Di-μ₂-chloro-bis­[(benzyl­diphenyl­phosphine)chloro­palladium(II)]

The molecule of the title compound, [Pd₂Cl₄(C₁₉H₁₇P)₂] or [Pd(μ₂-Cl)Cl(PPh₂Bz)]₂, where Bz = CH₂Ph, lies on an inversion centre. The Pd atom has a distorted square-planar coordination environment formed by a benzyl­diphenyl­phosphine [Pd—P = 2.2218 (6) Å], a terminal chloride [Pd—Cl = 2.2729 (5) Å] and two bridging chloride ligands. The Pd—Cl bond in the position trans to the phosphine ligand [Pd—Cl = 2.4123 (5) Å] is considerably longer than the Pd—Cl bond in the position trans to the terminal chloride [Pd—Cl = 2.3155 (5) Å].

Key indicators

• Single-crystal X-ray study
• T = 100 K
• Mean [sigma](C-C)= 0.004 Å
• R factor = 0.025
• wR factor = 0.064
• Data-to-parameter ratio = 21.8

checkCIF/PLATON results

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Computing details

Data collection: APEX2 (Bruker, 2005); cell refinement: SAINT-Plus (Bruker, 2004); data reduction: SAINT-Plus and XPREP (Bruker 2004); program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg & Putz, 2005); software used to prepare material for publication: WinGX (Farrugia, 1999).

(I)

Crystal data

[PdCl2(C19H17P)]2	Z = 1
Mr = 907.19	F(000) = 452
Triclinic, P1	Dx = 1.656 Mg m^−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 9.2060 (2) Å	Cell parameters from 6089 reflections
b = 10.2804 (2) Å	θ = 2.5–28.3°
c = 10.8020 (4) Å	µ = 1.40 mm^−1
α = 99.347 (2)°	T = 100 K
β = 96.505 (2)°	Block, red
γ = 113.143 (1)°	0.15 × 0.08 × 0.05 mm
V = 909.72 (4) Å^3

Data collection

Bruker X8 APEXII diffractometer	4530 independent reflections
Radiation source: fine-focus sealed tube	3853 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.032
Detector resolution: 512 pixels mm^-1	θmax = 28.3°, θmin = 2.2°
ω and φ scans	h = −11→12
Absorption correction: multi-scan (SADABS; Bruker, 1998)	k = −13→13
Tmin = 0.818, Tmax = 0.933	l = −14→14
15329 measured reflections

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	H-atom parameters constrained
R[F^2 > 2σ(F^2)] = 0.025	w = 1/[σ^2(Fo^2) + (0.0292P)^2 + 0.2322P] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.064	(Δ/σ)max = 0.001
S = 1.06	Δρmax = 0.45 e Å^−3
4530 reflections	Δρmin = −0.55 e Å^−3
208 parameters

Special details

Experimental. The intensity data was collected on a Bruker X8 ApexII diffractometer using an exposure time of 10 s/frame. A total of 1688 frames were collected with a frame width of 0.5° covering up to θ = 28.33° with 99.6% completeness accomplished.

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.

