trans-Diaqua-bis(2,2'-bipyridine-κN,N')ruthenium(II) bis-(trifluoro-methane-sulfonate).

The title compound, trans-[Ru(bpy)(2)(H(2)O)(2)](CF(3)SO(3))(2) (bpy = 2,2'-bipyridine, C(10)H(8)N(2)), crystallized from the decomposition of an aged aqueous solution of a dimeric complex of cis-Ru(bpy)(2) in 0.1 M triflic acid. The Ru(II) ion is located on a crystallographic inversion center and exhibits a distorted octa-hedral coordination with equivalent ligands trans to each other. The Ru-O distance is 2.1053 (16) Å and the Ru-N distances are 2.0727 (17) and 2.0739 (17) Å. The bpy ligands are bent, due to inter-ligand steric inter-actions between H atoms of opposite pyridyl units across the Ru center. The crystal structure exhibits an extensive hydrogen-bonding network involving the water ligands and the trifluoromethane-sulfonate counter-ions within two-dimensional layers, although no close hydrogen-bond inter-actions exist between different layers.

Related literature

For the crystal structures of related compounds, see: Weathers et al. (1997 ▶); Durham et al. (1980 ▶); Klüfers & Zangl (2007 ▶). For a comparative discussion, see the Comment section in the Supplementary materials. For the preparation of the title compound, see: Jude et al. (2008 ▶); Sullivan et al. (1978 ▶). For related literature, see: Walsh & Durham (1982 ▶).

Experimental

Crystal data

[Ru(C10H8N2)2(H2O)2](CF3SO3)2

M = 747.61

Monoclinic,

a = 8.6569 (5) Å

b = 14.1272 (8) Å

c = 11.3226 (6) Å

β = 93.095 (3)°

V = 1382.71 (13) Å3

Z = 2

Cu Kα radiation

μ = 6.88 mm−1

T = 100 (2) K

0.20 × 0.15 × 0.02 mm

Data collection

Bruker SMART APEXII CCD area-detector diffractometer

Absorption correction: numerical followed by SADABS (Bruker, 2007 ▶) T min = 0.340, T max = 0.875

15574 measured reflections

2538 independent reflections

2436 reflections with I > 2σ(I)

R int = 0.039

Refinement

R[F 2 > 2σ(F 2)] = 0.025

wR(F 2) = 0.061

S = 1.09

2538 reflections

204 parameters

H atoms treated by a mixture of independent and constrained refinement

Δρmax = 0.69 e Å−3

Δρmin = −0.45 e Å−3

Data collection: APEX2 (Bruker, 2007 ▶); cell refinement: APEX2; data reduction: SAINT (Bruker, 2007 ▶); 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.

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536808028195/pk2108sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808028195/pk2108Isup2.hkl

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

[Ru(C10H8N2)2(H2O)2](CF3O3S)2	F(000) = 748
Mr = 747.61	Dx = 1.796 Mg m−3
Monoclinic, P21/c	Cu Kα radiation, λ = 1.54178 Å
Hall symbol: -P 2ybc	Cell parameters from 1677 reflections
a = 8.6569 (5) Å	θ = 5.0–67.3°
b = 14.1272 (8) Å	µ = 6.88 mm−1
c = 11.3226 (6) Å	T = 100 K
β = 93.095 (3)°	Plate, brown
V = 1382.71 (13) Å3	0.20 × 0.15 × 0.02 mm
Z = 2

Bruker SMART APEXII CCD area-detector diffractometer	2538 independent reflections
Radiation source: fine-focus sealed tube	2436 reflections with I > 2σ(I)
graphite	Rint = 0.039
φ and ω scans	θmax = 69.7°, θmin = 5.0°
Absorption correction: numerical Numerical followed by SADABS (Bruker, 2007)	h = −9→10
Tmin = 0.340, Tmax = 0.875	k = −17→17
15574 measured reflections	l = −13→13

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: difference Fourier map
wR(F2) = 0.062	H atoms treated by a mixture of independent and constrained refinement
S = 1.09	w = 1/[σ2(Fo2) + (0.0273P)2 + 1.4103P] where P = (Fo2 + 2Fc2)/3
2538 reflections	(Δ/σ)max < 0.001
204 parameters	Δρmax = 0.69 e Å−3
0 restraints	Δρmin = −0.45 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 > 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.Hydrogen atoms were placed in calculated positions with the exception of H1A and H1A, which were located in a difference synthesis and subsequently allowed to refine with isotropic thermal parameters.

