trans-Bis[bis­(2-methoxy­phen­yl)phenyl­phosphine-κP]dichloridopalladium(II)

Blerk, C. van; Holzapfel, C.W.

doi:10.1107/S1600536809040744

metal-organic compounds

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ISSN: 2056-9890

Volume 65| Part 11| November 2009| Page m1341

https://doi.org/10.1107/S1600536809040744

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trans-Bis[bis(2-methoxyphenyl)phenylphosphine-κP]dichloridopalladium(II)

Charmaine van Blerk ^a ^* and Cedric W. Holzapfel ^a

^aUniversity of Johannesburg, Department of Chemistry, PO Box 524, Auckland Park, Johannesburg 2006, South Africa
^*Correspondence e-mail: cvanblerk@uj.ac.za

(Received 23 September 2009; accepted 6 October 2009; online 10 October 2009)

The structure of the title compound, [PdCl₂(C₂₀H₁₉O₂P)₂], shows a square-planar geometry for the Pd^II ion within a Cl₂Pd[PPh(PhOMe)₂]₂ ligand set. The Pd^II atom sits on an inversion centre and therefore the asymmetric unit contains the Pd^II atom, one Cl atom and one bis(2-methoxyphenyl)phenylphosphine ligand. The trans arrangement of ligands is also imposed by symmetry.

Related literature

For related structures of similar palladium complexes and their use in methoxycarbonylation reactions, see: Robertson & Cole-Hamilton (2002 ); Van Leeuwen et al. (2003 ); Williams et al. (2008 ).

Experimental

Crystal data

[PdCl₂(C₂₀H₁₉O₂P)₂]
M_r = 821.94
Monoclinic, P 2₁ /n
a = 9.1617 (2) Å
b = 12.7203 (3) Å
c = 16.4939 (4) Å
β = 94.114 (1)°
V = 1917.24 (8) Å³
Z = 2
Mo Kα radiation
μ = 0.75 mm⁻¹
T = 296 K
0.22 × 0.18 × 0.12 mm

Data collection

Bruker SMART CCD diffractometer
Absorption correction: multi-scan (APEX AXScale; Bruker, 2008 ) T_min = 0.853, T_max = 0.916
23435 measured reflections
4750 independent reflections
3339 reflections with I > 2σ(I)
R_int = 0.064

Refinement

R[F² > 2σ(F²)] = 0.036
wR(F²) = 0.089
S = 1.02
4750 reflections
225 parameters
H-atom parameters constrained
Δρ_max = 0.63 e Å⁻³
Δρ_min = −0.38 e Å⁻³

Table 1
Selected geometric parameters (Å, °)

P1—Pd1	2.3458 (6)
Cl1—Pd1	2.3048 (7)

Cl1—Pd1—P1	93.24 (2)
Cl1ⁱ—Pd1—P1	86.76 (2)
Symmetry code: (i) -x, -y, -z.

Data collection: SMART-NT (Bruker, 1999 ); cell refinement: SAINT (Bruker, 2008); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: X-SEED (Barbour, 2001 ) and Mercury (Macrae et al., 2006 ); software used to prepare material for publication: publCIF (Westrip, 2009 ).

Supporting information

Crystal structure: contains datablocks I, global. DOI: https://doi.org/10.1107/S1600536809040744/bh2252sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536809040744/bh2252Isup2.hkl

checkCIF report

Comment top

The palladium-catalysed methoxycarbonylation (Robertson & Cole-Hamilton, 2002) of 1-alkenes is an active area of research. The preferred (pre)-catalysts of general structure (Ar₃P)₂PdX₂ (X = Cl, DMS, OTf, etc.) are either preformed or generated in situ. The X-ray structures (Van Leeuwen et al., 2003; Williams et al., 2008) of several of this class of palladium(II) complexes have been determined. Only some of these have found application in the catalysis of the methoxycarbonylation reaction, but their use results mainly in the formation of linear esters (Robertson & Cole-Hamilton, 2002). However, we have identified some palladium(II) complexes which catalyse the regioselective formation of branched esters. We report here the structure of one of these.

