metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890
Volume 69| Part 5| May 2013| Pages m288-m289

cyclo-Tetra­kis(μ2-D-penicillaminato-κ4N,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

(Received 17 April 2013; accepted 22 April 2013; online 27 April 2013)

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 κ4N,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

  • α = 113.527 (8)°

  • β = 98.425 (7)°

  • γ = 108.557 (8)°

  • V = 2067.3 (3) Å3

  • Z = 2

  • Mo Kα radiation

  • μ = 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 > 2σ(I)

  • Rint = 0.027

Refinement
  • R[F2 > 2σ(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

  • Δρmax = 1.52 e Å−3

  • Δρmin = −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 DA 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.

Supporting information


Comment top

D-Penicillamine (C5H11NSO2, D—H2pen), which is a sulfur-containing amino acid, has been known as a unique multidentate chiral ligand that has three kinds of coordination sites, amine N, carboxylate O, and thiolate S atoms (Igashira-Kamiyama & Konno, 2011). Recently, we found that an S-bridged cyclic tetranuclear PdII complex with D-pen, [Pd4Cl4(D-Hpen)4].7H2O, gradually converts to an S-bridged cyclic trinuclear PdII structure in [Pd3(D-pen)3].4.5H2O (II), by treating with K2CO3 in water (Yoshinari et al., 2009). We assumed that some intermediate species exists in this reaction because not only the nuclearity of the complex (PdII4 versus. PdII3) but also the coordination mode of D-pen (κ2N,S:κS versus. κ2N,S:κ2S,O) are required to be changed for this structural conversion. In the course of our trials to find an intermediate species, we were able to isolate crystals (I), the composition of which is different from those of [Pd4Cl4(D-Hpen)4].7H2O and [Pd3(D-pen)3].4.5H2O, and its structure was determined by single-crystal X-ray crystallography. Herein we report that crystal (I) thus obtained has a new cyclic tetranuclear PdII structure in [PdII4(D-pen)4].9.75H2O, which forms an intriguing supramolecular dimer structure.

The asymmetric unit of (I) contains two tetranuclear PdII molecules, [Pd4(D-pen)4], and nineteen and a half solvated water molecules (Figure 1). The two tetranuclear molecules are essentially the same as each other, comprising of four square-planar PdII atoms and four D-pen ligands. Each D-pen ligand bridges two PdII centers in a κ2N,S:κ2S,O coordination mode, while each PdII atom is coordinated by two D-pen ligands in N,S- and S,O- chelating modes, forming a crown-type eight-membered Pd4S4 metallacycle. Note that amine and carboxy groups cover one face of the metallacycle, while thiolate and methyl groups cover another face in (I). It has been shown that similar hydrophilic and hydrophobic surfaces are formed in the S-bridged metallacycle structure in (II).

The Pd—S distances and S—Pd—S angles in (I) [Pd—S = 2.2261 (11)–2.2968 (10) Å, S—Pd—S = 89.76 (4)–93.65 (4)°] are similar to those in (II) [Pd—S = 2.2427 (15)–2.2934 (15) Å, S—Pd—S = 90.08 (6)–92.66 (6)°]. However, the Pd—S—Pd angles in (I) [96.90 (4)–102.42 (4)°] are closer to the ideal tetrahedral angle of 109.5° compared with those in (II) [Pd—S—Pd = 82.89 (5)–91.65 (6)°], while the trans angles around PdII atoms in (I) [167.45 (12)–172.13 (8)°] are slightly smaller than those in (II) [170.41 (13)–176.67 (16)°]. This implies that the distortion around S atoms is larger but the distortion around Pd atoms is smaller in (I), compared with those in (II).

The most remarkable structural feature in (I) is the construction of a cylindrical supramolecular structure, in which two cyclic tetranuclear molecules face to each other to form eight intermolecular N—H···O hydrogen bonds [N···O = 2.917 (4)–3.278 (5) Å] (Figure 2). None of solvent molecules are accommodated in the cylinder despite the presence of a void space with a diameter of ca 4 Å. All of the water molecules are participated in the formation of O—H···O and/or N—H···O hydrogen bonds with neighboring water molecules and/or tetranuclear molecules [O···O = 2.650 (5)–3.135 (9) Å, N···O = 2.886 (5)–3.326 (5) Å], completing three dimensional structure in (I) (Table 1).

Related literature top

For background to this class of compound, see: Igashira-Kamiyama & Konno (2011). For related structures, see: Yoshinari et al. (2009).

Experimental top

To an orange suspension containing 100 mg (0.08 mmol) of [Pd4(D-Hpen)4Cl4].7H2O in water (10 ml) was added an aqueous K2CO3 (0.2 M, 1 ml). From the resulting orange solution, a yellow crystalline powder of (I) was immediately precipitated, which was collected by filtration. Yield: 43 mg (46%). 1H NMR in DMSO-d6 (500 MHz): δ 5.84 (dd, J = 11.1, 7.5 Hz, 1H, NH2), 4.95 (d, J = 11.2 Hz, 1H, NH2), 3.15 (d, J = 7.6 Hz, 1H, CH), 1.64 (s, 3H, CH3), 1.64 (s, 3H, CH3). IR (KBr): 1610 cm-1 (νCO for COO-). Single-crystals of (I) suitable for X-ray analysis were obtained by recrystallization of the powder from a small amount of ethanol/water (1:1).

Refinement top

H atoms bound to C and N atoms were placed at calculated positions [C—H = 0.98 (CH3), 0.99 (CH2) or 1.00 Å (CH) and N—H = 0.92 Å (NH2)] and refined as riding with Uiso(H) = 1.2Ueq(C,N) for CH and NH2, and 1.5Ueq(C) for CH3. One and a half water molecules were disordered, and these molecules were refined with occupancies of 0.5. H atoms of water molecules were placed so as to form reasonable hydrogen bonding. All H atoms bound to O atoms were refined with restrained geometric and displacement parameters [O—H = 0.85 (2) Å, H···H = 1.38 (2) Å and Uiso(H) = 1.2Ueq(O)]. In addition, one H atom (H32F) was refined with an additional intermolecular H···O distance restraint so as to form reasonable hydrogen bonding. Reflections of (-6 14 -9), (-13 2 1), (-12 -3 0) and (-12 2 14) were removed to improve the data quality.

Computing details top

Data collection: PROCESS-AUTO (Rigaku, 2000); cell refinement: PROCESS-AUTO (Rigaku, 2000); data reduction: PROCESS-AUTO (Rigaku, 2000); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: Yadokari-XG 2009 (Kabuto et al., 2009); software used to prepare material for publication: Yadokari-XG 2009 (Kabuto et al., 2009).

Figures top
[Figure 1] Fig. 1. A perspective view of the title compound, showing the atom-numbering scheme. Displacement ellipsoids are drawn at the 50% probability level and H atoms have been omitted for clarity.
[Figure 2] Fig. 2. (a) Side and (b) top views of the cylindrical dimer structure in the title compound. H atoms have been omitted for clarity. Dashed lines indicate intermolecular N—H···O hydrogen bonds.
cyclo-Tetrakis(µ2-D-penicillaminato-κ4N,S:O,S)tetrapalladium(II) 9.75-hydrate top
Crystal data top
[Pd4(C5H9NO2S)4]·9.75H2OZ = 2
Mr = 1190.03F(000) = 1187
Triclinic, P1Dx = 1.912 Mg m3
Hall symbol: P 1Mo Kα radiation, λ = 0.71075 Å
a = 12.4517 (3) ÅCell parameters from 20017 reflections
b = 13.2680 (4) Åθ = 3.1–27.5°
c = 15.1666 (11) ŵ = 1.98 mm1
α = 113.527 (8)°T = 200 K
β = 98.425 (7)°Platelet, yellow
γ = 108.557 (8)°0.25 × 0.10 × 0.03 mm
V = 2067.3 (3) Å3
Data collection top
Rigaku R-AXIS RAPID
diffractometer
15410 independent reflections
Radiation source: fine-focus sealed tube15064 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.027
Detector resolution: 10.000 pixels mm-1θmax = 27.5°, θmin = 3.1°
ω scansh = 1614
Absorption correction: multi-scan
(ABSCOR; Rigaku, 1995)
k = 1617
Tmin = 0.730, Tmax = 0.916l = 1919
20447 measured reflections
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.025H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.062 w = 1/[σ2(Fo2) + (0.0317P)2 + 0.9989P]
where P = (Fo2 + 2Fc2)/3
S = 1.08(Δ/σ)max = 0.001
15410 reflectionsΔρmax = 1.52 e Å3
1052 parametersΔρmin = 0.68 e Å3
67 restraintsAbsolute structure: Flack (1983), 6026 Friedel pairs
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.024 (13)
Crystal data top
[Pd4(C5H9NO2S)4]·9.75H2Oγ = 108.557 (8)°
Mr = 1190.03V = 2067.3 (3) Å3
Triclinic, P1Z = 2
a = 12.4517 (3) ÅMo Kα radiation
b = 13.2680 (4) ŵ = 1.98 mm1
c = 15.1666 (11) ÅT = 200 K
α = 113.527 (8)°0.25 × 0.10 × 0.03 mm
β = 98.425 (7)°
Data collection top
Rigaku R-AXIS RAPID
diffractometer
15410 independent reflections
Absorption correction: multi-scan
(ABSCOR; Rigaku, 1995)
15064 reflections with I > 2σ(I)
Tmin = 0.730, Tmax = 0.916Rint = 0.027
20447 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.025H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.062Δρmax = 1.52 e Å3
S = 1.08Δρmin = 0.68 e Å3
15410 reflectionsAbsolute structure: Flack (1983), 6026 Friedel pairs
1052 parametersAbsolute structure parameter: 0.024 (13)
67 restraints
Special details top

