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In the title dinuclear palladium complex, [Pd2Cl4(C29H46N2)], the terminal ligands adopt an anti configuration, with an intra­molecular metal–metal distance of 3.3625 (5) Å. The dinuclear palladium complex adopts a V-shaped conformation, with a dihedral angle of 152.67 (3)° between the two chloride-bridged PdNCl3 square-planar systems. The benzene rings in the chelating amine ligand are at an angle of 74.9 (1)° with respect to each other. The complex is the first example of chloride-bridged dinuclear palladium complex with a bi­dentate secondary amine ligand.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807047745/dn2236sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807047745/dn2236Isup2.hkl
Contains datablock I

CCDC reference: 667131

Key indicators

  • Single-crystal X-ray study
  • T = 173 K
  • Mean [sigma](C-C) = 0.006 Å
  • R factor = 0.041
  • wR factor = 0.105
  • Data-to-parameter ratio = 18.0

checkCIF/PLATON results

No syntax errors found



Alert level C RINTA01_ALERT_3_C The value of Rint is greater than 0.10 Rint given 0.106 PLAT020_ALERT_3_C The value of Rint is greater than 0.10 ......... 0.11 PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Pd2 - Cl2 .. 6.39 su PLAT412_ALERT_2_C Short Intra XH3 .. XHn H1B .. H18C .. 1.89 Ang. PLAT420_ALERT_2_C D-H Without Acceptor N1 - H1 ... ? PLAT420_ALERT_2_C D-H Without Acceptor N2 - H2 ... ?
Alert level G PLAT793_ALERT_1_G Check the Absolute Configuration of N1 = ... S PLAT793_ALERT_1_G Check the Absolute Configuration of N2 = ... S
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 6 ALERT level C = Check and explain 2 ALERT level G = General alerts; check 2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 4 ALERT type 2 Indicator that the structure model may be wrong or deficient 2 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Comment top

The title compound [PdCl(µ-Cl) (NHtBu—CH2-2,4,6-C6HMe3—CH2-2,4,6-C6HMe3—CH2—NHtBu)]2 (1) is prepared from N,N'-{3,3'-methylenebis(2,4,6-trimethyl-3,1-phenylene)}bis(methylene)bis (2-methylpropan-2-amine) (Chahen et al., 2007) and 2 eq. of [PdCl2(C6H5CN)2]. The molecular structure of 1 shows the palladium atoms to be surrounded by a terminal chloro ligand, a nitrogen atom of the bidentate amine ligand, NHtBu—CH2-2,4,6-C6HMe3—CH2-2,4,6-C6HMe3—CH2—NHtBu, and two bridging chloro ligands. Each Pd atom and the four atoms comprising its square-planar coordination sphere are planar with a mean deviation of the fitted atoms of 0.009Å for Pd1 and 0.03Å for Pd2. The angle between these two planes is 152.67 (3)°. The intramolecular Pd—Pd distance of 3.3625 (5) Å is slightly longer then those observed for the pyrazolyl analogues [3.2004 (6) to 3.2569 (6) Å] (Guzei et al., 2003).

A characteristic helical conformation of the diphenyl methane moiety (Barnes et al., 1981), which occurs as enantiomeric pairs, is observed in the bis-amine ligand. The two C6HMe3 planes are inclined at an angle of 74.9 (1)° to each other.

Related literature top

For similar dinuclear chloro-bridged palladium complexes, see: Guzei et al. (2003). For the synthesis of NHtBu—CH2-2,4,6-C6HMe3—CH2-2,4,6-C6HMe3—CH2—NHtBu, see: Chahen et al. (2007). For structural information, see: Barnes et al. (1981).

Experimental top

A solution of di(ttbutylamino-methyl-mesityl)methane (178 mg, 0.42 mmol) and [PdCl2(C6H5CN)2] (322 mg, 0.84 mmol) in dichloromethane (80 ml) was stirred during 18 h. After that period the solvent was evaporated and the residue filtered through a short silicagel column using dichloromethane as eluent. The filtrate was evaporated to dryness and the orange product was washed with diethylether (10 ml) (78% yield).