	x	y	z	Uiso*/Ueq
Ru1	0.5000	0.5000	0.0000	0.01303 (9)
O1	0.64907 (19)	0.61137 (12)	0.05421 (17)	0.0181 (3)
N2	0.6089 (2)	0.42131 (12)	0.13474 (15)	0.0154 (4)
C3	0.5507 (3)	0.39407 (15)	0.23786 (19)	0.0192 (4)
H3	0.4431	0.4020	0.2475	0.023*
C4	0.6412 (3)	0.35501 (17)	0.3302 (2)	0.0243 (5)
H4	0.5965	0.3365	0.4014	0.029*
C5	0.7986 (3)	0.34355 (18)	0.3164 (2)	0.0271 (5)
H5	0.8644	0.3208	0.3800	0.033*
C6	0.8584 (3)	0.36563 (17)	0.2090 (2)	0.0230 (5)
H6	0.9650	0.3559	0.1970	0.028*
C7	0.7606 (3)	0.40225 (15)	0.11871 (19)	0.0179 (4)
C8	0.8048 (2)	0.41339 (15)	−0.00489 (19)	0.0170 (4)
C9	0.9491 (3)	0.38753 (16)	−0.0439 (2)	0.0208 (5)
H9	1.0312	0.3708	0.0113	0.025*
C10	0.9709 (3)	0.38668 (17)	−0.1642 (2)	0.0240 (5)
H10	1.0692	0.3716	−0.1926	0.029*
C11	0.8470 (3)	0.40816 (17)	−0.2426 (2)	0.0230 (5)
H11	0.8578	0.4043	−0.3255	0.028*
C12	0.7075 (3)	0.43527 (16)	−0.19861 (19)	0.0194 (4)
H12	0.6233	0.4499	−0.2528	0.023*
N13	0.6869 (2)	0.44164 (12)	−0.08110 (16)	0.0160 (4)
S1	0.31188 (6)	0.31728 (4)	0.61491 (5)	0.01857 (13)
C14	0.2290 (3)	0.3937 (2)	0.4986 (2)	0.0343 (6)
F15	0.1904 (2)	0.34309 (16)	0.40134 (15)	0.0556 (5)
F16	0.3298 (2)	0.45966 (12)	0.46821 (15)	0.0458 (4)
F17	0.1035 (2)	0.43667 (17)	0.53333 (18)	0.0652 (6)
O19	0.44116 (19)	0.27407 (11)	0.55926 (14)	0.0241 (4)
O20	0.3551 (2)	0.38361 (12)	0.70808 (14)	0.0271 (4)
O21	0.1893 (2)	0.25354 (14)	0.64049 (17)	0.0360 (5)
H1A	0.644 (3)	0.6198 (19)	0.120 (3)	0.016 (7)*
H1B	0.619 (4)	0.651 (2)	0.018 (3)	0.033 (9)*