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 F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Pd10.56254 (2)0.15412 (2)0.01146 (2)0.01755 (6)
Pd20.41117 (2)0.20457 (2)0.15893 (2)0.01745 (6)
Pd30.65618 (3)0.29031 (2)0.35747 (2)0.01965 (7)
Pd40.80963 (2)0.23751 (2)0.19018 (2)0.01745 (6)
Pd50.38317 (2)0.68823 (2)0.09373 (2)0.01653 (6)
Pd60.64056 (2)0.76363 (2)0.08388 (2)0.01663 (6)
Pd70.52043 (2)0.81899 (2)0.27928 (2)0.01811 (6)
Pd80.26082 (2)0.75142 (2)0.10469 (2)0.01650 (6)
S10.48748 (9)0.28612 (8)0.06247 (7)0.02000 (19)
S20.53843 (9)0.36787 (8)0.30163 (7)0.01988 (19)
S30.80787 (9)0.39725 (8)0.32436 (7)0.02019 (19)
S40.75113 (9)0.30047 (8)0.08309 (7)0.01972 (19)
S50.49291 (8)0.59918 (8)0.05455 (7)0.01876 (19)
S60.58784 (9)0.68416 (9)0.18395 (7)0.01953 (19)
S70.33138 (8)0.67908 (8)0.20419 (7)0.01933 (19)
S80.23872 (8)0.59553 (8)0.04008 (7)0.01813 (18)
O10.2813 (2)0.0429 (2)0.0384 (2)0.0231 (6)
O20.1159 (3)0.0122 (3)0.0646 (2)0.0332 (7)
O30.5311 (3)0.1763 (3)0.3917 (3)0.0332 (7)
O40.4366 (4)0.2102 (4)0.5046 (3)0.0484 (10)
O50.8676 (3)0.1593 (3)0.2715 (2)0.0272 (6)
O61.0310 (3)0.2146 (4)0.3895 (3)0.0510 (11)
O70.6082 (2)0.0152 (2)0.0941 (2)0.0231 (6)
O80.7179 (3)0.0477 (3)0.1856 (2)0.0299 (7)
O90.7102 (3)0.8570 (2)0.0075 (2)0.0238 (6)
O100.8157 (3)0.8105 (3)0.0954 (2)0.0333 (7)
O110.6842 (3)0.9670 (3)0.3624 (2)0.0282 (7)
O120.8575 (3)1.0212 (4)0.4671 (3)0.0553 (11)
O130.2651 (3)0.9032 (3)0.2224 (2)0.0260 (6)
O140.2040 (3)0.9751 (3)0.3530 (3)0.0410 (9)
O150.2990 (2)0.7811 (3)0.1378 (2)0.0229 (6)
O160.1355 (3)0.7755 (3)0.2233 (2)0.0275 (6)
N10.3900 (3)0.0411 (3)0.1125 (2)0.0203 (7)
H10.39350.02110.17720.024*
H1A0.36490.02920.10790.024*
N20.3325 (3)0.1506 (3)0.2542 (3)0.0240 (7)
H20.25170.12750.23010.029*
H2A0.34330.08310.24840.029*
N30.7798 (3)0.2570 (4)0.4357 (3)0.0296 (8)
H30.77630.28230.50080.036*
H3A0.75650.17480.40610.036*
N40.8342 (3)0.1127 (3)0.0675 (2)0.0203 (7)
H40.90890.11600.08870.024*
H4A0.77970.03690.05060.024*
N50.5071 (3)0.7408 (3)0.1641 (2)0.0194 (7)
H50.46590.71400.23030.023*
H5A0.54200.82390.13300.023*
N60.7913 (3)0.8925 (3)0.2088 (2)0.0236 (7)
H60.85740.89850.18740.028*
H6A0.78700.96600.23010.028*
N70.4558 (3)0.9259 (3)0.3788 (2)0.0208 (7)
H70.49720.94750.44360.025*
H7A0.47330.99570.37370.025*
N80.1709 (3)0.7980 (3)0.0124 (2)0.0210 (7)
H80.11110.81270.03700.025*
H8A0.22320.86980.01950.025*
C10.3559 (4)0.2285 (4)0.0483 (3)0.0234 (8)
C20.2972 (4)0.0906 (4)0.0983 (3)0.0209 (8)
H2B0.24140.06000.16680.025*
C30.2244 (4)0.0447 (4)0.0382 (3)0.0229 (8)
C40.4041 (5)0.2698 (4)0.1216 (3)0.0317 (10)
H4C0.33720.24620.17940.047*
H4D0.45700.23160.14580.047*
H4E0.44870.35780.08630.047*
C50.2723 (4)0.2883 (4)0.0111 (4)0.0348 (10)
H5C0.31250.37560.01370.052*
H5D0.25210.27340.04390.052*
H5E0.19920.25400.06720.052*
C60.4359 (4)0.3684 (4)0.3796 (3)0.0265 (9)
C70.3745 (4)0.2393 (4)0.3644 (3)0.0218 (8)
H7B0.30230.23380.38690.026*
C80.4521 (4)0.2079 (4)0.4268 (3)0.0258 (9)
C90.3439 (5)0.4063 (5)0.3404 (4)0.0391 (12)
H9C0.29430.41800.38490.059*
H9D0.29320.34320.27160.059*
H9E0.38490.48210.33940.059*
C100.5084 (5)0.4600 (4)0.4895 (4)0.0350 (11)
H10C0.54440.54070.49550.052*
H10D0.57160.43830.51200.052*
H10E0.45610.46000.53190.052*
C110.9312 (4)0.4296 (4)0.4314 (3)0.0254 (9)
C120.9076 (4)0.3144 (4)0.4416 (3)0.0249 (9)
H12B0.95890.33840.51010.030*
C130.9386 (4)0.2236 (4)0.3631 (3)0.0213 (8)
C140.9306 (5)0.5310 (5)0.5255 (4)0.0455 (13)
H14C1.00040.55870.58250.068*
H14D0.85760.50100.54190.068*
H14E0.93340.59830.51260.068*
C151.0490 (4)0.4763 (4)0.4098 (4)0.0375 (11)
H15C1.05450.54400.39650.056*
H15D1.05130.41110.35050.056*
H15E1.11630.50360.46870.056*
C160.8366 (3)0.2537 (3)0.0042 (3)0.0202 (8)
C170.8233 (3)0.1252 (4)0.0265 (3)0.0207 (8)
H17B0.89110.11370.05080.025*
C180.7080 (3)0.0242 (3)0.1089 (3)0.0200 (8)
C190.9684 (4)0.3435 (4)0.0515 (3)0.0288 (9)
H19C1.01580.32530.00600.043*
H19D0.99790.33640.11130.043*
H19E0.97530.42610.07260.043*
C200.7879 (4)0.2604 (4)0.0998 (3)0.0266 (9)
H20C0.78410.33880.08030.040*
H20D0.70780.19550.13870.040*
H20E0.84080.25130.14150.040*
C210.5636 (4)0.5795 (3)0.1569 (3)0.0206 (8)
C220.6039 (3)0.6977 (4)0.1639 (3)0.0197 (8)
H22B0.62040.68010.22980.024*
C230.7192 (4)0.7945 (4)0.0790 (3)0.0220 (8)
C240.4685 (4)0.4759 (4)0.2548 (3)0.0304 (10)
H24C0.50370.45900.30990.046*
H24D0.40340.49840.27120.046*
H24E0.43720.40370.24640.046*
C250.6677 (4)0.5470 (4)0.1301 (4)0.0303 (10)
H25C0.63610.46680.13450.045*
H25D0.72010.60700.06100.045*
H25E0.71320.54660.17760.045*
C260.7410 (4)0.7371 (4)0.2672 (3)0.0253 (9)
C270.8110 (4)0.8710 (4)0.2986 (3)0.0215 (8)
H27B0.89780.89080.32350.026*
C280.7823 (4)0.9590 (4)0.3831 (3)0.0262 (9)
C290.7994 (4)0.6606 (5)0.2034 (4)0.0359 (11)
H29C0.80810.67790.14710.054*
H29D0.74890.57460.17660.054*
H29E0.87810.68080.24610.054*
C300.7311 (5)0.7148 (5)0.3579 (4)0.0364 (11)
H30C0.81120.74470.40370.055*
H30D0.68880.62790.33390.055*
H30E0.68700.75730.39410.055*
C310.2743 (4)0.7331 (4)0.3133 (3)0.0211 (8)
C320.3264 (4)0.8728 (4)0.3654 (3)0.0190 (8)
H32B0.31720.90120.43450.023*
C330.2592 (4)0.9188 (3)0.3094 (3)0.0210 (8)
C340.3183 (4)0.6923 (4)0.3870 (3)0.0283 (9)
H34C0.29120.72070.44610.042*
H34D0.40570.72610.40880.042*
H34E0.28610.60380.35320.042*
C350.1378 (4)0.6754 (4)0.2741 (3)0.0266 (9)
H35C0.10880.58720.24010.040*
H35D0.11050.70100.22600.040*
H35E0.10670.70110.33110.040*
C360.1010 (3)0.5834 (3)0.1193 (3)0.0211 (8)
C370.1163 (3)0.7115 (3)0.0981 (3)0.0174 (7)
H37B0.03470.70790.11930.021*
C380.1877 (3)0.7582 (3)0.1584 (3)0.0176 (7)
C390.0021 (4)0.5281 (4)0.0858 (4)0.0327 (10)
H39C0.07720.51560.12850.049*
H39D0.01080.58270.01500.049*
H39E0.00590.45030.09260.049*
C400.0796 (4)0.4998 (4)0.2302 (3)0.0306 (10)
