Hexakis(acetonitrile-κN)ruthenium(II) bis­(hexa­bromo­carbadodeca­borate) aceto­nitrile solvate

Masland, J.; Diaz, J.; Eady, S.; Lobkovsky, E.; Larsen, A.

doi:10.1107/S1600536810006252

metal-organic compounds

CRYSTALLOGRAPHIC
COMMUNICATIONS

ISSN: 2056-9890

Volume 66| Part 3| March 2010| Pages m325-m326

doi:10.1107/S1600536810006252

Open

access

Hexakis(acetonitrile-κN)ruthenium(II) bis(hexabromocarbadodecaborate) acetonitrile solvate

Joshua Masland,^a Jason Diaz,^a Shawn Eady,^a Emil Lobkovsky ^b and Anna Larsen ^a ^*

^aDepartment of Chemistry, Ithaca College, 953 Danby Road, Ithaca, NY 14850, USA, and ^bX-Ray Diffraction Facility, 167 Spencer T. Olin Laboratory, Cornell University, Ithaca, NY 14850, USA
^*Correspondence e-mail: alarsen@ithaca.edu

(Received 15 January 2010; accepted 16 February 2010; online 24 February 2010)

The title compound, [Ru(NCCH₃)₆](CH₆B₁₁Br₆)₂·CH₃CN, consists of the 'naked' ruthenium(II) cation surrounded by six acetonitrile molecules, each coordinated via the nitrogen atoms in a linear or nearly-linear fashion in a typical octahedral over-all arrangement. The cation is balanced by the two hexa-bromocarborane cage anionic fragments [CB₁₁H₆Br₆]. Weak C—H⋯Br and B—H⋯Br interactions link neighboring anions.

Related literature

For related literature pertaining to ruthenium and ruthenium derivative structures, see: Bergman & Chang (1987 ); Burns & Hubbard (1994 ); Stasko et al. (2002 ); Brookhart et al. (1992 ). For related ruthenium structures, see: Pearsal et al. (2007 ).

Experimental

Crystal data

[Ru(C₂H₃N)₆](CH₆B₁₁Br₆)₂·C₂H₃N
M_r = 1621.30
Orthorhombic, P n a 2₁
a = 21.332 (2) Å
b = 11.7577 (10) Å
c = 20.2620 (17) Å
V = 5082.1 (8) Å³
Z = 4
Mo Kα radiation
μ = 9.77 mm⁻¹
T = 173 K
0.20 × 0.15 × 0.10 mm

Data collection

Bruker CCD-1000 area-detector diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2007 ) T_min = 0.245, T_max = 0.442
36328 measured reflections
13481 independent reflections
10985 reflections with I > 2σ(I)
R_int = 0.042

Refinement

R[F² > 2σ(F²)] = 0.033
wR(F²) = 0.062
S = 0.97
13481 reflections
531 parameters
1 restraint
H-atom parameters constrained
Δρ_max = 0.83 e Å⁻³
Δρ_min = −0.73 e Å⁻³
Absolute structure: Flack (1983 ), 6319 Friedel pairs
Flack parameter: 0.000 (5)

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
B10—H10⋯Br8ⁱ	1.12	2.85	3.612 (5)	125
C1AA—H1A⋯Br4ⁱⁱ	1.12	2.77	3.547 (5)	126
Symmetry codes: (i) x, y-1, z; (ii) $[-x+1, -y+1, z-{\script{1\over 2}}]$ .

Data collection: SMART (Bruker, 2000 ); cell refinement: SAINT (Bruker, 2007); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2008 ); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL and publCIF (Westrip, 2010 ).

Supporting information

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536810006252/ez2197sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536810006252/ez2197Isup2.hkl

checkCIF report

Comment top

Electrophilic complexes with the [Cp*Ru(NO)] core are reactive towards small molecular nucleophiles. In the presence of labile neutral ligands or weakly coordinating anions, such as trifluoromethanesulfonate, these complexes exhibit pro-catalytic reactivity with unsaturated hydrocarbons and alcohols (Burns and Hubbard, 1994; Pearsal et al., 2007). The present study's goal is introduction of the non-coordinating carborane cage anions of the [CB₁₁H₁₂] family in order to increase the reactivity of the ruthenium catalytic center (Stasko et al., 2002). The synthetic route to the desired complexes includes protonation of the dialkyl starting material with the solvated proton salt of the weakly-coordinating anion (similar to Brookhart, et al., 1992). This process eventually results in stripping all the ligands off the ruthenium center to give the title compound comprised of the 'naked' hexa-acetonitrile ruthenium cationic fragment balanced by two hexa-bromo-carborane anionic fragments. The catalytic activity of this complex is currently under investigation.

Related literature top

For related literature pertaining to ruthenium and ruthenium derivative structures, see: Bergman & Chang (1987); Burns & Hubbard (1994); Stasko et al. (2002); Brookhart et al. (1992). For related ruthenium structures, see: Pearsal et al. (2007).

