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Acta Cryst. (2010). E66, m638-m639
https://doi.org/10.1107/S1600536810016533
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Dichlorido(4,7-diaza-1-azoniacyclo­nonane-κ2N4,N7)palladium(II) p-toluene­sulfonate

T. A. Anthony, H. D. Arman and J. A. Walmsley
The title compound, [PdCl2(C6H16N3)](C7H7SO3), consists of a PdII atom bonded to two N atoms of the 1,4,7-triaza­cyclo­nonane (TACN) ligand and two chloride ions, which define a distorted square-planar geometry. The third N atom of the TACN ligand is protonated and hydrogen bonds to the p-toluene­sulfonate anion. The Cl—Pd—Cl angle is larger than the N—Pd—N angle. The packing is dominated by layers, which are formed by the criss-crossing of two different hydrogen-bonded chains. One chain is composed of hydrogen-bonded Pd(TACNH)Cl2+ cations, while the second is formed through hydrogen bonding between the p-toluene­sulfonate anion and the Pd(TACNH)Cl2+ cation.
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Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536810016533/tk2666sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536810016533/tk2666Isup2.hkl
Contains datablock I

CCDC reference: 781200

checkCIF report

Key indicators

  • Single-crystal X-ray study
  • T = 98 K
  • Mean [sigma](C-C) = 0.005 Å
  • R factor = 0.029
  • wR factor = 0.067
  • Data-to-parameter ratio = 18.2

checkCIF/PLATON results

No syntax errors found




Alert level C
PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low .......       0.98
PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor ....       2.31
PLAT352_ALERT_3_C Short   N-H Bond (0.87A)   N3     -   H3A    ...       0.75 Ang.
PLAT910_ALERT_3_C Missing # of FCF Reflections Below Th(Min) .....          2
PLAT911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L=  0.600         73
PLAT913_ALERT_3_C Missing # of Very Strong Reflections in FCF ....          6
PLAT912_ALERT_4_C Missing # of FCF Reflections Above STh/L=  0.600         19


Alert level G
PLAT380_ALERT_4_G Check Incorrectly? Oriented X(sp2)-Methyl Moiety        C13
PLAT793_ALERT_4_G The Model has Chirality at N1      (Verify) ....          R
PLAT793_ALERT_4_G The Model has Chirality at N2      (Verify) ....          S


   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
   7 ALERT level C = Check and explain
   3 ALERT level G = General alerts; check

   0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   1 ALERT type 2 Indicator that the structure model may be wrong or deficient
   5 ALERT type 3 Indicator that the structure quality may be low
   4 ALERT type 4 Improvement, methodology, query or suggestion
   0 ALERT type 5 Informative message, check
Comment top

Complexes of PdII and PtII with 1,4,7,-triazacyclononane (TACN) have been reported in which the metal ion is coordinated to all three of the TACN nitrogen atoms (McAuley & Whitcombe, 1988) or to only two of the N atoms (Blake et al., 1988; Blake et al., 1993; Margulis & Zompa, 1992; Hunter et al., 1988). In the latter case, under acidic conditions, the non-Pd bonded N atom becomes protonated. As a result, hydrogen bonding networks can be formed in the presence of an acceptor site. A similar type of complex has been reported for PtII (Davies et al., 2000).

The title salt is comprised of a protonated Pd(TACNH)Cl2+ cation and a p-toluenesulfonate ion, Fig. 1. The Pd—N and Pd—Cl bond distances, Table 1, are similar to the bond distances observed in Pd(en)Cl2 of 1.9798 (7) and 2.3084 (8) Å for Pd—N and Pd—Cl bonds, respectively (Iball et al., 1975). The geometry about the PdIIatom is essentially square planar, but with the Cl1—Pd—Cl2 bond angle larger than the N1—Pd—N2 bond angle., Table 1 The dimer associates into a supramolecular chain via a nine member, ···O1—S1—O2···H3a—N3—C—C—N1—H1a···, synthon, Fig 2. A second hydrogen bonded chain is observed that is formed between protonated Pd(TACNH)Cl2+ cations. These chains are composed of a seven member, ···Cl2—Pd—N1—C—C—N3—H3d···, repeat unit involving the protonated N atom, Fig 3. Hydrogen bonding distances are given in Table 1. These two hydrogen bonded chains are situated approximately perpendicular to one another which allows for the formation of 2-D hydrogen bonded layers, Fig 4.

