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The title compound, [Pd2I4(C34H24P2)2]·3CHCl3, was obtained from the direct reaction of PdI2 with 1,4-bis­[(diphenyl­phosphan­yl)ethyn­yl]benzene. The dimer complex mol­ecule is centrosymmetric, with each PdII atom in a slightly distorted square-planar coordination geometry.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680704620X/bt2515sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S160053680704620X/bt2515Isup2.hkl
Contains datablock I

CCDC reference: 672580

Key indicators

  • Single-crystal X-ray study
  • T = 150 K
  • Mean [sigma](C-C) = 0.014 Å
  • Disorder in solvent or counterion
  • R factor = 0.056
  • wR factor = 0.112
  • Data-to-parameter ratio = 16.2

checkCIF/PLATON results

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Alert level B PLAT366_ALERT_2_B Short? C(sp?)-C(sp?) Bond C1 - C2 ... 1.20 Ang.
Alert level C PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C15 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for C1S PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 11.00 Perc. PLAT320_ALERT_2_C Check Hybridisation of C1 in Main Residue . ? PLAT342_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang ... 14 PLAT371_ALERT_2_C Long C(sp2)-C(sp1) Bond C2 - C3 ... 1.43 Ang. PLAT371_ALERT_2_C Long C(sp2)-C(sp1) Bond C6 - C9 ... 1.43 Ang. PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 2 PLAT731_ALERT_1_C Bond Calc 1.727(12), Rep 1.728(5) ...... 2.40 su-Ra CL3 -C1S 1.555 1.555 PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 33.70 Deg. C2S -CL5 -C2S 2.756 1.555 1.555 PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 33.60 Deg. C2S -CL4 -C2S 1.555 1.555 2.756 PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 2 C H Cl3
Alert level G PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 4
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 12 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 7 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 4 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Comment top

The bidentate phosphane ligand used in this work has been previously found to form a triangle when reacted with PtCl2 (Baumgartner et al., 2002). In this work, we report the formation of a rectangle using PdI2 as the metal source. The Pd centres in the title compound exhibit a slightly distorted square planar geometry, where the P—Pd—I angles deviate from 90° by less than 3°.

Related literature top

Metal-containing rings are currently of interest as polymer precursors (Nguyen et al., 1999; Herbert et al., 2007). We have also determined the structure of a triclinic modification of the title compound (Baumgartner et al., 2007). A related complex containing PtII atoms and chloride ligands was found to form a triangle (Baumgartner et al., 2002).

Experimental top

PdI2 (11 mg, 0.031 mmol) and 1,4-bis-[(diphenylphosphanyl)-ethynyl]-benzene (15 mg, 0.030 mmol) was added to CDCl3 (0.6 ml). Crystals of the title compound was obtained after 2 days.

Refinement top

All hydrogen atoms were placed in calculated positions with C—H = 0.95 or 1.00 Å and were included in the refinement in the riding-motion approximation with Uiso(H) = 1.2Ueq(C). One of the CHCl3 solvent molecules is disordered over a twofold rotation axis. For each CHCl3 the three C—Cl distances were constrained to be equal with a standard uncertainty of 0.002Å [see: SADI command in SHELXTL (Sheldrick, 2001)]

Computing details top

Data collection: COLLECT (Nonius, 2002); cell refinement: DENZO-SMN (Otwinowski & Minor, 1997); data reduction: DENZO-SMN (Otwinowski & Minor, 1997); program(s) used to solve structure: SIR92 (Altomare et al., 1994); program(s) used to refine structure: SHELXTL (Sheldrick, 2001); molecular graphics: SHELXTL (Sheldrick, 2001); software used to prepare material for publication: SHELXTL (Sheldrick, 2001).

