μ-(2,2'-Bipyrimidine)-bis-[dichlorido-palladium(II)] dimethyl-formamide monosolvate.

In the title compound, [Pd(2)Cl(4)(C(8)H(6)N(4))]·C(3)H(7)NO, the two Pd(2+) cations have a distorted square-planar coordination sphere and are bridged by a bis-bidentate 2,2'-bipyrimidine ligand. Two terminal chloride anions are also bonded to each of the Pd(2+) cations. The dinuclear complex and the dimethylformamide solvate molecule lie on the inter-section of a twofold rotation axis and a mirror plane, with disorder present in the solvate mol-ecule. There is a slight distortion from the square-planar metal geometry, as indicated by the bite angles of 81.77 (13)° and 91.63 (5)°. The C and O atoms of the solvent mol-ecule are disordered over two sets of sites of equal occupancy.

Related literature

The title compound is structurally related to the mono-coord­inated species reported by Hudgens et al. (1997 ▶). For background literature on homogenous catalyst models, see: Van Leeuwen (2004 ▶); Meij et al. (2005 ▶); Otto et al. (2003 ▶); Steyn et al. (1997 ▶). For related structures, see: Inagaki et al. (2007 ▶); Maekawa et al. (1994 ▶). The mono-coordinated platinum counterpart was reported by Kawakami et al. (2006 ▶). For the synthetic procedure, see: Boyle et al. (2004 ▶).

Experimental

Crystal data

[Pd2Cl4(C8H6N4)]·C3H7NO

M = 578.81

Monoclinic,

a = 10.7299 (6) Å

b = 14.2399 (7) Å

c = 5.9381 (3) Å

β = 108.229 (2)°

V = 861.76 (8) Å3

Z = 2

Mo Kα radiation

μ = 2.71 mm−1

T = 100 K

0.09 × 0.09 × 0.08 mm

Data collection

Bruker APEXII diffractometer

Absorption correction: multi-scan (SADABS; Bruker, 2008) ▶ T min = 0.785, T max = 0.814

6102 measured reflections

1108 independent reflections

975 reflections with I > 2σ(I)

R int = 0.041

Refinement

R[F 2 > 2σ(F 2)] = 0.028

wR(F 2) = 0.059

S = 1.11

1108 reflections

68 parameters

H-atom parameters constrained

Δρmax = 0.75 e Å−3

Δρmin = −0.79 e Å−3

Data collection: APEX2 (Bruker, 2008) ▶; cell refinement: SAINT-Plus (Bruker, 2008 ▶); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: DIAMOND (Brandenburg & Putz, 2005) ▶; software used to prepare material for publication: WinGX (Farrugia, 1999 ▶).

Click here for additional data file.

Crystal structure: contains datablock(s) global, I. DOI: 10.1107/S1600536812040779/gg2102sup1.cif

Click here for additional data file.

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536812040779/gg2102Isup2.hkl

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

[Pd2Cl4(C8H6N4)]·C3H7NO	F(000) = 550
Mr = 578.81	Dx = 2.231 Mg m−3
Monoclinic, C2/m	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2y	Cell parameters from 1958 reflections
a = 10.7299 (6) Å	θ = 2.9–27.8°
b = 14.2399 (7) Å	µ = 2.71 mm−1
c = 5.9381 (3) Å	T = 100 K
β = 108.229 (2)°	Cuboid, red
V = 861.76 (8) Å3	0.09 × 0.09 × 0.08 mm
Z = 2

Bruker APEXII diffractometer	1108 independent reflections
Radiation source: sealed tube	975 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.041
phi and ω scans	θmax = 28.3°, θmin = 3.6°
Absorption correction: multi-scan (SADABS; Bruker, 2008)	h = −12→14
Tmin = 0.785, Tmax = 0.814	k = −18→18
6102 measured reflections	l = −7→7

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)] = 0.028	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.059	H-atom parameters constrained
S = 1.11	w = 1/[σ2(Fo2) + (0.0172P)2 + 2.5414P] where P = (Fo2 + 2Fc2)/3
1108 reflections	(Δ/σ)max < 0.001
68 parameters	Δρmax = 0.75 e Å−3
0 restraints	Δρmin = −0.79 e Å−3