Experimental top

The compound was obtained by a prolonged exposure of the Cp*Ru(NO)(CH₃)₂ complex to an excess of carborane-based protonating agent [(C₂H₅OC₂H₅)₂ H]⁺ [CB₁₁H₆Br₆]^- in acetonitrile.

All synthetic procedures were carried out in inert atmosphere and in anhydrous solvents. The protonating agent [(C₂H₅OC₂H₅)₂ H]⁺ [CB₁₁H₆Br₆]^- and starting ruthenium complex Cp*Ru(NO)(CH₃)₂ were synthesized according to the reported procedures (Stasko et al., 2002; Bergman & Chang,1987).

20 mg (0.065 mmol) of Cp*Ru(NO)(CH₃)₂ were dissolved in 10 ml of CH₃CN and the solution was added to 200 mg of solid [(C₂H₅OC₂H₅)₂ H]⁺ [CB₁₁H₆Br₆]^- (0.265 mmol). Vigorous evolution of a gas (methane) was observed. The color of the solution gradually changed from dark red to dark purple-red. Initial product of the reaction, [Cp*Ru(NO)(CH₃)(NCCH₃)] [CB₁₁H₆Br₆], formed via a mono-protonation process and loss of one methane molecule from the starting material, was observed spectroscopically (by 1H NMR) in the aliquot of the reaction mixture taken after 4 hrs. The red crystals of the [Ru(NCCH₃)₆]] [CB₁₁H₆Br₆]₂ were grown from the reaction mixture in acetonitrile at ambient temperature under nitrogen by slow evaporation over a period of 3 weeks.

Computing details top

Data collection: SMART (Bruker, 2000); cell refinement: SAINT (Bruker, 2007); data reduction: SAINT (Bruker, 2007); program(s) used to solve structure: SHELXTL (Sheldrick, 2008); program(s) used to refine structure: SHELXTL (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008) and publCIF (Westrip, 2010).

Figures top

Fig. 1. Molecular structure of (I)with atom numbering scheme. The thermal ellipsoids are shown at 50% probability level.

Hexakis(acetonitrile-κN)ruthenium(II) bis(hexabromocarbadodecaborate) acetonitrile solvate top

Crystal data top

[Ru(C₂H₃N)₆](CH₆B₁₁Br₆)₂·C₂H₃N	F(000) = 3008
M_r = 1621.30	D_x = 2.119 Mg m⁻³
Orthorhombic, Pna2₁	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2c -2n	Cell parameters from 999 reflections
a = 21.332 (2) Å	θ = 1.9–29.3°
b = 11.7577 (10) Å	µ = 9.77 mm⁻¹
c = 20.2620 (17) Å	T = 173 K
V = 5082.1 (8) Å³	Block, red
Z = 4	0.20 × 0.15 × 0.10 mm

Data collection top

Bruker CCD-1000 area-detector diffractometer	13481 independent reflections
Radiation source: fine-focus sealed tube	10985 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.042
0.30° ω and 0.4 ° ϕ scans	θ_max = 29.3°, θ_min = 1.9°
Absorption correction: multi-scan (SADABS; Bruker, 2007)	h = −29→28
T_min = 0.245, T_max = 0.442	k = −16→15
36328 measured reflections	l = −27→27

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.033	H-atom parameters constrained
wR(F²) = 0.062	w = 1/[σ²(F_o²) + (0.002P)²] where P = (F_o² + 2F_c²)/3
S = 0.97	(Δ/σ)_max = 0.001
13481 reflections	Δρ_max = 0.83 e Å⁻³
531 parameters	Δρ_min = −0.73 e Å⁻³
1 restraint	Absolute structure: Flack (1983), 6319 Friedel pairs
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: 0.000 (5)

Crystal data top

[Ru(C₂H₃N)₆](CH₆B₁₁Br₆)₂·C₂H₃N	V = 5082.1 (8) Å³
M_r = 1621.30	Z = 4
Orthorhombic, Pna2₁	Mo Kα radiation
a = 21.332 (2) Å	µ = 9.77 mm⁻¹
b = 11.7577 (10) Å	T = 173 K
c = 20.2620 (17) Å	0.20 × 0.15 × 0.10 mm

Data collection top

Bruker CCD-1000 area-detector diffractometer	13481 independent reflections
Absorption correction: multi-scan (SADABS; Bruker, 2007)	10985 reflections with I > 2σ(I)
T_min = 0.245, T_max = 0.442	R_int = 0.042
36328 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.033	H-atom parameters constrained
wR(F²) = 0.062	Δρ_max = 0.83 e Å⁻³
S = 0.97	Δρ_min = −0.73 e Å⁻³
13481 reflections	Absolute structure: Flack (1983), 6319 Friedel pairs
531 parameters	Absolute structure parameter: 0.000 (5)
1 restraint

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 > 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.

