Download citation
Download citation
link to html
The structure of the title compound, [PdI2(C18H15P)2]·2CH2Cl2, has previously been reported by Debaerdemaeker, Kutoglu, Schmid & Weber [Acta Cryst. (1973), B29, 1283-1288] at room temperature. We report the structure determination of this compound from a twinned crystal at 173 (2) K. The Pd atom is located on a centre of inversion and has square-planar coordination geometry.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806013262/lh2044sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806013262/lh2044Isup2.hkl
Contains datablock I

CCDC reference: 608452

Key indicators

  • Single-crystal X-ray study
  • T = 173 K
  • Mean [sigma](C-C) = 0.015 Å
  • R factor = 0.047
  • wR factor = 0.148
  • Data-to-parameter ratio = 18.8

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.92 PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) I1 - Pd1 .. 7.31 su PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 15
Alert level G ABSTM02_ALERT_3_G When printed, the submitted absorption T values will be replaced by the scaled T values. Since the ratio of scaled T's is identical to the ratio of reported T values, the scaling does not imply a change to the absorption corrections used in the study. Ratio of Tmax expected/reported 0.923 Tmax scaled 0.510 Tmin scaled 0.474
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 4 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 1 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 1 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: X-AREA (Stoe & Cie, 2001); cell refinement: X-AREA; data reduction: X-AREA; program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP in SHELXTL-Plus (Sheldrick, 1991); software used to prepare material for publication: SHELXL97 and PLATON (Spek, 2003).