The structure of the title compound, [PdCl₂(C₄₀H₃₈P₂O₄)], shows a square planar geometry for the Pd^II ion within the Cl₂(PPh(PhOMe)₂) ligand set. The palladium atom sits on a centre of inversion and therefore the asymmetric unit contains the palladium atom, one chlorine atom and one bis-(2-methoxyphenyl)phenylphosphine ligand. Figure 1 shows the molecular structure of the title compound.

Related literature top

For related structures of similar palladium complexes and literature about their use in methoxycarbonylation reactions, see: Robertson et al. (2002); Van Leeuwen et al. (2003); Williams et al. (2008).

Experimental top

Bis-(2-methoxyphenyl)phenylphosphine (1.288 g, 4 mmol) was added to a solution of palladium(II) chloride (354 mg, 2 mmol) and anhydrous lithium chloride (168 mg, 4 mmol) in methanol (15 ml). The mixture was refluxed in an atmosphere of nitrogen until all the phosphine reagent had reacted and a light yellow product had formed (ca. 45 min). The reaction mixture was cooled and the product collected by filtration, washed with fresh methanol and dried under vacuum. The crude product (1.37 g) was dissolved in dichloromethane and crystallization of the title compound was carried out by diethyl ether vapour diffusion into the dichloromethane. The crystals of the title compound were pale yellow blocks (m.p. > 503 K, decomp.) and a suitable crystal was selected for the single-crystal X-ray diffraction analysis.

Structure description top

Computing details top

Data collection: SMART-NT (Bruker, 1999); cell refinement: SAINT (Bruker, 2008); data reduction: SAINT (Bruker, 2008); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: X-SEED (Barbour, 2001) and Mercury (Macrae et al., 2006); software used to prepare material for publication: publCIF (Westrip, 2009).

Figures top

Fig. 1. Molecular structure of (I) with displacement ellipsoids drawn at the 50% probability level. Atoms labelled with (i) are at symmetry position (-x, -y, -z).

trans-Bis[bis(2-methoxyphenyl)phenylphosphine- κP]dichloridopalladium(II) top

Crystal data top

[PdCl₂(C₂₀H₁₉O₂P)₂]	F(000) = 840
M_r = 821.94	D_x = 1.424 Mg m⁻³
Monoclinic, P2₁/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 5078 reflections
a = 9.1617 (2) Å	θ = 2.5–24.7°
b = 12.7203 (3) Å	µ = 0.75 mm⁻¹
c = 16.4939 (4) Å	T = 296 K
β = 94.114 (1)°	Block, yellow
V = 1917.24 (8) Å³	0.22 × 0.18 × 0.12 mm
Z = 2

Data collection top

Bruker SMART CCD diffractometer	4750 independent reflections
Radiation source: fine-focus sealed tube	3339 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.064
φ and ω scans	θ_max = 28.3°, θ_min = 2.0°
Absorption correction: multi-scan (APEX AXScale; Bruker, 2008)	h = −12→12
T_min = 0.853, T_max = 0.916	k = −16→16
23435 measured reflections	l = −21→21

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.036	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.089	H-atom parameters constrained
S = 1.02	w = 1/[σ²(F_o²) + (0.0441P)²] where P = (F_o² + 2F_c²)/3
4750 reflections	(Δ/σ)_max = 0.001
225 parameters	Δρ_max = 0.63 e Å⁻³
0 restraints	Δρ_min = −0.38 e Å⁻³
0 constraints

Crystal data top

[PdCl₂(C₂₀H₁₉O₂P)₂]	V = 1917.24 (8) Å³
M_r = 821.94	Z = 2
Monoclinic, P2₁/n	Mo Kα radiation
a = 9.1617 (2) Å	µ = 0.75 mm⁻¹
b = 12.7203 (3) Å	T = 296 K
c = 16.4939 (4) Å	0.22 × 0.18 × 0.12 mm
β = 94.114 (1)°

Data collection top

Bruker SMART CCD diffractometer	4750 independent reflections
Absorption correction: multi-scan (APEX AXScale; Bruker, 2008)	3339 reflections with I > 2σ(I)
T_min = 0.853, T_max = 0.916	R_int = 0.064
23435 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.036	0 restraints
wR(F²) = 0.089	H-atom parameters constrained
S = 1.02	Δρ_max = 0.63 e Å⁻³
4750 reflections	Δρ_min = −0.38 e Å⁻³
225 parameters