Figures top
[Figure 1] Fig. 1. The molecular structure with displacement ellipsoids drawn at the 30% probability level. Neither the chloroform solvent molecules nor H atoms are shown. Atoms labeled with the suffix 'a' are related by the symmetry operator (-x + 3/2,-y + 1/2,-z + 1).
Bis{µ-1,4-bis[(diphenylphosphanyl)ethynyl]benzene-κ2P:P'}bis[trans- diiodidopalladium(II)] chloroform trisolvate top
Crystal data top
[Pd2I4(C34H24P2)2]·3CHCl3F(000) = 3976
Mr = 2067.45Dx = 1.790 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 19576 reflections
a = 20.8960 (9) Åθ = 2.6–25.0°
b = 9.5920 (5) ŵ = 2.52 mm1
c = 38.832 (2) ÅT = 150 K
β = 99.804 (3)°Needle, colourless
V = 7669.6 (7) Å30.14 × 0.06 × 0.02 mm
Z = 4
Data collection top
Nonius KappaCCD
diffractometer
6672 independent reflections
Radiation source: fine-focus sealed tube3732 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.086
Detector resolution: 9 pixels mm-1θmax = 25.0°, θmin = 2.6°
ϕ scans and ω scans with κ offsetsh = 2424
Absorption correction: multi-scan
(SORTAV; Blessing, 1995)
k = 1111
Tmin = 0.827, Tmax = 0.958l = 4546
19576 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)] = 0.056Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.112H-atom parameters constrained
S = 1.01 w = 1/[σ2(Fo2) + (0.024P)2 + 42.7375P]
where P = (Fo2 + 2Fc2)/3
6672 reflections(Δ/σ)max = 0.002
411 parametersΔρmax = 1.06 e Å3
4 restraintsΔρmin = 0.91 e Å3
Crystal data top
[Pd2I4(C34H24P2)2]·3CHCl3V = 7669.6 (7) Å3
Mr = 2067.45Z = 4
Monoclinic, C2/cMo Kα radiation
a = 20.8960 (9) ŵ = 2.52 mm1
b = 9.5920 (5) ÅT = 150 K
c = 38.832 (2) Å0.14 × 0.06 × 0.02 mm
β = 99.804 (3)°
Data collection top
Nonius KappaCCD
diffractometer
6672 independent reflections
Absorption correction: multi-scan
(SORTAV; Blessing, 1995)
3732 reflections with I > 2σ(I)
Tmin = 0.827, Tmax = 0.958Rint = 0.086
19576 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0564 restraints
wR(F2) = 0.112H-atom parameters constrained
S = 1.01 w = 1/[σ2(Fo2) + (0.024P)2 + 42.7375P]
where P = (Fo2 + 2Fc2)/3
6672 reflectionsΔρmax = 1.06 e Å3
411 parametersΔρmin = 0.91 e Å3
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)
Pd10.67135 (3)0.12571 (7)0.633756 (18)0.0337 (2)
I10.72848 (3)0.04250 (7)0.595490 (18)0.0489 (2)
I20.61881 (3)0.24764 (6)0.681462 (16)0.04193 (19)
P10.57291 (10)0.0364 (2)0.60639 (6)0.0338 (6)
P20.77171 (11)0.2254 (2)0.65447 (6)0.0363 (6)
C10.5693 (4)0.0548 (9)0.5615 (3)0.044 (3)
C20.5810 (4)0.0764 (9)0.5327 (2)0.040 (2)
C30.6019 (4)0.1060 (10)0.5002 (2)0.040 (2)
C40.6216 (5)0.2398 (11)0.4932 (3)0.061 (3)
H4A0.61920.31230.50960.073*
C50.6448 (5)0.2686 (11)0.4626 (3)0.059 (3)
H5A0.65770.36080.45800.071*
C60.6491 (4)0.1649 (10)0.4388 (2)0.043 (2)
C70.6299 (4)0.0311 (9)0.4456 (2)0.043 (2)
H7A0.63290.04110.42910.051*
C80.6064 (4)0.0008 (10)0.4760 (2)0.043 (2)
H8A0.59330.09150.48030.052*