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

	x	y	z	U_iso*/U_eq
Ru1	0.399141 (18)	0.77943 (3)	0.705666 (18)	0.02190 (8)
N1	0.3418 (2)	0.8915 (3)	0.75141 (19)	0.0252 (9)
N2	0.3486 (2)	0.6518 (3)	0.74612 (18)	0.0232 (9)
N3	0.4578 (2)	0.7767 (3)	0.7844 (2)	0.0289 (9)
N4	0.4530 (2)	0.6611 (3)	0.66043 (19)	0.0245 (9)
N5	0.4493 (2)	0.9056 (3)	0.66337 (19)	0.0261 (9)
N6	0.34097 (19)	0.7832 (3)	0.62615 (19)	0.0229 (8)
C1	0.3052 (3)	0.9451 (4)	0.7782 (2)	0.0264 (11)
C2	0.2595 (3)	1.0150 (4)	0.8113 (3)	0.0371 (13)
H2C	0.2802	1.0603	0.8455	0.056*
H2B	0.2276	0.9663	0.8317	0.056*
H2A	0.2395	1.0659	0.7793	0.056*
C3	0.3216 (2)	0.5780 (4)	0.7671 (2)	0.0271 (11)
C4	0.2864 (3)	0.4804 (4)	0.7934 (3)	0.0355 (13)
H4C	0.3127	0.4390	0.8250	0.053*
H4A	0.2747	0.4297	0.7570	0.053*
H4B	0.2485	0.5076	0.8156	0.053*
C5	0.4903 (2)	0.7721 (4)	0.8281 (2)	0.0256 (10)
C6	0.5326 (3)	0.7672 (4)	0.8846 (2)	0.0354 (12)
H6B	0.5756	0.7821	0.8699	0.053*
H6A	0.5304	0.6915	0.9047	0.053*
H6C	0.5202	0.8246	0.9171	0.053*
C7	0.4787 (2)	0.5888 (4)	0.6358 (2)	0.0261 (10)
C8	0.5105 (3)	0.4935 (4)	0.6042 (3)	0.0370 (13)
H8C	0.5355	0.4524	0.6370	0.055*
H8B	0.5382	0.5222	0.5693	0.055*
H8A	0.4794	0.4420	0.5849	0.055*
C9	0.4757 (2)	0.9733 (4)	0.6354 (3)	0.0299 (11)
C10	0.5104 (3)	1.0596 (4)	0.5984 (3)	0.0435 (15)
H10B	0.4837	1.1264	0.5917	0.065*
H10A	0.5229	1.0285	0.5555	0.065*
H10C	0.5479	1.0817	0.6233	0.065*
C11	0.3105 (2)	0.7833 (4)	0.5804 (2)	0.0256 (11)
C12	0.2710 (3)	0.7818 (4)	0.5225 (2)	0.0324 (12)
H12A	0.2539	0.7052	0.5163	0.049*
H12B	0.2958	0.8032	0.4838	0.049*
H12C	0.2365	0.8360	0.5282	0.049*
Br1	0.09098 (2)	0.22557 (4)	0.51235 (3)	0.02750 (11)
Br2	0.17891 (3)	0.50024 (3)	0.48909 (2)	0.02850 (11)
Br3	0.32771 (2)	0.48584 (3)	0.59669 (2)	0.02548 (10)
Br4	0.33173 (3)	0.19992 (4)	0.68133 (3)	0.03209 (12)
Br5	0.18567 (3)	0.03424 (4)	0.63167 (3)	0.03231 (12)
Br6	0.17687 (2)	0.35779 (4)	0.65791 (2)	0.02565 (10)
C0AA	0.2963 (2)	0.1822 (4)	0.4613 (2)	0.0220 (10)
H0A	0.3221	0.1438	0.4186	0.026*
B1	0.1813 (2)	0.2282 (4)	0.5161 (3)	0.0195 (10)
B2	0.2239 (2)	0.3581 (4)	0.5052 (2)	0.0191 (10)
B3	0.2923 (2)	0.3521 (4)	0.5546 (2)	0.0180 (10)
B4	0.2940 (2)	0.2181 (4)	0.5941 (3)	0.0197 (10)
B5	0.2248 (3)	0.1416 (4)	0.5710 (2)	0.0188 (10)
B6	0.2212 (2)	0.2911 (4)	0.5838 (2)	0.0147 (10)
B7	0.2284 (3)	0.2502 (4)	0.4441 (3)	0.0229 (12)
H7	0.2077	0.2598	0.3937	0.028*
B8	0.2965 (3)	0.3270 (4)	0.4675 (3)	0.0233 (11)
H8	0.3204	0.3869	0.4327	0.028*
B9	0.3402 (3)	0.2401 (4)	0.5234 (3)	0.0225 (11)
H9	0.3926	0.2433	0.5250	0.027*
B10	0.2980 (3)	0.1107 (4)	0.5337 (3)	0.0232 (11)
H10	0.3232	0.0283	0.5422	0.028*
B11	0.2287 (3)	0.1170 (4)	0.4860 (3)	0.0218 (11)
H11	0.2080	0.0389	0.4630	0.026*