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

	x	y	z	Uiso*/Ueq
Pd	0.84148 (2)	0.328676 (17)	0.951948 (14)	0.01312 (6)
P	0.71935 (7)	0.15169 (6)	0.77710 (5)	0.01475 (12)
Cl1	1.01892 (7)	0.48850 (5)	0.85316 (5)	0.01782 (11)
Cl2	0.67930 (7)	0.17734 (6)	1.05986 (5)	0.02234 (13)
C1	0.4991 (3)	0.0784 (2)	0.7454 (2)	0.0193 (5)
H1A	0.4566	0.0049	0.6634	0.023*
H1B	0.4591	0.0282	0.8136	0.023*
C11	0.4325 (3)	0.1899 (2)	0.7384 (2)	0.0202 (5)
C12	0.3877 (3)	0.2176 (3)	0.6210 (2)	0.0250 (5)
H12	0.3999	0.1657	0.5446	0.03*
C13	0.3259 (3)	0.3192 (3)	0.6144 (2)	0.0320 (6)
H13	0.2965	0.3372	0.5339	0.038*
C14	0.3066 (4)	0.3948 (3)	0.7241 (3)	0.0368 (7)
H14	0.264	0.4648	0.7194	0.044*
C15	0.3495 (3)	0.3682 (3)	0.8411 (2)	0.0335 (6)
H15	0.3356	0.4196	0.9168	0.04*
C16	0.4127 (3)	0.2670 (3)	0.8486 (2)	0.0259 (5)
H16	0.4426	0.2501	0.9295	0.031*
C21	0.7808 (3)	0.2041 (2)	0.63209 (19)	0.0178 (5)
C22	0.7589 (3)	0.3207 (3)	0.5962 (2)	0.0256 (5)
H22	0.7153	0.3736	0.6487	0.031*
C23	0.8009 (3)	0.3591 (3)	0.4836 (2)	0.0318 (6)
H23	0.7845	0.4375	0.4585	0.038*
C24	0.8669 (3)	0.2830 (3)	0.4074 (2)	0.0330 (6)
H24	0.8948	0.3089	0.33	0.04*
C25	0.8915 (3)	0.1707 (3)	0.4440 (2)	0.0315 (6)
H25	0.9381	0.1199	0.3925	0.038*
C26	0.8488 (3)	0.1303 (3)	0.5561 (2)	0.0236 (5)
H26	0.8662	0.0521	0.5806	0.028*
C31	0.7707 (3)	0.0017 (2)	0.79246 (19)	0.0190 (5)
C32	0.9330 (3)	0.0320 (3)	0.8290 (2)	0.0259 (5)
H32	1.0123	0.1291	0.844	0.031*
C33	0.9791 (4)	−0.0782 (3)	0.8437 (2)	0.0342 (7)
H33	1.0899	−0.057	0.868	0.041*
C34	0.8643 (4)	−0.2185 (3)	0.8229 (2)	0.0407 (8)
H34	0.8962	−0.2941	0.8335	0.049*
C35	0.7035 (4)	−0.2503 (3)	0.7869 (3)	0.0415 (8)
H35	0.6253	−0.3477	0.7727	0.05*
C36	0.6549 (3)	−0.1409 (3)	0.7710 (2)	0.0299 (6)
H36	0.5439	−0.1631	0.7459	0.036*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Pd	0.01295 (10)	0.01352 (9)	0.01400 (8)	0.00498 (7)	0.00497 (6)	0.00595 (6)
P	0.0144 (3)	0.0150 (3)	0.0153 (2)	0.0052 (2)	0.0039 (2)	0.0066 (2)
Cl1	0.0206 (3)	0.0150 (2)	0.0161 (2)	0.0039 (2)	0.0083 (2)	0.00478 (18)
Cl2	0.0191 (3)	0.0245 (3)	0.0194 (2)	0.0020 (2)	0.0056 (2)	0.0114 (2)
C1	0.0148 (12)	0.0186 (11)	0.0221 (10)	0.0036 (9)	0.0025 (9)	0.0076 (9)
C11	0.0127 (12)	0.0225 (12)	0.0247 (11)	0.0051 (9)	0.0037 (9)	0.0092 (9)
C12	0.0214 (13)	0.0311 (13)	0.0230 (11)	0.0116 (11)	0.0030 (10)	0.0072 (10)
C13	0.0299 (15)	0.0493 (17)	0.0295 (12)	0.0253 (13)	0.0062 (11)	0.0202 (12)
C14	0.0376 (17)	0.0516 (18)	0.0450 (15)	0.0345 (15)	0.0193 (13)	0.0260 (14)
C15	0.0360 (17)	0.0468 (17)	0.0334 (13)	0.0294 (14)	0.0170 (12)	0.0132 (12)
C16	0.0238 (14)	0.0366 (14)	0.0231 (11)	0.0158 (12)	0.0071 (10)	0.0123 (10)
C21	0.0146 (12)	0.0190 (11)	0.0146 (9)	0.0016 (9)	−0.0005 (8)	0.0068 (8)
C22	0.0225 (14)	0.0261 (13)	0.0252 (11)	0.0057 (11)	0.0014 (10)	0.0122 (10)
C23	0.0314 (16)	0.0305 (14)	0.0276 (12)	0.0036 (12)	−0.0001 (11)	0.0195 (11)
C24	0.0298 (15)	0.0371 (15)	0.0176 (11)	−0.0024 (12)	0.0022 (10)	0.0115 (10)
C25	0.0308 (15)	0.0373 (15)	0.0183 (11)	0.0047 (12)	0.0079 (10)	0.0073 (10)
C26	0.0214 (13)	0.0264 (12)	0.0168 (10)	0.0035 (10)	0.0025 (9)	0.0058 (9)
C31	0.0290 (14)	0.0216 (11)	0.0133 (9)	0.0153 (10)	0.0077 (9)	0.0079 (8)
C32	0.0331 (15)	0.0321 (14)	0.0163 (10)	0.0193 (12)	0.0018 (10)	0.0029 (9)
C33	0.0490 (19)	0.0528 (18)	0.0190 (11)	0.0405 (16)	0.0060 (11)	0.0073 (11)
C34	0.074 (2)	0.0459 (18)	0.0335 (14)	0.0490 (18)	0.0252 (15)	0.0207 (13)
C35	0.062 (2)	0.0267 (14)	0.0523 (17)	0.0265 (15)	0.0310 (16)	0.0193 (13)
C36	0.0338 (16)	0.0259 (13)	0.0383 (14)	0.0160 (12)	0.0178 (12)	0.0133 (11)