	U11	U22	U33	U12	U13	U23
Ru1	0.01032 (13)	0.01596 (13)	0.01305 (13)	0.00058 (8)	0.00289 (8)	−0.00017 (7)
O1	0.0178 (8)	0.0206 (8)	0.0159 (9)	−0.0017 (6)	0.0017 (6)	0.0007 (7)
N2	0.0146 (9)	0.0163 (8)	0.0155 (9)	0.0011 (7)	0.0015 (7)	−0.0003 (7)
C3	0.0195 (11)	0.0191 (10)	0.0196 (11)	0.0000 (8)	0.0064 (9)	−0.0007 (8)
C4	0.0310 (13)	0.0241 (11)	0.0185 (11)	0.0024 (9)	0.0070 (10)	0.0042 (9)
C5	0.0291 (14)	0.0300 (12)	0.0219 (11)	0.0101 (10)	−0.0011 (10)	0.0028 (9)
C6	0.0164 (11)	0.0288 (12)	0.0240 (11)	0.0054 (9)	0.0022 (9)	0.0008 (9)
C7	0.0174 (11)	0.0169 (10)	0.0196 (11)	0.0008 (8)	0.0041 (9)	−0.0011 (8)
C8	0.0149 (11)	0.0164 (10)	0.0198 (11)	−0.0002 (8)	0.0016 (9)	−0.0010 (8)
C9	0.0163 (11)	0.0228 (11)	0.0232 (11)	0.0020 (9)	0.0018 (9)	−0.0001 (9)
C10	0.0180 (12)	0.0285 (12)	0.0265 (12)	0.0039 (9)	0.0102 (10)	0.0003 (9)
C11	0.0228 (12)	0.0281 (12)	0.0188 (11)	0.0033 (9)	0.0063 (9)	−0.0001 (9)
C12	0.0192 (12)	0.0227 (11)	0.0167 (10)	0.0016 (9)	0.0027 (9)	−0.0003 (8)
N13	0.0137 (9)	0.0160 (8)	0.0185 (9)	−0.0004 (7)	0.0037 (7)	−0.0005 (7)
S1	0.0180 (3)	0.0219 (3)	0.0161 (2)	−0.0016 (2)	0.0032 (2)	−0.00187 (19)
C14	0.0296 (15)	0.0488 (17)	0.0245 (13)	0.0170 (12)	−0.0003 (11)	0.0023 (11)
F15	0.0536 (12)	0.0841 (14)	0.0270 (9)	0.0107 (10)	−0.0172 (8)	−0.0078 (9)
F16	0.0665 (12)	0.0385 (9)	0.0332 (9)	0.0124 (8)	0.0110 (8)	0.0147 (7)
F17	0.0458 (11)	0.0919 (16)	0.0583 (12)	0.0474 (11)	0.0068 (9)	0.0086 (11)
O19	0.0218 (9)	0.0244 (8)	0.0266 (8)	0.0029 (6)	0.0054 (7)	0.0001 (6)
O20	0.0347 (10)	0.0275 (9)	0.0191 (8)	−0.0044 (7)	0.0015 (7)	−0.0040 (7)
O21	0.0340 (11)	0.0391 (10)	0.0366 (10)	−0.0155 (8)	0.0171 (8)	−0.0102 (8)