Geometry. All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'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 > 2σ(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	Occ. (<1)
C11	0.5	0.4487 (3)	0.5	0.0149 (8)
C12	0.5694 (3)	0.3120 (2)	0.6987 (6)	0.0270 (8)
H12	0.6167	0.2793	0.8341	0.032*
C13	0.5	0.2637 (3)	0.5	0.0370 (13)
H13	0.5	0.1984	0.5	0.044*
N1	0.5696 (2)	0.40577 (17)	0.6995 (4)	0.0152 (5)
Cl11	0.72957 (8)	0.61422 (6)	1.23998 (14)	0.0303 (2)
Pd01	0.65034 (3)	0.5	0.96630 (6)	0.01736 (12)
N22	0.5	0	0	0.0288 (14)
O22	0.5	0.1536 (5)	0	0.052 (2)	0.5
C21	0.4476 (8)	0.0853 (5)	−0.1298 (13)	0.0356 (18)	0.5
C22	0.4325 (11)	0	−0.2451 (19)	0.053 (4)	0.5

	U11	U22	U33	U12	U13	U23
C11	0.013 (2)	0.015 (2)	0.018 (2)	0	0.0063 (17)	0
C12	0.0231 (18)	0.0158 (15)	0.035 (2)	0.0002 (13)	−0.0007 (15)	0.0069 (13)
C13	0.034 (3)	0.012 (2)	0.051 (3)	0	−0.008 (3)	0
N1	0.0112 (12)	0.0180 (12)	0.0155 (13)	0.0008 (10)	0.0027 (10)	0.0040 (10)
Cl11	0.0220 (4)	0.0488 (5)	0.0189 (4)	−0.0109 (4)	0.0045 (3)	−0.0137 (4)
Pd01	0.01263 (19)	0.0256 (2)	0.01300 (18)	0	0.00278 (13)	0
N22	0.052 (4)	0.016 (3)	0.026 (3)	0	0.025 (3)	0
O22	0.095 (7)	0.019 (4)	0.064 (6)	0	0.058 (6)	0
C21	0.037 (5)	0.038 (4)	0.041 (4)	−0.001 (3)	0.025 (4)	0.002 (4)
C22	0.015 (5)	0.123 (12)	0.018 (5)	0	0.003 (4)	0

C11—N1i	1.335 (3)	N22—C22	1.408 (11)
C11—N1	1.335 (3)	N22—C22iv	1.408 (11)
C11—C11ii	1.462 (8)	N22—C21v	1.454 (8)
C12—N1	1.336 (4)	N22—C21vi	1.454 (8)
C12—C13	1.368 (4)	N22—C21	1.454 (8)
C12—H12	0.93	N22—C21iv	1.454 (8)
C13—C12i	1.368 (4)	O22—C21	1.258 (9)
C13—H13	0.93	O22—C21v	1.258 (9)
N1—Pd01	2.050 (2)	C21—C22	1.379 (9)
Cl11—Pd01	2.2682 (8)	C21—C21v	1.598 (16)
Pd01—N1iii	2.050 (2)	C22—C21vi	1.379 (9)
Pd01—Cl11iii	2.2682 (8)
N1i—C11—N1	125.5 (4)	C22iv—N22—C21vi	122.4 (3)
N1i—C11—C11ii	117.24 (18)	C21v—N22—C21vi	180.0 (3)
N1—C11—C11ii	117.24 (18)	C22—N22—C21	57.6 (3)
N1—C12—C13	120.4 (3)	C22iv—N22—C21	122.4 (3)
N1—C12—H12	119.8	C21v—N22—C21	66.7 (6)
C13—C12—H12	119.8	C21vi—N22—C21	113.3 (6)
C12—C13—C12i	119.6 (4)	C22—N22—C21iv	122.4 (3)
C12—C13—H13	120.2	C22iv—N22—C21iv	57.6 (3)
C12i—C13—H13	120.2	C21v—N22—C21iv	113.3 (6)
C11—N1—C12	117.1 (3)	C21vi—N22—C21iv	66.7 (6)
C11—N1—Pd01	111.7 (2)	C21—N22—C21iv	180.0 (6)
C12—N1—Pd01	131.1 (2)	C21—O22—C21v	78.9 (8)
N1—Pd01—N1iii	81.77 (13)	O22—C21—C22	160.9 (9)
N1—Pd01—Cl11	174.98 (7)	O22—C21—N22	107.2 (6)
N1iii—Pd01—Cl11	93.29 (7)	C22—C21—N22	59.5 (5)
N1—Pd01—Cl11iii	93.29 (7)	O22—C21—C21v	50.6 (4)
N1iii—Pd01—Cl11iii	174.98 (7)	C22—C21—C21v	114.6 (6)
Cl11—Pd01—Cl11iii	91.63 (5)	N22—C21—C21v	56.7 (3)
C22—N22—C22iv	180.0000 (10)	C21—C22—C21vi	123.5 (10)
C22—N22—C21v	122.4 (3)	C21—C22—N22	62.9 (5)
C22iv—N22—C21v	57.6 (3)	C21vi—C22—N22	62.9 (5)
C22—N22—C21vi	57.6 (3)