trans-Di­chloro­bis­(cyclo­hexyl­di­phenyl­phosphine)­palladium(II)

As part of a systematic investigation for a number of Pd^II complexes in order to find correlations between molecular structure and chemical behaviour, crystals of the title compound, trans-[PdCl₂(PPh₂Cy)₂] or [PdCl₂(C₁₈H₂₁P)₂], were prepared. The Pd atom is located on an inversion cneter. Selected geometrical parameters are: Pd-P 2.3256 (10) and Pd-Cl 2.3007 (11) Å, and P-Pd-Cl 91.38 (4)°. The effective and Tolman cone angles for the PPh₂Cy ligand were determined as 151.0 and 154.6°, respectively.

Key indicators

• Single-crystal X-ray study
• T = 293 K
• Mean [sigma](C-C) = 0.006 Å
• R factor = 0.042
• wR factor = 0.105
• Data-to-parameter ratio = 22.7

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


 Alert Level A:



DIFF_019  Alert A _diffrn_standards_number is missing
          Number of standards used in measurement.

DIFF_020  Alert A _diffrn_standards_interval_count and
          _diffrn_standards_interval_time are missing. Number of measurements
          between standards or time (min) between standards.


 2 Alert Level A = Potentially serious problem

 0 Alert Level B = Potential problem

 0 Alert Level C = Please check

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Computing details

Data collection: SMART (Bruker, 1998); cell refinement: SAINT (Bruker, 1998); data reduction: SAINT; program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandendurg & Brendt, 2001); software used to prepare material for publication: WinGX (Farrugia, 1999).

(I)

Crystal data

[PdCl2(C18H21P)2]	F(000) = 736
Mr = 713.98	Dx = 1.373 Mg m^−3
Monoclinic, P21/n	Mo Kα radiation, λ = 0.71069 Å
Hall symbol: -P 2yn	Cell parameters from 204 reflections
a = 9.797 (5) Å	θ = 3–23°
b = 12.552 (5) Å	µ = 0.81 mm^−1
c = 14.087 (5) Å	T = 293 K
β = 94.357 (5)°	Cuboid, yellow
V = 1727.3 (13) Å^3	0.20 × 0.19 × 0.10 mm
Z = 2

Data collection

Bruker 1000 SMART diffractometer	2604 reflections with I > 2σ(I)
ω scans	Rint = 0.050
Absorption correction: multi-scan (SADABS; Siemens, 1998)	θmax = 28.3°, θmin = 2.2°
Tmin = 0.86, Tmax = 0.92	h = −10→13
11930 measured reflections	k = −15→16
4236 independent reflections	l = −15→18

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	H-atom parameters constrained
R[F^2 > 2σ(F^2)] = 0.042	w = 1/[σ^2(Fo^2) + (0.0541P)^2 + 0.0819P] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.106	(Δ/σ)max = 0.007
S = 0.95	Δρmax = 0.65 e Å^−3
4236 reflections	Δρmin = −0.74 e Å^−3
187 parameters

