trans-Diaqua­bis(2,2′-bipyridine-κ2N,N′)ruthenium(II) bis­(trifluoro­methane­sulfonate)

Jude, H.; White, P.S.; Dattelbaum, D.M.; Rocha, R.C.

doi:10.1107/S1600536808028195

metal-organic compounds

CRYSTALLOGRAPHIC
COMMUNICATIONS

ISSN: 2056-9890

Volume 64| Part 11| November 2008| Pages m1388-m1389

doi:10.1107/S1600536808028195

Open

access

trans-Diaquabis(2,2′-bipyridine-κ²N,N′)ruthenium(II) bis(trifluoromethanesulfonate)

Hershel Jude,^a ^* Peter S. White,^b Dana M. Dattelbaum ^c and Reginaldo C. Rocha ^a

^aLos Alamos National Laboratory, MPA-CINT, Mail Stop G755, Los Alamos, NM 87545, USA, ^bUniversity of North Carolina, Department of Chemistry, Chapel Hill, NC 27599-3290, USA, and ^cLos Alamos National Laboratory, DE-9, Mail Stop P952, Los Alamos, NM 87545, USA
^*Correspondence e-mail: judeh3@lanl.gov

(Received 21 July 2008; accepted 3 September 2008; online 11 October 2008)

The title compound, trans-[Ru(bpy)₂(H₂O)₂](CF₃SO₃)₂ (bpy = 2,2′-bipyridine, C₁₀H₈N₂), 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 octahedral 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 interactions 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 trifluoromethanesulfonate counter-ions within two-dimensional layers, although no close hydrogen-bond interactions 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_r = 747.61
Monoclinic, P 2₁ /c
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[F² > 2σ(F²)] = 0.025
wR(F²) = 0.061
S = 1.09
2538 reflections
204 parameters
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 0.69 e Å⁻³
Δρ_min = −0.45 e Å⁻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) $[-x+1, y+{\script{1\over 2}}, -z+{\script{1\over 2}}]$ ; (ii) -x+1, -y+1, -z+1.

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.

Supporting information

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

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

checkCIF report

Comment top

The water ligands in cis- and trans-[Ru(bpy)₂(H₂O)₂]²⁺ can undergo facile ligand substitution under mild reaction conditions and thus these complexes have been important synthetic precursors to derivatives of the general type [Ru(bpy)₂(X)(Y)]ⁿ. Although the trans isomer is usually obtained from the photo-induced isomerization of the more common cis isomer (Durham et al., 1980; Walsh & Durham, 1982), formation of the trans isomer as a by-product in synthetic preparations involving the cis-Ru(bpy)₂ moiety has also been reported (e.g. Weathers et al., 1997).

The title compound trans-[Ru(bpy)₂(H₂O)₂](CF₃SO₃)₂, (I), was unintentionally obtained and crystallized from an acidic (0.1 M CF₃SO₃H) aqueous solution of [(bpy)₂Ru(OMe)(pyz)Ru(bpy)₂](PF₆)₂ (Jude et al., 2008) that was left aging in ambient conditions for several weeks. Its crystal structure is shown in Figs. 1 and 2, and detailed structural information is available herein as supplementary materials as well as in the archived CIF.

The structure of the analogous compound as a hexafluorophosphate salt, i.e. trans-[Ru(bpy)₂(H₂O)₂](PF₆)₂, (II), was previosuly reported (Weathers et al., 1997). In this case, the compound crystallized in the triclinic (P1) space group. The Ru—O distance of 2.116 (2) Å in the PF₆^- salt is similar to that reported here for the CF₃SO₃^- analogue, and the mean Ru—N distance of 2.074 (2) Å in II is essentially identical to those observed for I. The dihedral angle between the pyridyl (C₅N) ring planes in the distorted, non-planar bpy ligands is also similar in these compounds: 162.68 (12)° for II and 160.1 (1)° for I.

Another related structure was reported earlier for the oxidized/deprotonated Ru(III)-hydroxy species, trans-[Ru(bpy)₂(H₂O)(OH)](ClO₄)₂ (Durham et al., 1980). This perchlorate salt, (III), crystallized in the trigonal space group (P3₁21). In this case, however, the sterically strained bpy ligands adopted a twisted conformation, in contrast to the bowed conformation in both I and II. Shorter Ru—N distances are exhibited by the Ru(II)-diaqua species compared to III (2.090 (3) and 2.099 (3) Å), owing to the characteristic π-backbonding involving Ru(II) and π-acceptor pyridyl ligands. Consistent with the higher Ru(III) oxidation state, however, the Ru—O bond distance is shorter in III (2.007 (3) Å).

The trans-[Ru(bpy)₂(H₂O)₂]²⁺ cations pack in alternating layers with the CF₃SO₃^- anions packed between the cations. An extensive hydrogen bonding network exists within two-dimensional layers as a result of the hydrogen bonds between the water ligand molecules in the cationic complex and the sulfonate groups in the trifluoromethanesulfonate anions (Table 1 and Figure 2). However, no significant hydrogen-bond interactions are present between different layers.

Related literature top

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 top

cis-Ru(bpy)₂Cl₂ was prepared as described by Sullivan et al. (1978). The title compound was a product of the decomposition of [(bpy)₂Ru(OMe)(pyz)Ru(bpy)₂](PF₆)₂ (Jude et al., 2008) in a highly acidic (0.1 M CF₃SO₃H) aqueous solution that was kept for several weeks in a sealed clear glass jar in ambient lighting and temperature conditions. Red–orange blocks suitable for single-crystal X-ray analysis were isolated from the mixture.