Related literature top

For background to complexes of PdII and PtII with 1,4,7,-triazacyclononane (TACN), see: McAuley & Whitcombe (1988); Blake et al. (1988, 1993); Margulis & Zompa (1992); Hunter et al. (1988); Davies et al. (2000). For the synthesis of TACN, see: Kang & Jo (2003). For Pd—N and Pd—Cl bond distances in Pd(en)Cl2, see: Iball et al. (1975).

Experimental top

The ligand (TACN) was prepared according to the procedure reported in the literature (Kang & Jo, 2003). K2PdCl4 (0.126 g, 0.387 mmol) was dissolved in deionized H2O (20 ml) and heated to 343 K. TACN (0.0500 g, 0.387 mmol) was dissolved in 50% 2-propanol/50% water solution (20 ml) and heated to 343 K. The two hot solutions were combined, removed from the heat and allowed to stir for 48 h. Yellow-brown crystals precipitated and were isolated by suction filtration. These were recrystallized from a 50% 2-propanol/50% water mixture to obtain crystals suitable for X-ray analysis.

Refinement top

Carbon-bound H-atoms were placed in calculated positions(C—H 0.93 - 0.97 Å) and were included in the refinement in the riding model approximation with Uiso(H) set to 1.2-1.5 Ueq(C). The nitrogen-bound H-atoms were located in a difference Fourier map and were refined with Uiso(H) = 1.2Ueq(N).

Structure description top

Complexes of PdII and PtII with 1,4,7,-triazacyclononane (TACN) have been reported in which the metal ion is coordinated to all three of the TACN nitrogen atoms (McAuley & Whitcombe, 1988) or to only two of the N atoms (Blake et al., 1988; Blake et al., 1993; Margulis & Zompa, 1992; Hunter et al., 1988). In the latter case, under acidic conditions, the non-Pd bonded N atom becomes protonated. As a result, hydrogen bonding networks can be formed in the presence of an acceptor site. A similar type of complex has been reported for PtII (Davies et al., 2000).

The title salt is comprised of a protonated Pd(TACNH)Cl2+ cation and a p-toluenesulfonate ion, Fig. 1. The Pd—N and Pd—Cl bond distances, Table 1, are similar to the bond distances observed in Pd(en)Cl2 of 1.9798 (7) and 2.3084 (8) Å for Pd—N and Pd—Cl bonds, respectively (Iball et al., 1975). The geometry about the PdIIatom is essentially square planar, but with the Cl1—Pd—Cl2 bond angle larger than the N1—Pd—N2 bond angle., Table 1 The dimer associates into a supramolecular chain via a nine member, ···O1—S1—O2···H3a—N3—C—C—N1—H1a···, synthon, Fig 2. A second hydrogen bonded chain is observed that is formed between protonated Pd(TACNH)Cl2+ cations. These chains are composed of a seven member, ···Cl2—Pd—N1—C—C—N3—H3d···, repeat unit involving the protonated N atom, Fig 3. Hydrogen bonding distances are given in Table 1. These two hydrogen bonded chains are situated approximately perpendicular to one another which allows for the formation of 2-D hydrogen bonded layers, Fig 4.

For background to complexes of PdII and PtII with 1,4,7,-triazacyclononane (TACN), see: McAuley & Whitcombe (1988); Blake et al. (1988, 1993); Margulis & Zompa (1992); Hunter et al. (1988); Davies et al. (2000). For the synthesis of TACN, see: Kang & Jo (2003). For Pd—N and Pd—Cl bond distances in Pd(en)Cl2, see: Iball et al. (1975).

Computing details top

Data collection: CrystalClear (Rigaku/MSC, 2005); cell refinement: CrystalClear (Rigaku/MSC, 2005); data reduction: CrystalClear (Rigaku/MSC, 2005); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: publCIF (Westrip, 2010).