Br7	0.32987 (2)	0.77287 (4)	0.33363 (2)	0.02870 (11)
Br8	0.42000 (3)	0.93866 (4)	0.46079 (3)	0.03373 (12)
Br9	0.56818 (3)	0.76830 (4)	0.50431 (3)	0.03494 (12)
Br10	0.56984 (2)	0.50141 (4)	0.39952 (3)	0.02875 (11)
Br11	0.42319 (3)	0.49971 (4)	0.29036 (3)	0.03068 (11)
Br12	0.41484 (2)	0.61228 (4)	0.46759 (2)	0.02423 (10)
C1AA	0.5353 (3)	0.8272 (4)	0.2853 (2)	0.0291 (11)
H1A	0.5610	0.8742	0.2455	0.035*
B13	0.4202 (3)	0.7666 (4)	0.3357 (3)	0.0220 (11)
B14	0.4631 (3)	0.8445 (4)	0.3960 (3)	0.0246 (12)
B15	0.5318 (3)	0.7669 (4)	0.4164 (3)	0.0235 (11)
B16	0.5325 (3)	0.6418 (4)	0.3670 (2)	0.0195 (11)
B17	0.4641 (3)	0.6413 (4)	0.3173 (2)	0.0212 (11)
B18	0.4606 (2)	0.6923 (4)	0.4001 (2)	0.0170 (10)
B19	0.4671 (3)	0.8845 (4)	0.3124 (3)	0.0263 (12)
H19	0.4458	0.9654	0.2937	0.032*
B20	0.5362 (3)	0.8849 (5)	0.3618 (3)	0.0286 (13)
H20	0.5607	0.9658	0.3756	0.034*
B21	0.5796 (3)	0.7595 (4)	0.3441 (3)	0.0277 (13)
H21	0.6321	0.7578	0.3462	0.033*
B22	0.5369 (3)	0.6817 (4)	0.2831 (3)	0.0252 (12)
H22	0.5615	0.6288	0.2452	0.030*
B23	0.4681 (3)	0.7597 (5)	0.2636 (3)	0.0277 (13)
H23	0.4479	0.7584	0.2126	0.033*
N1S	0.6665 (3)	0.8100 (6)	0.7904 (3)	0.083 (2)
C1S	0.6582 (4)	0.8053 (6)	0.7357 (4)	0.063 (2)
C2S	0.6476 (6)	0.8005 (6)	0.6695 (4)	0.126 (5)
H2SC	0.6778	0.8495	0.6466	0.189*
H2SB	0.6050	0.8266	0.6600	0.189*
H2SA	0.6526	0.7220	0.6542	0.189*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Ru1	0.0257 (2)	0.01802 (17)	0.02196 (19)	−0.00100 (15)	0.00163 (16)	−0.00001 (15)
N1	0.032 (3)	0.0193 (18)	0.024 (2)	0.0028 (17)	0.0022 (19)	0.0000 (16)
N2	0.030 (2)	0.0195 (18)	0.019 (2)	0.0012 (16)	0.0004 (17)	0.0005 (16)
N3	0.033 (3)	0.0214 (19)	0.033 (2)	−0.0021 (18)	0.002 (2)	−0.0021 (18)
N4	0.030 (2)	0.0212 (19)	0.022 (2)	0.0006 (17)	−0.0014 (18)	−0.0010 (16)
N5	0.031 (2)	0.0239 (19)	0.024 (2)	−0.0030 (17)	0.0016 (19)	−0.0023 (17)
N6	0.028 (2)	0.0170 (18)	0.023 (2)	0.0010 (15)	0.0021 (18)	0.0010 (16)
C1	0.036 (3)	0.021 (2)	0.021 (3)	0.002 (2)	0.004 (2)	0.0048 (19)
C2	0.039 (4)	0.046 (3)	0.026 (3)	0.010 (3)	0.005 (2)	0.001 (2)
C3	0.028 (3)	0.031 (3)	0.022 (3)	0.002 (2)	−0.006 (2)	−0.004 (2)
C4	0.044 (4)	0.029 (3)	0.034 (3)	−0.015 (2)	−0.006 (3)	0.005 (2)
C5	0.026 (3)	0.024 (2)	0.026 (3)	−0.005 (2)	0.004 (2)	−0.002 (2)
C6	0.033 (3)	0.044 (3)	0.029 (3)	−0.011 (2)	−0.005 (2)	−0.004 (2)
C7	0.026 (3)	0.028 (2)	0.024 (3)	−0.007 (2)	−0.006 (2)	0.003 (2)
C8	0.036 (3)	0.037 (3)	0.037 (3)	0.014 (2)	0.003 (3)	−0.004 (2)
C9	0.030 (3)	0.028 (2)	0.031 (3)	−0.008 (2)	−0.002 (2)	−0.007 (2)
C10	0.057 (4)	0.042 (3)	0.032 (3)	−0.023 (3)	0.008 (3)	−0.002 (3)
C11	0.032 (3)	0.019 (2)	0.026 (3)	−0.0016 (19)	0.005 (2)	0.0027 (19)
C12	0.037 (3)	0.027 (2)	0.033 (3)	−0.001 (2)	−0.008 (2)	0.004 (2)