Complex 1 was disolved in chloroform, and crystals suitable for X-ray diffraction analysis were obtained by slow evaporation of the chloroform solution.

1H NMR (400 MHz, CDCl3): 7.09 (s, 2H), 4.59 (d, 3J = 11.4 Hz, 2H), 4.38 (s, 2H), 3.81 (dd, 2J = 12.7 Hz, 2H), 3.14 (d, 2J = 12.7 Hz, 2H), 2.60 (s, 6H), 2.49 (s, 6H), 2.37 (s, 6H), 1.57 (s, 18H) p.p.m.. 13C {1H} NMR (100 MHz, CDCl3): 138.23, 137.67, 137.42, 135.05, 132.27, 130.18, 60.83, 47.11, 33.94, 29.35, 22.68, 20.72, 19.24 p.p.m.. Calcd. for C29H46Cl4N2Pd2: C 44.81 H 5.96 N 3.60 Found: C 44.56 H 5.92 N 3.57.

Refinement top

The H atoms were included in calculated positions and refined using a riding model, with C—H (N—H)= 0.93–0.96 Å and with Uiso(H) = 1.2 (1.5 for methyl groups) times Ueq(C).

Structure description top

The title compound [PdCl(µ-Cl) (NHtBu—CH2-2,4,6-C6HMe3—CH2-2,4,6-C6HMe3—CH2—NHtBu)]2 (1) is prepared from N,N'-{3,3'-methylenebis(2,4,6-trimethyl-3,1-phenylene)}bis(methylene)bis (2-methylpropan-2-amine) (Chahen et al., 2007) and 2 eq. of [PdCl2(C6H5CN)2]. The molecular structure of 1 shows the palladium atoms to be surrounded by a terminal chloro ligand, a nitrogen atom of the bidentate amine ligand, NHtBu—CH2-2,4,6-C6HMe3—CH2-2,4,6-C6HMe3—CH2—NHtBu, and two bridging chloro ligands. Each Pd atom and the four atoms comprising its square-planar coordination sphere are planar with a mean deviation of the fitted atoms of 0.009Å for Pd1 and 0.03Å for Pd2. The angle between these two planes is 152.67 (3)°. The intramolecular Pd—Pd distance of 3.3625 (5) Å is slightly longer then those observed for the pyrazolyl analogues [3.2004 (6) to 3.2569 (6) Å] (Guzei et al., 2003).

A characteristic helical conformation of the diphenyl methane moiety (Barnes et al., 1981), which occurs as enantiomeric pairs, is observed in the bis-amine ligand. The two C6HMe3 planes are inclined at an angle of 74.9 (1)° to each other.

For similar dinuclear chloro-bridged palladium complexes, see: Guzei et al. (2003). For the synthesis of NHtBu—CH2-2,4,6-C6HMe3—CH2-2,4,6-C6HMe3—CH2—NHtBu, see: Chahen et al. (2007). For structural information, see: Barnes et al. (1981).

Computing details top

Data collection: EXPOSE in IPDS Software (Stoe & Cie, 2000); cell refinement: CELL in IPDS Software (Stoe & Cie, 2000); data reduction: INTEGRATE in IPDS Software (Stoe & Cie, 2000); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: SHELXL97 (Sheldrick, 1997).