H40C0.07870.42260.23790.046*
H40D0.14370.53730.25260.046*
H40E0.00270.48570.27140.046*
O170.2360 (3)0.7792 (3)0.6258 (3)0.0368 (8)
H17F0.295 (4)0.846 (3)0.647 (3)0.044*
H17G0.213 (4)0.779 (4)0.676 (3)0.044*
O180.3581 (3)0.6315 (3)0.6191 (3)0.0376 (8)
H18F0.323 (4)0.677 (4)0.632 (4)0.045*
H18G0.422 (3)0.665 (4)0.609 (4)0.045*
O190.9512 (3)0.0057 (3)0.7877 (3)0.0372 (8)
H19F0.881 (2)0.021 (5)0.792 (4)0.045*
H19G0.997 (3)0.010 (5)0.823 (4)0.045*
O200.5778 (3)0.7806 (3)0.6202 (2)0.0372 (8)
H20F0.635 (3)0.768 (5)0.601 (3)0.045*
H20G0.603 (4)0.826 (4)0.6846 (16)0.045*
O210.7559 (3)0.7161 (4)0.5734 (3)0.0460 (9)
H21F0.782 (4)0.694 (5)0.615 (4)0.055*
H21G0.818 (3)0.772 (4)0.576 (4)0.055*
O220.8781 (3)0.6974 (4)0.7329 (3)0.0414 (9)
H22F0.859 (4)0.728 (5)0.786 (3)0.050*
H22G0.947 (3)0.749 (4)0.742 (4)0.050*
O230.5672 (3)0.9673 (3)0.5820 (3)0.0363 (8)
H23F0.563 (4)0.904 (3)0.585 (4)0.044*
H23G0.641 (2)1.013 (4)0.600 (4)0.044*
O240.0002 (3)0.2202 (4)0.7741 (3)0.0449 (9)
H24F0.012 (5)0.157 (4)0.779 (5)0.054*
H24G0.060 (4)0.235 (5)0.753 (4)0.054*
O250.7894 (3)0.1475 (3)0.6288 (3)0.0416 (8)
H25F0.858 (3)0.178 (5)0.674 (3)0.050*
H25G0.802 (4)0.116 (5)0.572 (2)0.050*
O260.4061 (3)0.0111 (3)0.6861 (3)0.0386 (8)
H26F0.464 (3)0.007 (5)0.663 (4)0.046*
H26G0.362 (4)0.026 (5)0.649 (4)0.046*
O270.0682 (3)0.0366 (3)0.2512 (2)0.0374 (8)
H27F0.040 (4)0.077 (4)0.293 (3)0.045*
H27G0.115 (4)0.018 (5)0.282 (3)0.045*
O280.9639 (3)0.8198 (4)0.0690 (3)0.0405 (8)
H28F0.930 (5)0.835 (5)0.028 (3)0.049*
H28G0.996 (5)0.875 (4)0.1274 (18)0.049*
O290.0768 (3)0.1372 (4)0.1199 (3)0.0439 (9)
H29F0.078 (6)0.096 (4)0.059 (2)0.053*
H29G0.069 (6)0.091 (4)0.147 (4)0.053*
O300.9422 (4)0.9185 (4)0.5849 (3)0.0563 (11)
H30F0.961 (6)0.983 (3)0.578 (4)0.068*
H30G0.954 (6)0.940 (5)0.6485 (19)0.068*
O310.2735 (4)0.0901 (4)0.5859 (3)0.0523 (10)
H31F0.213 (4)0.025 (4)0.549 (4)0.063*
H31G0.315 (5)0.109 (5)0.550 (4)0.063*
O320.1683 (6)0.2489 (5)0.6778 (5)0.094 (2)
H32F0.144 (4)0.263 (5)0.626 (4)0.113*
H32G0.202 (8)0.202 (7)0.651 (6)0.113*
O330.0993 (5)0.8375 (5)0.4988 (4)0.0651 (13)
H33F0.111 (6)0.797 (6)0.530 (5)0.078*
H33G0.056 (6)0.871 (6)0.529 (5)0.078*
O340.2066 (5)0.3892 (5)0.5768 (4)0.0731 (15)
H34F0.267 (4)0.450 (5)0.587 (5)0.088*
H34G0.164 (5)0.353 (6)0.514 (2)0.088*
O35A0.6203 (8)0.2636 (7)0.6738 (6)0.0473 (18)0.50
H35F0.673 (8)0.236 (11)0.662 (8)0.057*0.50
H35G0.562 (7)0.227 (10)0.620 (5)0.057*0.50
O35B0.7105 (7)0.3189 (8)0.6173 (6)0.0428 (18)0.50
H35H0.645 (5)0.323 (10)0.613 (9)0.051*0.50
H35I0.710 (9)0.258 (7)0.622 (10)0.051*0.50
O36A0.7793 (9)0.4317 (7)0.6403 (6)0.060 (3)0.50
H36F0.790 (12)0.506 (4)0.669 (10)0.072*0.50
H36G0.736 (12)0.395 (9)0.666 (10)0.072*0.50
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pd10.01898 (15)0.01577 (14)0.01867 (14)0.00661 (11)0.00782 (11)0.00872 (11)
Pd20.01978 (15)0.01643 (14)0.01862 (14)0.00832 (11)0.00777 (11)0.00939 (11)
Pd30.02208 (15)0.02032 (15)0.02266 (15)0.01175 (12)0.01158 (12)0.01195 (12)
Pd40.01941 (15)0.01653 (14)0.01521 (13)0.00718 (11)0.00666 (10)0.00626 (11)
Pd50.01712 (14)0.01635 (13)0.01776 (13)0.00712 (11)0.00635 (10)0.00918 (11)
Pd60.01805 (14)0.01675 (13)0.01560 (13)0.00801 (11)0.00604 (10)0.00728 (11)
Pd70.02024 (15)0.01885 (14)0.01730 (14)0.01009 (11)0.00649 (11)0.00875 (12)
Pd80.02006 (14)0.01697 (14)0.01576 (13)0.00908 (11)0.00712 (10)0.00920 (11)
S10.0235 (5)0.0168 (4)0.0221 (5)0.0086 (4)0.0102 (4)0.0104 (4)
S20.0233 (5)0.0166 (4)0.0219 (4)0.0090 (4)0.0090 (4)0.0098 (4)
S30.0230 (5)0.0175 (4)0.0194 (4)0.0084 (4)0.0091 (4)0.0074 (4)
S40.0221 (5)0.0164 (4)0.0191 (4)0.0065 (4)0.0075 (3)0.0078 (4)
S50.0205 (5)0.0167 (4)0.0191 (4)0.0081 (3)0.0059 (3)0.0082 (4)
S60.0226 (5)0.0199 (4)0.0191 (4)0.0102 (4)0.0081 (3)0.0103 (4)
S70.0225 (5)0.0186 (4)0.0198 (4)0.0110 (4)0.0076 (3)0.0095 (4)
S80.0210 (5)0.0170 (4)0.0194 (4)0.0082 (4)0.0083 (3)0.0104 (4)
O10.0247 (15)0.0210 (14)0.0206 (14)0.0049 (11)0.0053 (11)0.0114 (12)
O20.0210 (15)0.050 (2)0.0358 (17)0.0146 (14)0.0108 (12)0.0262 (16)
O30.0333 (17)0.0367 (17)0.057 (2)0.0233 (14)0.0292 (15)0.0353 (16)
O40.057 (2)0.083 (3)0.037 (2)0.045 (2)0.0266 (17)0.041 (2)
O50.0362 (17)0.0256 (15)0.0163 (13)0.0162 (13)0.0044 (11)0.0057 (12)
O60.042 (2)0.056 (2)0.0342 (19)0.0325 (18)0.0008 (15)0.0023 (17)
O70.0176 (13)0.0153 (13)0.0292 (15)0.0049 (10)0.0078 (11)0.0054 (11)
O80.0266 (15)0.0299 (16)0.0197 (14)0.0110 (13)0.0062 (11)0.0004 (12)
O90.0273 (15)0.0221 (14)0.0219 (14)0.0072 (11)0.0127 (11)0.0111 (12)
O100.0231 (16)0.0492 (19)0.0283 (16)0.0150 (14)0.0128 (12)0.0174 (15)
O110.0262 (15)0.0218 (14)0.0311 (16)0.0112 (12)0.0068 (12)0.0075 (13)
O120.040 (2)0.072 (3)0.0229 (17)0.0284 (19)0.0025 (14)0.0044 (18)
O130.0420 (18)0.0267 (15)0.0194 (14)0.0219 (14)0.0109 (12)0.0138 (12)
O140.062 (2)0.064 (2)0.0338 (18)0.055 (2)0.0265 (16)0.0299 (17)
O150.0225 (14)0.0262 (15)0.0283 (15)0.0109 (12)0.0103 (11)0.0191 (12)
O160.0275 (16)0.0426 (18)0.0295 (15)0.0192 (13)0.0126 (12)0.0278 (14)
N10.0219 (17)0.0180 (16)0.0216 (16)0.0065 (13)0.0098 (13)0.0104 (13)
N20.0240 (18)0.0231 (17)0.0253 (17)0.0060 (14)0.0113 (14)0.0135 (15)
N30.038 (2)0.043 (2)0.034 (2)0.0275 (18)0.0237 (16)0.0291 (18)
N40.0210 (16)0.0196 (16)0.0208 (16)0.0101 (13)0.0092 (13)0.0080 (13)
N50.0165 (15)0.0218 (16)0.0188 (15)0.0073 (13)0.0074 (12)0.0087 (13)
N60.0226 (17)0.0241 (17)0.0196 (16)0.0041 (13)0.0060 (13)0.0109 (14)
N70.0251 (17)0.0187 (16)0.0194 (16)0.0102 (13)0.0054 (13)0.0096 (13)
N80.0234 (17)0.0212 (16)0.0224 (16)0.0105 (13)0.0120 (13)0.0113 (14)
C10.029 (2)0.022 (2)0.024 (2)0.0120 (16)0.0071 (16)0.0146 (17)
C20.025 (2)0.027 (2)0.0171 (18)0.0140 (16)0.0090 (15)0.0131 (16)
C30.023 (2)0.022 (2)0.0225 (19)0.0092 (16)0.0086 (15)0.0095 (16)
