Download citation
Download citation
link to html
The title complex, [PdI2(dppe)], where dppe is 1,2-bis­(di­phenyl­phosphino)­ethane (C26H24P2), has a square-planar coordination of the Pd atom with a small tetrahedral distortion and an envelope conformation of the five-membered metallocycle, similar to those observed in [PdI2(dppe)]·CHCl3.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536801007589/bt6044sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536801007589/bt6044Isup2.hkl
Contains datablock I

CCDC reference: 170275

Key indicators

  • Single-crystal X-ray study
  • T = 150 K
  • Mean [sigma](C-C) = 0.009 Å
  • R factor = 0.041
  • wR factor = 0.080
  • Data-to-parameter ratio = 21.1

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry

General Notes

REFLT_03 From the CIF: _diffrn_reflns_theta_max 27.50 From the CIF: _reflns_number_total 5903 From the CIF: _diffrn_reflns_limit_ max hkl 12. 27. 20. From the CIF: _diffrn_reflns_limit_ min hkl -12. -27. -20. TEST1: Expected hkl limits for theta max Calculated maximum hkl 12. 25. 18. Calculated minimum hkl -12. -25. -18. ALERT: Expected hkl max differ from CIF values

Computing details top

Data collection: SMART (Siemens, 1995); cell refinement: SMART; data reduction: SAINT (Siemens, 1995); program(s) used to solve structure: SHELXS86 (Sheldrick, 1990); program(s) used to refine structure: SHELXL93 (Sheldrick, 1993); molecular graphics: SHELXTL (Siemens, 1995); software used to prepare material for publication: SHELXTL.

[1,2-bis(diphenylphosphino)ethane-P,P]diiodopalladium(II) top
Crystal data top
[PdI2(C26H24P2)]F(000) = 1448
Mr = 758.59Dx = 1.962 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
a = 9.465 (1) ÅCell parameters from 432 reflections
b = 19.821 (1) Åθ = 12–20°
c = 14.208 (1) ŵ = 3.26 mm1
β = 105.51 (1)°T = 150 K
V = 2568.4 (4) Å3Plate, yellow
Z = 40.30 × 0.12 × 0.06 mm
Data collection top
SMART 1K CCD area-detector
diffractometer
5903 independent reflections
Radiation source: fine-focus sealed tube4690 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.056
ω scansθmax = 27.5°, θmin = 1.8°
Absorption correction: integration
(XPREP SHELXTL; Siemens, 1995), Rint = 0.107 before correction
h = 1212
Tmin = 0.355, Tmax = 0.832k = 2727
18477 measured reflectionsl = 2020
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) = 0.080H-atom parameters constrained
S = 1.16 w = 1/[σ2(Fo2) + (0.0102P)2 + 11.804P]
where P = (Fo2 + 2Fc2)/3
5903 reflections(Δ/σ)max < 0.001
280 parametersΔρmax = 0.66 e Å3
0 restraintsΔρmin = 1.05 e Å3
Special details top

Experimental. The data collection nominally covered over a hemisphere of reciprocal space, by a combination of 4 sets of ω scans; each set at different φ and/or 2θ angles and each scan (10 sec exposure) covering 0.3° in ω. Crystal to detector distance 4.51 cm. Crystal decay was monitored by repeating 50 initial frames at the end of data collection and comparing 279 duplicate reflections.