Figures top
[Figure 1] Fig. 1. The molecular structure of [PdCl(µ-Cl) (NHtBu—CH2-2,4,6-C6HMe3—CH2-2,4,6-C6HMe3—CH2—NHtBu)]2. Displacement ellipsoids are drawn at the 50% probability level. H atoms have been omitted for clarity
(±)-Di-µ-chlorido-[µ-N,N'-{[3,3'-methylenebis(2,4,6-trimethyl- 3,1-phenylene)]dimethylene}bis(2-methylpropan-2- amine)]bis[chloridopalladium(II)] top
Crystal data top
[Pd2Cl4(C29H46N2)]F(000) = 3152
Mr = 777.28Dx = 1.607 Mg m3
Orthorhombic, PbcaMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2abCell parameters from 8003 reflections
a = 18.7173 (11) Åθ = 2.1–26.0°
b = 14.7968 (8) ŵ = 1.47 mm1
c = 23.1967 (18) ÅT = 173 K
V = 6424.5 (7) Å3Plate, yellow
Z = 80.22 × 0.19 × 0.16 mm
Data collection top
Stoe IPDS
diffractometer
4450 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.106
Graphite monochromatorθmax = 25.9°, θmin = 2.2°
φ oscillation scansh = 2322
47318 measured reflectionsk = 1717
6218 independent reflectionsl = 2828
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)] = 0.041Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.105H-atom parameters constrained
S = 0.92 w = 1/[σ2(Fo2) + (0.0695P)2]
where P = (Fo2 + 2Fc2)/3
6218 reflections(Δ/σ)max = 0.001
346 parametersΔρmax = 0.83 e Å3
0 restraintsΔρmin = 1.24 e Å3
Crystal data top
[Pd2Cl4(C29H46N2)]V = 6424.5 (7) Å3
Mr = 777.28Z = 8
Orthorhombic, PbcaMo Kα radiation
a = 18.7173 (11) ŵ = 1.47 mm1
b = 14.7968 (8) ÅT = 173 K
c = 23.1967 (18) Å0.22 × 0.19 × 0.16 mm
Data collection top
Stoe IPDS
diffractometer
4450 reflections with I > 2σ(I)
47318 measured reflectionsRint = 0.106
6218 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0410 restraints
wR(F2) = 0.105H-atom parameters constrained
S = 0.92Δρmax = 0.83 e Å3
6218 reflectionsΔρmin = 1.24 e Å3
346 parameters
Special details top

Experimental. A crystal was mounted at 173 K on a Stoe Image Plate Diffraction System (Stoe & Cie, 2000) using Mo Kα graphite monochromated radiation. Image plate distance 70 mm, φ oscillation scans 0 - 100°, step Δφ = 0.8°, 5 minutes per frame.

