trans-Dichloridobis[tris-(2-methoxy-phen-yl)phosphine]palladium(II).

The structure of the title compound, [PdCl(2)(C(21)H(21)O(3)P)(2)], shows a nearly square-planar geometry for the Pd(II) atom within the Cl(2)Pd[P(PhOMe)(3)](2) ligand set. The Pd(II) atom sits on a centre of inversion and therefore the asymmetric unit contains one half-mol-ecule, i.e. half of one Pd(II) atom, one Cl atom and one tris-(2-methoxy-phen-yl)phosphine ligand.

Related literature

For related structures and literature on similar palladium complexes, see: Robertson & Cole-Hamilton (2002 ▶); Van Leeuwen et al. (2003 ▶); Williams et al. (2008 ▶).

Experimental

Crystal data

[PdCl2(C21H21O3P)2]

M = 882.00

Triclinic,

a = 9.1415 (2) Å

b = 10.8985 (3) Å

c = 12.0287 (3) Å

α = 103.691 (2)°

β = 109.275 (3)°

γ = 108.438 (2)°

V = 992.26 (5) Å3

Z = 1

Mo Kα radiation

μ = 0.73 mm−1

T = 294 K

0.30 × 0.16 × 0.10 mm

Data collection

Bruker SMART CCD diffractometer

Absorption correction: multi-scan (APEX2 AXScale; Bruker, 2008 ▶) T min = 0.811, T max = 0.931

11296 measured reflections

4894 independent reflections

3672 reflections with I > 2σ(I)

R int = 0.039

Refinement

R[F 2 > 2σ(F 2)] = 0.037

wR(F 2) = 0.094

S = 0.97

4894 reflections

244 parameters

H-atom parameters constrained

Δρmax = 0.35 e Å−3

Δρmin = −0.43 e Å−3

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 ▶).

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536809040719/bq2163sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809040719/bq2163Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[PdCl2(C42H42O6P2)]	Z = 1
Mr = 882.00	F(000) = 452
Triclinic, P1	Dx = 1.476 Mg m−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 9.1415 (2) Å	Cell parameters from 3513 reflections
b = 10.8985 (3) Å	θ = 2.3–25.9°
c = 12.0287 (3) Å	µ = 0.73 mm−1
α = 103.691 (2)°	T = 294 K
β = 109.275 (3)°	Plate, yellow
γ = 108.438 (2)°	0.30 × 0.16 × 0.10 mm
V = 992.26 (5) Å3

Bruker SMART CCD diffractometer	4894 independent reflections
Radiation source: fine-focus sealed tube	3672 reflections with I > 2σ(I)
graphite	Rint = 0.039
φ and ω scans	θmax = 28.3°, θmin = 1.9°
Absorption correction: multi-scan (APEX2 AXScale; Bruker, 2008)	h = −12→11
Tmin = 0.811, Tmax = 0.931	k = −14→13
11296 measured reflections	l = −15→16

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)] = 0.037	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.094	H-atom parameters constrained
S = 0.97	w = 1/[σ2(Fo2) + (0.051P)2] where P = (Fo2 + 2Fc2)/3
4894 reflections	(Δ/σ)max < 0.001
244 parameters	Δρmax = 0.35 e Å−3
0 restraints	Δρmin = −0.43 e Å−3

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.