Special details

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. The intensity data were collected on a Siemens SMART CCD diffractometer using an exposure time of 10 s per frame. A total of 1315 frames were collected, with a frame width of 0.3° being used, covering up to τ = 28.32°, with a completeness of 98.6% being achieved. The first 50 frames were recollected at the end of the data collection to check for decay; none was found. The minimum residual electron density is located within 1.0 Å of the Pd atom.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Pd	0	0	0	0.03438 (12)
P	0.08843 (8)	0.12606 (7)	0.10897 (6)	0.0353 (2)
Cl	−0.14801 (11)	0.12314 (8)	−0.07185 (7)	0.0637 (3)
C11	−0.0168 (3)	0.2445 (3)	0.1267 (2)	0.0416 (8)
H11	−0.0423	0.2701	0.0621	0.05*
C31	0.1360 (3)	0.0815 (3)	0.2298 (2)	0.0407 (8)
C36	0.0555 (4)	0.0032 (3)	0.2688 (3)	0.0510 (9)
H36	−0.017	−0.0268	0.2315	0.061*
C23	0.3598 (7)	0.2752 (5)	−0.0538 (3)	0.102 (2)
H23	0.3592	0.3304	−0.0978	0.123*
C32	0.2316 (3)	0.1371 (3)	0.2905 (2)	0.0468 (9)
H32	0.2767	0.1963	0.2683	0.056*
C21	0.2447 (3)	0.1705 (3)	0.0595 (2)	0.0445 (9)
C13	−0.0447 (4)	0.4311 (3)	0.1802 (3)	0.0698 (12)
H13A	0	0.4857	0.2202	0.084*
H13B	−0.0614	0.4605	0.1168	0.084*
C34	0.1784 (5)	0.0253 (3)	0.4217 (3)	0.0622 (12)
H34	0.1886	0.0101	0.4865	0.075*
C26	0.3664 (4)	0.1153 (4)	0.0798 (3)	0.0646 (11)
H26	0.37	0.0607	0.1244	0.078*
C33	0.2584 (4)	0.1029 (3)	0.3844 (3)	0.0545 (10)
H33	0.3307	0.1327	0.422	0.065*
C35	0.0824 (4)	−0.0306 (3)	0.3629 (3)	0.0551 (10)
H35	0.0371	−0.0893	0.3858	0.066*
C12	0.0503 (4)	0.3381 (3)	0.1758 (3)	0.0574 (10)
H12A	0.129	0.3591	0.1423	0.069*
H12B	0.083	0.3178	0.2399	0.069*
C16	−0.1504 (4)	0.2151 (3)	0.1648 (3)	0.0571 (10)
H16A	−0.1329	0.1838	0.2275	0.068*
H16B	−0.1955	0.1618	0.1236	0.068*
C22	0.2401 (5)	0.2491 (3)	−0.0091 (3)	0.0698 (12)
H22	0.1585	0.2847	−0.0259	0.084*
C15	−0.2443 (4)	0.3091 (3)	0.1716 (3)	0.0638 (11)
H15A	−0.2809	0.3282	0.108	0.077*
H15B	−0.3207	0.2881	0.2074	0.077*
C24	0.4786 (7)	0.2174 (6)	−0.0309 (5)	0.110 (2)
H24	0.5571	0.2325	−0.0617	0.132*
C25	0.4814 (5)	0.1406 (5)	0.0344 (4)	0.0907 (17)
H25	0.5624	0.1036	0.0496	0.109*
C14	−0.1782 (5)	0.4051 (3)	0.2176 (4)	0.0803 (14)
H14A	−0.2392	0.4655	0.2076	0.096*
H14B	−0.1644	0.3929	0.2857	0.096*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Pd	0.02859 (18)	0.03465 (19)	0.0390 (2)	0.00197 (16)	−0.00313 (14)	−0.00181 (17)
P	0.0292 (4)	0.0375 (5)	0.0387 (5)	−0.0010 (4)	−0.0006 (4)	−0.0019 (4)
Cl	0.0719 (7)	0.0522 (6)	0.0619 (6)	0.0254 (5)	−0.0275 (5)	−0.0109 (5)
C11	0.0408 (18)	0.041 (2)	0.0421 (19)	0.0043 (15)	−0.0010 (16)	−0.0050 (15)
C31	0.0347 (18)	0.046 (2)	0.0410 (19)	−0.0020 (15)	−0.0025 (16)	−0.0012 (15)
C36	0.045 (2)	0.059 (2)	0.049 (2)	−0.0128 (19)	0.0000 (17)	−0.003 (2)
C23	0.157 (6)	0.087 (4)	0.071 (3)	−0.039 (4)	0.062 (4)	−0.011 (3)
C32	0.044 (2)	0.044 (2)	0.051 (2)	−0.0015 (16)	−0.0030 (18)	−0.0045 (17)
C21	0.042 (2)	0.046 (2)	0.045 (2)	−0.0108 (16)	0.0075 (17)	−0.0105 (16)
C13	0.072 (3)	0.056 (3)	0.079 (3)	0.011 (2)	−0.008 (3)	−0.016 (2)
C34	0.081 (3)	0.063 (3)	0.041 (2)	0.004 (2)	−0.005 (2)	0.0043 (18)
C26	0.037 (2)	0.081 (3)	0.077 (3)	−0.008 (2)	0.009 (2)	−0.013 (2)
C33	0.059 (2)	0.052 (2)	0.049 (2)	0.0053 (19)	−0.017 (2)	−0.0096 (18)
C35	0.060 (3)	0.056 (2)	0.049 (2)	−0.0054 (18)	0.002 (2)	0.0062 (18)
C12	0.052 (2)	0.047 (2)	0.073 (3)	0.0034 (17)	0.002 (2)	−0.0077 (19)
C16	0.043 (2)	0.055 (2)	0.073 (3)	0.0060 (17)	0.006 (2)	−0.007 (2)
C22	0.084 (3)	0.068 (3)	0.060 (3)	−0.009 (2)	0.027 (2)	−0.005 (2)
C15	0.045 (2)	0.078 (3)	0.070 (3)	0.015 (2)	0.007 (2)	−0.001 (2)
C24	0.089 (4)	0.132 (6)	0.118 (5)	−0.045 (4)	0.067 (4)	−0.051 (4)
C25	0.052 (3)	0.114 (5)	0.110 (4)	−0.020 (3)	0.031 (3)	−0.037 (4)
C14	0.071 (3)	0.066 (3)	0.104 (4)	0.025 (2)	0.008 (3)	−0.006 (3)