Br1	0.0190 (2)	0.0286 (2)	0.0349 (3)	−0.00053 (19)	−0.0065 (2)	−0.0091 (2)
Br2	0.0357 (3)	0.0201 (2)	0.0297 (3)	0.00673 (19)	−0.0053 (2)	0.00434 (19)
Br3	0.0292 (3)	0.0224 (2)	0.0248 (2)	−0.01019 (18)	−0.0001 (2)	−0.00055 (19)
Br4	0.0332 (3)	0.0362 (3)	0.0269 (3)	−0.0033 (2)	−0.0145 (2)	0.0097 (2)
Br5	0.0342 (3)	0.0264 (2)	0.0362 (3)	−0.0099 (2)	−0.0006 (2)	0.0116 (2)
Br6	0.0253 (3)	0.0345 (2)	0.0171 (2)	−0.0024 (2)	0.0058 (2)	−0.00666 (19)
C0AA	0.026 (3)	0.024 (2)	0.017 (2)	0.0020 (19)	0.002 (2)	−0.0049 (18)
B1	0.017 (2)	0.018 (2)	0.023 (3)	0.001 (2)	−0.002 (2)	−0.005 (2)
B2	0.018 (3)	0.024 (2)	0.015 (3)	−0.0007 (19)	0.000 (2)	0.001 (2)
B3	0.017 (3)	0.019 (2)	0.019 (3)	−0.0014 (19)	0.002 (2)	0.0022 (19)
B4	0.017 (2)	0.017 (2)	0.025 (3)	−0.0018 (19)	−0.002 (2)	0.001 (2)
B5	0.019 (3)	0.018 (2)	0.020 (3)	0.001 (2)	−0.003 (2)	0.0040 (19)
B6	0.019 (3)	0.015 (2)	0.010 (2)	−0.0009 (18)	0.0012 (18)	0.0004 (18)
B7	0.025 (3)	0.026 (3)	0.018 (3)	0.001 (2)	−0.003 (2)	−0.0032 (19)
B8	0.025 (3)	0.026 (3)	0.019 (3)	0.004 (2)	0.000 (2)	0.000 (2)
B9	0.023 (3)	0.024 (3)	0.021 (3)	0.004 (2)	−0.002 (2)	0.000 (2)
B10	0.023 (3)	0.020 (2)	0.027 (3)	0.003 (2)	0.001 (2)	0.000 (2)
B11	0.021 (3)	0.020 (2)	0.025 (3)	0.001 (2)	0.000 (2)	−0.006 (2)
Br7	0.0210 (3)	0.0375 (3)	0.0276 (3)	0.0067 (2)	−0.0004 (2)	0.0066 (2)
Br8	0.0399 (3)	0.0236 (2)	0.0376 (3)	0.0011 (2)	0.0123 (2)	−0.0059 (2)
Br9	0.0384 (3)	0.0375 (3)	0.0290 (3)	−0.0131 (2)	−0.0098 (2)	0.0016 (2)
Br10	0.0275 (3)	0.0234 (2)	0.0353 (3)	0.0061 (2)	−0.0020 (2)	0.00958 (19)
Br11	0.0340 (3)	0.0301 (2)	0.0279 (3)	0.0008 (2)	−0.0059 (2)	−0.0072 (2)
Br12	0.0267 (3)	0.0265 (2)	0.0195 (2)	−0.00456 (18)	0.0039 (2)	0.00747 (18)
C1AA	0.030 (3)	0.029 (2)	0.028 (3)	0.006 (2)	0.008 (2)	0.014 (2)
B13	0.024 (3)	0.030 (3)	0.012 (2)	0.003 (2)	0.004 (2)	0.004 (2)
B14	0.030 (3)	0.017 (2)	0.027 (3)	0.002 (2)	0.007 (2)	−0.002 (2)
B15	0.026 (3)	0.022 (2)	0.023 (3)	−0.003 (2)	−0.001 (2)	0.007 (2)
B16	0.022 (3)	0.023 (3)	0.013 (2)	0.004 (2)	0.002 (2)	0.011 (2)
B17	0.021 (3)	0.025 (3)	0.017 (3)	0.005 (2)	0.000 (2)	0.003 (2)
B18	0.017 (3)	0.021 (2)	0.013 (2)	−0.0002 (19)	0.002 (2)	0.0072 (19)
B19	0.024 (3)	0.024 (3)	0.032 (3)	0.005 (2)	0.007 (2)	0.017 (2)
B20	0.026 (3)	0.024 (3)	0.036 (3)	−0.006 (2)	0.009 (3)	0.002 (2)
B21	0.019 (3)	0.030 (3)	0.035 (3)	−0.002 (2)	0.007 (2)	0.010 (2)
B22	0.029 (3)	0.029 (3)	0.018 (3)	0.006 (2)	0.007 (2)	0.008 (2)
B23	0.025 (3)	0.036 (3)	0.022 (3)	0.008 (2)	0.007 (2)	0.013 (2)
N1S	0.069 (5)	0.136 (6)	0.044 (4)	−0.032 (4)	−0.001 (3)	0.016 (4)
C1S	0.067 (5)	0.067 (5)	0.053 (5)	0.000 (4)	0.000 (4)	0.016 (4)
C2S	0.236 (15)	0.059 (5)	0.083 (7)	0.032 (7)	−0.043 (8)	−0.017 (5)