diiodobis(triphenylphosphine)palladium(II) dichloromethane disolvate top
Crystal data top
[PdI2(C18H15P)2]·2CH2Cl2F(000) = 1024
Mr = 1054.59Dx = 1.768 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 43265 reflections
a = 11.8422 (6) Åθ = 2.0–26.7°
b = 20.3802 (7) ŵ = 2.41 mm1
c = 8.2420 (4) ÅT = 173 K
β = 95.364 (4)°Block, dark red
V = 1980.47 (15) Å30.32 × 0.30 × 0.28 mm
Z = 2
Data collection top
Stoe IPDS-II two-circle
diffractometer
4044 independent reflections
Radiation source: fine-focus sealed tube3868 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.074
ω scansθmax = 26.5°, θmin = 2.0°
Absorption correction: multi-scan
(MULABS; Spek, 2003; Blessing, 1995)
h = 1414
Tmin = 0.513, Tmax = 0.553k = 2525
43265 measured reflectionsl = 810
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)] = 0.047Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.148H-atom parameters constrained
S = 1.37 w = 1/[σ2(Fo2) + (0.0112P)2 + 25.7032P]
where P = (Fo2 + 2Fc2)/3
4044 reflections(Δ/σ)max < 0.001
215 parametersΔρmax = 1.36 e Å3
0 restraintsΔρmin = 1.20 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*/Ueq
Pd10.50000.50000.50000.0179 (2)
I10.61286 (5)0.39141 (3)0.47747 (8)0.02967 (18)
P10.36134 (18)0.43787 (10)0.6144 (3)0.0192 (4)
C110.2503 (7)0.4805 (4)0.7140 (12)0.0253 (19)
C120.2500 (9)0.4838 (5)0.8822 (13)0.032 (2)
H120.30780.46220.94990.038*
C130.1657 (10)0.5185 (6)0.9528 (15)0.043 (3)
H130.16740.52151.06800.051*
C140.0799 (9)0.5485 (6)0.8551 (16)0.044 (3)
H140.02220.57200.90310.052*
C150.0775 (9)0.5444 (6)0.6864 (17)0.045 (3)
H150.01790.56480.61950.054*
C160.1617 (8)0.5108 (5)0.6156 (14)0.033 (2)
H160.15970.50810.50030.040*
C210.2785 (7)0.3875 (4)0.4635 (11)0.0231 (18)
C220.1838 (8)0.3533 (4)0.5056 (12)0.028 (2)
H220.16370.35560.61430.034*
C230.1183 (9)0.3160 (5)0.3920 (14)0.037 (2)
H230.05480.29220.42280.044*
C240.1471 (9)0.3140 (5)0.2316 (14)0.037 (2)
H240.10240.28880.15280.045*
C250.2388 (9)0.3479 (5)0.1862 (13)0.036 (2)
H250.25720.34620.07660.044*
C260.3061 (8)0.3853 (5)0.3025 (12)0.029 (2)
H260.36980.40890.27140.035*
C310.4239 (7)0.3834 (4)0.7736 (11)0.0205 (17)
C320.5071 (8)0.4101 (5)0.8858 (11)0.0270 (19)
H320.52810.45480.87580.032*
C330.5598 (8)0.3724 (5)1.0118 (12)0.032 (2)
H330.61430.39131.09010.038*
C340.5306 (8)0.3059 (5)1.0203 (13)0.034 (2)
H340.56560.27931.10520.040*
C350.4507 (9)0.2786 (5)0.9052 (13)0.033 (2)
H350.43310.23320.90990.039*
C360.3975 (8)0.3170 (4)0.7853 (11)0.0242 (18)
H360.34180.29820.70880.029*
C10.8212 (10)0.3169 (7)0.829 (2)0.064 (4)
H1A0.75520.33840.76830.077*
H1B0.81790.32650.94640.077*
Cl10.8113 (3)0.2321 (2)0.7992 (7)0.0814 (13)
Cl20.9452 (3)0.3500 (2)0.7662 (6)0.0732 (11)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pd10.0170 (4)0.0151 (4)0.0221 (4)0.0002 (3)0.0036 (4)0.0013 (3)
I10.0305 (3)0.0214 (3)0.0385 (3)0.0045 (2)0.0109 (3)0.0026 (2)
P10.0183 (10)0.0173 (10)0.0225 (11)0.0016 (8)0.0041 (8)0.0012 (8)
C110.018 (4)0.020 (4)0.038 (5)0.000 (3)0.004 (4)0.004 (4)
C120.035 (5)0.028 (5)0.034 (5)0.006 (4)0.010 (4)0.003 (4)
C130.046 (6)0.043 (6)0.041 (6)0.002 (5)0.020 (5)0.007 (5)
C140.032 (5)0.037 (6)0.064 (8)0.002 (5)0.014 (5)0.007 (6)
C150.027 (5)0.041 (6)0.068 (8)0.008 (5)0.009 (5)0.009 (6)
C160.025 (5)0.033 (5)0.041 (6)0.004 (4)0.001 (4)0.001 (5)
C210.020 (4)0.018 (4)0.031 (5)0.000 (3)0.001 (4)0.001 (4)
C220.027 (5)0.026 (5)0.032 (5)0.004 (4)0.004 (4)0.000 (4)
C230.030 (5)0.030 (5)0.050 (6)0.006 (4)0.002 (5)0.002 (5)
C240.036 (5)0.028 (5)0.045 (6)0.002 (4)0.012 (5)0.012 (5)
C250.037 (6)0.041 (6)0.029 (5)0.007 (5)0.005 (4)0.003 (5)
C260.030 (5)0.031 (5)0.028 (5)0.001 (4)0.006 (4)0.002 (4)
C310.022 (4)0.019 (4)0.021 (4)0.000 (3)0.004 (3)0.004 (3)
C320.025 (4)0.026 (4)0.029 (5)0.007 (4)0.002 (4)0.001 (4)