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 on F2 for ALL reflections except for 97 with very negative F2. Weighted R-factors wR and all goodnesses of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The observed criterion of F2 > σ(F2) is used only for calculating _R_factor_gt etc. and is not relevant to the choice of reflections for refinement.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Pd0.18303 (4)0.326237 (19)0.21618 (3)0.01517 (9)
I10.05634 (4)0.213028 (18)0.13280 (3)0.02293 (9)
I20.06742 (4)0.387890 (19)0.21131 (3)0.02568 (10)
P10.40705 (14)0.28443 (7)0.21606 (10)0.0165 (3)
P20.31003 (15)0.41505 (7)0.29652 (10)0.0178 (3)
C10.5489 (6)0.3438 (3)0.2838 (4)0.0234 (12)
H1A0.63840.31840.31720.030*
H1B0.57470.37570.23750.030*
C20.4926 (6)0.3828 (3)0.3592 (4)0.0212 (11)
H2A0.55970.42060.38610.028*
H2B0.48670.35280.41380.028*
C110.4493 (5)0.2046 (2)0.2801 (4)0.0164 (10)
C120.4064 (7)0.1959 (3)0.3658 (4)0.0283 (13)
H120.35600.23130.38840.034*
C130.4355 (7)0.1362 (3)0.4185 (4)0.0366 (15)
H130.40680.13110.47730.044*
C140.5075 (6)0.0843 (3)0.3855 (4)0.0300 (14)
H140.52590.04310.42100.036*
C150.5518 (7)0.0920 (3)0.3016 (5)0.0328 (14)
H150.60150.05630.27940.039*
C160.5237 (7)0.1524 (3)0.2488 (4)0.0281 (13)
H160.55560.15760.19120.034*
C210.4477 (6)0.2758 (3)0.0986 (4)0.0181 (11)
C220.5951 (6)0.2674 (3)0.0975 (4)0.0221 (11)
H220.67040.26620.15710.026*
C230.6307 (6)0.2609 (3)0.0093 (4)0.0268 (13)
H230.73000.25510.00860.032*
C240.5215 (7)0.2628 (3)0.0777 (4)0.0282 (13)
H240.54560.25710.13790.034*
C250.3774 (7)0.2732 (3)0.0771 (4)0.0288 (13)
H250.30350.27610.13720.035*
C260.3395 (6)0.2790 (3)0.0104 (4)0.0219 (11)
H260.23990.28530.01010.026*
C310.2524 (6)0.4582 (3)0.3927 (4)0.0223 (12)
C320.2213 (6)0.5271 (3)0.3899 (5)0.0301 (13)
H320.22690.55320.33490.036*
C330.1832 (6)0.5575 (3)0.4675 (5)0.0347 (15)
H330.16270.60440.46510.042*
C340.1738 (6)0.5204 (4)0.5478 (5)0.0398 (17)
H340.14570.54150.60010.048*
C350.2059 (7)0.4519 (4)0.5512 (5)0.0412 (17)
H350.20130.42630.60680.049*
C360.2446 (7)0.4207 (3)0.4747 (4)0.0307 (14)
H360.26590.37380.47780.037*
C410.3480 (6)0.4757 (3)0.2123 (4)0.0197 (11)
C420.4484 (6)0.5287 (3)0.2444 (4)0.0260 (12)
H420.48920.53570.31240.031*
C430.4887 (7)0.5708 (3)0.1776 (5)0.0338 (14)
H430.55730.60610.20010.041*
C440.4278 (7)0.5615 (3)0.0778 (5)0.0354 (15)
H440.45570.59020.03220.043*
C450.3277 (7)0.5106 (3)0.0452 (4)0.0320 (14)