C40.051 (3)0.023 (2)0.029 (2)0.015 (2)0.0132 (19)0.0197 (18)
C50.039 (3)0.033 (2)0.042 (3)0.024 (2)0.014 (2)0.020 (2)
C60.031 (2)0.023 (2)0.029 (2)0.0149 (18)0.0151 (17)0.0095 (17)
C70.0203 (19)0.023 (2)0.0229 (19)0.0114 (16)0.0115 (15)0.0083 (16)
C80.025 (2)0.021 (2)0.031 (2)0.0094 (16)0.0098 (17)0.0129 (17)
C90.041 (3)0.044 (3)0.058 (3)0.033 (2)0.030 (2)0.032 (3)
C100.047 (3)0.027 (2)0.030 (2)0.015 (2)0.021 (2)0.0093 (19)
C110.025 (2)0.022 (2)0.0207 (19)0.0097 (16)0.0010 (15)0.0043 (16)
C120.024 (2)0.033 (2)0.0173 (19)0.0167 (18)0.0050 (15)0.0083 (17)
C130.0222 (19)0.0197 (19)0.0174 (18)0.0094 (15)0.0030 (14)0.0053 (15)
C140.064 (4)0.033 (3)0.024 (2)0.028 (3)0.002 (2)0.002 (2)
C150.024 (2)0.036 (3)0.043 (3)0.0050 (19)0.0066 (19)0.017 (2)
C160.0216 (19)0.0176 (18)0.0190 (18)0.0039 (15)0.0084 (14)0.0091 (15)
C170.0177 (19)0.0222 (19)0.0198 (19)0.0048 (15)0.0080 (14)0.0099 (16)
C180.0191 (19)0.0199 (18)0.0218 (19)0.0088 (15)0.0060 (14)0.0102 (16)
C190.021 (2)0.027 (2)0.028 (2)0.0012 (16)0.0053 (16)0.0099 (18)
C200.030 (2)0.027 (2)0.023 (2)0.0080 (18)0.0112 (17)0.0152 (18)
C210.024 (2)0.0187 (18)0.0196 (18)0.0116 (16)0.0088 (15)0.0073 (15)
C220.0201 (19)0.0228 (19)0.0169 (18)0.0093 (15)0.0081 (14)0.0090 (16)
C230.027 (2)0.0194 (19)0.0212 (19)0.0105 (16)0.0061 (15)0.0103 (16)
C240.040 (3)0.020 (2)0.022 (2)0.0063 (18)0.0077 (18)0.0076 (17)
C250.035 (2)0.036 (2)0.036 (2)0.026 (2)0.0180 (19)0.021 (2)
C260.026 (2)0.027 (2)0.025 (2)0.0132 (17)0.0029 (16)0.0146 (18)
C270.0210 (19)0.0220 (19)0.0197 (18)0.0094 (16)0.0053 (14)0.0083 (16)
C280.027 (2)0.024 (2)0.023 (2)0.0088 (17)0.0052 (16)0.0087 (17)
C290.032 (2)0.038 (3)0.045 (3)0.025 (2)0.010 (2)0.020 (2)
C300.042 (3)0.037 (3)0.037 (3)0.016 (2)0.007 (2)0.026 (2)
C310.026 (2)0.0209 (19)0.0189 (18)0.0138 (16)0.0083 (15)0.0080 (15)
C320.025 (2)0.0220 (19)0.0166 (17)0.0142 (16)0.0104 (14)0.0110 (15)
C330.026 (2)0.0161 (18)0.0185 (18)0.0102 (15)0.0037 (15)0.0063 (15)
C340.036 (2)0.031 (2)0.030 (2)0.0193 (19)0.0162 (18)0.0196 (19)
C350.028 (2)0.030 (2)0.031 (2)0.0139 (18)0.0149 (17)0.0183 (19)
C360.022 (2)0.0158 (18)0.0212 (19)0.0032 (15)0.0026 (15)0.0094 (16)
C370.0155 (18)0.0196 (18)0.0205 (18)0.0055 (14)0.0063 (14)0.0139 (16)
C380.0199 (19)0.0171 (17)0.0180 (17)0.0086 (14)0.0080 (14)0.0088 (15)
C390.025 (2)0.032 (2)0.036 (2)0.0030 (18)0.0062 (18)0.020 (2)
C400.037 (3)0.024 (2)0.020 (2)0.0036 (18)0.0021 (17)0.0098 (18)
O170.040 (2)0.0383 (19)0.0361 (18)0.0147 (15)0.0203 (15)0.0197 (16)
O180.040 (2)0.0367 (19)0.0373 (19)0.0171 (15)0.0110 (15)0.0177 (16)
O190.0335 (18)0.051 (2)0.0362 (19)0.0196 (16)0.0129 (15)0.0269 (17)
O200.0357 (19)0.0325 (18)0.0287 (17)0.0126 (15)0.0022 (13)0.0051 (14)
O210.047 (2)0.057 (2)0.040 (2)0.0277 (18)0.0133 (17)0.0246 (19)
O220.0326 (18)0.060 (2)0.0297 (17)0.0237 (17)0.0130 (14)0.0149 (17)
O230.0358 (18)0.044 (2)0.0336 (17)0.0187 (15)0.0064 (14)0.0221 (16)
O240.037 (2)0.048 (2)0.062 (3)0.0216 (18)0.0201 (18)0.032 (2)
O250.047 (2)0.043 (2)0.0327 (18)0.0220 (17)0.0151 (15)0.0127 (17)
O260.043 (2)0.050 (2)0.039 (2)0.0259 (18)0.0221 (16)0.0283 (18)
O270.050 (2)0.051 (2)0.0245 (15)0.0407 (17)0.0119 (14)0.0145 (15)
O280.0282 (18)0.056 (2)0.0349 (19)0.0183 (16)0.0068 (14)0.0201 (18)
O290.0353 (19)0.059 (2)0.047 (2)0.0236 (18)0.0222 (17)0.0268 (19)
O300.061 (3)0.067 (3)0.041 (2)0.033 (2)0.0171 (19)0.020 (2)
O310.071 (3)0.071 (3)0.043 (2)0.046 (2)0.032 (2)0.036 (2)
O320.113 (5)0.093 (4)0.161 (6)0.074 (4)0.103 (4)0.093 (4)
O330.072 (3)0.087 (4)0.055 (3)0.046 (3)0.028 (2)0.038 (3)
O340.068 (3)0.063 (3)0.055 (3)0.001 (2)0.010 (2)0.030 (3)
O35A0.053 (5)0.046 (4)0.045 (4)0.025 (4)0.012 (3)0.022 (4)
O35B0.055 (5)0.051 (5)0.031 (4)0.026 (4)0.017 (3)0.023 (3)
O36A0.096 (7)0.037 (4)0.045 (5)0.017 (5)0.049 (5)0.017 (4)
Geometric parameters (Å, º) top
Pd1—O72.079 (3)C12—C131.518 (5)
Pd1—N12.089 (3)C12—H12B1.0000
Pd1—S12.2315 (10)C14—H14C0.9800
Pd1—S42.2867 (10)C14—H14D0.9800
Pd2—O12.086 (3)C14—H14E0.9800
Pd2—N22.087 (3)C15—H15C0.9800
Pd2—S22.2261 (11)C15—H15D0.9800
Pd2—S12.2871 (10)C15—H15E0.9800
Pd3—N32.070 (4)C16—C201.536 (6)
Pd3—O32.085 (3)C16—C191.540 (5)
Pd3—S32.2302 (10)C16—C171.547 (6)
Pd3—S22.2843 (11)C17—C181.527 (5)
Pd4—N42.080 (3)C17—H17B1.0000
Pd4—O52.088 (3)C19—H19C0.9800
Pd4—S42.2338 (11)C19—H19D0.9800
Pd4—S32.2876 (10)C19—H19E0.9800
Pd5—O152.082 (3)C20—H20C0.9800
Pd5—N52.097 (3)C20—H20D0.9800
Pd5—S52.2285 (11)C20—H20E0.9800
Pd5—S82.2869 (9)C21—C241.522 (5)
Pd6—N62.089 (3)C21—C221.539 (6)
Pd6—O92.095 (3)C21—C251.541 (6)
Pd6—S62.2306 (10)C22—C231.527 (5)
Pd6—S52.2819 (10)C22—H22B1.0000
Pd7—N72.076 (3)C24—H24C0.9800
Pd7—O112.080 (3)C24—H24D0.9800
Pd7—S72.2427 (10)C24—H24E0.9800
Pd7—S62.2894 (10)C25—H25C0.9800
Pd8—N82.065 (3)C25—H25D0.9800
Pd8—O132.068 (3)C25—H25E0.9800
Pd8—S82.2382 (10)C26—C301.532 (6)
Pd8—S72.2968 (10)C26—C271.536 (6)
S1—C11.861 (4)C26—C291.544 (6)
S2—C61.863 (4)C27—C281.529 (6)
S3—C111.863 (4)C27—H27B1.0000
S4—C161.856 (4)C29—H29C0.9800
S5—C211.864 (4)C29—H29D0.9800
S6—C261.860 (4)C29—H29E0.9800
S7—C311.865 (4)C30—H30C0.9800
S8—C361.864 (4)C30—H30D0.9800
O1—C31.282 (5)C30—H30E0.9800
O2—C31.226 (5)C31—C341.528 (6)
O3—C81.291 (5)C31—C351.529 (6)
O4—C81.214 (5)C31—C321.548 (5)
O5—C131.285 (5)C32—C331.525 (6)
O6—C131.221 (5)C32—H32B1.0000
O7—C181.273 (5)C34—H34C0.9800
O8—C181.228 (5)C34—H34D0.9800
O9—C231.286 (5)C34—H34E0.9800
O10—C231.233 (5)C35—H35C0.9800
O11—C281.263 (5)C35—H35D0.9800
O12—C281.225 (5)C35—H35E0.9800
O13—C331.269 (5)C36—C401.524 (6)
O14—C331.238 (5)C36—C391.527 (6)
O15—C381.280 (5)C36—C371.538 (5)
O16—C381.238 (5)C37—C381.533 (5)
N1—C21.502 (5)C37—H37B1.0000
N1—H10.9200C39—H39C0.9800
N1—H1A0.9200C39—H39D0.9800
N2—C71.494 (5)C39—H39E0.9800
N2—H20.9200C40—H40C0.9800