Geometric parameters (Å, º) top

Ru1—N5	2.020 (4)	B4—B6	1.785 (7)
Ru1—N2	2.021 (4)	B4—B5	1.790 (7)
Ru1—N1	2.022 (4)	B5—B11	1.750 (7)
Ru1—N4	2.024 (4)	B5—B10	1.773 (7)
Ru1—N3	2.028 (4)	B5—B6	1.777 (6)
Ru1—N6	2.034 (4)	B7—B8	1.776 (8)
N1—C1	1.142 (6)	B7—B11	1.780 (7)
N2—C3	1.126 (6)	B7—H7	1.1200
N3—C5	1.127 (6)	B8—B9	1.786 (7)
N4—C7	1.127 (6)	B8—H8	1.1200
N5—C9	1.126 (6)	B9—B10	1.781 (7)
N6—C11	1.132 (6)	B9—H9	1.1200
C1—C2	1.441 (7)	B10—B11	1.768 (8)
C2—H2C	0.9800	B10—H10	1.1200
C2—H2B	0.9800	B11—H11	1.1200
C2—H2A	0.9800	Br7—B13	1.928 (6)
C3—C4	1.470 (7)	Br8—B14	1.948 (5)
C4—H4C	0.9800	Br9—B15	1.944 (5)
C4—H4A	0.9800	Br10—B16	1.947 (5)
C4—H4B	0.9800	Br11—B17	1.958 (5)
C5—C6	1.457 (7)	Br12—B18	1.926 (5)
C6—H6B	0.9800	C1AA—B20	1.694 (7)
C6—H6A	0.9800	C1AA—B19	1.695 (7)
C6—H6C	0.9800	C1AA—B23	1.696 (8)
C7—C8	1.459 (7)	C1AA—B22	1.712 (7)
C8—H8C	0.9800	C1AA—B21	1.717 (7)
C8—H8B	0.9800	C1AA—H1A	1.1200
C8—H8A	0.9800	B13—B19	1.774 (7)
C9—C10	1.463 (7)	B13—B14	1.780 (8)
C10—H10B	0.9800	B13—B17	1.785 (7)
C10—H10A	0.9800	B13—B23	1.787 (8)
C10—H10C	0.9800	B13—B18	1.791 (7)
C11—C12	1.445 (7)	B14—B19	1.759 (7)
C12—H12A	0.9800	B14—B20	1.773 (8)
C12—H12B	0.9800	B14—B15	1.776 (8)
C12—H12C	0.9800	B14—B18	1.792 (6)
Br1—B1	1.929 (5)	B15—B20	1.776 (7)
Br2—B2	1.955 (5)	B15—B16	1.778 (7)
Br3—B3	1.943 (5)	B15—B18	1.784 (7)
Br4—B4	1.954 (5)	B15—B21	1.786 (8)
Br5—B5	1.950 (5)	B16—B22	1.767 (7)
Br6—B6	1.940 (5)	B16—B21	1.772 (7)
C0AA—B7	1.690 (7)	B16—B17	1.773 (7)
C0AA—B10	1.693 (7)	B16—B18	1.776 (7)
C0AA—B8	1.707 (7)	B17—B22	1.765 (8)
C0AA—B11	1.707 (7)	B17—B23	1.770 (7)
C0AA—B9	1.710 (7)	B17—B18	1.782 (7)
C0AA—H0A	1.1200	B19—B23	1.770 (8)
B1—B11	1.761 (7)	B19—B20	1.782 (8)
B1—B5	1.770 (7)	B19—H19	1.1200
B1—B6	1.776 (7)	B20—B21	1.778 (8)
B1—B7	1.789 (7)	B20—H20	1.1200
B1—B2	1.790 (7)	B21—B22	1.788 (8)
B2—B8	1.765 (7)	B21—H21	1.1200
B2—B3	1.770 (7)	B22—B23	1.774 (8)
B2—B7	1.774 (7)	B22—H22	1.1200
B2—B6	1.779 (7)	B23—H23	1.1200
B3—B4	1.767 (7)	N1S—C1S	1.124 (9)
B3—B6	1.779 (7)	C1S—C2S	1.361 (10)
B3—B9	1.782 (7)	C2S—H2SC	0.9800
B3—B8	1.790 (7)	C2S—H2SB	0.9800
B4—B9	1.759 (7)	C2S—H2SA	0.9800
B4—B10	1.760 (7)