	x	y	z	Uiso*/Ueq
Pd1	0.0000	0.0000	0.5000	0.02713 (10)
Cl1	0.15837 (9)	−0.10437 (8)	0.59870 (7)	0.04185 (18)
P1	−0.08161 (8)	−0.18084 (7)	0.30980 (7)	0.02821 (16)
O1	−0.0797 (3)	−0.3741 (2)	0.0829 (2)	0.0456 (5)
O2	−0.0304 (3)	0.0196 (2)	0.1933 (2)	0.0514 (6)
O3	−0.3775 (3)	−0.2921 (2)	0.3590 (2)	0.0499 (6)
C11	0.0985 (3)	−0.1701 (3)	0.2718 (3)	0.0330 (6)
C12	0.2580 (4)	−0.0560 (3)	0.3521 (3)	0.0389 (7)
H12	0.2748	0.0032	0.4295	0.047*
C13	0.3914 (4)	−0.0308 (3)	0.3165 (3)	0.0460 (8)
H13	0.4969	0.0453	0.3702	0.055*
C14	0.3682 (4)	−0.1176 (4)	0.2026 (3)	0.0477 (8)
H14	0.4581	−0.1002	0.1796	0.057*
C15	0.2113 (4)	−0.2308 (3)	0.1219 (3)	0.0449 (8)
H15	0.1958	−0.2890	0.0446	0.054*
C16	0.0765 (4)	−0.2577 (3)	0.1565 (3)	0.0367 (7)
C17	−0.1525 (5)	−0.4108 (4)	−0.0510 (3)	0.0573 (9)
H17A	−0.1702	−0.3344	−0.0698	0.086*
H17B	−0.2605	−0.4919	−0.0906	0.086*
H17C	−0.0761	−0.4309	−0.0832	0.086*
C21	−0.2402 (3)	−0.1916 (3)	0.1633 (3)	0.0321 (6)
C22	−0.4005 (4)	−0.3027 (3)	0.0900 (3)	0.0374 (7)
H22	−0.4308	−0.3776	0.1153	0.045*
C23	−0.5172 (4)	−0.3056 (4)	−0.0200 (3)	0.0471 (8)
H23	−0.6235	−0.3822	−0.0693	0.056*
C24	−0.4724 (5)	−0.1919 (4)	−0.0553 (3)	0.0572 (9)
H24	−0.5514	−0.1908	−0.1270	0.069*
C25	−0.3139 (5)	−0.0814 (4)	0.0140 (3)	0.0540 (9)
H25	−0.2853	−0.0065	−0.0115	0.065*
C26	−0.1954 (4)	−0.0806 (3)	0.1223 (3)	0.0388 (7)
C27	0.0186 (6)	0.1455 (4)	0.1722 (5)	0.0838 (14)
H27A	−0.0617	0.1842	0.1745	0.126*
H27B	0.0196	0.1268	0.0904	0.126*
H27C	0.1313	0.2110	0.2374	0.126*
C31	−0.1653 (3)	−0.3488 (3)	0.3249 (3)	0.0311 (6)
C32	−0.0820 (4)	−0.4361 (3)	0.3219 (3)	0.0397 (7)
H32	0.0107	−0.4142	0.3021	0.048*
C33	−0.1362 (5)	−0.5554 (3)	0.3482 (3)	0.0507 (9)
H33	−0.0805	−0.6135	0.3454	0.061*
C34	−0.2717 (5)	−0.5873 (3)	0.3784 (3)	0.0574 (9)
H34	−0.3069	−0.6668	0.3969	0.069*
C35	−0.3573 (5)	−0.5032 (3)	0.3817 (3)	0.0522 (9)
H35	−0.4505	−0.5267	0.4009	0.063*
C36	−0.3034 (4)	−0.3833 (3)	0.3561 (3)	0.0403 (7)
C37	−0.5075 (5)	−0.3122 (4)	0.4017 (4)	0.0604 (10)
H37A	−0.4612	−0.3054	0.4882	0.091*
H37B	−0.6007	−0.4031	0.3488	0.091*
H37C	−0.5486	−0.2418	0.3968	0.091*