H450.28530.50490.02290.038*
C460.2879 (6)0.4672 (3)0.1112 (4)0.0245 (12)
H460.21970.43190.08780.029*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pd0.01245 (19)0.01539 (19)0.01755 (18)0.00116 (15)0.00381 (14)0.00207 (16)
I10.02370 (19)0.01948 (18)0.02451 (18)0.00400 (15)0.00452 (14)0.00343 (15)
I20.01920 (18)0.0271 (2)0.0311 (2)0.00150 (15)0.00725 (15)0.00585 (16)
P10.0140 (6)0.0167 (6)0.0192 (6)0.0001 (5)0.0049 (5)0.0001 (5)
P20.0165 (7)0.0172 (7)0.0191 (7)0.0006 (5)0.0037 (5)0.0024 (5)
C10.016 (3)0.025 (3)0.029 (3)0.002 (2)0.006 (2)0.001 (2)
C20.020 (3)0.020 (3)0.021 (3)0.002 (2)0.000 (2)0.002 (2)
C110.015 (2)0.016 (3)0.018 (2)0.001 (2)0.003 (2)0.000 (2)
C120.035 (3)0.027 (3)0.026 (3)0.002 (3)0.013 (3)0.002 (2)
C130.045 (4)0.042 (4)0.024 (3)0.002 (3)0.012 (3)0.006 (3)
C140.025 (3)0.027 (3)0.032 (3)0.005 (3)0.002 (3)0.010 (3)
C150.040 (4)0.017 (3)0.043 (4)0.009 (3)0.013 (3)0.001 (3)
C160.036 (3)0.021 (3)0.030 (3)0.004 (3)0.014 (3)0.001 (2)
C210.017 (3)0.019 (3)0.019 (2)0.001 (2)0.006 (2)0.001 (2)
C220.019 (3)0.024 (3)0.024 (3)0.002 (2)0.008 (2)0.006 (2)
C230.025 (3)0.029 (3)0.031 (3)0.007 (2)0.016 (3)0.006 (3)
C240.039 (4)0.024 (3)0.026 (3)0.002 (3)0.016 (3)0.003 (2)
C250.030 (3)0.030 (3)0.023 (3)0.011 (3)0.001 (2)0.002 (2)
C260.017 (3)0.026 (3)0.022 (3)0.004 (2)0.004 (2)0.001 (2)
C310.016 (3)0.030 (3)0.020 (3)0.003 (2)0.003 (2)0.008 (2)
C320.024 (3)0.031 (3)0.034 (3)0.002 (3)0.006 (3)0.010 (3)
C330.025 (3)0.036 (4)0.042 (4)0.003 (3)0.007 (3)0.023 (3)
C340.018 (3)0.071 (5)0.032 (3)0.010 (3)0.009 (3)0.021 (3)
C350.036 (4)0.063 (5)0.025 (3)0.007 (3)0.009 (3)0.006 (3)
C360.033 (3)0.034 (3)0.026 (3)0.007 (3)0.010 (3)0.002 (3)
C410.019 (3)0.019 (3)0.023 (3)0.002 (2)0.008 (2)0.002 (2)
C420.026 (3)0.025 (3)0.026 (3)0.005 (2)0.006 (2)0.001 (2)
C430.034 (3)0.027 (3)0.041 (4)0.011 (3)0.011 (3)0.003 (3)
C440.051 (4)0.021 (3)0.043 (4)0.003 (3)0.028 (3)0.001 (3)
C450.042 (4)0.031 (3)0.023 (3)0.001 (3)0.009 (3)0.004 (3)
C460.029 (3)0.023 (3)0.022 (3)0.002 (2)0.008 (2)0.001 (2)
Geometric parameters (Å, º) top
Pd—P22.2612 (14)C23—C241.384 (8)
Pd—P12.2769 (14)C23—H230.9504
Pd—I22.6514 (6)C24—C251.381 (8)
Pd—I12.6678 (5)C24—H240.9505
P1—C111.815 (5)C25—C261.387 (8)
P1—C211.818 (5)C25—H250.9503
P1—C11.850 (6)C26—H260.9503
P2—C411.798 (5)C31—C321.394 (8)
P2—C311.815 (5)C31—C361.402 (8)
P2—C21.834 (5)C32—C331.386 (8)
C1—C21.528 (7)C32—H320.9502
C1—H1A0.9901C33—C341.381 (9)