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*/Ueq
C10.5736 (2)0.4144 (3)0.31830 (17)0.0296 (9)
H1A0.62440.41840.31030.036*
H1B0.55540.47530.32300.036*
C20.5361 (2)0.3695 (3)0.26755 (17)0.0271 (9)
C30.5634 (2)0.2868 (3)0.24702 (17)0.0288 (9)
C40.5300 (2)0.2459 (3)0.20064 (18)0.0328 (10)
H40.54910.19230.18640.039*
C50.4696 (2)0.2807 (3)0.17434 (18)0.0316 (9)
C60.4423 (2)0.3634 (3)0.19445 (17)0.0303 (9)
C70.4773 (2)0.4101 (3)0.23907 (17)0.0289 (9)
C80.3776 (2)0.4033 (4)0.16409 (18)0.0389 (11)
H8A0.35630.35490.14160.047*
H8B0.39540.44740.13680.047*
C90.3170 (2)0.4485 (3)0.19724 (17)0.0293 (9)
C100.2895 (2)0.5295 (3)0.17559 (17)0.0319 (9)
C110.2326 (2)0.5708 (3)0.20403 (16)0.0286 (9)
H110.21490.62490.18950.034*
C120.2015 (2)0.5345 (3)0.25317 (17)0.0271 (9)
C130.2288 (2)0.4529 (3)0.27535 (16)0.0274 (9)
C140.2851 (2)0.4084 (3)0.24643 (17)0.0268 (9)
C150.1935 (2)0.4135 (3)0.32872 (17)0.0283 (9)
H15A0.14270.40600.32180.034*
H15B0.21360.35450.33680.034*
C160.6282 (2)0.2403 (3)0.2727 (2)0.0360 (10)
H16A0.61390.20500.30540.054*
H16B0.66240.28490.28460.054*
H16C0.64950.20140.24430.054*
C170.4378 (3)0.2303 (4)0.1237 (2)0.0464 (12)
H17A0.46640.17800.11540.070*
H17B0.43690.26920.09060.070*
H17C0.39010.21180.13300.070*
C180.4534 (2)0.5050 (3)0.25403 (19)0.0334 (10)
H18A0.41260.50210.27910.050*
H18B0.44080.53670.21940.050*
H18C0.49160.53630.27320.050*
C190.3112 (2)0.3161 (3)0.26521 (19)0.0320 (10)
H19A0.35290.32280.28890.048*
H19B0.32290.28070.23180.048*
H19C0.27430.28630.28680.048*
C200.3157 (3)0.5732 (4)0.12039 (19)0.0431 (12)
H20A0.30570.53410.08840.065*
H20B0.36630.58310.12290.065*
H20C0.29180.62990.11490.065*
C210.1385 (2)0.5844 (3)0.27893 (19)0.0325 (9)
H21A0.15480.62310.30950.049*
H21B0.10480.54160.29400.049*
H21C0.11590.62030.24960.049*
C220.6132 (2)0.3860 (3)0.42283 (18)0.0307 (9)
C230.6175 (2)0.4873 (3)0.43222 (19)0.0354 (10)
H23A0.63450.51590.39770.053*
H23B0.64970.49990.46340.053*
H23C0.57090.51020.44150.053*
C240.5848 (3)0.3393 (3)0.47687 (19)0.0397 (11)
H24A0.61920.34480.50740.060*
H24B0.57650.27660.46880.060*
H24C0.54080.36730.48850.060*
C250.6874 (2)0.3479 (4)0.4085 (2)0.0451 (13)
H25A0.70630.37850.37540.068*
H25B0.68350.28440.40040.068*
H25C0.71870.35680.44080.068*
C260.1549 (2)0.4595 (3)0.43174 (16)0.0291 (9)
C270.0767 (2)0.4595 (4)0.4113 (2)0.0399 (11)
H27A0.06940.41030.38490.060*
H27B0.06640.51560.39220.060*
H27C0.04560.45260.44390.060*
C280.1667 (3)0.5402 (3)0.47139 (19)0.0390 (11)
H28A0.13910.53260.50590.058*
H28B0.15200.59450.45210.058*