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
C11	0.0228 (3)	0.1927 (2)	−0.15944 (16)	0.0323 (6)
C12	0.0094 (3)	0.1268 (2)	−0.22659 (16)	0.0401 (7)
H12	−0.0432	0.0646	−0.2240	0.048*
C13	0.0734 (3)	0.1526 (3)	−0.29741 (18)	0.0505 (8)
H13	0.0647	0.1072	−0.3417	0.061*
C14	0.1500 (3)	0.2454 (3)	−0.3024 (2)	0.0528 (8)
H14	0.1927	0.2628	−0.3501	0.063*
C15	0.1626 (3)	0.3112 (3)	−0.2373 (2)	0.0505 (8)
H15	0.2128	0.3744	−0.2409	0.061*
C16	0.1016 (3)	0.2850 (2)	−0.16577 (18)	0.0426 (7)
H16	0.1136	0.3299	−0.1213	0.051*
C21	−0.2607 (3)	0.1459 (2)	−0.10562 (17)	0.0363 (6)
C22	−0.3400 (3)	0.0578 (2)	−0.08536 (18)	0.0434 (7)
H22	−0.2954	0.0076	−0.0508	0.052*
C23	−0.4839 (3)	0.0426 (3)	−0.1152 (2)	0.0569 (9)
H23	−0.5358	−0.0163	−0.1002	0.068*
C24	−0.5481 (4)	0.1156 (3)	−0.1671 (2)	0.0670 (10)
H24	−0.6444	0.1055	−0.1876	0.080*
C25	−0.4735 (4)	0.2040 (3)	−0.1898 (2)	0.0631 (10)
H25	−0.5191	0.2525	−0.2254	0.076*
C26	−0.3300 (3)	0.2201 (3)	−0.15904 (19)	0.0472 (8)
C27	−0.3017 (6)	0.3742 (4)	−0.2385 (3)	0.1117 (19)
H27A	−0.3180	0.3354	−0.2882	0.167*
H27B	−0.2311	0.4286	−0.2454	0.167*
H27C	−0.3921	0.4052	−0.2245	0.167*
C31	−0.0464 (3)	0.2692 (2)	−0.00191 (17)	0.0403 (7)
C32	−0.1582 (4)	0.3370 (2)	0.0142 (2)	0.0518 (8)
H32	−0.2510	0.3276	−0.0114	0.062*
C33	−0.1318 (5)	0.4201 (3)	0.0691 (2)	0.0707 (11)
H33	−0.2066	0.4664	0.0796	0.085*
C34	0.0048 (6)	0.4326 (3)	0.1071 (2)	0.0805 (13)
H34	0.0212	0.4869	0.1444	0.097*
C35	0.1175 (5)	0.3675 (3)	0.0916 (2)	0.0737 (12)
H35	0.2099	0.3779	0.1175	0.088*
C36	0.0933 (4)	0.2854 (2)	0.03693 (19)	0.0505 (8)
C37	0.3458 (4)	0.2356 (4)	0.0401 (3)	0.1033 (17)
H37A	0.3705	0.3048	0.0224	0.155*
H37B	0.4060	0.1847	0.0154	0.155*
H37C	0.3618	0.2312	0.0981	0.155*
O1	−0.2494 (2)	0.30626 (18)	−0.17624 (15)	0.0639 (7)
O2	0.1969 (2)	0.21487 (18)	0.01702 (15)	0.0628 (7)
P1	−0.06893 (7)	0.15556 (5)	−0.06890 (4)	0.03007 (16)
Cl1	0.12498 (8)	−0.06305 (6)	−0.10623 (4)	0.04534 (19)
Pd1	0.0000	0.0000	0.0000	0.02642 (9)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
C11	0.0277 (13)	0.0311 (14)	0.0378 (14)	0.0047 (11)	0.0009 (11)	0.0057 (11)
C12	0.0412 (16)	0.0401 (16)	0.0384 (16)	−0.0050 (13)	−0.0002 (13)	0.0031 (13)
C13	0.056 (2)	0.059 (2)	0.0359 (16)	0.0035 (16)	0.0020 (15)	0.0028 (15)
C14	0.0448 (19)	0.069 (2)	0.0461 (18)	0.0056 (17)	0.0128 (15)	0.0177 (17)
C15	0.0432 (18)	0.0463 (19)	0.063 (2)	−0.0063 (15)	0.0130 (16)	0.0168 (16)
C16	0.0434 (17)	0.0356 (16)	0.0492 (17)	−0.0033 (13)	0.0056 (14)	0.0043 (13)
C21	0.0268 (14)	0.0406 (16)	0.0415 (15)	0.0064 (12)	0.0030 (12)	0.0073 (12)
C22	0.0336 (16)	0.0468 (18)	0.0492 (17)	0.0012 (13)	0.0001 (13)	0.0083 (14)
C23	0.0321 (17)	0.062 (2)	0.076 (2)	−0.0062 (15)	−0.0007 (16)	0.0080 (19)
C24	0.0341 (18)	0.091 (3)	0.074 (2)	0.0017 (19)	−0.0093 (17)	0.004 (2)
C25	0.0407 (19)	0.080 (3)	0.067 (2)	0.0151 (18)	−0.0095 (17)	0.022 (2)
C26	0.0381 (17)	0.0505 (19)	0.0529 (18)	0.0081 (14)	0.0027 (14)	0.0131 (15)
C27	0.128 (4)	0.086 (3)	0.114 (4)	−0.004 (3)	−0.035 (3)	0.063 (3)
C31	0.0531 (18)	0.0263 (14)	0.0425 (16)	0.0021 (12)	0.0100 (15)	0.0037 (12)
C32	0.062 (2)	0.0367 (17)	0.060 (2)	0.0031 (15)	0.0236 (17)	0.0025 (15)
C33	0.099 (3)	0.039 (2)	0.079 (3)	0.009 (2)	0.046 (2)	−0.0043 (19)
C34	0.124 (4)	0.054 (3)	0.064 (3)	−0.007 (3)	0.016 (3)	−0.018 (2)
C35	0.102 (3)	0.049 (2)	0.068 (2)	−0.010 (2)	−0.014 (2)	−0.0157 (19)
C36	0.067 (2)	0.0352 (16)	0.0484 (18)	−0.0089 (15)	−0.0040 (16)	−0.0039 (14)
C37	0.059 (3)	0.094 (3)	0.151 (4)	−0.009 (2)	−0.033 (3)	−0.026 (3)
O1	0.0490 (13)	0.0574 (14)	0.0837 (17)	0.0081 (11)	−0.0064 (12)	0.0361 (13)
O2	0.0521 (14)	0.0522 (14)	0.0802 (16)	0.0009 (11)	−0.0218 (12)	−0.0140 (12)
P1	0.0294 (3)	0.0265 (3)	0.0342 (4)	0.0024 (3)	0.0015 (3)	0.0036 (3)
Cl1	0.0549 (5)	0.0435 (4)	0.0395 (4)	0.0124 (3)	0.0169 (3)	0.0021 (3)
Pd1	0.02524 (14)	0.02514 (14)	0.02887 (14)	0.00229 (12)	0.00193 (10)	0.00150 (12)