C90.6710 (4)0.1963 (9)0.4067 (3)0.045 (3)
C100.6902 (4)0.2313 (9)0.3808 (2)0.039 (2)
C110.5605 (4)0.1473 (9)0.6139 (2)0.034 (2)
C120.5926 (4)0.2073 (10)0.6446 (2)0.045 (3)
H12A0.62270.15410.66040.054*
C130.5805 (4)0.3451 (10)0.6522 (3)0.047 (3)
H13A0.60240.38670.67310.056*
C140.5369 (5)0.4205 (10)0.6294 (3)0.053 (3)
H14A0.52830.51450.63480.063*
C150.5047 (5)0.3619 (11)0.5983 (3)0.064 (3)
H15A0.47450.41550.58260.077*
C160.5172 (4)0.2262 (9)0.5908 (3)0.044 (3)
H16A0.49600.18580.56950.053*
C210.4980 (4)0.1166 (9)0.6141 (2)0.034 (2)
C220.4672 (4)0.0657 (10)0.6404 (2)0.045 (3)
H22A0.48460.01300.65360.054*
C230.4114 (4)0.1278 (11)0.6476 (3)0.051 (3)
H23A0.39040.09110.66550.061*
C240.3862 (5)0.2435 (11)0.6288 (3)0.061 (3)
H24A0.34790.28640.63390.073*
C250.4161 (4)0.2965 (9)0.6030 (3)0.057 (3)
H25A0.39880.37630.59030.069*
C260.4718 (4)0.2337 (9)0.5956 (2)0.045 (2)
H26A0.49240.27080.57760.053*
C310.7750 (4)0.3889 (10)0.6778 (3)0.041 (2)
C320.8069 (5)0.4039 (11)0.7117 (3)0.055 (3)
H32A0.82680.32490.72380.066*
C330.8103 (5)0.5302 (14)0.7282 (3)0.076 (4)
H33A0.83240.53860.75170.092*
C340.7823 (5)0.6428 (14)0.7111 (4)0.080 (4)
H34A0.78430.72970.72300.096*
C350.7511 (5)0.6362 (12)0.6771 (4)0.068 (4)
H35A0.73210.71680.66540.082*
C360.7483 (4)0.5061 (11)0.6601 (3)0.053 (3)
H36A0.72790.49880.63640.063*
C410.8270 (4)0.1125 (9)0.6827 (2)0.038 (2)
C420.8062 (5)0.0596 (10)0.7121 (3)0.056 (3)
H42A0.76330.07720.71600.067*
C430.8482 (6)0.0186 (11)0.7354 (3)0.067 (3)
H43A0.83430.05080.75610.080*
C440.9086 (6)0.0514 (11)0.7300 (3)0.071 (3)
H44A0.93640.10860.74610.085*
C450.9286 (5)0.0010 (11)0.7005 (3)0.066 (3)
H45A0.97100.02050.69630.080*
C460.8881 (5)0.0846 (10)0.6767 (3)0.053 (3)
H46A0.90290.12140.65670.064*
Cl10.56608 (16)0.6246 (3)0.51296 (10)0.0983 (11)
Cl20.7013 (2)0.6345 (6)0.5168 (2)0.255 (4)
Cl30.6484 (3)0.4900 (7)0.56931 (13)0.206 (3)
C1S0.63949 (19)0.6309 (12)0.5412 (2)0.150 (8)
H1SA0.64120.71850.55530.180*
Cl51.03790 (18)0.6728 (4)0.72255 (9)0.1068 (12)
Cl41.00000.4169 (5)0.75000.125 (2)
C2S0.9795 (9)0.5888 (12)0.7413 (6)0.110 (13)0.50
H2SA0.94040.58880.72420.132*0.50
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pd10.0336 (4)0.0372 (4)0.0304 (4)0.0009 (3)0.0059 (3)0.0015 (4)
I10.0401 (4)0.0537 (4)0.0545 (5)0.0011 (3)0.0122 (3)0.0148 (4)
I20.0428 (4)0.0494 (4)0.0349 (4)0.0031 (3)0.0102 (3)0.0075 (3)
P10.0339 (13)0.0402 (15)0.0282 (15)0.0027 (11)0.0075 (11)0.0005 (12)
P20.0398 (14)0.0423 (16)0.0275 (14)0.0021 (12)0.0076 (12)0.0013 (12)
C10.045 (6)0.042 (6)0.048 (7)0.003 (5)0.015 (5)0.009 (5)
C20.043 (6)0.041 (6)0.037 (6)0.012 (5)0.009 (5)0.003 (5)
C30.051 (6)0.044 (6)0.027 (6)0.006 (5)0.012 (5)0.001 (5)
C40.101 (9)0.050 (7)0.036 (7)0.014 (6)0.024 (6)0.004 (5)
C50.081 (8)0.058 (7)0.044 (7)0.025 (6)0.023 (6)0.002 (6)
C60.050 (6)0.044 (6)0.036 (6)0.009 (5)0.009 (5)0.001 (5)
C70.051 (6)0.044 (6)0.033 (6)0.014 (5)0.009 (5)0.001 (5)