H28C0.21650.54440.48110.058*
C290.1720 (3)0.3719 (3)0.4619 (2)0.0435 (12)
H29A0.21970.37440.47700.065*
H29B0.16840.32280.43500.065*
H29C0.13880.36260.49290.065*
Cl10.47124 (6)0.19910 (8)0.38347 (5)0.0417 (3)
Cl20.33518 (5)0.33643 (8)0.41655 (5)0.0344 (2)
Cl30.43593 (5)0.50561 (7)0.40657 (5)0.0319 (2)
Cl40.29904 (6)0.63889 (8)0.37556 (5)0.0365 (3)
N10.56226 (17)0.3624 (2)0.37331 (15)0.0285 (8)
H10.57490.30500.36370.034*
N20.20462 (17)0.4748 (2)0.37997 (14)0.0265 (7)
H20.19140.53010.36660.032*
Pd10.455757 (16)0.35125 (2)0.393763 (13)0.02669 (11)
Pd20.312726 (15)0.48875 (2)0.395103 (12)0.02541 (10)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.029 (2)0.024 (2)0.037 (2)0.0035 (17)0.0036 (17)0.0001 (17)
C20.0269 (19)0.025 (2)0.030 (2)0.0020 (17)0.0095 (16)0.0003 (16)
C30.029 (2)0.027 (3)0.031 (2)0.0009 (17)0.0086 (17)0.0002 (17)
C40.039 (2)0.023 (2)0.037 (2)0.0015 (18)0.0088 (19)0.0029 (18)
C50.035 (2)0.027 (3)0.033 (2)0.0056 (18)0.0076 (17)0.0027 (18)
C60.032 (2)0.032 (3)0.027 (2)0.0001 (17)0.0074 (16)0.0002 (17)
C70.032 (2)0.022 (2)0.033 (2)0.0028 (17)0.0105 (17)0.0001 (17)
C80.046 (3)0.045 (3)0.025 (2)0.011 (2)0.0036 (19)0.0042 (19)
C90.034 (2)0.030 (3)0.024 (2)0.0003 (18)0.0033 (16)0.0045 (16)
C100.040 (2)0.032 (3)0.025 (2)0.0011 (19)0.0018 (17)0.0014 (17)
C110.038 (2)0.020 (2)0.027 (2)0.0018 (17)0.0049 (17)0.0009 (16)
C120.0267 (19)0.027 (2)0.028 (2)0.0006 (16)0.0058 (16)0.0071 (17)
C130.030 (2)0.028 (2)0.0247 (19)0.0050 (17)0.0073 (16)0.0009 (16)
C140.031 (2)0.022 (2)0.028 (2)0.0027 (17)0.0051 (16)0.0025 (16)
C150.0285 (19)0.027 (2)0.030 (2)0.0012 (17)0.0032 (16)0.0023 (17)
C160.034 (2)0.027 (3)0.047 (3)0.0050 (19)0.0043 (19)0.002 (2)
C170.055 (3)0.042 (3)0.041 (3)0.002 (2)0.000 (2)0.012 (2)
C180.036 (2)0.027 (3)0.037 (2)0.0058 (18)0.0002 (19)0.0044 (18)
C190.033 (2)0.027 (3)0.036 (2)0.0016 (18)0.0012 (17)0.0034 (18)
C200.062 (3)0.042 (3)0.025 (2)0.003 (2)0.006 (2)0.002 (2)
C210.033 (2)0.027 (3)0.037 (2)0.0006 (18)0.0013 (18)0.0038 (18)
C220.0252 (19)0.029 (3)0.038 (2)0.0021 (17)0.0070 (17)0.0061 (18)
C230.035 (2)0.032 (3)0.039 (2)0.0034 (19)0.0075 (19)0.0055 (19)
C240.043 (3)0.034 (3)0.043 (3)0.003 (2)0.014 (2)0.001 (2)
C250.031 (2)0.039 (3)0.065 (3)0.006 (2)0.009 (2)0.014 (2)
C260.030 (2)0.033 (3)0.024 (2)0.0016 (18)0.0053 (16)0.0028 (17)
C270.027 (2)0.051 (3)0.042 (2)0.004 (2)0.0018 (18)0.002 (2)
C280.045 (3)0.044 (3)0.028 (2)0.003 (2)0.0036 (19)0.005 (2)
C290.048 (3)0.040 (3)0.043 (3)0.005 (2)0.016 (2)0.011 (2)
