trans-Dibromidotetra-kis-(pyridine-κN)ruthenium(II).

The title complex, [RuBr(2)(C(5)H(5)N)(4)], contains two independent complex mol-ecules in each of which the Ru(II) atom is located on a site of 222 symmetry and has a distorted octa-hedral coordination geometry with four pyridine N atoms and two Br atoms. The Br aroms are trans-disposed as a result of symmetry.

Related literature

For background to ruthenium complexes: see: Pagliaro et al. (2005 ▶); van Rijt & Sadler (2009 ▶); Wu et al. (2009 ▶); Zhang et al. (2005 ▶). For related structures, see: Mirza et al. (2003 ▶); Wong & Lau (1994 ▶); Zhang et al. (2006 ▶). For a description of the Cambridge Structural Database, see: Allen (2002 ▶).

Experimental

Crystal data

[RuBr2(C5H5N)4]

M = 577.29

Orthorhombic,

a = 16.830 (4) Å

b = 22.032 (5) Å

c = 23.221 (5) Å

V = 8610 (3) Å3

Z = 16

Mo Kα radiation

μ = 4.45 mm−1

T = 296 K

0.22 × 0.18 × 0.13 mm

Data collection

Bruker APEXII CCD diffractometer

Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T min = 0.441, T max = 0.595

13382 measured reflections

2430 independent reflections

1631 reflections with I > 2σ(I)

R int = 0.034

Refinement

R[F 2 > 2σ(F 2)] = 0.025

wR(F 2) = 0.069

S = 1.04

2430 reflections

125 parameters

H-atom parameters constrained

Δρmax = 0.58 e Å−3

Δρmin = −0.34 e Å−3

Data collection: APEX2 (Bruker, 2007 ▶); cell refinement: SAINT (Bruker, 2007 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: SHELXTL (Sheldrick, 2008 ▶); software used to prepare material for publication: SHELXTL.

Click here for additional data file.

Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536813000871/hy2613sup1.cif

Click here for additional data file.

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536813000871/hy2613Isup2.hkl

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

[RuBr2(C5H5N)4]	F(000) = 4512
Mr = 577.29	Dx = 1.781 Mg m−3
Orthorhombic, Fddd	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -F 2uv 2vw	Cell parameters from 2149 reflections
a = 16.830 (4) Å	θ = 2.2–26.4°
b = 22.032 (5) Å	µ = 4.45 mm−1
c = 23.221 (5) Å	T = 296 K
V = 8610 (3) Å3	Block, red
Z = 16	0.22 × 0.18 × 0.13 mm

Bruker APEXII CCD diffractometer	2430 independent reflections
Radiation source: fine-focus sealed tube	1631 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.034
φ and ω scans	θmax = 27.5°, θmin = 3.0°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −21→21
Tmin = 0.441, Tmax = 0.595	k = −28→28
13382 measured reflections	l = −29→26

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)] = 0.025	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.069	H-atom parameters constrained
S = 1.04	w = 1/[σ2(Fo2) + (0.0292P)2 + 11.6805P] where P = (Fo2 + 2Fc2)/3
2430 reflections	(Δ/σ)max < 0.001
125 parameters	Δρmax = 0.58 e Å−3
0 restraints	Δρmin = −0.34 e Å−3