	U11	U22	U33	U12	U13	U23
Pd1	0.02580 (16)	0.02587 (16)	0.02807 (18)	0.01139 (13)	0.01105 (13)	0.00837 (13)
Cl1	0.0434 (4)	0.0428 (4)	0.0399 (4)	0.0256 (4)	0.0126 (4)	0.0151 (4)
P1	0.0270 (4)	0.0260 (4)	0.0292 (4)	0.0104 (3)	0.0123 (3)	0.0080 (3)
O1	0.0460 (13)	0.0431 (12)	0.0391 (13)	0.0129 (11)	0.0218 (11)	0.0058 (11)
O2	0.0507 (14)	0.0417 (12)	0.0597 (16)	0.0118 (11)	0.0254 (12)	0.0255 (12)
O3	0.0570 (14)	0.0500 (13)	0.0703 (17)	0.0293 (12)	0.0437 (13)	0.0363 (13)
C11	0.0313 (14)	0.0336 (15)	0.0346 (16)	0.0148 (12)	0.0158 (13)	0.0107 (13)
C12	0.0347 (16)	0.0396 (16)	0.0374 (17)	0.0140 (14)	0.0153 (14)	0.0104 (14)
C13	0.0309 (16)	0.0493 (19)	0.056 (2)	0.0150 (15)	0.0182 (16)	0.0205 (17)
C14	0.0445 (18)	0.060 (2)	0.060 (2)	0.0299 (17)	0.0343 (18)	0.0301 (19)
C15	0.0510 (19)	0.0494 (19)	0.045 (2)	0.0264 (17)	0.0296 (17)	0.0175 (17)
C16	0.0381 (16)	0.0345 (15)	0.0401 (18)	0.0169 (13)	0.0199 (14)	0.0128 (14)
C17	0.062 (2)	0.055 (2)	0.040 (2)	0.0152 (19)	0.0176 (18)	0.0142 (18)
C21	0.0349 (15)	0.0357 (15)	0.0280 (15)	0.0174 (13)	0.0150 (13)	0.0111 (13)
C22	0.0354 (16)	0.0389 (16)	0.0338 (16)	0.0168 (14)	0.0134 (14)	0.0089 (14)
C23	0.0415 (18)	0.053 (2)	0.0350 (18)	0.0240 (16)	0.0079 (15)	0.0063 (16)
C24	0.061 (2)	0.073 (3)	0.0312 (18)	0.039 (2)	0.0069 (17)	0.0153 (18)
C25	0.076 (3)	0.054 (2)	0.044 (2)	0.035 (2)	0.026 (2)	0.0282 (18)
C26	0.0434 (17)	0.0390 (16)	0.0357 (17)	0.0185 (14)	0.0191 (15)	0.0135 (14)
C27	0.092 (3)	0.052 (2)	0.102 (4)	0.013 (2)	0.041 (3)	0.047 (3)
C31	0.0337 (14)	0.0236 (13)	0.0253 (14)	0.0084 (12)	0.0070 (12)	0.0056 (12)
C32	0.0413 (17)	0.0349 (16)	0.0309 (16)	0.0145 (14)	0.0073 (14)	0.0079 (13)
C33	0.067 (2)	0.0354 (17)	0.042 (2)	0.0262 (17)	0.0112 (18)	0.0138 (16)
C34	0.082 (3)	0.0341 (18)	0.047 (2)	0.0177 (18)	0.021 (2)	0.0208 (17)
C35	0.064 (2)	0.0405 (18)	0.056 (2)	0.0166 (17)	0.0304 (19)	0.0270 (18)
C36	0.0459 (17)	0.0335 (15)	0.0386 (18)	0.0135 (14)	0.0178 (15)	0.0153 (14)
C37	0.064 (2)	0.067 (2)	0.073 (3)	0.030 (2)	0.048 (2)	0.036 (2)