N2—H2A0.9200C40—H40D0.9800
N3—C121.501 (6)C40—H40E0.9800
N3—H30.9200O17—H17F0.847 (19)
N3—H3A0.9200O17—H17G0.856 (19)
N4—C171.491 (5)O18—H18F0.841 (19)
N4—H40.9200O18—H18G0.852 (19)
N4—H4A0.9200O19—H19F0.851 (19)
N5—C221.490 (5)O19—H19G0.854 (19)
N5—H50.9200O20—H20F0.845 (19)
N5—H5A0.9200O20—H20G0.858 (19)
N6—C271.501 (5)O21—H21F0.863 (19)
N6—H60.9200O21—H21G0.869 (19)
N6—H6A0.9200O22—H22F0.854 (19)
N7—C321.484 (5)O22—H22G0.859 (19)
N7—H70.9200O23—H23F0.851 (19)
N7—H7A0.9200O23—H23G0.854 (19)
N8—C371.491 (5)O24—H24F0.849 (19)
N8—H80.9200O24—H24G0.851 (19)
N8—H8A0.9200O25—H25F0.865 (19)
C1—C21.529 (6)O25—H25G0.852 (19)
C1—C41.539 (6)O26—H26F0.860 (19)
C1—C51.541 (6)O26—H26G0.851 (19)
C2—C31.535 (5)O27—H27F0.847 (19)
C2—H2B1.0000O27—H27G0.844 (19)
C4—H4C0.9800O28—H28F0.822 (19)
C4—H4D0.9800O28—H28G0.821 (19)
C4—H4E0.9800O29—H29F0.868 (19)
C5—H5C0.9800O29—H29G0.854 (19)
C5—H5D0.9800O30—H30F0.861 (19)
C5—H5E0.9800O30—H30G0.864 (19)
C6—C101.521 (6)O31—H31F0.839 (19)
C6—C91.525 (7)O31—H31G0.858 (19)
C6—C71.540 (6)O32—H32F0.917 (19)
C7—C81.518 (6)O32—H32G0.86 (2)
C7—H7B1.0000O33—H33F0.875 (19)
C9—H9C0.9800O33—H33G0.87 (2)
C9—H9D0.9800O34—H34F0.85 (2)
C9—H9E0.9800O34—H34G0.86 (2)
C10—H10C0.9800O35A—H35F0.85 (2)
C10—H10D0.9800O35A—H35G0.85 (2)
C10—H10E0.9800O35B—H35H0.83 (2)
C11—C141.524 (6)O35B—H35I0.84 (2)
C11—C121.537 (6)O36A—H36F0.85 (2)
C11—C151.539 (6)O36A—H36G0.85 (2)
O7—Pd1—N185.63 (12)C14—C11—C15108.8 (4)
O7—Pd1—S1171.94 (8)C12—C11—C15113.5 (4)
N1—Pd1—S186.31 (9)C14—C11—S3106.2 (3)
O7—Pd1—S498.20 (8)C12—C11—S3109.0 (3)
N1—Pd1—S4168.53 (10)C15—C11—S3107.6 (3)
S1—Pd1—S489.76 (4)N3—C12—C13110.1 (3)
O1—Pd2—N286.93 (12)N3—C12—C11110.2 (3)
O1—Pd2—S2171.92 (8)C13—C12—C11112.9 (4)
N2—Pd2—S285.00 (10)N3—C12—H12B107.8
O1—Pd2—S196.38 (8)C13—C12—H12B107.8
N2—Pd2—S1171.42 (11)C11—C12—H12B107.8
S2—Pd2—S191.67 (4)O6—C13—O5122.2 (4)
N3—Pd3—O385.09 (14)O6—C13—C12118.4 (4)
N3—Pd3—S386.53 (10)O5—C13—C12119.4 (4)
O3—Pd3—S3170.89 (9)C11—C14—H14C109.5
N3—Pd3—S2167.45 (12)C11—C14—H14D109.5
O3—Pd3—S298.63 (9)H14C—C14—H14D109.5
S3—Pd3—S290.31 (4)C11—C14—H14E109.5
N4—Pd4—O585.91 (12)H14C—C14—H14E109.5
N4—Pd4—S485.40 (10)H14D—C14—H14E109.5
O5—Pd4—S4171.31 (8)C11—C15—H15C109.5
N4—Pd4—S3170.89 (9)C11—C15—H15D109.5
O5—Pd4—S397.34 (8)H15C—C15—H15D109.5
S4—Pd4—S391.28 (4)C11—C15—H15E109.5
O15—Pd5—N586.31 (12)H15C—C15—H15E109.5
O15—Pd5—S5172.13 (8)H15D—C15—H15E109.5
N5—Pd5—S585.87 (10)C20—C16—C19111.0 (3)
O15—Pd5—S897.94 (8)C20—C16—C17112.9 (3)
N5—Pd5—S8169.40 (9)C19—C16—C17109.6 (4)
S5—Pd5—S889.92 (4)C20—C16—S4107.7 (3)
N6—Pd6—O986.45 (12)C19—C16—S4107.0 (3)
N6—Pd6—S685.64 (10)C17—C16—S4108.5 (3)
O9—Pd6—S6172.08 (8)N4—C17—C18109.7 (3)
N6—Pd6—S5169.28 (11)N4—C17—C16111.1 (3)
O9—Pd6—S596.66 (8)C18—C17—C16114.0 (4)
S6—Pd6—S591.20 (4)N4—C17—H17B107.2
N7—Pd7—O1184.28 (12)C18—C17—H17B107.2
N7—Pd7—S786.56 (9)C16—C17—H17B107.2
O11—Pd7—S7170.76 (9)O8—C18—O7123.4 (4)
N7—Pd7—S6170.75 (10)O8—C18—C17117.0 (4)
O11—Pd7—S698.17 (9)O7—C18—C17119.6 (3)
S7—Pd7—S691.07 (4)C16—C19—H19C109.5
N8—Pd8—O1384.85 (12)C16—C19—H19D109.5
N8—Pd8—S885.18 (9)H19C—C19—H19D109.5
O13—Pd8—S8170.03 (9)C16—C19—H19E109.5
N8—Pd8—S7170.92 (9)H19C—C19—H19E109.5
O13—Pd8—S796.17 (8)H19D—C19—H19E109.5
S8—Pd8—S793.65 (4)C16—C20—H20C109.5
C1—S1—Pd197.60 (14)C16—C20—H20D109.5
C1—S1—Pd2104.04 (13)H20C—C20—H20D109.5
Pd1—S1—Pd297.42 (4)C16—C20—H20E109.5
C6—S2—Pd297.34 (14)H20C—C20—H20E109.5
C6—S2—Pd3102.37 (15)H20D—C20—H20E109.5
Pd2—S2—Pd3100.53 (4)C24—C21—C22110.5 (3)
C11—S3—Pd397.93 (14)C24—C21—C25110.5 (4)
C11—S3—Pd4103.18 (14)C22—C21—C25113.1 (3)
Pd3—S3—Pd496.90 (4)C24—C21—S5106.9 (3)
C16—S4—Pd498.06 (14)C22—C21—S5108.0 (3)
C16—S4—Pd1101.06 (12)C25—C21—S5107.6 (3)
Pd4—S4—Pd1102.42 (4)N5—C22—C23111.5 (3)
C21—S5—Pd598.24 (13)N5—C22—C21110.6 (3)
C21—S5—Pd6102.92 (12)C23—C22—C21111.3 (3)
Pd5—S5—Pd699.24 (4)N5—C22—H22B107.8
C26—S6—Pd697.13 (14)C23—C22—H22B107.8
C26—S6—Pd7103.20 (14)C21—C22—H22B107.8
Pd6—S6—Pd799.03 (4)O10—C23—O9122.8 (4)
C31—S7—Pd797.98 (13)O10—C23—C22119.7 (4)
C31—S7—Pd8102.32 (14)O9—C23—C22117.5 (4)
Pd7—S7—Pd899.57 (4)C21—C24—H24C109.5
C36—S8—Pd897.79 (13)C21—C24—H24D109.5
C36—S8—Pd5102.08 (13)H24C—C24—H24D109.5
Pd8—S8—Pd5101.17 (4)C21—C24—H24E109.5
C3—O1—Pd2119.2 (3)H24C—C24—H24E109.5
C8—O3—Pd3119.8 (3)H24D—C24—H24E109.5
C13—O5—Pd4121.7 (3)C21—C25—H25C109.5
C18—O7—Pd1127.7 (2)C21—C25—H25D109.5
C23—O9—Pd6117.0 (2)H25C—C25—H25D109.5
C28—O11—Pd7124.1 (3)C21—C25—H25E109.5
C33—O13—Pd8127.9 (3)H25C—C25—H25E109.5
C38—O15—Pd5127.3 (2)H25D—C25—H25E109.5
C2—N1—Pd1116.6 (2)C30—C26—C27112.9 (4)
C2—N1—H1108.1C30—C26—C29110.1 (4)
Pd1—N1—H1108.1C27—C26—C29109.9 (4)
C2—N1—H1A108.1C30—C26—S6108.5 (3)
Pd1—N1—H1A108.1C27—C26—S6108.7 (3)
H1—N1—H1A107.3C29—C26—S6106.6 (3)
C7—N2—Pd2118.2 (2)N6—C27—C28108.8 (3)
C7—N2—H2107.8N6—C27—C26110.5 (3)
Pd2—N2—H2107.8C28—C27—C26114.7 (3)
C7—N2—H2A107.8N6—C27—H27B107.5
Pd2—N2—H2A107.8C28—C27—H27B107.5
H2—N2—H2A107.1C26—C27—H27B107.5
C12—N3—Pd3117.4 (3)O12—C28—O11123.1 (4)
C12—N3—H3108.0O12—C28—C27118.1 (4)
Pd3—N3—H3108.0O11—C28—C27118.7 (4)
C12—N3—H3A108.0C26—C29—H29C109.5
Pd3—N3—H3A108.0C26—C29—H29D109.5
H3—N3—H3A107.2H29C—C29—H29D109.5
C17—N4—Pd4118.0 (3)C26—C29—H29E109.5
C17—N4—H4107.8H29C—C29—H29E109.5
Pd4—N4—H4107.8H29D—C29—H29E109.5
C17—N4—H4A107.8C26—C30—H30C109.5
Pd4—N4—H4A107.8C26—C30—H30D109.5
H4—N4—H4A107.1H30C—C30—H30D109.5
C22—N5—Pd5116.9 (2)C26—C30—H30E109.5
C22—N5—H5108.1H30C—C30—H30E109.5
Pd5—N5—H5108.1H30D—C30—H30E109.5
C22—N5—H5A108.1C34—C31—C35110.1 (3)
Pd5—N5—H5A108.1C34—C31—C32109.8 (3)
H5—N5—H5A107.3C35—C31—C32112.2 (3)
C27—N6—Pd6117.2 (2)C34—C31—S7107.3 (3)
C27—N6—H6108.0C35—C31—S7108.7 (3)
Pd6—N6—H6108.0C32—C31—S7108.6 (3)
C27—N6—H6A108.0N7—C32—C33110.7 (3)