Figures top
[Figure 1] Fig. 1. Thermal ellipsoid plot (50% probability) of the asymmetric unit of the title salt. Carbon bound hydrogen atoms are removed for clarity.
[Figure 2] Fig. 2. Hydrogen bonded chain formed between the protonated Pd(TACNH)Cl2+ cation and the p-toluenesulfonate anion; non-participating hydrogen atoms have been removed for clarity. Thermal ellipsoids are shown at 50% probability.
[Figure 3] Fig. 3. Hydrogen bonded chain formed between protonated Pd(TACNH)Cl2+ ions; non- participating hydrogen atoms have been removed for clarity. Thermal ellipsoids are shown at 50% probability.
[Figure 4] Fig. 4. Illustration of the hydrogen bonded layer (view down the c axis); non-participating hydrogen atoms have been removed for clarity. Thermal ellipsoids are shown at 50% probability.
Dichlorido(4,7-diaza-1-azoniacyclononane- κ2N4,N7)palladium(II) p-toluenesulfonate top
Crystal data top
[PdCl2(C6H16N3)](C7H7O3S)Z = 2
Mr = 478.70F(000) = 484
Triclinic, P1Dx = 1.783 Mg m−3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 6.6663 (11) ÅCell parameters from 4441 reflections
b = 7.0023 (11) Åθ = 3.0–40.2°
c = 19.646 (3) ŵ = 1.47 mm−1
α = 92.149 (3)°T = 98 K
β = 92.301 (3)°Prism, orange
γ = 103.084 (4)°0.39 × 0.25 × 0.14 mm
V = 891.5 (2) Å3
Data collection top
Rigaku AFC12 Kappa goniometer
diffractometer		3998 independent reflections
Radiation source: sealed tube3941 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.018
Detector resolution: 14.286 pixels mm-1θmax = 27.5°, θmin = 3.0°
ω scansh = −8→8
Absorption correction: multi-scan
(ABSCOR; Higashi, 1995)		k = −9→8
Tmin = 0.839, Tmax = 1.000l = −25→24
6224 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.029Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.067H atoms treated by a mixture of independent and constrained refinement
S = 1.00 w = 1/[σ2(Fo2) + (0.007P)2 + 4.1P]
where P = (Fo2 + 2Fc2)/3
3998 reflections(Δ/σ)max = 0.001
220 parametersΔρmax = 0.62 e Å−3
0 restraintsΔρmin = −0.98 e Å−3
Crystal data top
[PdCl2(C6H16N3)](C7H7O3S)γ = 103.084 (4)°
Mr = 478.70V = 891.5 (2) Å3
Triclinic, P1Z = 2
a = 6.6663 (11) ÅMo Kα radiation
b = 7.0023 (11) ŵ = 1.47 mm−1
c = 19.646 (3) ÅT = 98 K
α = 92.149 (3)°0.39 × 0.25 × 0.14 mm
β = 92.301 (3)°
Data collection top
Rigaku AFC12 Kappa goniometer
diffractometer		3998 independent reflections
Absorption correction: multi-scan
(ABSCOR; Higashi, 1995)		3941 reflections with I > 2σ(I)
Tmin = 0.839, Tmax = 1.000Rint = 0.018
6224 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0290 restraints
wR(F2) = 0.067H atoms treated by a mixture of independent and constrained refinement
S = 1.00Δρmax = 0.62 e Å−3
3998 reflectionsΔρmin = −0.98 e Å−3
220 parameters
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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*/Ueq
Pd10.97009 (3)1.13904 (3)0.126918 (10)0.00972 (6)
Cl20.84514 (10)1.25666 (9)0.02940 (3)0.01338 (13)