Cl10.0401 (6)0.0243 (6)0.0607 (7)0.0071 (5)0.0001 (5)0.0003 (5)
Cl20.0273 (5)0.0312 (6)0.0447 (6)0.0032 (4)0.0012 (4)0.0070 (5)
Cl30.0251 (5)0.0291 (6)0.0414 (6)0.0036 (4)0.0009 (4)0.0043 (4)
Cl40.0377 (5)0.0265 (6)0.0453 (6)0.0051 (4)0.0040 (5)0.0035 (4)
N10.0280 (17)0.024 (2)0.0331 (17)0.0002 (14)0.0008 (14)0.0036 (14)
N20.0269 (17)0.025 (2)0.0275 (17)0.0028 (14)0.0029 (14)0.0017 (14)
Pd10.02492 (17)0.0251 (2)0.03005 (17)0.00315 (12)0.00053 (12)0.00089 (13)
Pd20.02467 (17)0.0255 (2)0.02605 (17)0.00274 (12)0.00058 (12)0.00051 (12)
Geometric parameters (Å, º) top
C1—N11.505 (5)C19—H19C0.9600
C1—C21.523 (6)C20—H20A0.9600
C1—H1A0.9700C20—H20B0.9600
C1—H1B0.9700C20—H20C0.9600
C2—C31.410 (6)C21—H21A0.9600
C2—C71.418 (6)C21—H21B0.9600
C3—C41.384 (6)C21—H21C0.9600
C3—C161.516 (6)C22—C231.517 (6)
C4—C51.383 (6)C22—C241.527 (6)
C4—H40.9300C22—N11.533 (5)
C5—C61.407 (6)C22—C251.535 (6)
C5—C171.513 (6)C23—H23A0.9600
C6—C71.407 (6)C23—H23B0.9600
C6—C81.520 (6)C23—H23C0.9600
C7—C181.513 (6)C24—H24A0.9600
C8—C91.525 (6)C24—H24B0.9600
C8—H8A0.9700C24—H24C0.9600
C8—H8B0.9700C25—H25A0.9600
C9—C101.397 (6)C25—H25B0.9600
C9—C141.418 (6)C25—H25C0.9600
C10—C111.394 (6)C26—C291.508 (6)
C10—C201.516 (6)C26—C281.523 (6)
C11—C121.388 (6)C26—N21.536 (5)
C11—H110.9300C26—C271.538 (6)
C12—C131.409 (6)C27—H27A0.9600
C12—C211.514 (6)C27—H27B0.9600
C13—C141.412 (6)C27—H27C0.9600
C13—C151.520 (6)C28—H28A0.9600
C14—C191.514 (6)C28—H28B0.9600
C15—N21.510 (5)C28—H28C0.9600
C15—H15A0.9700C29—H29A0.9600
C15—H15B0.9700C29—H29B0.9600
C16—H16A0.9600C29—H29C0.9600
C16—H16B0.9600Cl1—Pd12.2825 (12)
C16—H16C0.9600Cl2—Pd12.3283 (10)
C17—H17A0.9600Cl2—Pd22.3460 (12)
C17—H17B0.9600Cl3—Pd12.3329 (11)
C17—H17C0.9600Cl3—Pd22.3347 (10)
C18—H18A0.9600Cl4—Pd22.2818 (12)
C18—H18B0.9600N1—Pd12.056 (3)
C18—H18C0.9600N1—H10.9100
C19—H19A0.9600N2—Pd22.064 (3)
C19—H19B0.9600N2—H20.9100
N1—C1—C2111.6 (3)H20A—C20—H20C109.5
N1—C1—H1A109.3H20B—C20—H20C109.5
C2—C1—H1A109.3C12—C21—H21A109.5
N1—C1—H1B109.3C12—C21—H21B109.5
C2—C1—H1B109.3H21A—C21—H21B109.5
H1A—C1—H1B108.0C12—C21—H21C109.5
C3—C2—C7119.5 (4)H21A—C21—H21C109.5
C3—C2—C1118.2 (4)H21B—C21—H21C109.5
C7—C2—C1122.2 (4)C23—C22—C24110.3 (4)
C4—C3—C2118.6 (4)C23—C22—N1111.4 (3)
C4—C3—C16118.0 (4)C24—C22—N1107.2 (3)
C2—C3—C16123.5 (4)C23—C22—C25110.3 (4)
C5—C4—C3123.4 (4)C24—C22—C25109.1 (4)
C5—C4—H4118.3N1—C22—C25108.5 (3)
C3—C4—H4118.3C22—C23—H23A109.5
C4—C5—C6118.4 (4)C22—C23—H23B109.5
C4—C5—C17118.7 (4)H23A—C23—H23B109.5
C6—C5—C17122.9 (4)C22—C23—H23C109.5
C7—C6—C5120.1 (4)H23A—C23—H23C109.5