Pd6—N6—H6A108.0N7—C32—C31111.4 (3)
H6—N6—H6A107.2C33—C32—C31112.4 (3)
C32—N7—Pd7117.2 (2)N7—C32—H32B107.4
C32—N7—H7108.0C33—C32—H32B107.4
Pd7—N7—H7108.0C31—C32—H32B107.4
C32—N7—H7A108.0O14—C33—O13122.0 (4)
Pd7—N7—H7A108.0O14—C33—C32118.1 (4)
H7—N7—H7A107.2O13—C33—C32119.8 (4)
C37—N8—Pd8118.7 (2)C31—C34—H34C109.5
C37—N8—H8107.6C31—C34—H34D109.5
Pd8—N8—H8107.6H34C—C34—H34D109.5
C37—N8—H8A107.6C31—C34—H34E109.5
Pd8—N8—H8A107.6H34C—C34—H34E109.5
H8—N8—H8A107.1H34D—C34—H34E109.5
C2—C1—C4110.4 (3)C31—C35—H35C109.5
C2—C1—C5113.6 (4)C31—C35—H35D109.5
C4—C1—C5109.2 (4)H35C—C35—H35D109.5
C2—C1—S1108.8 (3)C31—C35—H35E109.5
C4—C1—S1106.4 (3)H35C—C35—H35E109.5
C5—C1—S1108.2 (3)H35D—C35—H35E109.5
N1—C2—C1110.1 (3)C40—C36—C39109.5 (3)
N1—C2—C3110.5 (3)C40—C36—C37113.2 (3)
C1—C2—C3112.4 (3)C39—C36—C37109.8 (4)
N1—C2—H2B107.9C40—C36—S8109.0 (3)
C1—C2—H2B107.9C39—C36—S8106.9 (3)
C3—C2—H2B107.9C37—C36—S8108.3 (3)
O2—C3—O1123.1 (4)N8—C37—C38110.4 (3)
O2—C3—C2119.4 (4)N8—C37—C36110.9 (3)
O1—C3—C2117.6 (4)C38—C37—C36113.3 (3)
C1—C4—H4C109.5N8—C37—H37B107.3
C1—C4—H4D109.5C38—C37—H37B107.3
H4C—C4—H4D109.5C36—C37—H37B107.3
C1—C4—H4E109.5O16—C38—O15122.7 (3)
H4C—C4—H4E109.5O16—C38—C37118.2 (3)
H4D—C4—H4E109.5O15—C38—C37119.1 (3)
C1—C5—H5C109.5C36—C39—H39C109.5
C1—C5—H5D109.5C36—C39—H39D109.5
H5C—C5—H5D109.5H39C—C39—H39D109.5
C1—C5—H5E109.5C36—C39—H39E109.5
H5C—C5—H5E109.5H39C—C39—H39E109.5
H5D—C5—H5E109.5H39D—C39—H39E109.5
C10—C6—C9110.3 (4)C36—C40—H40C109.5
C10—C6—C7112.6 (4)C36—C40—H40D109.5
C9—C6—C7110.4 (4)H40C—C40—H40D109.5
C10—C6—S2108.4 (3)C36—C40—H40E109.5
C9—C6—S2106.8 (3)H40C—C40—H40E109.5
C7—C6—S2108.2 (3)H40D—C40—H40E109.5
N2—C7—C8111.4 (3)H17F—O17—H17G108 (3)
N2—C7—C6109.7 (3)H18F—O18—H18G109 (3)
C8—C7—C6113.4 (3)H19F—O19—H19G110 (3)
N2—C7—H7B107.3H20F—O20—H20G108 (3)
C8—C7—H7B107.3H21F—O21—H21G105 (3)
C6—C7—H7B107.3H22F—O22—H22G107 (3)
O4—C8—O3122.7 (4)H23F—O23—H23G107 (3)
O4—C8—C7120.2 (4)H24F—O24—H24G108 (3)
O3—C8—C7117.0 (4)H25F—O25—H25G105 (3)
C6—C9—H9C109.5H26F—O26—H26G107 (3)
C6—C9—H9D109.5H27F—O27—H27G109 (3)
H9C—C9—H9D109.5H28F—O28—H28G116 (3)
C6—C9—H9E109.5H29F—O29—H29G106 (3)
H9C—C9—H9E109.5H30F—O30—H30G108 (3)
H9D—C9—H9E109.5H31F—O31—H31G110 (3)
C6—C10—H10C109.5H32F—O32—H32G101 (3)
C6—C10—H10D109.5H33F—O33—H33G103 (3)
H10C—C10—H10D109.5H34F—O34—H34G108 (3)
C6—C10—H10E109.5H35F—O35A—H35G109 (3)
H10C—C10—H10E109.5H35H—O35B—H35I113 (4)
H10D—C10—H10E109.5H36F—O36A—H36G109 (3)
C14—C11—C12111.5 (4)
N1—Pd1—S1—C123.21 (16)Pd2—N2—C7—C8105.8 (3)
S4—Pd1—S1—C1146.02 (13)Pd2—N2—C7—C620.7 (4)
N1—Pd1—S1—Pd282.11 (9)C10—C6—C7—N2165.2 (4)
S4—Pd1—S1—Pd2108.66 (4)C9—C6—C7—N271.1 (4)
O1—Pd2—S1—C133.51 (16)S2—C6—C7—N245.5 (4)
S2—Pd2—S1—C1145.78 (14)C10—C6—C7—C839.9 (5)
O1—Pd2—S1—Pd166.29 (9)C9—C6—C7—C8163.7 (4)
S2—Pd2—S1—Pd1114.43 (4)S2—C6—C7—C879.8 (4)
N2—Pd2—S2—C627.85 (19)Pd3—O3—C8—O4126.5 (4)
S1—Pd2—S2—C6144.23 (15)Pd3—O3—C8—C755.4 (5)
N2—Pd2—S2—Pd376.25 (11)N2—C7—C8—O4134.5 (4)
S1—Pd2—S2—Pd3111.67 (4)C6—C7—C8—O4101.2 (5)
N3—Pd3—S2—C674.5 (5)N2—C7—C8—O343.7 (5)
O3—Pd3—S2—C631.90 (17)C6—C7—C8—O380.7 (5)
S3—Pd3—S2—C6149.81 (14)Pd3—S3—C11—C1477.6 (3)
N3—Pd3—S2—Pd2174.5 (4)Pd4—S3—C11—C14176.7 (3)
O3—Pd3—S2—Pd268.11 (10)Pd3—S3—C11—C1242.6 (3)
S3—Pd3—S2—Pd2110.18 (4)Pd4—S3—C11—C1256.4 (3)
N3—Pd3—S3—C1122.52 (17)Pd3—S3—C11—C15166.0 (3)
S2—Pd3—S3—C11145.32 (14)Pd4—S3—C11—C1567.0 (3)
N3—Pd3—S3—Pd481.89 (11)Pd3—N3—C12—C1399.3 (4)
S2—Pd3—S3—Pd4110.27 (4)Pd3—N3—C12—C1125.9 (4)
O5—Pd4—S3—C1131.59 (17)C14—C11—C12—N371.2 (4)
S4—Pd4—S3—C11147.27 (15)C15—C11—C12—N3165.5 (3)
O5—Pd4—S3—Pd368.27 (9)S3—C11—C12—N345.7 (4)
S4—Pd4—S3—Pd3112.87 (4)C14—C11—C12—C13165.2 (4)
N4—Pd4—S4—C1626.63 (15)C15—C11—C12—C1341.9 (5)
S3—Pd4—S4—C16144.88 (12)S3—C11—C12—C1377.9 (4)
N4—Pd4—S4—Pd176.65 (10)Pd4—O5—C13—O6127.5 (4)
S3—Pd4—S4—Pd1111.85 (4)Pd4—O5—C13—C1252.3 (5)
O7—Pd1—S4—C1629.29 (16)N3—C12—C13—O6133.1 (4)
N1—Pd1—S4—C1679.6 (5)C11—C12—C13—O6103.3 (5)
S1—Pd1—S4—C16149.39 (14)N3—C12—C13—O547.2 (5)
O7—Pd1—S4—Pd471.63 (9)C11—C12—C13—O576.4 (5)
N1—Pd1—S4—Pd4179.5 (5)Pd4—S4—C16—C20166.7 (2)
S1—Pd1—S4—Pd4109.69 (4)Pd1—S4—C16—C2062.3 (3)
N5—Pd5—S5—C2123.67 (15)Pd4—S4—C16—C1974.0 (3)
S8—Pd5—S5—C21146.60 (12)Pd1—S4—C16—C19178.4 (3)
N5—Pd5—S5—Pd680.95 (9)Pd4—S4—C16—C1744.2 (3)
S8—Pd5—S5—Pd6108.78 (4)Pd1—S4—C16—C1760.3 (3)
N6—Pd6—S5—C2170.4 (5)Pd4—N4—C17—C18108.1 (3)
O9—Pd6—S5—C2135.97 (16)Pd4—N4—C17—C1618.9 (4)
S6—Pd6—S5—C21143.07 (14)C20—C16—C17—N4161.8 (3)
N6—Pd6—S5—Pd5171.1 (5)C19—C16—C17—N473.9 (4)
O9—Pd6—S5—Pd564.77 (9)S4—C16—C17—N442.5 (4)
S6—Pd6—S5—Pd5116.19 (4)C20—C16—C17—C1837.2 (5)
N6—Pd6—S6—C2627.51 (18)C19—C16—C17—C18161.4 (3)
S5—Pd6—S6—C26142.24 (14)S4—C16—C17—C1882.1 (3)
N6—Pd6—S6—Pd777.14 (11)Pd1—O7—C18—O8149.9 (3)
S5—Pd6—S6—Pd7113.11 (4)Pd1—O7—C18—C1733.2 (5)
O11—Pd7—S6—C2628.82 (17)N4—C17—C18—O8116.7 (4)
S7—Pd7—S6—C26151.02 (15)C16—C17—C18—O8117.9 (4)
O11—Pd7—S6—Pd670.75 (10)N4—C17—C18—O760.4 (5)
S7—Pd7—S6—Pd6109.40 (4)C16—C17—C18—O765.0 (5)
N7—Pd7—S7—C3122.31 (16)Pd5—S5—C21—C2474.9 (3)
S6—Pd7—S7—C31148.75 (14)Pd6—S5—C21—C24176.4 (3)
N7—Pd7—S7—Pd881.70 (10)Pd5—S5—C21—C2244.1 (3)
S6—Pd7—S7—Pd8107.25 (4)Pd6—S5—C21—C2257.4 (3)
O13—Pd8—S7—C3130.71 (16)Pd5—S5—C21—C25166.4 (3)
S8—Pd8—S7—C31147.56 (13)Pd6—S5—C21—C2564.9 (3)
O13—Pd8—S7—Pd769.71 (9)Pd5—N5—C22—C2398.2 (3)
S8—Pd8—S7—Pd7112.02 (4)Pd5—N5—C22—C2126.2 (4)
N8—Pd8—S8—C3626.71 (15)C24—C21—C22—N569.7 (4)
S7—Pd8—S8—C36144.26 (12)C25—C21—C22—N5165.8 (3)
N8—Pd8—S8—Pd577.31 (10)S5—C21—C22—N546.9 (4)
S7—Pd8—S8—Pd5111.73 (4)C24—C21—C22—C23165.7 (3)
O15—Pd5—S8—C3627.72 (15)C25—C21—C22—C2341.3 (4)
N5—Pd5—S8—C3685.4 (6)S5—C21—C22—C2377.6 (4)
S5—Pd5—S8—C36151.84 (13)Pd6—O9—C23—O10117.2 (4)
O15—Pd5—S8—Pd872.85 (9)Pd6—O9—C23—C2263.4 (4)
N5—Pd5—S8—Pd8174.1 (5)N5—C22—C23—O10138.9 (4)