Geometric parameters (Å, º) top

C11—C16	1.386 (4)	C27—O1	1.400 (4)
C11—C12	1.387 (4)	C27—H27A	0.9600
C11—P1	1.827 (3)	C27—H27B	0.9600
C12—C13	1.383 (4)	C27—H27C	0.9600
C12—H12	0.9300	C31—C32	1.379 (4)
C13—C14	1.379 (4)	C31—C36	1.405 (4)
C13—H13	0.9300	C31—P1	1.822 (3)
C14—C15	1.361 (5)	C32—C33	1.402 (5)
C14—H14	0.9300	C32—H32	0.9300
C15—C16	1.382 (4)	C33—C34	1.368 (6)
C15—H15	0.9300	C33—H33	0.9300
C16—H16	0.9300	C34—C35	1.362 (6)
C21—C22	1.390 (4)	C34—H34	0.9300
C21—C26	1.410 (4)	C35—C36	1.388 (4)
C21—P1	1.821 (3)	C35—H35	0.9300
C22—C23	1.387 (4)	C36—O2	1.363 (4)
C22—H22	0.9300	C37—O2	1.414 (4)
C23—C24	1.367 (5)	C37—H37A	0.9600
C23—H23	0.9300	C37—H37B	0.9600
C24—C25	1.381 (5)	C37—H37C	0.9600
C24—H24	0.9300	P1—Pd1	2.3458 (6)
C25—C26	1.390 (4)	Cl1—Pd1	2.3048 (7)
C25—H25	0.9300	Pd1—Cl1ⁱ	2.3048 (7)
C26—O1	1.363 (4)	Pd1—P1ⁱ	2.3458 (6)

