acta Cryst. A39, 876-881.  [CrossRef] [details]
Igashira-Kamiyama, A. & Konno, T. (2011). Dalton Trans. 40, 7249-7263.  [ChemPort] [PubMed]
Kabuto, C., Akine, S., Nemoto, T. & Kwon, E. (2009). Nihon Kessho Gakkaishi, 51, 218-224.  [CrossRef]
Rigaku (1995). ABSCOR. Rigaku Corporation, Tokyo, Japan.
Rigaku (2000). PROCESS-AUTO. Rigaku Corporation, Tokyo, Japan.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [ChemPort] [details]
Yoshinari, N., Hirai, Y., Kawamoto, T., Igasihra-Kamiyama, A., Tsuge, K. & Konno, T. (2009). Chem. Lett. 38, 1056-1057.  [CSD] [CrossRef] [ChemPort]


Acta Cryst (2013). E69, m288-m289   [ doi:10.1107/S160053681301088X ]

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