S5—Pd5—S8—Pd8107.59 (4)C21—C22—C23—O1097.1 (5)
N2—Pd2—O1—C3132.9 (3)N5—C22—C23—O940.6 (5)
S1—Pd2—O1—C339.1 (3)C21—C22—C23—O983.4 (4)
N3—Pd3—O3—C8133.2 (4)Pd6—S6—C26—C30169.5 (3)
S2—Pd3—O3—C834.8 (3)Pd7—S6—C26—C3068.4 (3)
N4—Pd4—O5—C13139.1 (3)Pd6—S6—C26—C2746.4 (3)
S3—Pd4—O5—C1332.4 (3)Pd7—S6—C26—C2754.6 (3)
N1—Pd1—O7—C18149.4 (3)Pd6—S6—C26—C2972.0 (3)
S4—Pd1—O7—C1819.7 (3)Pd7—S6—C26—C29173.0 (3)
N6—Pd6—O9—C23128.3 (3)Pd6—N6—C27—C28106.6 (3)
S5—Pd6—O9—C2341.4 (3)Pd6—N6—C27—C2620.1 (4)
N7—Pd7—O11—C28143.1 (3)C30—C26—C27—N6165.3 (4)
S6—Pd7—O11—C2827.9 (3)C29—C26—C27—N671.4 (4)
N8—Pd8—O13—C33145.6 (4)S6—C26—C27—N644.9 (4)
S7—Pd8—O13—C3325.3 (3)C30—C26—C27—C2842.0 (5)
N5—Pd5—O15—C38150.5 (3)C29—C26—C27—C28165.3 (4)
S8—Pd5—O15—C3819.8 (3)S6—C26—C27—C2878.4 (4)
O7—Pd1—N1—C2178.3 (3)Pd7—O11—C28—O12135.9 (4)
S1—Pd1—N1—C21.9 (2)Pd7—O11—C28—C2746.5 (5)
S4—Pd1—N1—C268.3 (6)N6—C27—C28—O12127.5 (5)
O1—Pd2—N2—C7171.9 (3)C26—C27—C28—O12108.3 (5)
S2—Pd2—N2—C78.5 (3)N6—C27—C28—O1150.2 (5)
O3—Pd3—N3—C12178.3 (3)C26—C27—C28—O1174.0 (5)
S3—Pd3—N3—C121.8 (3)Pd7—S7—C31—C3477.1 (3)
S2—Pd3—N3—C1273.8 (6)Pd8—S7—C31—C34178.8 (2)
O5—Pd4—N4—C17171.7 (3)Pd7—S7—C31—C35163.9 (3)
S4—Pd4—N4—C178.5 (2)Pd8—S7—C31—C3562.2 (3)
O15—Pd5—N5—C22178.4 (3)Pd7—S7—C31—C3241.5 (3)
S5—Pd5—N5—C222.5 (2)Pd8—S7—C31—C3260.2 (3)
S8—Pd5—N5—C2264.3 (6)Pd7—N7—C32—C33100.4 (3)
O9—Pd6—N6—C27171.9 (3)Pd7—N7—C32—C3125.4 (4)
S6—Pd6—N6—C278.6 (3)C34—C31—C32—N772.0 (4)
S5—Pd6—N6—C2764.6 (6)C35—C31—C32—N7165.2 (3)
O11—Pd7—N7—C32179.3 (3)S7—C31—C32—N745.0 (4)
S7—Pd7—N7—C322.0 (3)C34—C31—C32—C33163.1 (3)
O13—Pd8—N8—C37171.1 (3)C35—C31—C32—C3340.3 (4)
S8—Pd8—N8—C378.7 (2)S7—C31—C32—C3379.9 (3)
Pd1—S1—C1—C244.4 (3)Pd8—O13—C33—O14142.1 (4)
Pd2—S1—C1—C255.3 (3)Pd8—O13—C33—C3240.9 (5)
Pd1—S1—C1—C474.6 (3)N7—C32—C33—O14119.8 (4)
Pd2—S1—C1—C4174.3 (3)C31—C32—C33—O14115.0 (4)
Pd1—S1—C1—C5168.2 (3)N7—C32—C33—O1357.4 (5)
Pd2—S1—C1—C568.5 (3)C31—C32—C33—O1367.9 (5)
Pd1—N1—C2—C126.9 (4)Pd8—S8—C36—C40167.9 (2)
Pd1—N1—C2—C397.9 (3)Pd5—S8—C36—C4064.6 (3)
C4—C1—C2—N168.7 (4)Pd8—S8—C36—C3973.9 (3)
C5—C1—C2—N1168.2 (3)Pd5—S8—C36—C39177.1 (3)
S1—C1—C2—N147.7 (4)Pd8—S8—C36—C3744.3 (3)
C4—C1—C2—C3167.6 (4)Pd5—S8—C36—C3758.9 (3)
C5—C1—C2—C344.5 (5)Pd8—N8—C37—C38107.5 (3)
S1—C1—C2—C376.0 (4)Pd8—N8—C37—C3618.9 (4)
Pd2—O1—C3—O2118.8 (4)C40—C36—C37—N8163.6 (3)
Pd2—O1—C3—C260.9 (4)C39—C36—C37—N873.8 (4)
N1—C2—C3—O2137.9 (4)S8—C36—C37—N842.6 (4)
C1—C2—C3—O298.6 (5)C40—C36—C37—C3838.7 (5)
N1—C2—C3—O142.4 (5)C39—C36—C37—C38161.4 (3)
C1—C2—C3—O181.1 (5)S8—C36—C37—C3882.3 (3)
Pd2—S2—C6—C10169.6 (3)Pd5—O15—C38—O16146.6 (3)
Pd3—S2—C6—C1067.1 (3)Pd5—O15—C38—C3735.6 (5)
Pd2—S2—C6—C971.5 (3)N8—C37—C38—O16120.8 (4)
Pd3—S2—C6—C9174.1 (3)C36—C37—C38—O16114.1 (4)
Pd2—S2—C6—C747.3 (3)N8—C37—C38—O1557.1 (5)
Pd3—S2—C6—C755.3 (3)C36—C37—C38—O1568.0 (4)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1···O26i0.922.062.963 (5)169
N1—H1A···O15ii0.922.213.109 (4)166
N2—H2···O270.922.353.139 (5)143
N2—H2A···O13ii0.922.112.928 (5)148
N3—H3···O35B0.922.012.889 (8)160
N3—H3···O36A0.922.233.045 (8)147
N3—H3A···O11ii0.922.373.278 (5)167
N4—H4···O29iii0.921.982.886 (5)170
N4—H4A···O9ii0.922.042.917 (4)160
N5—H5···O18i0.922.093.008 (5)172
N5—H5A···O7iv0.922.193.094 (4)167
N6—H6···O27v0.922.443.183 (5)138
N6—H6···O280.922.483.326 (5)153
N6—H6A···O5iv0.922.213.041 (5)151
N7—H7···O230.922.032.938 (5)170
N7—H7A···O3iv0.922.163.066 (5)169
N8—H8···O28vi0.921.982.896 (5)171
N8—H8A···O1iv0.922.062.930 (4)157
O17—H17F···O26iv0.85 (2)1.96 (2)2.798 (5)167 (6)
O17—H17G···O16vii0.86 (2)1.93 (2)2.775 (4)170 (5)
O18—H18F···O170.84 (2)2.00 (3)2.818 (5)165 (6)
O18—H18G···O200.85 (2)1.98 (2)2.814 (5)165 (5)
O19—H19F···O8vii0.85 (2)2.05 (2)2.892 (5)168 (5)
O19—H19G···O2viii0.85 (2)1.94 (3)2.760 (5)160 (6)
O20—H20F···O210.85 (2)1.88 (2)2.709 (5)167 (6)
O20—H20G···O8ix0.86 (2)1.94 (3)2.742 (4)156 (5)
O21—H21F···O220.86 (2)1.97 (3)2.805 (6)162 (5)
O21—H21G···O300.87 (2)2.00 (2)2.857 (6)169 (6)
O22—H22F···O10vii0.85 (2)1.95 (2)2.802 (5)174 (6)
O22—H22G···O16viii0.86 (2)2.21 (4)2.915 (5)139 (6)
O23—H23F···O200.85 (2)1.96 (2)2.796 (5)168 (5)
O23—H23G···O25iv0.85 (2)1.96 (2)2.782 (5)162 (5)
O24—H24F···O19vi0.85 (2)1.97 (2)2.814 (5)177 (6)
O24—H24G···O320.85 (2)1.90 (2)2.736 (6)168 (6)
O25—H25F···O24iii0.87 (2)1.91 (2)2.770 (6)170 (6)
O25—H25G···O12ii0.85 (2)1.97 (3)2.788 (5)159 (5)
O26—H26F···O23ii0.86 (2)1.95 (2)2.791 (5)167 (6)
O26—H26G···O310.85 (2)1.95 (2)2.788 (6)169 (6)
O27—H27F···O6vi0.85 (2)1.88 (3)2.687 (5)158 (5)
O27—H27G···O14ii0.84 (2)1.81 (2)2.650 (5)175 (5)
O28—H28F···O100.82 (2)2.02 (2)2.810 (5)161 (5)
O28—H28G···O27v0.82 (2)2.00 (3)2.797 (5)164 (5)
O29—H29F···O20.87 (2)1.98 (2)2.834 (5)168 (6)
O29—H29G···O270.85 (2)1.98 (2)2.802 (5)160 (5)
O30—H30F···O120.86 (2)2.28 (5)2.911 (7)130 (6)
O30—H30G···O19iv0.86 (2)1.95 (3)2.791 (5)165 (6)
O31—H31F···O33ii0.84 (2)2.17 (3)2.946 (8)154 (7)
O31—H31G···O40.86 (2)2.08 (2)2.902 (6)161 (5)
O32—H32F···O340.92 (2)2.07 (2)2.823 (7)139 (3)
O32—H32G···O310.86 (2)1.98 (2)2.837 (7)178 (9)
O33—H33F···O170.88 (2)2.11 (4)2.877 (6)146 (7)
O33—H33G···O30vi0.87 (2)1.90 (2)2.766 (6)170 (7)
O34—H34F···O180.85 (2)2.12 (4)2.906 (6)154 (8)
O34—H34G···O6vi0.86 (2)2.02 (3)2.815 (6)154 (6)
O35A—H35F···O250.85 (2)2.14 (3)2.986 (9)174 (13)
O35A—H35G···O40.85 (2)2.05 (5)2.848 (9)157 (12)
O35B—H35H···O40.83 (2)2.45 (8)3.135 (9)141 (10)
O35B—H35I···O250.84 (2)2.03 (5)2.802 (10)152 (9)
O36A—H36F···O220.85 (2)2.14 (5)2.949 (9)159 (12)
O36A—H36G···O35A0.85 (2)1.93 (5)2.746 (12)158 (12)
Symmetry codes: (i) x, y, z1; (ii) x, y1, z; (iii) x+1, y, z; (iv) x, y+1, z; (v) x+1, y+1, z; (vi) x1, y, z; (vii) x, y, z+1; (viii) x+1, y, z+1; (ix) x, y+1, z+1.