Cl11.31092 (10)1.25684 (10)0.10367 (3)0.01477 (13)
N11.0477 (4)1.0307 (3)0.21612 (12)0.0107 (4)
N20.6749 (3)1.0232 (3)0.15540 (12)0.0119 (4)
N30.8065 (4)0.6217 (4)0.12108 (13)0.0131 (5)
C51.0277 (4)0.7097 (4)0.14512 (15)0.0135 (5)
H5A1.09020.79780.11100.016*
H5B1.10000.60420.14650.016*
C40.6940 (4)0.7353 (4)0.07501 (14)0.0133 (5)
H4A0.60680.64280.04220.016*
H4B0.79540.82250.04970.016*
C61.0657 (4)0.8215 (4)0.21375 (14)0.0125 (5)
H6A0.96930.75110.24490.015*
H6B1.20320.81870.23110.015*
C30.5617 (4)0.8563 (4)0.10909 (15)0.0139 (5)
H3B0.48580.90820.07390.017*
H3C0.46160.77000.13520.017*
C20.6799 (4)0.9703 (4)0.22882 (14)0.0150 (5)
H2B0.65670.82900.23150.018*
H2C0.57151.01370.25220.018*
C10.8864 (4)1.0674 (4)0.26239 (14)0.0143 (5)
H1B0.89751.20730.26940.017*
H1C0.90361.01280.30630.017*
S10.48600 (10)0.43932 (10)0.28213 (3)0.01295 (14)
O10.3964 (3)0.2362 (3)0.29720 (10)0.0153 (4)
O20.6622 (3)0.4531 (3)0.23865 (10)0.0162 (4)
O30.3348 (4)0.5425 (3)0.25768 (12)0.0240 (5)
C70.5938 (5)0.5596 (4)0.36084 (15)0.0168 (6)
C80.7933 (5)0.5552 (5)0.38198 (17)0.0244 (7)
H8A0.87250.49370.35450.029*
C90.8743 (6)0.6442 (5)0.44501 (18)0.0316 (8)
H9A1.00870.64220.45900.038*
C120.4771 (6)0.6539 (5)0.40103 (18)0.0286 (7)
H12A0.34470.66020.38610.034*
C110.5605 (6)0.7399 (6)0.4645 (2)0.0373 (9)
H11A0.48110.80140.49190.045*
C100.7584 (6)0.7355 (5)0.48716 (17)0.0329 (9)
C130.8478 (8)0.8282 (7)0.55589 (19)0.0492 (13)
H13A0.74740.88420.57810.074*
H13B0.96860.92930.54960.074*
H13C0.88420.72990.58360.074*
H1A1.158 (8)1.102 (8)0.230 (3)0.059*
H2A0.624 (8)1.114 (8)0.151 (3)0.059*
H3A0.742 (8)0.592 (8)0.151 (3)0.059*
H3D0.809 (8)0.516 (8)0.100 (3)0.059*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pd10.00972 (10)0.00856 (10)0.01090 (11)0.00177 (7)0.00143 (7)0.00151 (7)
Cl20.0159 (3)0.0127 (3)0.0122 (3)0.0043 (2)0.0012 (2)0.0019 (2)
Cl10.0111 (3)0.0167 (3)0.0161 (3)0.0015 (2)0.0024 (2)0.0038 (2)
N10.0111 (11)0.0110 (11)0.0091 (11)0.0001 (8)0.0017 (8)0.0009 (8)
N20.0092 (10)0.0109 (11)0.0162 (12)0.0035 (8)0.0025 (8)0.0011 (9)
N30.0149 (11)0.0112 (11)0.0130 (12)0.0024 (9)0.0021 (9)0.0012 (9)
C50.0099 (12)0.0132 (13)0.0180 (14)0.0033 (10)0.0018 (10)0.0020 (10)
C40.0147 (13)0.0126 (12)0.0118 (13)0.0019 (10)−0.0008 (10)0.0000 (10)
C60.0120 (12)0.0114 (12)0.0145 (13)0.0032 (10)0.0009 (10)0.0030 (10)
C30.0103 (12)0.0135 (13)0.0171 (14)0.0009 (10)0.0007 (10)0.0006 (10)
C20.0159 (13)0.0154 (13)0.0140 (13)0.0032 (11)0.0049 (10)0.0028 (10)
C10.0167 (13)0.0149 (13)0.0117 (13)0.0043 (11)0.0049 (10)−0.0007 (10)
S10.0134 (3)0.0117 (3)0.0133 (3)0.0020 (2)0.0007 (2)0.0011 (2)
O10.0175 (10)0.0135 (9)0.0128 (10)−0.0013 (8)0.0019 (8)0.0007 (7)
O20.0141 (10)0.0204 (10)0.0132 (10)0.0018 (8)0.0024 (7)0.0027 (8)
O30.0238 (11)0.0224 (11)0.0288 (12)0.0118 (9)−0.0025 (9)0.0027 (9)
C70.0227 (15)0.0121 (13)0.0132 (13)−0.0012 (11)0.0032 (11)0.0002 (10)
C80.0283 (17)0.0235 (16)0.0201 (16)0.0042 (13)−0.0022 (13)−0.0014 (12)