Geometric parameters (Å, º)

Pd—Cl	2.3007 (11)	C13—H13A	0.97
Pd—Cl^i	2.3007 (11)	C13—H13B	0.97
Pd—P	2.3256 (10)	C34—C33	1.380 (5)
Pd—P^i	2.3256 (10)	C34—C35	1.395 (6)
P—C31	1.819 (3)	C34—H34	0.93
P—C21	1.817 (3)	C26—C25	1.374 (6)
P—C11	1.837 (3)	C26—H26	0.93
C11—C12	1.490 (5)	C33—H33	0.93
C11—C16	1.498 (5)	C35—H35	0.93
C11—H11	0.98	C12—H12A	0.97
C31—C36	1.398 (4)	C12—H12B	0.97
C31—C32	1.405 (5)	C16—C15	1.503 (5)
C36—C35	1.397 (5)	C16—H16A	0.97
C36—H36	0.93	C16—H16B	0.97
C23—C24	1.389 (8)	C22—H22	0.93
C23—C22	1.411 (6)	C15—C14	1.492 (6)
C23—H23	0.93	C15—H15A	0.97
C32—C33	1.397 (5)	C15—H15B	0.97
C32—H32	0.93	C24—C25	1.332 (8)
C21—C22	1.379 (5)	C24—H24	0.93
C21—C26	1.390 (5)	C25—H25	0.93
C13—C14	1.483 (6)	C14—H14A	0.97
C13—C12	1.497 (5)	C14—H14B	0.97
Cl—Pd—Cl^i	180.00	C25—C26—C21	120.7 (5)
Cl—Pd—P	91.38 (4)	C25—C26—H26	119.7
Cl^i—Pd—P	88.62 (4)	C21—C26—H26	119.7
Cl—Pd—P^i	88.62 (4)	C34—C33—C32	120.4 (4)
Cl^i—Pd—P^i	91.38 (4)	C34—C33—H33	119.8
P—Pd—P^i	180.00	C32—C33—H33	119.8
C31—P—C21	106.85 (16)	C36—C35—C34	118.7 (4)
C31—P—C11	103.19 (15)	C36—C35—H35	120.6
C21—P—C11	107.53 (16)	C34—C35—H35	120.6
C31—P—Pd	117.68 (11)	C11—C12—C13	112.3 (3)
C21—P—Pd	103.79 (11)	C11—C12—H12A	109.1
C11—P—Pd	117.12 (11)	C13—C12—H12A	109.1
C12—C11—C16	113.3 (3)	C11—C12—H12B	109.1
C12—C11—P	118.0 (2)	C13—C12—H12B	109.1
C16—C11—P	111.3 (2)	H12A—C12—H12B	107.9
C12—C11—H11	104.2	C11—C16—C15	112.7 (3)
C16—C11—H11	104.2	C11—C16—H16A	109.1
P—C11—H11	104.2	C15—C16—H16A	109.1
C36—C31—C32	118.7 (3)	C11—C16—H16B	109.1
C36—C31—P	118.2 (3)	C15—C16—H16B	109.1
C32—C31—P	121.9 (3)	H16A—C16—H16B	107.8
C35—C36—C31	121.0 (3)	C21—C22—C23	119.6 (5)
C35—C36—H36	119.5	C21—C22—H22	120.2
C31—C36—H36	119.5	C23—C22—H22	120.2
C24—C23—C22	119.1 (5)	C14—C15—C16	114.4 (3)
C24—C23—H23	120.5	C14—C15—H15A	108.7
C22—C23—H23	120.5	C16—C15—H15A	108.7
C33—C32—C31	119.5 (3)	C14—C15—H15B	108.7
C33—C32—H32	120.3	C16—C15—H15B	108.7
C31—C32—H32	120.3	H15A—C15—H15B	107.6
C22—C21—C26	118.8 (3)	C25—C24—C23	120.7 (5)
C22—C21—P	120.3 (3)	C25—C24—H24	119.6
C26—C21—P	120.2 (3)	C23—C24—H24	119.6
C14—C13—C12	114.3 (4)	C24—C25—C26	120.9 (6)
C14—C13—H13A	108.7	C24—C25—H25	119.5
C12—C13—H13A	108.7	C26—C25—H25	119.5
C14—C13—H13B	108.7	C13—C14—C15	112.9 (4)
C12—C13—H13B	108.7	C13—C14—H14A	109
H13A—C13—H13B	107.6	C15—C14—H14A	109
C33—C34—C35	120.4 (4)	C13—C14—H14B	109
C33—C34—H34	119.8	C15—C14—H14B	109
C35—C34—H34	119.8	H14A—C14—H14B	107.8

Symmetry code: (i) −x, −y, −z.