C330.025 (5)0.040 (5)0.029 (5)0.001 (4)0.005 (4)0.000 (4)
C340.032 (5)0.039 (5)0.030 (5)0.009 (4)0.005 (4)0.012 (4)
C350.039 (5)0.023 (4)0.038 (5)0.003 (4)0.006 (4)0.009 (4)
C360.023 (4)0.020 (4)0.030 (5)0.004 (3)0.005 (4)0.001 (4)
C10.032 (6)0.078 (10)0.082 (11)0.010 (6)0.007 (7)0.018 (9)
Cl10.057 (2)0.072 (3)0.111 (4)0.0132 (18)0.017 (2)0.016 (3)
Cl20.063 (2)0.074 (2)0.088 (3)0.0106 (19)0.037 (2)0.012 (2)
Geometric parameters (Å, º) top
Pd1—P1i2.340 (2)C23—C241.397 (16)
Pd1—P12.340 (2)C23—H230.9500
Pd1—I12.6009 (6)C24—C251.368 (15)
Pd1—I1i2.6009 (6)C24—H240.9500
P1—C311.823 (9)C25—C261.412 (14)
P1—C211.826 (9)C25—H250.9500
P1—C111.834 (9)C26—H260.9500
C11—C121.388 (14)C31—C361.394 (12)
C11—C161.407 (13)C31—C321.397 (12)
C12—C131.394 (14)C32—C331.391 (13)
C12—H120.9500C32—H320.9500
C13—C141.380 (17)C33—C341.403 (14)
C13—H130.9500C33—H330.9500
C14—C151.391 (18)C34—C351.392 (15)
C14—H140.9500C34—H340.9500
C15—C161.383 (14)C35—C361.367 (13)
C15—H150.9500C35—H350.9500
C16—H160.9500C36—H360.9500
C21—C221.391 (12)C1—Cl21.739 (14)
C21—C261.397 (13)C1—Cl11.748 (16)
C22—C231.385 (14)C1—H1A0.9900
C22—H220.9500C1—H1B0.9900
P1i—Pd1—P1180.0C22—C23—C24119.0 (10)
P1i—Pd1—I192.70 (5)C22—C23—H23120.5
P1—Pd1—I187.30 (5)C24—C23—H23120.5
P1i—Pd1—I1i87.30 (5)C25—C24—C23121.0 (10)
P1—Pd1—I1i92.70 (5)C25—C24—H24119.5
I1—Pd1—I1i179.999 (1)C23—C24—H24119.5
C31—P1—C21107.7 (4)C24—C25—C26120.0 (10)
C31—P1—C11103.1 (4)C24—C25—H25120.0
C21—P1—C11102.1 (4)C26—C25—H25120.0
C31—P1—Pd1111.5 (3)C21—C26—C25119.6 (9)
C21—P1—Pd1112.5 (3)C21—C26—H26120.2
C11—P1—Pd1118.9 (3)C25—C26—H26120.2
C12—C11—C16118.9 (9)C36—C31—C32118.7 (8)
C12—C11—P1122.6 (8)C36—C31—P1124.2 (7)
C16—C11—P1118.5 (8)C32—C31—P1117.0 (6)
C11—C12—C13120.6 (10)C33—C32—C31121.3 (9)
C11—C12—H12119.7C33—C32—H32119.4
C13—C12—H12119.7C31—C32—H32119.4
C14—C13—C12119.9 (11)C32—C33—C34118.3 (9)
C14—C13—H13120.0C32—C33—H33120.8
C12—C13—H13120.0C34—C33—H33120.8
C13—C14—C15120.1 (10)C35—C34—C33120.5 (9)
C13—C14—H14119.9C35—C34—H34119.7
C15—C14—H14119.9C33—C34—H34119.7
C16—C15—C14120.3 (11)C36—C35—C34120.1 (9)
C16—C15—H15119.9C36—C35—H35120.0
C14—C15—H15119.9C34—C35—H35120.0
C15—C16—C11120.1 (11)C35—C36—C31121.0 (9)
C15—C16—H16119.9C35—C36—H36119.5
C11—C16—H16119.9C31—C36—H36119.5
C22—C21—C26119.1 (9)Cl2—C1—Cl1112.9 (8)
C22—C21—P1120.4 (7)Cl2—C1—H1A109.0
C26—C21—P1120.4 (7)Cl1—C1—H1A109.0
C23—C22—C21121.3 (10)Cl2—C1—H1B109.0
C23—C22—H22119.3Cl1—C1—H1B109.0
C21—C22—H22119.3H1A—C1—H1B107.8
I1—Pd1—P1—C3147.6 (3)C11—P1—C21—C26133.0 (8)
I1i—Pd1—P1—C31132.4 (3)Pd1—P1—C21—C264.4 (8)
I1—Pd1—P1—C2173.5 (3)C26—C21—C22—C231.7 (14)
I1i—Pd1—P1—C21106.5 (3)P1—C21—C22—C23178.5 (8)
I1—Pd1—P1—C11167.3 (4)C21—C22—C23—C241.3 (15)
I1i—Pd1—P1—C1112.7 (4)C22—C23—C24—C250.4 (16)
C31—P1—C11—C1219.5 (9)C23—C24—C25—C260.3 (16)
C21—P1—C11—C12131.2 (8)C22—C21—C26—C251.0 (14)
Pd1—P1—C11—C12104.4 (8)P1—C21—C26—C25177.8 (7)
C31—P1—C11—C16160.1 (7)C24—C25—C26—C210.1 (15)
C21—P1—C11—C1648.4 (8)C21—P1—C31—C368.4 (9)
Pd1—P1—C11—C1676.0 (8)C11—P1—C31—C3699.1 (8)
C16—C11—C12—C132.4 (15)Pd1—P1—C31—C36132.2 (7)
P1—C11—C12—C13178.0 (8)C21—P1—C31—C32168.7 (7)
C11—C12—C13—C141.8 (16)C11—P1—C31—C3283.9 (7)
C12—C13—C14—C150.2 (17)Pd1—P1—C31—C3244.8 (8)
C13—C14—C15—C160.6 (18)C36—C31—C32—C332.8 (14)
C14—C15—C16—C110.1 (17)P1—C31—C32—C33180.0 (7)
C12—C11—C16—C151.5 (15)C31—C32—C33—C342.4 (15)
P1—C11—C16—C15178.8 (8)C32—C33—C34—C350.1 (15)
C31—P1—C21—C2264.4 (8)C33—C34—C35—C361.9 (15)
C11—P1—C21—C2243.7 (8)C34—C35—C36—C311.5 (15)
Pd1—P1—C21—C22172.4 (6)C32—C31—C36—C350.8 (13)
C31—P1—C21—C26118.8 (8)P1—C31—C36—C35177.8 (7)
Symmetry code: (i) x+1, y+1, z+1.
 

Follow Acta Cryst. E
Sign up for e-alerts
Follow Acta Cryst. on Twitter
Follow us on facebook
Sign up for RSS feeds