C90.0343 (19)0.0331 (19)0.0211 (17)−0.0046 (15)−0.0055 (14)0.0012 (14)
C120.0277 (17)0.0256 (17)0.0291 (18)−0.0008 (14)0.0098 (14)−0.0090 (14)
C110.046 (2)0.0320 (19)0.0274 (19)−0.0054 (17)0.0191 (17)−0.0105 (15)
C100.047 (2)0.0265 (17)0.0144 (16)−0.0148 (15)0.0065 (14)−0.0030 (13)
C130.068 (3)0.044 (2)0.0176 (18)−0.024 (2)0.0062 (18)−0.0074 (16)
Geometric parameters (Å, º) top
Pd1—N12.030 (2)C2—C11.504 (4)
Pd1—N22.060 (2)C2—H2B0.9700
Pd1—Cl12.3053 (8)C2—H2C0.9700
Pd1—Cl22.3115 (7)C1—H1B0.9700
N1—C11.495 (3)C1—H1C0.9700
N1—C61.495 (3)S1—O31.444 (2)
N1—H1A0.82 (5)S1—O11.459 (2)
N2—C31.493 (3)S1—O21.468 (2)
N2—C21.504 (4)S1—C71.777 (3)
N2—H2A0.79 (5)C7—C121.381 (4)
N3—C41.511 (4)C7—C81.385 (5)
N3—C51.512 (4)C8—C91.396 (5)
N3—H3A0.76 (6)C8—H8A0.9300
N3—H3D0.83 (6)C9—C101.388 (6)
C5—C61.516 (4)C9—H9A0.9300
C5—H5A0.9700C12—C111.400 (5)
C5—H5B0.9700C12—H12A0.9300
C4—C31.512 (4)C11—C101.383 (6)
C4—H4A0.9700C11—H11A0.9300
C4—H4B0.9700C10—C131.515 (5)
C6—H6A0.9700C13—H13A0.9600
C6—H6B0.9700C13—H13B0.9600
C3—H3B0.9700C13—H13C0.9600
C3—H3C0.9700
N1—Pd1—N282.71 (9)N2—C3—H3C108.4
N1—Pd1—Cl192.14 (7)C4—C3—H3C108.4
N2—Pd1—Cl1174.84 (7)H3B—C3—H3C107.4
N1—Pd1—Cl2173.69 (7)N2—C2—C1109.3 (2)
N2—Pd1—Cl291.14 (7)N2—C2—H2B109.8
Cl1—Pd1—Cl294.02 (3)C1—C2—H2B109.8
C1—N1—C6112.8 (2)N2—C2—H2C109.8
C1—N1—Pd1103.19 (17)C1—C2—H2C109.8
C6—N1—Pd1116.87 (17)H2B—C2—H2C108.3
C1—N1—H1A108 (4)N1—C1—C2107.4 (2)
C6—N1—H1A109 (4)N1—C1—H1B110.2
Pd1—N1—H1A106 (4)C2—C1—H1B110.2
C3—N2—C2112.6 (2)N1—C1—H1C110.2
C3—N2—Pd1113.10 (17)C2—C1—H1C110.2
C2—N2—Pd1109.76 (17)H1B—C1—H1C108.5
C3—N2—H2A109 (4)O3—S1—O1113.12 (13)
C2—N2—H2A110 (4)O3—S1—O2113.98 (13)
Pd1—N2—H2A101 (4)O1—S1—O2111.41 (12)
C4—N3—C5119.6 (2)O3—S1—C7106.63 (14)
C4—N3—H3A108 (4)O1—S1—C7106.18 (13)
C5—N3—H3A110 (4)O2—S1—C7104.72 (13)
C4—N3—H3D107 (4)C12—C7—C8120.5 (3)
C5—N3—H3D105 (4)C12—C7—S1119.9 (3)
H3A—N3—H3D105 (5)C8—C7—S1119.7 (2)
N3—C5—C6117.7 (2)C7—C8—C9119.3 (3)
N3—C5—H5A107.9C7—C8—H8A120.3
C6—C5—H5A107.9C9—C8—H8A120.3
N3—C5—H5B107.9C10—C9—C8121.4 (4)
C6—C5—H5B107.9C10—C9—H9A119.3
H5A—C5—H5B107.2C8—C9—H9A119.3
N3—C4—C3116.7 (2)C7—C12—C11119.3 (4)
N3—C4—H4A108.1C7—C12—H12A120.4
C3—C4—H4A108.1C11—C12—H12A120.4
N3—C4—H4B108.1C10—C11—C12121.4 (3)
C3—C4—H4B108.1C10—C11—H11A119.3
H4A—C4—H4B107.3C12—C11—H11A119.3
N1—C6—C5117.5 (2)C11—C10—C9118.1 (3)
N1—C6—H6A107.9C11—C10—C13121.3 (4)
C5—C6—H6A107.9C9—C10—C13120.6 (4)
N1—C6—H6B107.9C10—C13—H13A109.5
C5—C6—H6B107.9C10—C13—H13B109.5
H6A—C6—H6B107.2H13A—C13—H13B109.5
N2—C3—C4115.6 (2)C10—C13—H13C109.5
N2—C3—H3B108.4H13A—C13—H13C109.5
C4—C3—H3B108.4H13B—C13—H13C109.5
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1a···O1i0.82 (6)2.05 (6)2.833 (3)159 (6)
N2—H2a···Cl1ii0.79 (5)2.66 (6)3.365 (2)149 (5)
N3—H3a···O20.75 (6)2.04 (6)2.743 (3)156 (6)
N3—H3d···Cl2iii0.84 (5)2.31 (6)3.136 (3)171 (5)
Symmetry codes: (i) x+1, y+1, z; (ii) x−1, y, z; (iii) x, y−1, z.