C16—C11—C12	117.9 (3)	H27A—C27—H27C	109.5
C16—C11—P1	123.6 (2)	H27B—C27—H27C	109.5
C12—C11—P1	118.5 (2)	C32—C31—C36	119.0 (3)
C13—C12—C11	120.9 (3)	C32—C31—P1	124.0 (3)
C13—C12—H12	119.6	C36—C31—P1	116.9 (2)
C11—C12—H12	119.6	C31—C32—C33	120.0 (3)
C14—C13—C12	120.1 (3)	C31—C32—H32	120.0
C14—C13—H13	119.9	C33—C32—H32	120.0
C12—C13—H13	119.9	C34—C33—C32	119.6 (4)
C15—C14—C13	119.6 (3)	C34—C33—H33	120.2
C15—C14—H14	120.2	C32—C33—H33	120.2
C13—C14—H14	120.2	C35—C34—C33	121.6 (4)
C14—C15—C16	120.6 (3)	C35—C34—H34	119.2
C14—C15—H15	119.7	C33—C34—H34	119.2
C16—C15—H15	119.7	C34—C35—C36	119.5 (4)
C15—C16—C11	120.9 (3)	C34—C35—H35	120.3
C15—C16—H16	119.5	C36—C35—H35	120.3
C11—C16—H16	119.5	O2—C36—C35	124.8 (3)
C22—C21—C26	118.1 (3)	O2—C36—C31	114.9 (3)
C22—C21—P1	118.9 (2)	C35—C36—C31	120.3 (3)
C26—C21—P1	122.9 (2)	O2—C37—H37A	109.5
C23—C22—C21	121.8 (3)	O2—C37—H37B	109.5
C23—C22—H22	119.1	H37A—C37—H37B	109.5
C21—C22—H22	119.1	O2—C37—H37C	109.5
C24—C23—C22	118.9 (3)	H37A—C37—H37C	109.5
C24—C23—H23	120.6	H37B—C37—H37C	109.5
C22—C23—H23	120.6	C26—O1—C27	119.1 (3)
C23—C24—C25	121.6 (3)	C36—O2—C37	119.2 (3)
C23—C24—H24	119.2	C21—P1—C31	108.64 (14)
C25—C24—H24	119.2	C21—P1—C11	103.58 (12)
C24—C25—C26	119.7 (3)	C31—P1—C11	104.58 (13)
C24—C25—H25	120.2	C21—P1—Pd1	108.91 (9)
C26—C25—H25	120.2	C31—P1—Pd1	111.13 (9)
O1—C26—C25	123.7 (3)	C11—P1—Pd1	119.37 (8)
O1—C26—C21	116.2 (3)	Cl1—Pd1—Cl1ⁱ	180.00 (4)
C25—C26—C21	120.0 (3)	Cl1—Pd1—P1ⁱ	86.76 (2)
O1—C27—H27A	109.5	Cl1ⁱ—Pd1—P1ⁱ	93.24 (2)
O1—C27—H27B	109.5	Cl1—Pd1—P1	93.24 (2)
H27A—C27—H27B	109.5	Cl1ⁱ—Pd1—P1	86.76 (2)
O1—C27—H27C	109.5	P1ⁱ—Pd1—P1	180.00 (5)