C7—C6—C8121.5 (4)H23B—C23—H23C109.5
C5—C6—C8118.3 (4)C22—C24—H24A109.5
C6—C7—C2119.8 (4)C22—C24—H24B109.5
C6—C7—C18119.1 (4)H24A—C24—H24B109.5
C2—C7—C18121.1 (4)C22—C24—H24C109.5
C6—C8—C9121.9 (3)H24A—C24—H24C109.5
C6—C8—H8A106.8H24B—C24—H24C109.5
C9—C8—H8A106.8C22—C25—H25A109.5
C6—C8—H8B106.8C22—C25—H25B109.5
C9—C8—H8B106.8H25A—C25—H25B109.5
H8A—C8—H8B106.7C22—C25—H25C109.5
C10—C9—C14119.6 (4)H25A—C25—H25C109.5
C10—C9—C8118.0 (4)H25B—C25—H25C109.5
C14—C9—C8122.3 (4)C29—C26—C28111.3 (4)
C11—C10—C9119.2 (4)C29—C26—N2111.1 (3)
C11—C10—C20117.4 (4)C28—C26—N2105.6 (3)
C9—C10—C20123.4 (4)C29—C26—C27110.2 (4)
C12—C11—C10122.6 (4)C28—C26—C27109.0 (4)
C12—C11—H11118.7N2—C26—C27109.6 (3)
C10—C11—H11118.7C26—C27—H27A109.5
C11—C12—C13118.6 (4)C26—C27—H27B109.5
C11—C12—C21117.5 (4)H27A—C27—H27B109.5
C13—C12—C21123.8 (4)C26—C27—H27C109.5
C12—C13—C14119.8 (4)H27A—C27—H27C109.5
C12—C13—C15117.9 (4)H27B—C27—H27C109.5
C14—C13—C15122.2 (4)C26—C28—H28A109.5
C13—C14—C9120.1 (4)C26—C28—H28B109.5
C13—C14—C19121.6 (4)H28A—C28—H28B109.5
C9—C14—C19118.3 (4)C26—C28—H28C109.5
N2—C15—C13110.6 (3)H28A—C28—H28C109.5
N2—C15—H15A109.5H28B—C28—H28C109.5
C13—C15—H15A109.5C26—C29—H29A109.5
N2—C15—H15B109.5C26—C29—H29B109.5
C13—C15—H15B109.5H29A—C29—H29B109.5
H15A—C15—H15B108.1C26—C29—H29C109.5
C3—C16—H16A109.5H29A—C29—H29C109.5
C3—C16—H16B109.5H29B—C29—H29C109.5
H16A—C16—H16B109.5Pd1—Cl2—Pd292.01 (4)
C3—C16—H16C109.5Pd1—Cl3—Pd292.18 (4)
H16A—C16—H16C109.5C1—N1—C22115.6 (3)
H16B—C16—H16C109.5C1—N1—Pd1111.9 (2)
C5—C17—H17A109.5C22—N1—Pd1116.6 (3)
C5—C17—H17B109.5C1—N1—H1103.5
H17A—C17—H17B109.5C22—N1—H1103.5
C5—C17—H17C109.5Pd1—N1—H1103.5
H17A—C17—H17C109.5C15—N2—C26116.3 (3)
H17B—C17—H17C109.5C15—N2—Pd2109.2 (2)
C7—C18—H18A109.5C26—N2—Pd2118.4 (2)
C7—C18—H18B109.5C15—N2—H2103.6
H18A—C18—H18B109.5C26—N2—H2103.6
C7—C18—H18C109.5Pd2—N2—H2103.6
H18A—C18—H18C109.5N1—Pd1—Cl186.11 (11)
H18B—C18—H18C109.5N1—Pd1—Cl2179.19 (11)
C14—C19—H19A109.5Cl1—Pd1—Cl293.09 (4)
C14—C19—H19B109.5N1—Pd1—Cl396.02 (10)
H19A—C19—H19B109.5Cl1—Pd1—Cl3177.71 (4)
C14—C19—H19C109.5Cl2—Pd1—Cl384.78 (4)
H19A—C19—H19C109.5N2—Pd2—Cl487.33 (10)
H19B—C19—H19C109.5N2—Pd2—Cl3176.73 (9)
C10—C20—H20A109.5Cl4—Pd2—Cl391.69 (4)
C10—C20—H20B109.5N2—Pd2—Cl296.64 (10)
H20A—C20—H20B109.5Cl4—Pd2—Cl2176.02 (4)
C10—C20—H20C109.5Cl3—Pd2—Cl284.35 (4)
N1—C1—C2—C370.0 (4)C12—C13—C14—C19173.8 (4)
N1—C1—C2—C7112.9 (4)C15—C13—C14—C193.2 (6)
C7—C2—C3—C42.4 (6)C10—C9—C14—C133.8 (6)
C1—C2—C3—C4179.5 (4)C8—C9—C14—C13179.5 (4)
C7—C2—C3—C16177.0 (4)C10—C9—C14—C19173.9 (4)