C80.047 (6)0.045 (6)0.038 (6)0.008 (5)0.010 (5)0.007 (5)
C90.039 (6)0.051 (6)0.045 (7)0.012 (5)0.009 (5)0.006 (5)
C100.037 (5)0.040 (6)0.042 (6)0.016 (5)0.010 (5)0.001 (5)
C110.032 (5)0.041 (6)0.033 (6)0.002 (5)0.012 (5)0.003 (5)
C120.054 (6)0.048 (7)0.036 (7)0.011 (5)0.012 (5)0.000 (5)
C130.038 (6)0.047 (7)0.052 (7)0.000 (5)0.002 (5)0.004 (6)
C140.062 (7)0.033 (6)0.065 (8)0.005 (5)0.018 (6)0.012 (6)
C150.068 (7)0.043 (7)0.079 (10)0.021 (6)0.007 (7)0.009 (7)
C160.043 (6)0.033 (6)0.054 (7)0.009 (5)0.000 (5)0.001 (5)
C210.034 (5)0.034 (6)0.035 (6)0.000 (4)0.006 (5)0.001 (5)
C220.045 (6)0.055 (6)0.040 (6)0.002 (5)0.023 (5)0.004 (5)
C230.050 (6)0.060 (7)0.043 (7)0.003 (6)0.009 (5)0.005 (6)
C240.038 (6)0.056 (7)0.089 (9)0.005 (6)0.012 (6)0.018 (7)
C250.035 (6)0.034 (6)0.102 (10)0.006 (5)0.006 (6)0.006 (6)
C260.044 (6)0.039 (6)0.051 (7)0.009 (5)0.010 (5)0.001 (5)
C310.040 (6)0.054 (7)0.029 (6)0.014 (5)0.003 (5)0.001 (5)
C320.059 (7)0.048 (7)0.061 (8)0.000 (5)0.017 (6)0.014 (6)
C330.067 (8)0.091 (10)0.071 (10)0.005 (8)0.012 (7)0.029 (9)
C340.047 (8)0.072 (10)0.126 (14)0.017 (7)0.026 (8)0.049 (10)
C350.047 (7)0.052 (8)0.111 (12)0.007 (6)0.025 (8)0.002 (8)
C360.046 (6)0.053 (7)0.059 (8)0.011 (6)0.006 (6)0.001 (6)
C410.036 (5)0.039 (6)0.037 (6)0.001 (5)0.001 (5)0.001 (5)
C420.052 (6)0.064 (7)0.049 (7)0.005 (6)0.004 (6)0.024 (6)
C430.071 (8)0.064 (8)0.056 (8)0.009 (7)0.017 (7)0.032 (6)
C440.064 (8)0.058 (8)0.080 (10)0.004 (7)0.021 (7)0.023 (7)
C450.050 (7)0.074 (9)0.073 (9)0.026 (6)0.005 (7)0.000 (7)
C460.049 (6)0.062 (7)0.048 (7)0.008 (6)0.005 (6)0.002 (6)
Cl10.106 (3)0.084 (2)0.103 (3)0.009 (2)0.012 (2)0.011 (2)
Cl20.114 (4)0.210 (6)0.467 (11)0.044 (4)0.127 (5)0.152 (7)
Cl30.205 (5)0.282 (7)0.101 (4)0.136 (5)0.064 (4)0.085 (4)
C1S0.059 (9)0.165 (16)0.21 (2)0.002 (10)0.009 (11)0.137 (15)
Cl50.127 (3)0.115 (3)0.084 (3)0.009 (2)0.033 (2)0.017 (2)
Cl40.150 (5)0.084 (4)0.159 (6)0.0000.081 (4)0.000
C2S0.042 (18)0.12 (2)0.18 (4)0.011 (13)0.05 (2)0.10 (2)
Geometric parameters (Å, º) top
Pd1—P12.313 (2)C23—C241.383 (13)
Pd1—P22.321 (2)C23—H23A0.9500
Pd1—I22.5880 (9)C24—C251.365 (13)
Pd1—I12.6155 (9)C24—H24A0.9500
P1—C11.743 (10)C25—C261.384 (11)
P1—C111.812 (9)C25—H25A0.9500
P1—C211.813 (8)C26—H26A0.9500
P2—C10i1.749 (9)C31—C321.379 (12)
P2—C311.806 (10)C31—C361.384 (12)
P2—C411.809 (9)C32—C331.367 (13)
C1—C21.202 (11)C32—H32A0.9500
C2—C31.434 (12)C33—C341.349 (16)
C3—C41.388 (12)C33—H33A0.9500
C3—C81.393 (11)C34—C351.370 (15)
C4—C51.388 (12)C34—H34A0.9500
C4—H4A0.9500C35—C361.408 (13)
C5—C61.371 (12)C35—H35A0.9500
C5—H5A0.9500C36—H36A0.9500
C6—C71.384 (11)C41—C461.364 (11)
C6—C91.430 (12)C41—C421.386 (12)
C7—C81.384 (11)C42—C431.373 (12)
C7—H7A0.9500C42—H42A0.9500
C8—H8A0.9500C43—C441.351 (13)
C9—C101.191 (11)C43—H43A0.9500
C10—P2i1.749 (9)C44—C451.381 (14)
C11—C161.386 (11)C44—H44A0.9500
C11—C121.390 (11)C45—C461.396 (13)
C12—C131.386 (12)C45—H45A0.9500
C12—H12A0.9500C46—H46A0.9500