C1—H1B0.9902C33—H330.9499
C2—H2A0.9899C34—C351.390 (10)
C2—H2B0.9902C34—H340.9504
C11—C161.391 (7)C35—C361.381 (9)
C11—C121.394 (7)C35—H350.9503
C12—C131.389 (8)C36—H360.9497
C12—H120.9500C41—C461.407 (7)
C13—C141.383 (9)C41—C421.408 (8)
C13—H130.9506C42—C431.392 (8)
C14—C151.374 (9)C42—H420.9503
C14—H140.9500C43—C441.393 (9)
C15—C161.400 (8)C43—H430.9500
C15—H150.9501C44—C451.378 (9)
C16—H160.9504C44—H440.9502
C21—C261.392 (7)C45—C461.396 (8)
C21—C221.410 (7)C45—H450.9503
C22—C231.386 (7)C46—H460.9500
C22—H220.9502
P2—Pd—P185.08 (5)C23—C22—C21120.1 (5)
P2—Pd—I290.30 (4)C23—C22—H22119.9
P1—Pd—I2173.71 (4)C21—C22—H22120.0
P2—Pd—I1173.81 (4)C24—C23—C22120.0 (5)
P1—Pd—I190.09 (4)C24—C23—H23119.9
I2—Pd—I194.790 (18)C22—C23—H23120.0
C11—P1—C21107.8 (2)C25—C24—C23120.1 (5)
C11—P1—C1105.1 (2)C25—C24—H24119.9
C21—P1—C1103.6 (2)C23—C24—H24120.0
C11—P1—Pd113.39 (17)C24—C25—C26120.6 (5)
C21—P1—Pd117.44 (17)C24—C25—H25119.6
C1—P1—Pd108.34 (18)C26—C25—H25119.7
C41—P2—C31109.8 (3)C25—C26—C21119.9 (5)
C41—P2—C2103.1 (3)C25—C26—H26120.1
C31—P2—C2103.4 (2)C21—C26—H26120.0
C41—P2—Pd110.99 (18)C32—C31—C36119.1 (5)
C31—P2—Pd121.39 (18)C32—C31—P2122.9 (4)
C2—P2—Pd106.18 (18)C36—C31—P2117.9 (5)
C2—C1—P1110.3 (4)C33—C32—C31120.1 (6)
C2—C1—H1A109.6C33—C32—H32120.0
P1—C1—H1A109.6C31—C32—H32120.0
C2—C1—H1B109.6C34—C33—C32121.0 (6)
P1—C1—H1B109.6C34—C33—H33119.6
H1A—C1—H1B108.1C32—C33—H33119.5
C1—C2—P2107.2 (4)C33—C34—C35119.1 (6)
C1—C2—H2A110.2C33—C34—H34120.4
P2—C2—H2A110.3C35—C34—H34120.5
C1—C2—H2B110.3C36—C35—C34120.8 (6)
P2—C2—H2B110.3C36—C35—H35119.7
H2A—C2—H2B108.5C34—C35—H35119.5
C16—C11—C12118.6 (5)C35—C36—C31120.0 (6)
C16—C11—P1123.4 (4)C35—C36—H36120.0
C12—C11—P1118.0 (4)C31—C36—H36120.0
C13—C12—C11120.9 (5)C46—C41—C42118.2 (5)
C13—C12—H12119.5C46—C41—P2120.1 (4)
C11—C12—H12119.6C42—C41—P2121.4 (4)
C14—C13—C12119.8 (6)C43—C42—C41120.7 (5)
C14—C13—H13120.1C43—C42—H42119.7
C12—C13—H13120.1C41—C42—H42119.6
C15—C14—C13120.2 (6)C42—C43—C44120.1 (6)
C15—C14—H14120.0C42—C43—H43119.9
C13—C14—H14119.8C44—C43—H43120.0
C14—C15—C16120.2 (5)C45—C44—C43119.9 (6)
C14—C15—H15119.9C45—C44—H44120.0
C16—C15—H15119.9C43—C44—H44120.1
C11—C16—C15120.3 (5)C44—C45—C46120.7 (6)
C11—C16—H16119.9C44—C45—H45119.7
C15—C16—H16119.8C46—C45—H45119.6
C26—C21—C22119.1 (5)C45—C46—C41120.3 (5)
C26—C21—P1122.5 (4)C45—C46—H46119.9
C22—C21—P1118.4 (4)C41—C46—H46119.8
 

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