C1—C2—C3—C160.1 (6)C8—C9—C14—C191.9 (6)
C2—C3—C4—C52.0 (6)C12—C13—C15—N265.6 (4)
C16—C3—C4—C5178.6 (4)C14—C13—C15—N2117.3 (4)
C3—C4—C5—C62.3 (6)C2—C1—N1—C22163.9 (3)
C3—C4—C5—C17179.7 (4)C2—C1—N1—Pd159.3 (4)
C4—C5—C6—C71.9 (6)C23—C22—N1—C149.3 (5)
C17—C5—C6—C7175.4 (4)C24—C22—N1—C1170.1 (4)
C4—C5—C6—C8177.8 (4)C25—C22—N1—C172.3 (5)
C17—C5—C6—C80.5 (6)C23—C22—N1—Pd185.4 (4)
C5—C6—C7—C26.2 (6)C24—C22—N1—Pd135.3 (4)
C8—C6—C7—C2178.0 (4)C25—C22—N1—Pd1153.0 (3)
C5—C6—C7—C18171.1 (4)C13—C15—N2—C26162.7 (3)
C8—C6—C7—C184.6 (6)C13—C15—N2—Pd260.0 (4)
C3—C2—C7—C66.5 (6)C29—C26—N2—C1570.3 (5)
C1—C2—C7—C6176.5 (4)C28—C26—N2—C15168.9 (3)
C3—C2—C7—C18170.8 (4)C27—C26—N2—C1551.7 (5)
C1—C2—C7—C186.2 (6)C29—C26—N2—Pd263.0 (4)
C7—C6—C8—C944.5 (6)C28—C26—N2—Pd257.8 (4)
C5—C6—C8—C9139.7 (4)C27—C26—N2—Pd2175.0 (3)
C6—C8—C9—C10136.6 (5)C1—N1—Pd1—Cl1117.2 (3)
C6—C8—C9—C1447.6 (7)C22—N1—Pd1—Cl1106.5 (3)
C14—C9—C10—C112.1 (6)C1—N1—Pd1—Cl363.7 (3)
C8—C9—C10—C11178.0 (4)C22—N1—Pd1—Cl372.6 (3)
C14—C9—C10—C20174.5 (4)Pd2—Cl2—Pd1—Cl1161.48 (4)
C8—C9—C10—C201.4 (6)Pd2—Cl2—Pd1—Cl319.38 (4)
C9—C10—C11—C120.5 (6)Pd2—Cl3—Pd1—N1160.38 (10)
C20—C10—C11—C12176.4 (4)Pd2—Cl3—Pd1—Cl219.48 (4)
C10—C11—C12—C130.4 (6)C15—N2—Pd2—Cl4117.0 (2)
C10—C11—C12—C21178.0 (4)C26—N2—Pd2—Cl4106.7 (3)
C11—C12—C13—C142.1 (6)C15—N2—Pd2—Cl263.1 (2)
C21—C12—C13—C14176.3 (4)C26—N2—Pd2—Cl273.1 (3)
C11—C12—C13—C15179.3 (3)Pd1—Cl3—Pd2—Cl4161.03 (4)
C21—C12—C13—C150.9 (6)Pd1—Cl3—Pd2—Cl219.34 (4)
C12—C13—C14—C93.8 (6)Pd1—Cl2—Pd2—N2157.49 (10)
C15—C13—C14—C9179.2 (4)Pd1—Cl2—Pd2—Cl319.38 (4)

Experimental details

Crystal data
Chemical formula[Pd2Cl4(C29H46N2)]
Mr777.28
Crystal system, space groupOrthorhombic, Pbca
Temperature (K)173
a, b, c (Å)18.7173 (11), 14.7968 (8), 23.1967 (18)
V3)6424.5 (7)
Z8
Radiation typeMo Kα
µ (mm1)1.47
Crystal size (mm)0.22 × 0.19 × 0.16
Data collection
DiffractometerStoe IPDS
Absorption correction
No. of measured, independent and
observed [I > 2σ(I)] reflections
47318, 6218, 4450
Rint0.106
(sin θ/λ)max1)0.615
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.041, 0.105, 0.92
No. of reflections6218
No. of parameters346
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.83, 1.24

Computer programs: EXPOSE in IPDS Software (Stoe & Cie, 2000), CELL in IPDS Software (Stoe & Cie, 2000), INTEGRATE in IPDS Software (Stoe & Cie, 2000), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), ORTEP-3 (Farrugia, 1997).

 

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