N5—Ru1—N2	178.82 (15)	B4—B10—B11	108.0 (4)
N5—Ru1—N1	92.08 (16)	C0AA—B10—B5	104.4 (4)
N2—Ru1—N1	88.58 (15)	B4—B10—B5	60.9 (3)
N5—Ru1—N4	90.67 (15)	B11—B10—B5	59.2 (3)
N2—Ru1—N4	88.65 (15)	C0AA—B10—B9	58.9 (3)
N1—Ru1—N4	177.05 (16)	B4—B10—B9	59.5 (3)
N5—Ru1—N3	91.08 (16)	B11—B10—B9	108.8 (4)
N2—Ru1—N3	89.88 (16)	B5—B10—B9	108.6 (4)
N1—Ru1—N3	91.28 (16)	C0AA—B10—H10	125.0
N4—Ru1—N3	89.73 (16)	B4—B10—H10	122.5
N5—Ru1—N6	88.36 (15)	B11—B10—H10	121.4
N2—Ru1—N6	90.68 (15)	B5—B10—H10	122.3
N1—Ru1—N6	88.86 (16)	B9—B10—H10	121.0
N4—Ru1—N6	90.16 (15)	C0AA—B11—B5	104.8 (4)
N3—Ru1—N6	179.43 (17)	C0AA—B11—B1	104.7 (3)
C1—N1—Ru1	172.6 (4)	B5—B11—B1	60.6 (3)
C3—N2—Ru1	177.4 (4)	C0AA—B11—B10	58.3 (3)
C5—N3—Ru1	178.2 (4)	B5—B11—B10	60.5 (3)
C7—N4—Ru1	173.9 (4)	B1—B11—B10	108.8 (4)
C9—N5—Ru1	174.9 (4)	C0AA—B11—B7	57.9 (3)
C11—N6—Ru1	177.2 (4)	B5—B11—B7	108.8 (3)
N1—C1—C2	178.8 (5)	B1—B11—B7	60.7 (3)
C1—C2—H2C	109.5	B10—B11—B7	107.5 (4)
C1—C2—H2B	109.5	C0AA—B11—H11	125.4
H2C—C2—H2B	109.5	B5—B11—H11	121.7
C1—C2—H2A	109.5	B1—B11—H11	121.7
H2C—C2—H2A	109.5	B10—B11—H11	121.5
H2B—C2—H2A	109.5	B7—B11—H11	121.5
N2—C3—C4	178.9 (5)	B20—C1AA—B19	63.5 (3)
C3—C4—H4C	109.5	B20—C1AA—B23	115.8 (4)
C3—C4—H4A	109.5	B19—C1AA—B23	62.9 (3)
H4C—C4—H4A	109.5	B20—C1AA—B22	115.1 (4)
C3—C4—H4B	109.5	B19—C1AA—B22	115.0 (4)
H4C—C4—H4B	109.5	B23—C1AA—B22	62.8 (3)
H4A—C4—H4B	109.5	B20—C1AA—B21	62.8 (3)
N3—C5—C6	179.6 (6)	B19—C1AA—B21	115.5 (4)
C5—C6—H6B	109.5	B23—C1AA—B21	115.4 (4)
C5—C6—H6A	109.5	B22—C1AA—B21	62.8 (3)
H6B—C6—H6A	109.5	B20—C1AA—H1A	117.1
C5—C6—H6C	109.5	B19—C1AA—H1A	117.2
H6B—C6—H6C	109.5	B23—C1AA—H1A	117.2
H6A—C6—H6C	109.5	B22—C1AA—H1A	117.8
N4—C7—C8	178.6 (5)	B21—C1AA—H1A	117.3
C7—C8—H8C	109.5	B19—B13—B14	59.4 (3)
C7—C8—H8B	109.5	B19—B13—B17	107.0 (4)
H8C—C8—H8B	109.5	B14—B13—B17	107.3 (4)
C7—C8—H8A	109.5	B19—B13—B23	59.6 (3)
H8C—C8—H8A	109.5	B14—B13—B23	106.9 (4)
H8B—C8—H8A	109.5	B17—B13—B23	59.4 (3)
N5—C9—C10	179.0 (6)	B19—B13—B18	107.6 (4)
C9—C10—H10B	109.5	B14—B13—B18	60.2 (3)
C9—C10—H10A	109.5	B17—B13—B18	59.8 (3)
H10B—C10—H10A	109.5	B23—B13—B18	107.4 (4)
C9—C10—H10C	109.5	B19—B13—Br7	121.9 (3)
H10B—C10—H10C	109.5	B14—B13—Br7	120.6 (3)
H10A—C10—H10C	109.5	B17—B13—Br7	123.5 (3)
N6—C11—C12	179.0 (5)	B23—B13—Br7	123.8 (4)
C11—C12—H12A	109.5	B18—B13—Br7	121.1 (3)
C11—C12—H12B	109.5	B19—B14—B20	60.6 (3)
H12A—C12—H12B	109.5	B19—B14—B15	108.7 (4)
C11—C12—H12C	109.5	B20—B14—B15	60.1 (3)
H12A—C12—H12C	109.5	B19—B14—B13	60.2 (3)
H12B—C12—H12C	109.5	B20—B14—B13	108.8 (4)