Geometric parameters (Å, º)

Pd—P	2.2218 (6)	C21—C26	1.389 (3)
Pd—Cl2	2.2729 (5)	C21—C22	1.397 (3)
Pd—Cl1	2.3155 (5)	C22—C23	1.388 (3)
Pd—Cl1^i	2.4123 (5)	C22—H22	0.95
P—C31	1.808 (2)	C23—C24	1.392 (4)
P—C21	1.816 (2)	C23—H23	0.95
P—C1	1.832 (2)	C24—C25	1.369 (4)
Cl1—Pd^i	2.4123 (5)	C24—H24	0.95
C1—C11	1.505 (3)	C25—C26	1.391 (3)
C1—H1A	0.99	C25—H25	0.95
C1—H1B	0.99	C26—H26	0.95
C11—C16	1.391 (3)	C31—C32	1.394 (3)
C11—C12	1.397 (3)	C31—C36	1.395 (3)
C12—C13	1.379 (4)	C32—C33	1.382 (3)
C12—H12	0.95	C32—H32	0.95
C13—C14	1.377 (4)	C33—C34	1.375 (4)
C13—H13	0.95	C33—H33	0.95
C14—C15	1.383 (4)	C34—C35	1.378 (5)
C14—H14	0.95	C34—H34	0.95
C15—C16	1.385 (3)	C35—C36	1.392 (4)
C15—H15	0.95	C35—H35	0.95
C16—H16	0.95	C36—H36	0.95
P—Pd—Cl2	87.18 (2)	C26—C21—C22	119.3 (2)
P—Pd—Cl1	95.735 (19)	C26—C21—P	121.30 (17)
Cl2—Pd—Cl1	176.50 (2)	C22—C21—P	119.36 (17)
P—Pd—Cl1^i	176.47 (2)	C23—C22—C21	119.9 (2)
Cl2—Pd—Cl1^i	91.437 (19)	C23—C22—H22	120
Cl1—Pd—Cl1^i	85.544 (18)	C21—C22—H22	120
C31—P—C21	106.16 (10)	C22—C23—C24	120.1 (2)
C31—P—C1	106.71 (11)	C22—C23—H23	119.9
C21—P—C1	106.02 (10)	C24—C23—H23	119.9
C31—P—Pd	109.12 (7)	C25—C24—C23	119.9 (2)
C21—P—Pd	113.50 (7)	C25—C24—H24	120
C1—P—Pd	114.78 (7)	C23—C24—H24	120
Pd—Cl1—Pd^i	94.457 (18)	C24—C25—C26	120.6 (2)
C11—C1—P	114.65 (15)	C24—C25—H25	119.7
C11—C1—H1A	108.6	C26—C25—H25	119.7
P—C1—H1A	108.6	C21—C26—C25	120.1 (2)
C11—C1—H1B	108.6	C21—C26—H26	120
P—C1—H1B	108.6	C25—C26—H26	120
H1A—C1—H1B	107.6	C32—C31—C36	119.5 (2)
C16—C11—C12	118.3 (2)	C32—C31—P	117.91 (18)
C16—C11—C1	120.8 (2)	C36—C31—P	122.58 (19)
C12—C11—C1	120.8 (2)	C33—C32—C31	120.4 (3)
C13—C12—C11	120.9 (2)	C33—C32—H32	119.8
C13—C12—H12	119.6	C31—C32—H32	119.8
C11—C12—H12	119.6	C34—C33—C32	119.9 (3)
C14—C13—C12	120.3 (2)	C34—C33—H33	120.1