C16—C11—C12—C13	0.2 (4)	P1—C31—C36—C35	−177.1 (3)
P1—C11—C12—C13	178.3 (2)	C25—C26—O1—C27	−11.5 (5)
C11—C12—C13—C14	−0.9 (4)	C21—C26—O1—C27	169.7 (3)
C12—C13—C14—C15	0.2 (5)	C35—C36—O2—C37	−12.9 (5)
C13—C14—C15—C16	1.2 (5)	C31—C36—O2—C37	167.9 (3)
C14—C15—C16—C11	−1.9 (5)	C22—C21—P1—C31	−117.1 (2)
C12—C11—C16—C15	1.1 (4)	C26—C21—P1—C31	67.9 (3)
P1—C11—C16—C15	−176.8 (2)	C22—C21—P1—C11	132.1 (2)
C26—C21—C22—C23	−1.0 (5)	C26—C21—P1—C11	−42.9 (3)
P1—C21—C22—C23	−176.2 (3)	C22—C21—P1—Pd1	4.1 (3)
C21—C22—C23—C24	1.2 (5)	C26—C21—P1—Pd1	−170.9 (2)
C22—C23—C24—C25	−0.5 (6)	C32—C31—P1—C21	−2.3 (3)
C23—C24—C25—C26	−0.4 (6)	C36—C31—P1—C21	175.8 (2)
C24—C25—C26—O1	−178.1 (3)	C32—C31—P1—C11	107.8 (3)
C24—C25—C26—C21	0.6 (5)	C36—C31—P1—C11	−74.1 (2)
C22—C21—C26—O1	178.9 (3)	C32—C31—P1—Pd1	−122.1 (2)
P1—C21—C26—O1	−6.1 (4)	C36—C31—P1—Pd1	56.0 (2)
C22—C21—C26—C25	0.0 (5)	C16—C11—P1—C21	119.4 (2)
P1—C21—C26—C25	175.0 (3)	C12—C11—P1—C21	−58.5 (2)
C36—C31—C32—C33	−0.5 (5)	C16—C11—P1—C31	5.7 (3)
P1—C31—C32—C33	177.5 (2)	C12—C11—P1—C31	−172.3 (2)
C31—C32—C33—C34	−0.7 (5)	C16—C11—P1—Pd1	−119.4 (2)
C32—C33—C34—C35	1.4 (6)	C12—C11—P1—Pd1	62.7 (2)
C33—C34—C35—C36	−0.9 (6)	C21—P1—Pd1—Cl1	103.82 (10)
C34—C35—C36—O2	−179.6 (3)	C31—P1—Pd1—Cl1	−136.53 (11)
C34—C35—C36—C31	−0.3 (6)	C11—P1—Pd1—Cl1	−14.71 (10)
C32—C31—C36—O2	−179.7 (3)	C21—P1—Pd1—Cl1ⁱ	−76.18 (10)
P1—C31—C36—O2	2.2 (4)	C31—P1—Pd1—Cl1ⁱ	43.47 (11)
C32—C31—C36—C35	1.0 (5)	C11—P1—Pd1—Cl1ⁱ	165.29 (10)

Symmetry code: (i) −x, −y, −z.

Experimental details

Crystal data
Chemical formula	[PdCl₂(C₂₀H₁₉O₂P)₂]
M_r	821.94
Crystal system, space group	Monoclinic, P2₁/n
Temperature (K)	296
a, b, c (Å)	9.1617 (2), 12.7203 (3), 16.4939 (4)
β (°)	94.114 (1)
V (Å³)	1917.24 (8)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	0.75
Crystal size (mm)	0.22 × 0.18 × 0.12

Data collection
Diffractometer	Bruker SMART CCD
Absorption correction	Multi-scan (APEX AXScale; Bruker, 2008)
T_min, T_max	0.853, 0.916
No. of measured, independent and observed [I > 2σ(I)] reflections	23435, 4750, 3339
R_int	0.064
(sin θ/λ)_max (Å⁻¹)	0.667

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.036, 0.089, 1.02
No. of reflections	4750
No. of parameters	225
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.63, −0.38

Computer programs: SMART-NT (Bruker, 1999), SAINT (Bruker, 2008), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), X-SEED (Barbour, 2001) and Mercury (Macrae et al., 2006), publCIF (Westrip, 2009).

Selected geometric parameters (Å, º) top

P1—Pd1	2.3458 (6)	Cl1—Pd1	2.3048 (7)

Cl1—Pd1—P1	93.24 (2)	Cl1ⁱ—Pd1—P1	86.76 (2)

Symmetry code: (i) −x, −y, −z.

Acknowledgements

The authors acknowledge the University of the Witwatersrand for their facilities and the use of the diffractometer in the Jan Boeyens Structural Chemistry Laboratory.

References

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