Experimental details

Crystal data
Chemical formula[PdCl2(C6H16N3)](C7H7O3S)
Mr478.70
Crystal system, space groupTriclinic, P1
Temperature (K)98
a, b, c (Å)6.6663 (11), 7.0023 (11), 19.646 (3)
α, β, γ (°)92.149 (3), 92.301 (3), 103.084 (4)
V (Å3)891.5 (2)
Z2
Radiation typeMo Kα
µ (mm−1)1.47
Crystal size (mm)0.39 × 0.25 × 0.14
Data collection
DiffractometerRigaku AFC12 Kappa goniometer
Absorption correctionMulti-scan
(ABSCOR; Higashi, 1995)
Tmin, Tmax0.839, 1.000
No. of measured, independent and
observed [I > 2σ(I)] reflections		6224, 3998, 3941
Rint0.018
(sin θ/λ)max (Å−1)0.650
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.029, 0.067, 1.00
No. of reflections3998
No. of parameters220
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å−3)0.62, −0.98

Computer programs: CrystalClear (Rigaku/MSC, 2005), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), ORTEPII (Johnson, 1976), publCIF (Westrip, 2010).

Selected geometric parameters (Å, º) top
Pd1—N12.030 (2)Pd1—Cl12.3053 (8)
Pd1—N22.060 (2)Pd1—Cl22.3115 (7)
N1—Pd1—N282.71 (9)Cl1—Pd1—Cl294.02 (3)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1a···O1i0.82 (6)2.05 (6)2.833 (3)159 (6)
N2—H2a···Cl1ii0.79 (5)2.66 (6)3.365 (2)149 (5)
N3—H3a···O20.75 (6)2.04 (6)2.743 (3)156 (6)
N3—H3d···Cl2iii0.84 (5)2.31 (6)3.136 (3)171 (5)
Symmetry codes: (i) x+1, y+1, z; (ii) x−1, y, z; (iii) x, y−1, z.
Bond distances and angles for hydrogen-bonding interactions (Å, °) top
D···OX—D···AS=O···D
C1,C6—N1···O1i2.833 (3)97.42 (16), 104.83 (15)
N1—H1a···O1i2.05 (5)159 (5)
C4,C5—N3···O22.743 (3)125.55 (18), 99.40 (17)
N3—H3a···O22.04 (6)156 (6)
N3—H3d···Cl2ii2.31 (6)171 (5)
C4,C5—N3···Cl2ii3.136 (3)104.10 (16), 102.66 (16)
Pd—Cl2—H3diii85 (1)
Pd—Cl2—N3iii86.58 (5)
S1—O1···N1iv118.00 (12)
S1—O1···H1aiv113.3 (15)
S1—O2···N3139.70 (12)
S1—O2···H3a133.4 (16)
Symmetry codes: (i) 1+x, 1+y, z; (ii) x, -1+y, z; (iii) x, 1+y, z; (iv) -1+x, -1+y, z.
 

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