Experimental details

Crystal data
Chemical formula[Pd4(C5H9NO2S)4]·9.75H2O
Mr1190.03
Crystal system, space groupTriclinic, P1
Temperature (K)200
a, b, c (Å)12.4517 (3), 13.2680 (4), 15.1666 (11)
α, β, γ (°)113.527 (8), 98.425 (7), 108.557 (8)
V3)2067.3 (3)
Z2
Radiation typeMo Kα
µ (mm1)1.98
Crystal size (mm)0.25 × 0.10 × 0.03
Data collection
DiffractometerRigaku R-AXIS RAPID
diffractometer
Absorption correctionMulti-scan
(ABSCOR; Rigaku, 1995)
Tmin, Tmax0.730, 0.916
No. of measured, independent and
observed [I > 2σ(I)] reflections
20447, 15410, 15064
Rint0.027
(sin θ/λ)max1)0.649
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.025, 0.062, 1.08
No. of reflections15410
No. of parameters1052
No. of restraints67
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)1.52, 0.68
Absolute structureFlack (1983), 6026 Friedel pairs
Absolute structure parameter0.024 (13)

Computer programs: PROCESS-AUTO (Rigaku, 2000), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), Yadokari-XG 2009 (Kabuto et al., 2009).

Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1···O26i0.922.062.963 (5)169
N1—H1A···O15ii0.922.213.109 (4)166
N2—H2···O270.922.353.139 (5)143
N2—H2A···O13ii0.922.112.928 (5)148
N3—H3···O35B0.922.012.889 (8)160
N3—H3···O36A0.922.233.045 (8)147
N3—H3A···O11ii0.922.373.278 (5)167
N4—H4···O29iii0.921.982.886 (5)170
N4—H4A···O9ii0.922.042.917 (4)160
N5—H5···O18i0.922.093.008 (5)172
N5—H5A···O7iv0.922.193.094 (4)167
N6—H6···O27v0.922.443.183 (5)138
N6—H6···O280.922.483.326 (5)153
N6—H6A···O5iv0.922.213.041 (5)151
N7—H7···O230.922.032.938 (5)170
N7—H7A···O3iv0.922.163.066 (5)169
N8—H8···O28vi0.921.982.896 (5)171
N8—H8A···O1iv0.922.062.930 (4)157
O17—H17F···O26iv0.847 (19)1.96 (2)2.798 (5)167 (6)
O17—H17G···O16vii0.856 (19)1.93 (2)2.775 (4)170 (5)
O18—H18F···O170.841 (19)2.00 (3)2.818 (5)165 (6)
O18—H18G···O200.852 (19)1.98 (2)2.814 (5)165 (5)
O19—H19F···O8vii0.851 (19)2.05 (2)2.892 (5)168 (5)
O19—H19G···O2viii0.854 (19)1.94 (3)2.760 (5)160 (6)
O20—H20F···O210.845 (19)1.88 (2)2.709 (5)167 (6)
O20—H20G···O8ix0.858 (19)1.94 (3)2.742 (4)156 (5)
O21—H21F···O220.863 (19)1.97 (3)2.805 (6)162 (5)
O21—H21G···O300.869 (19)2.00 (2)2.857 (6)169 (6)
O22—H22F···O10vii0.854 (19)1.95 (2)2.802 (5)174 (6)
O22—H22G···O16viii0.859 (19)2.21 (4)2.915 (5)139 (6)
O23—H23F···O200.851 (19)1.96 (2)2.796 (5)168 (5)
O23—H23G···O25iv0.854 (19)1.96 (2)2.782 (5)162 (5)
O24—H24F···O19vi0.849 (19)1.97 (2)2.814 (5)177 (6)
O24—H24G···O320.851 (19)1.90 (2)2.736 (6)168 (6)
O25—H25F···O24iii0.865 (19)1.91 (2)2.770 (6)170 (6)
O25—H25G···O12ii0.852 (19)1.97 (3)2.788 (5)159 (5)
O26—H26F···O23ii0.860 (19)1.95 (2)2.791 (5)167 (6)
O26—H26G···O310.851 (19)1.95 (2)2.788 (6)169 (6)
O27—H27F···O6vi0.847 (19)1.88 (3)2.687 (5)158 (5)
O27—H27G···O14ii0.844 (19)1.81 (2)2.650 (5)175 (5)
O28—H28F···O100.822 (19)2.02 (2)2.810 (5)161 (5)
O28—H28G···O27v0.821 (19)2.00 (3)2.797 (5)164 (5)
O29—H29F···O20.868 (19)1.98 (2)2.834 (5)168 (6)
O29—H29G···O270.854 (19)1.98 (2)2.802 (5)160 (5)
O30—H30F···O120.861 (19)2.28 (5)2.911 (7)130 (6)
O30—H30G···O19iv0.864 (19)1.95 (3)2.791 (5)165 (6)
O31—H31F···O33ii0.839 (19)2.17 (3)2.946 (8)154 (7)
O31—H31G···O40.858 (19)2.08 (2)2.902 (6)161 (5)
O32—H32F···O340.917 (19)2.07 (2)2.823 (7)139 (3)
O32—H32G···O310.86 (2)1.98 (2)2.837 (7)178 (9)
O33—H33F···O170.875 (19)2.11 (4)2.877 (6)146 (7)
O33—H33G···O30vi0.87 (2)1.90 (2)2.766 (6)170 (7)
O34—H34F···O180.85 (2)2.12 (4)2.906 (6)154 (8)
O34—H34G···O6vi0.86 (2)2.02 (3)2.815 (6)154 (6)
O35A—H35F···O250.85 (2)2.14 (3)2.986 (9)174 (13)
O35A—H35G···O40.85 (2)2.05 (5)2.848 (9)157 (12)
O35B—H35H···O40.83 (2)2.45 (8)3.135 (9)141 (10)
O35B—H35I···O250.84 (2)2.03 (5)2.802 (10)152 (9)
O36A—H36F···O220.85 (2)2.14 (5)2.949 (9)159 (12)
O36A—H36G···O35A0.85 (2)1.93 (5)2.746 (12)158 (12)
Symmetry codes: (i) x, y, z1; (ii) x, y1, z; (iii) x+1, y, z; (iv) x, y+1, z; (v) x+1, y+1, z; (vi) x1, y, z; (vii) x, y, z+1; (viii) x+1, y, z+1; (ix) x, y+1, z+1.
 

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.

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Volume 69| Part 5| May 2013| Pages m288-m289
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