Ru1—N2i	2.0727 (17)	C7—C8	1.479 (3)
Ru1—N2	2.0727 (17)	C8—N13	1.360 (3)
Ru1—N13i	2.0739 (17)	C8—C9	1.396 (3)
Ru1—N13	2.0739 (17)	C9—C10	1.385 (3)
Ru1—O1i	2.1053 (16)	C9—H9	0.9500
Ru1—O1	2.1053 (16)	C10—C11	1.389 (4)
O1—H1A	0.75 (3)	C10—H10	0.9500
O1—H1B	0.73 (4)	C11—C12	1.384 (3)
N2—C3	1.352 (3)	C11—H11	0.9500
N2—C7	1.363 (3)	C12—N13	1.355 (3)
C3—C4	1.387 (3)	C12—H12	0.9500
C3—H3	0.9500	S1—O21	1.4334 (18)
C4—C5	1.389 (4)	S1—O20	1.4451 (17)
C4—H4	0.9500	S1—O19	1.4486 (16)
C5—C6	1.383 (3)	S1—C14	1.820 (3)
C5—H5	0.9500	C14—F17	1.323 (3)
C6—C7	1.391 (3)	C14—F16	1.334 (3)
C6—H6	0.9500	C14—F15	1.340 (3)
N2i—Ru1—N2	180.00 (8)	N2—C7—C6	121.9 (2)
N2i—Ru1—N13i	77.18 (7)	N2—C7—C8	113.93 (19)
N2—Ru1—N13i	102.82 (7)	C6—C7—C8	123.8 (2)
N2i—Ru1—N13	102.82 (7)	N13—C8—C9	122.0 (2)
N2—Ru1—N13	77.18 (7)	N13—C8—C7	114.07 (18)
N13i—Ru1—N13	180.0	C9—C8—C7	123.6 (2)
N2i—Ru1—O1i	86.51 (7)	C10—C9—C8	119.0 (2)
N2—Ru1—O1i	93.49 (7)	C10—C9—H9	120.5
N13i—Ru1—O1i	86.88 (7)	C8—C9—H9	120.5
N13—Ru1—O1i	93.12 (7)	C9—C10—C11	119.0 (2)
N2i—Ru1—O1	93.49 (7)	C9—C10—H10	120.5
N2—Ru1—O1	86.51 (7)	C11—C10—H10	120.5
N13i—Ru1—O1	93.12 (7)	C12—C11—C10	119.3 (2)
N13—Ru1—O1	86.88 (7)	C12—C11—H11	120.4
O1i—Ru1—O1	180.0	C10—C11—H11	120.4
Ru1—O1—H1A	110 (2)	N13—C12—C11	122.4 (2)
Ru1—O1—H1B	102 (3)	N13—C12—H12	118.8
H1A—O1—H1B	113 (3)	C11—C12—H12	118.8
C3—N2—C7	117.74 (19)	C12—N13—C8	117.98 (18)
C3—N2—Ru1	127.77 (15)	C12—N13—Ru1	127.48 (15)
C7—N2—Ru1	114.28 (14)	C8—N13—Ru1	114.35 (14)
N2—C3—C4	122.9 (2)	O21—S1—O20	115.16 (10)
N2—C3—H3	118.6	O21—S1—O19	114.90 (11)
C4—C3—H3	118.6	O20—S1—O19	114.53 (10)
C3—C4—C5	118.6 (2)	O21—S1—C14	104.58 (13)
C3—C4—H4	120.7	O20—S1—C14	102.69 (12)
C5—C4—H4	120.7	O19—S1—C14	102.65 (11)
C6—C5—C4	119.2 (2)	F17—C14—F16	108.4 (2)
C6—C5—H5	120.4	F17—C14—F15	108.5 (2)
C4—C5—H5	120.4	F16—C14—F15	107.4 (2)
C5—C6—C7	119.2 (2)	F17—C14—S1	110.79 (19)
C5—C6—H6	120.4	F16—C14—S1	111.30 (19)
C7—C6—H6	120.4	F15—C14—S1	110.4 (2)
N13i—Ru1—N2—C3	16.01 (19)	C9—C10—C11—C12	3.8 (4)
N13—Ru1—N2—C3	−163.99 (19)	C10—C11—C12—N13	−0.1 (4)
O1i—Ru1—N2—C3	−71.58 (18)	C11—C12—N13—C8	−5.0 (3)
O1—Ru1—N2—C3	108.42 (18)	C11—C12—N13—Ru1	169.81 (17)
N13i—Ru1—N2—C7	−158.51 (14)	C9—C8—N13—C12	6.5 (3)
N13—Ru1—N2—C7	21.49 (14)	C7—C8—N13—C12	−166.89 (19)
O1i—Ru1—N2—C7	113.90 (15)	C9—C8—N13—Ru1	−169.01 (16)
O1—Ru1—N2—C7	−66.10 (15)	C7—C8—N13—Ru1	17.6 (2)
C7—N2—C3—C4	5.3 (3)	N2i—Ru1—N13—C12	−16.10 (19)
Ru1—N2—C3—C4	−169.07 (17)	N2—Ru1—N13—C12	163.90 (19)
N2—C3—C4—C5	0.2 (4)	O1i—Ru1—N13—C12	71.02 (18)
C3—C4—C5—C6	−4.1 (4)	O1—Ru1—N13—C12	−108.98 (18)
C4—C5—C6—C7	2.5 (4)	N2i—Ru1—N13—C8	158.85 (14)
C3—N2—C7—C6	−7.0 (3)	N2—Ru1—N13—C8	−21.15 (14)
Ru1—N2—C7—C6	168.14 (17)	O1i—Ru1—N13—C8	−114.03 (15)
C3—N2—C7—C8	166.29 (18)	O1—Ru1—N13—C8	65.97 (15)
Ru1—N2—C7—C8	−18.6 (2)	O21—S1—C14—F17	57.2 (2)
C5—C6—C7—N2	3.2 (3)	O20—S1—C14—F17	−63.4 (2)
C5—C6—C7—C8	−169.4 (2)	O19—S1—C14—F17	177.4 (2)
N2—C7—C8—N13	0.6 (3)	O21—S1—C14—F16	177.87 (17)
C6—C7—C8—N13	173.7 (2)	O20—S1—C14—F16	57.3 (2)
N2—C7—C8—C9	−172.6 (2)	O19—S1—C14—F16	−61.9 (2)
C6—C7—C8—C9	0.5 (3)	O21—S1—C14—F15	−63.0 (2)
N13—C8—C9—C10	−2.8 (3)	O20—S1—C14—F15	176.41 (18)
C7—C8—C9—C10	169.9 (2)	O19—S1—C14—F15	57.3 (2)
C8—C9—C10—C11	−2.4 (3)

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1B···O19ii	0.73 (4)	2.01 (4)	2.727 (2)	169 (4)
O1—H1A···O20iii	0.75 (3)	1.95 (3)	2.695 (2)	169 (3)

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1—H1B⋯O19i	0.73 (4)	2.01 (4)	2.727 (2)	169 (4)
O1—H1A⋯O20ii	0.75 (3)	1.95 (3)	2.695 (2)	169 (3)

Symmetry codes: (i) ; (ii) .