C13—C141.363 (12)Cl1—C1S1.728 (5)
C13—H13A0.9500Cl2—C1S1.728 (5)
C14—C151.396 (13)Cl3—C1S1.728 (5)
C14—H14A0.9500C1S—H1SA1.0000
C15—C161.370 (12)Cl5—C2Sii1.71 (2)
C15—H15A0.9500Cl5—C2S1.723 (11)
C16—H16A0.9500Cl4—C2S1.723 (11)
C21—C221.384 (11)Cl4—C2Sii1.723 (11)
C21—C261.395 (11)C2S—C2Sii1.00 (4)
C22—C231.379 (11)C2S—Cl5ii1.71 (2)
C22—H22A0.9500C2S—H2SA0.9600
P1—Pd1—P2172.93 (9)C22—C23—H23A120.1
P1—Pd1—I292.51 (6)C24—C23—H23A120.1
P2—Pd1—I291.96 (6)C25—C24—C23120.3 (9)
P1—Pd1—I188.09 (6)C25—C24—H24A119.8
P2—Pd1—I188.75 (6)C23—C24—H24A119.8
I2—Pd1—I1167.36 (4)C24—C25—C26119.9 (10)
C1—P1—C11106.1 (4)C24—C25—H25A120.1
C1—P1—C21103.4 (4)C26—C25—H25A120.1
C11—P1—C21103.6 (4)C25—C26—C21120.8 (9)
C1—P1—Pd1107.8 (3)C25—C26—H26A119.6
C11—P1—Pd1115.3 (3)C21—C26—H26A119.6
C21—P1—Pd1119.5 (3)C32—C31—C36118.5 (10)
C10i—P2—C31101.7 (4)C32—C31—P2122.7 (8)
C10i—P2—C41106.7 (4)C36—C31—P2118.6 (8)
C31—P2—C41104.5 (4)C33—C32—C31121.3 (11)
C10i—P2—Pd1109.3 (3)C33—C32—H32A119.4
C31—P2—Pd1119.1 (3)C31—C32—H32A119.4
C41—P2—Pd1114.2 (3)C34—C33—C32119.6 (12)
C2—C1—P1165.4 (9)C34—C33—H33A120.2
C1—C2—C3173.7 (10)C32—C33—H33A120.2
C4—C3—C8118.9 (8)C33—C34—C35122.2 (13)
C4—C3—C2120.0 (8)C33—C34—H34A118.9
C8—C3—C2121.1 (8)C35—C34—H34A118.9
C3—C4—C5120.6 (9)C34—C35—C36117.9 (12)
C3—C4—H4A119.7C34—C35—H35A121.0
C5—C4—H4A119.7C36—C35—H35A121.0
C6—C5—C4120.4 (9)C31—C36—C35120.4 (10)
C6—C5—H5A119.8C31—C36—H36A119.8
C4—C5—H5A119.8C35—C36—H36A119.8
C5—C6—C7119.3 (9)C46—C41—C42120.2 (9)
C5—C6—C9120.1 (9)C46—C41—P2122.3 (7)
C7—C6—C9120.5 (9)C42—C41—P2117.4 (7)
C6—C7—C8120.9 (9)C43—C42—C41119.3 (10)
C6—C7—H7A119.5C43—C42—H42A120.3
C8—C7—H7A119.5C41—C42—H42A120.3
C7—C8—C3119.8 (8)C44—C43—C42122.2 (11)
C7—C8—H8A120.1C44—C43—H43A118.9
C3—C8—H8A120.1C42—C43—H43A118.9
C10—C9—C6175.6 (10)C43—C44—C45117.9 (10)
C9—C10—P2i172.5 (9)C43—C44—H44A121.0
C16—C11—C12119.8 (8)C45—C44—H44A121.0
C16—C11—P1121.5 (7)C44—C45—C46121.6 (10)
C12—C11—P1118.7 (7)C44—C45—H45A119.2
C13—C12—C11119.9 (9)C46—C45—H45A119.2
C13—C12—H12A120.1C41—C46—C45118.7 (10)
C11—C12—H12A120.1C41—C46—H46A120.6
C14—C13—C12119.6 (10)C45—C46—H46A120.6
C14—C13—H13A120.2Cl2—C1S—Cl1108.6 (5)
C12—C13—H13A120.2Cl2—C1S—Cl3110.6 (6)
C13—C14—C15121.1 (9)Cl1—C1S—Cl3111.2 (5)
C13—C14—H14A119.4Cl2—C1S—H1SA108.8
C15—C14—H14A119.4Cl1—C1S—H1SA108.8
C16—C15—C14119.1 (10)Cl3—C1S—H1SA108.8
C16—C15—H15A120.5C2Sii—Cl5—C2S33.7 (14)
C14—C15—H15A120.5C2S—Cl4—C2Sii33.6 (15)
C15—C16—C11120.5 (10)C2Sii—C2S—Cl5ii74 (2)
C15—C16—H16A119.8C2Sii—C2S—Cl473.2 (7)
C11—C16—H16A119.8Cl5ii—C2S—Cl4111.7 (10)
C22—C21—C26118.2 (8)C2Sii—C2S—Cl572.5 (17)
C22—C21—P1119.7 (7)Cl5ii—C2S—Cl5113.0 (10)
C26—C21—P1122.0 (7)Cl4—C2S—Cl5111.2 (10)
C23—C22—C21121.0 (9)C2Sii—C2S—H2SA179.2
C23—C22—H22A119.5Cl5ii—C2S—H2SA106.9
C21—C22—H22A119.5Cl4—C2S—H2SA106.8
C22—C23—C24119.8 (9)Cl5—C2S—H2SA106.8
Symmetry codes: (i) x+3/2, y+1/2, z+1; (ii) x+2, y, z+3/2.