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 > 2sigma(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
Ru1	0.1250	0.1250	0.1250	0.03562 (11)
Ru2	0.6250	0.1250	0.1250	0.03634 (11)
Br1	0.1250	0.009537 (19)	0.1250	0.05758 (14)
Br2	0.6250	0.1250	0.015713 (18)	0.06143 (15)
N1	0.03782 (12)	0.12460 (9)	0.18885 (9)	0.0409 (5)
N2	0.71241 (13)	0.19195 (10)	0.12552 (9)	0.0428 (5)
C1	−0.02375 (16)	0.08600 (14)	0.18763 (12)	0.0513 (7)
H1	−0.0280	0.0594	0.1567	0.062*
C2	−0.08052 (18)	0.08388 (16)	0.22953 (14)	0.0643 (9)
H2	−0.1223	0.0564	0.2268	0.077*
C3	−0.0757 (2)	0.12230 (16)	0.27562 (15)	0.0664 (9)
H3	−0.1137	0.1216	0.3047	0.080*
C4	−0.01284 (18)	0.16198 (15)	0.27768 (13)	0.0565 (8)
H4	−0.0077	0.1887	0.3084	0.068*
C5	0.04201 (16)	0.16198 (13)	0.23442 (11)	0.0463 (6)
H5	0.0842	0.1891	0.2366	0.056*
C6	0.77437 (16)	0.19016 (13)	0.16161 (13)	0.0513 (7)
H6	0.7783	0.1577	0.1870	0.062*
C7	0.83202 (18)	0.23371 (16)	0.16297 (15)	0.0655 (9)
H7	0.8740	0.2304	0.1888	0.079*
C8	0.8280 (2)	0.28178 (15)	0.12661 (16)	0.0721 (10)
H8	0.8670	0.3117	0.1269	0.086*
C9	0.76494 (19)	0.28493 (15)	0.08948 (16)	0.0656 (9)
H9	0.7601	0.3175	0.0642	0.079*
C10	0.70898 (16)	0.23981 (13)	0.08982 (13)	0.0509 (7)
H10	0.6667	0.2424	0.0642	0.061*

	U11	U22	U33	U12	U13	U23
Ru1	0.0287 (2)	0.0399 (2)	0.0383 (2)	0.000	0.000	0.000
Ru2	0.0285 (2)	0.0431 (2)	0.0374 (2)	0.000	0.000	0.000
Br1	0.0600 (3)	0.0459 (2)	0.0668 (3)	0.000	−0.0158 (2)	0.000
Br2	0.0616 (3)	0.0806 (3)	0.0421 (2)	−0.0070 (2)	0.000	0.000
N1	0.0331 (11)	0.0465 (12)	0.0430 (12)	−0.0042 (10)	−0.0006 (9)	0.0007 (10)
N2	0.0326 (11)	0.0461 (12)	0.0497 (13)	0.0005 (9)	−0.0006 (10)	0.0022 (11)
C1	0.0398 (15)	0.0614 (18)	0.0526 (17)	−0.0119 (14)	−0.0014 (13)	0.0002 (14)
C2	0.0449 (18)	0.081 (2)	0.067 (2)	−0.0174 (16)	0.0047 (15)	0.0060 (18)
C3	0.0495 (18)	0.091 (2)	0.0590 (19)	−0.0018 (18)	0.0172 (15)	0.0106 (18)
C4	0.0482 (17)	0.072 (2)	0.0490 (17)	0.0020 (15)	0.0079 (13)	−0.0041 (15)
C5	0.0392 (15)	0.0486 (16)	0.0512 (17)	−0.0019 (12)	0.0030 (12)	−0.0028 (13)
C6	0.0382 (15)	0.0530 (17)	0.0627 (19)	0.0023 (13)	−0.0086 (14)	−0.0006 (14)
C7	0.0407 (17)	0.068 (2)	0.088 (2)	−0.0039 (15)	−0.0146 (17)	−0.0092 (18)
C8	0.0504 (19)	0.053 (2)	0.112 (3)	−0.0150 (15)	−0.001 (2)	−0.004 (2)
C9	0.0528 (19)	0.056 (2)	0.088 (2)	−0.0023 (15)	0.0069 (18)	0.0133 (18)
C10	0.0380 (15)	0.0549 (18)	0.0597 (18)	−0.0009 (13)	0.0018 (13)	0.0077 (14)