C14—C13—H13	119.8	C32—C33—H33	120.1
C12—C13—H13	119.8	C33—C34—C35	120.5 (3)
C13—C14—C15	119.6 (2)	C33—C34—H34	119.8
C13—C14—H14	120.2	C35—C34—H34	119.8
C15—C14—H14	120.2	C34—C35—C36	120.5 (3)
C14—C15—C16	120.5 (2)	C34—C35—H35	119.8
C14—C15—H15	119.8	C36—C35—H35	119.8
C16—C15—H15	119.8	C35—C36—C31	119.3 (3)
C15—C16—C11	120.4 (2)	C35—C36—H36	120.4
C15—C16—H16	119.8	C31—C36—H36	120.4
C11—C16—H16	119.8
Cl2—Pd—P—C31	−67.18 (8)	C1—P—C21—C22	68.0 (2)
Cl1—Pd—P—C31	110.86 (8)	Pd—P—C21—C22	−58.9 (2)
Cl2—Pd—P—C21	174.66 (9)	C26—C21—C22—C23	1.8 (3)
Cl1—Pd—P—C21	−7.30 (9)	P—C21—C22—C23	−178.09 (19)
Cl2—Pd—P—C1	52.50 (8)	C21—C22—C23—C24	−0.9 (4)
Cl1—Pd—P—C1	−129.45 (8)	C22—C23—C24—C25	−0.5 (4)
P—Pd—Cl1—Pd^i	−176.69 (2)	C23—C24—C25—C26	1.0 (4)
Cl1^i—Pd—Cl1—Pd^i	0	C22—C21—C26—C25	−1.3 (3)
C31—P—C1—C11	176.03 (15)	P—C21—C26—C25	178.59 (19)
C21—P—C1—C11	−71.10 (17)	C24—C25—C26—C21	−0.1 (4)
Pd—P—C1—C11	55.02 (17)	C21—P—C31—C32	73.15 (18)
P—C1—C11—C16	−85.8 (2)	C1—P—C31—C32	−174.07 (16)
P—C1—C11—C12	94.9 (2)	Pd—P—C31—C32	−49.52 (18)
C16—C11—C12—C13	0.3 (4)	C21—P—C31—C36	−107.78 (19)
C1—C11—C12—C13	179.6 (2)	C1—P—C31—C36	5.0 (2)
C11—C12—C13—C14	−0.4 (4)	Pd—P—C31—C36	129.54 (17)
C12—C13—C14—C15	0.0 (5)	C36—C31—C32—C33	0.2 (3)
C13—C14—C15—C16	0.5 (5)	P—C31—C32—C33	179.28 (17)
C14—C15—C16—C11	−0.5 (4)	C31—C32—C33—C34	−0.4 (3)
C12—C11—C16—C15	0.2 (4)	C32—C33—C34—C35	0.4 (4)
C1—C11—C16—C15	−179.2 (2)	C33—C34—C35—C36	−0.1 (4)
C31—P—C21—C26	1.4 (2)	C34—C35—C36—C31	−0.2 (4)
C1—P—C21—C26	−111.85 (19)	C32—C31—C36—C35	0.1 (3)
Pd—P—C21—C26	121.25 (17)	P—C31—C36—C35	−178.92 (19)
C31—P—C21—C22	−178.75 (18)

Symmetry code: (i) −x+2, −y+1, −z+2.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
C1—H1B···Cl2^ii	0.99	2.68	3.636 (2)	163

Symmetry code: (ii) −x+1, −y, −z+2.