Computing details top

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

Figures top

	Fig. 1. Single crystal structure of the title compound with 50% probability displacement ellipsoids. H atoms are omitted for clarity.
	Fig. 2. A packing diagram showing the hydrogen bonds (as dotted lines) between the water ligands in the ruthenium complex and the sulfonate group in the trifluoromethanesulfonate counterions.

trans-Diaquabis(2,2'-bipyridine-κ²N,N')ruthenium(II) bis(trifluoromethanesulfonate) top

Crystal data top

[Ru(C₁₀H₈N₂)₂(H₂O)₂](CF₃O₃S)₂	F(000) = 748
M_r = 747.61	D_x = 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

Data collection top

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

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)] = 0.025	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(F_o²) + (0.0273P)² + 1.4103P] where P = (F_o² + 2F_c²)/3
2538 reflections	(Δ/σ)_max < 0.001
204 parameters	Δρ_max = 0.69 e Å⁻³
0 restraints	Δρ_min = −0.45 e Å⁻³

Crystal data top

[Ru(C₁₀H₈N₂)₂(H₂O)₂](CF₃O₃S)₂	V = 1382.71 (13) Å³
M_r = 747.61	Z = 2
Monoclinic, P2₁/c	Cu Kα radiation
a = 8.6569 (5) Å	µ = 6.88 mm⁻¹
b = 14.1272 (8) Å	T = 100 K
c = 11.3226 (6) Å	0.20 × 0.15 × 0.02 mm
β = 93.095 (3)°

Data collection top

Bruker SMART APEXII CCD area-detector diffractometer	2538 independent reflections
Absorption correction: numerical Numerical followed by SADABS (Bruker, 2007)	2436 reflections with I > 2σ(I)
T_min = 0.340, T_max = 0.875	R_int = 0.039
15574 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.025	0 restraints
wR(F²) = 0.062	H atoms treated by a mixture of independent and constrained refinement
S = 1.09	Δρ_max = 0.69 e Å⁻³
2538 reflections	Δρ_min = −0.45 e Å⁻³
204 parameters

Special details top

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.

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

	x	y	z	U_iso*/U_eq
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)*

Atomic displacement parameters (Å²) top

	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)

Geometric parameters (Å, º) top

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)

Symmetry code: (i) −x+1, −y+1, −z.

Hydrogen-bond geometry (Å, º) top

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)

Symmetry codes: (ii) −x+1, y+1/2, −z+1/2; (iii) −x+1, −y+1, −z+1.

Experimental details

Crystal data
Chemical formula	[Ru(C₁₀H₈N₂)₂(H₂O)₂](CF₃O₃S)₂
M_r	747.61
Crystal system, space group	Monoclinic, P2₁/c
Temperature (K)	100
a, b, c (Å)	8.6569 (5), 14.1272 (8), 11.3226 (6)
β (°)	93.095 (3)
V (Å³)	1382.71 (13)
Z	2
Radiation type	Cu Kα
µ (mm⁻¹)	6.88
Crystal size (mm)	0.20 × 0.15 × 0.02

Data collection
Diffractometer	Bruker SMART APEXII CCD area-detector diffractometer
Absorption correction	Numerical Numerical followed by SADABS (Bruker, 2007)
T_min, T_max	0.340, 0.875
No. of measured, independent and observed [I > 2σ(I)] reflections	15574, 2538, 2436
R_int	0.039
(sin θ/λ)_max (Å⁻¹)	0.608

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.025, 0.062, 1.09
No. of reflections	2538
No. of parameters	204
H-atom treatment	H atoms treated by a mixture of independent and constrained refinement
Δρ_max, Δρ_min (e Å⁻³)	0.69, −0.45

Computer programs: APEX2 (Bruker, 2007), SAINT (Bruker, 2007), SHELXS (Sheldrick, 2008), SHELXL (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

Hydrogen-bond geometry (Å, º) top

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) −x+1, y+1/2, −z+1/2; (ii) −x+1, −y+1, −z+1.

Acknowledgements

Support by the US Department of Energy through the Laboratory Directed Research and Development (LDRD) program at LANL is gratefully acknowledged.

References

Bruker (2007). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Durham, B., Wilson, S. R., Hodgson, D. J. & Meyer, T. J. (1980). J. Am. Chem. Soc. 102, 600–607. CSD CrossRef CAS Web of Science Google Scholar
Jude, H., Rein, F. N., White, P. S., Dattelbaum, D. M. & Rocha, R. C. (2008). Inorg. Chem. 47, 7695–7702. Web of Science CSD CrossRef PubMed CAS Google Scholar
Klüfers, P. & Zangl, A. (2007). Acta Cryst. E63, m3088. Web of Science CSD CrossRef IUCr Journals Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Sullivan, B. P., Salmon, D. J. & Meyer, T. J. (1978). Inorg. Chem. 17, 3334–3341. CrossRef CAS Web of Science Google Scholar
Walsh, J. L. & Durham, B. (1982). Inorg. Chem. 21, 329–332. CrossRef CAS Web of Science Google Scholar
Weathers, N. R., Sadoski, R. C., Durham, B. & Cordes, A. W. (1997). Acta Cryst. C53, 1047–1049. CSD CrossRef CAS Web of Science IUCr Journals Google Scholar

This is an open-access article distributed under the terms of the Creative Commons Attribution (CC-BY) Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.