Pd1—Cl1i	2.3120 (7)	C21—C22	1.382 (4)
Pd1—Cl1	2.3120 (7)	C21—C26	1.406 (4)
Pd1—P1i	2.3417 (7)	C22—C23	1.385 (4)
Pd1—P1	2.3417 (7)	C22—H22	0.9300
P1—C11	1.826 (3)	C23—C24	1.388 (5)
P1—C31	1.825 (3)	C23—H23	0.9300
P1—C21	1.824 (3)	C24—C25	1.367 (5)
O1—C16	1.386 (3)	C24—H24	0.9300
O1—C17	1.420 (4)	C25—C26	1.389 (4)
O2—C26	1.365 (4)	C25—H25	0.9300
O2—C27	1.415 (4)	C27—H27A	0.9600
O3—C36	1.370 (4)	C27—H27B	0.9600
O3—C37	1.419 (4)	C27—H27C	0.9600
C11—C16	1.394 (4)	C31—C32	1.395 (4)
C11—C12	1.400 (4)	C31—C36	1.398 (4)
C12—C13	1.391 (4)	C32—C33	1.388 (4)
C12—H12	0.9300	C32—H32	0.9300
C13—C14	1.373 (5)	C33—C34	1.368 (5)
C13—H13	0.9300	C33—H33	0.9300
C14—C15	1.384 (5)	C34—C35	1.383 (5)
C14—H14	0.9300	C34—H34	0.9300
C15—C16	1.395 (4)	C35—C36	1.388 (4)
C15—H15	0.9300	C35—H35	0.9300
C17—H17A	0.9600	C37—H37A	0.9600
C17—H17B	0.9600	C37—H37B	0.9600
C17—H17C	0.9600	C37—H37C	0.9600
Cl1i—Pd1—Cl1	180.00 (4)	C21—C22—H22	119.1
Cl1i—Pd1—P1i	85.73 (3)	C22—C23—C24	118.7 (3)
Cl1—Pd1—P1i	94.27 (3)	C22—C23—H23	120.7
Cl1i—Pd1—P1	94.27 (3)	C24—C23—H23	120.7
Cl1—Pd1—P1	85.73 (3)	C25—C24—C23	120.9 (3)
P1i—Pd1—P1	180.0	C25—C24—H24	119.5
C11—P1—C31	107.32 (13)	C23—C24—H24	119.5
C11—P1—C21	102.23 (13)	C24—C25—C26	120.2 (3)
C31—P1—C21	107.11 (13)	C24—C25—H25	119.9
C11—P1—Pd1	112.29 (9)	C26—C25—H25	119.9
C31—P1—Pd1	109.33 (9)	O2—C26—C25	124.9 (3)
C21—P1—Pd1	117.89 (9)	O2—C26—C21	115.1 (3)
C16—O1—C17	117.7 (2)	C25—C26—C21	120.0 (3)
C26—O2—C27	119.1 (3)	O2—C27—H27A	109.5
C36—O3—C37	119.0 (2)	O2—C27—H27B	109.5
C16—C11—C12	118.9 (2)	H27A—C27—H27B	109.5
C16—C11—P1	122.1 (2)	O2—C27—H27C	109.5
C12—C11—P1	118.1 (2)	H27A—C27—H27C	109.5
C13—C12—C11	120.2 (3)	H27B—C27—H27C	109.5
C13—C12—H12	119.9	C32—C31—C36	118.6 (3)
C11—C12—H12	119.9	C32—C31—P1	121.6 (2)
C14—C13—C12	120.4 (3)	C36—C31—P1	119.3 (2)
C14—C13—H13	119.8	C33—C32—C31	120.7 (3)
C12—C13—H13	119.8	C33—C32—H32	119.7
C13—C14—C15	120.2 (3)	C31—C32—H32	119.7
C13—C14—H14	119.9	C34—C33—C32	119.8 (3)
C15—C14—H14	119.9	C34—C33—H33	120.1
C14—C15—C16	120.1 (3)	C32—C33—H33	120.1
C14—C15—H15	120.0	C33—C34—C35	120.9 (3)
C16—C15—H15	120.0	C33—C34—H34	119.5
O1—C16—C11	117.3 (2)	C35—C34—H34	119.5
O1—C16—C15	122.4 (3)	C34—C35—C36	119.6 (3)
C11—C16—C15	120.2 (3)	C34—C35—H35	120.2
O1—C17—H17A	109.5	C36—C35—H35	120.2
O1—C17—H17B	109.5	O3—C36—C35	124.1 (3)
H17A—C17—H17B	109.5	O3—C36—C31	115.5 (2)
O1—C17—H17C	109.5	C35—C36—C31	120.4 (3)
H17A—C17—H17C	109.5	O3—C37—H37A	109.5
H17B—C17—H17C	109.5	O3—C37—H37B	109.5
C22—C21—C26	118.3 (3)	H37A—C37—H37B	109.5
C22—C21—P1	123.9 (2)	O3—C37—H37C	109.5
C26—C21—P1	117.8 (2)	H37A—C37—H37C	109.5
C23—C22—C21	121.8 (3)	H37B—C37—H37C	109.5
C23—C22—H22	119.1

Pd1—Cl1	2.3120 (7)
Pd1—P1	2.3417 (7)

Cl1—Pd1—P1i	94.27 (3)
Cl1—Pd1—P1	85.73 (3)

Symmetry code: (i) .