Ru1—N1i	2.086 (2)	C1—H1	0.9300
Ru1—N1ii	2.086 (2)	C2—C3	1.367 (5)
Ru1—N1	2.086 (2)	C2—H2	0.9300
Ru1—N1iii	2.086 (2)	C3—C4	1.373 (4)
Ru1—Br1	2.5439 (7)	C3—H3	0.9300
Ru1—Br1ii	2.5439 (7)	C4—C5	1.364 (4)
Ru2—N2iv	2.083 (2)	C4—H4	0.9300
Ru2—N2	2.083 (2)	C5—H5	0.9300
Ru2—N2i	2.083 (2)	C6—C7	1.365 (4)
Ru2—N2v	2.083 (2)	C6—H6	0.9300
Ru2—Br2	2.5378 (7)	C7—C8	1.356 (5)
Ru2—Br2v	2.5378 (7)	C7—H7	0.9300
N1—C1	1.341 (3)	C8—C9	1.370 (5)
N1—C5	1.343 (3)	C8—H8	0.9300
N2—C6	1.339 (3)	C9—C10	1.369 (4)
N2—C10	1.342 (3)	C9—H9	0.9300
C1—C2	1.365 (4)	C10—H10	0.9300
N1i—Ru1—N1ii	179.52 (12)	C6—N2—C10	116.3 (2)
N1i—Ru1—N1	90.60 (12)	C6—N2—Ru2	122.20 (18)
N1ii—Ru1—N1	89.40 (12)	C10—N2—Ru2	121.48 (18)
N1i—Ru1—N1iii	89.40 (12)	N1—C1—C2	123.2 (3)
N1ii—Ru1—N1iii	90.60 (12)	N1—C1—H1	118.4
N1—Ru1—N1iii	179.52 (12)	C2—C1—H1	118.4
N1i—Ru1—Br1	90.24 (6)	C1—C2—C3	119.7 (3)
N1ii—Ru1—Br1	90.24 (6)	C1—C2—H2	120.2
N1—Ru1—Br1	89.76 (6)	C3—C2—H2	120.2
N1iii—Ru1—Br1	89.76 (6)	C2—C3—C4	117.9 (3)
N1i—Ru1—Br1ii	89.76 (6)	C2—C3—H3	121.1
N1ii—Ru1—Br1ii	89.76 (6)	C4—C3—H3	121.1
N1—Ru1—Br1ii	90.24 (6)	C5—C4—C3	119.7 (3)
N1iii—Ru1—Br1ii	90.24 (6)	C5—C4—H4	120.2
Br1—Ru1—Br1ii	180.0	C3—C4—H4	120.2
N2iv—Ru2—N2	179.34 (11)	N1—C5—C4	123.0 (3)
N2iv—Ru2—N2i	89.84 (12)	N1—C5—H5	118.5
N2—Ru2—N2i	90.16 (12)	C4—C5—H5	118.5
N2iv—Ru2—N2v	90.16 (12)	N2—C6—C7	123.2 (3)
N2—Ru2—N2v	89.84 (12)	N2—C6—H6	118.4
N2i—Ru2—N2v	179.34 (11)	C7—C6—H6	118.4
N2iv—Ru2—Br2	90.33 (6)	C8—C7—C6	120.0 (3)
N2—Ru2—Br2	90.33 (6)	C8—C7—H7	120.0
N2i—Ru2—Br2	89.67 (6)	C6—C7—H7	120.0
N2v—Ru2—Br2	89.67 (6)	C7—C8—C9	118.0 (3)
N2iv—Ru2—Br2v	89.67 (6)	C7—C8—H8	121.0
N2—Ru2—Br2v	89.67 (6)	C9—C8—H8	121.0
N2i—Ru2—Br2v	90.33 (6)	C10—C9—C8	119.5 (3)
N2v—Ru2—Br2v	90.33 (6)	C10—C9—H9	120.2
Br2—Ru2—Br2v	180.0	C8—C9—H9	120.2
C1—N1—C5	116.5 (2)	N2—C10—C9	123.0 (3)
C1—N1—Ru1	122.09 (18)	N2—C10—H10	118.5
C5—N1—Ru1	121.38 (17)	C9—C10—H10	118.5

Table 1

Selected bond lengths (Å)

Ru1—N1	2.086 (2)
Ru1—Br1	2.5439 (7)
Ru2—N2	2.083 (2)
Ru2—Br2	2.5378 (7)