Experimental details

Crystal data
Chemical formula[Pd2I4(C34H24P2)2]·3CHCl3
Mr2067.45
Crystal system, space groupMonoclinic, C2/c
Temperature (K)150
a, b, c (Å)20.8960 (9), 9.5920 (5), 38.832 (2)
β (°) 99.804 (3)
V3)7669.6 (7)
Z4
Radiation typeMo Kα
µ (mm1)2.52
Crystal size (mm)0.14 × 0.06 × 0.02
Data collection
DiffractometerNonius KappaCCD
diffractometer
Absorption correctionMulti-scan
(SORTAV; Blessing, 1995)
Tmin, Tmax0.827, 0.958
No. of measured, independent and
observed [I > 2σ(I)] reflections
19576, 6672, 3732
Rint0.086
(sin θ/λ)max1)0.595
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.056, 0.112, 1.01
No. of reflections6672
No. of parameters411
No. of restraints4
H-atom treatmentH-atom parameters constrained
w = 1/[σ2(Fo2) + (0.024P)2 + 42.7375P]
where P = (Fo2 + 2Fc2)/3
Δρmax, Δρmin (e Å3)1.06, 0.91

Computer programs: COLLECT (Nonius, 2002), DENZO-SMN (Otwinowski & Minor, 1997), SIR92 (Altomare et al., 1994), SHELXTL (Sheldrick, 2001).

 

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