B7—C0AA—B10	115.6 (4)	B15—B14—B13	108.6 (3)
B7—C0AA—B8	63.0 (3)	B19—B14—B18	108.2 (4)
B10—C0AA—B8	115.5 (3)	B20—B14—B18	108.1 (4)
B7—C0AA—B11	63.2 (3)	B15—B14—B18	60.0 (3)
B10—C0AA—B11	62.7 (3)	B13—B14—B18	60.2 (3)
B8—C0AA—B11	115.4 (4)	B19—B14—Br8	121.4 (3)
B7—C0AA—B9	115.6 (3)	B20—B14—Br8	121.8 (3)
B10—C0AA—B9	63.1 (3)	B15—B14—Br8	121.6 (4)
B8—C0AA—B9	63.0 (3)	B13—B14—Br8	120.9 (4)
B11—C0AA—B9	115.2 (4)	B18—B14—Br8	121.5 (3)
B7—C0AA—H0A	117.0	B14—B15—B20	59.9 (3)
B10—C0AA—H0A	117.3	B14—B15—B16	107.6 (4)
B8—C0AA—H0A	117.3	B20—B15—B16	107.2 (4)
B11—C0AA—H0A	117.5	B14—B15—B18	60.5 (3)
B9—C0AA—H0A	117.3	B20—B15—B18	108.3 (4)
B11—B1—B5	59.4 (3)	B16—B15—B18	59.8 (3)
B11—B1—B6	107.6 (4)	B14—B15—B21	107.8 (4)
B5—B1—B6	60.2 (3)	B20—B15—B21	59.9 (3)
B11—B1—B7	60.2 (3)	B16—B15—B21	59.6 (3)
B5—B1—B7	107.6 (4)	B18—B15—B21	108.1 (4)
B6—B1—B7	107.5 (3)	B14—B15—Br9	122.6 (3)
B11—B1—B2	107.4 (4)	B20—B15—Br9	122.8 (3)
B5—B1—B2	107.6 (4)	B16—B15—Br9	121.2 (3)
B6—B1—B2	59.8 (3)	B18—B15—Br9	120.9 (3)
B7—B1—B2	59.4 (3)	B21—B15—Br9	121.6 (4)
B11—B1—Br1	123.2 (3)	B22—B16—B21	60.7 (3)
B5—B1—Br1	122.6 (3)	B22—B16—B17	59.8 (3)
B6—B1—Br1	121.0 (3)	B21—B16—B17	108.7 (4)
B7—B1—Br1	122.1 (3)	B22—B16—B18	108.6 (4)
B2—B1—Br1	121.0 (3)	B21—B16—B18	109.1 (4)
B8—B2—B3	60.8 (3)	B17—B16—B18	60.3 (3)
B8—B2—B7	60.2 (3)	B22—B16—B15	108.8 (3)
B3—B2—B7	108.7 (4)	B21—B16—B15	60.4 (3)
B8—B2—B6	108.9 (4)	B17—B16—B15	108.3 (4)
B3—B2—B6	60.2 (3)	B18—B16—B15	60.3 (3)
B7—B2—B6	108.0 (3)	B22—B16—Br10	121.9 (3)
B8—B2—B1	108.8 (3)	B21—B16—Br10	121.3 (3)
B3—B2—B1	108.3 (3)	B17—B16—Br10	121.7 (3)
B7—B2—B1	60.2 (3)	B18—B16—Br10	120.6 (3)
B6—B2—B1	59.7 (3)	B15—B16—Br10	121.0 (3)
B8—B2—Br2	122.4 (3)	B22—B17—B23	60.3 (3)
B3—B2—Br2	122.2 (3)	B22—B17—B16	59.9 (3)
B7—B2—Br2	121.5 (3)	B23—B17—B16	107.9 (4)
B6—B2—Br2	120.8 (3)	B22—B17—B18	108.4 (4)
B1—B2—Br2	120.1 (3)	B23—B17—B18	108.5 (4)
B4—B3—B2	108.0 (4)	B16—B17—B18	59.9 (3)
B4—B3—B6	60.5 (3)	B22—B17—B13	108.8 (4)
B2—B3—B6	60.2 (3)	B23—B17—B13	60.3 (3)
B4—B3—B9	59.4 (3)	B16—B17—B13	108.1 (4)
B2—B3—B9	107.6 (4)	B18—B17—B13	60.3 (3)
B6—B3—B9	108.0 (3)	B22—B17—Br11	120.7 (3)
B4—B3—B8	107.4 (3)	B23—B17—Br11	121.2 (3)
B2—B3—B8	59.4 (3)	B16—B17—Br11	121.9 (3)
B6—B3—B8	107.8 (4)	B18—B17—Br11	122.0 (3)
B9—B3—B8	60.0 (3)	B13—B17—Br11	121.7 (4)
B4—B3—Br3	120.9 (3)	B16—B18—B17	59.8 (3)
B2—B3—Br3	122.5 (3)	B16—B18—B15	59.9 (3)
B6—B3—Br3	120.8 (3)	B17—B18—B15	107.7 (4)
B9—B3—Br3	122.0 (3)	B16—B18—B13	107.7 (3)
B8—B3—Br3	123.1 (3)	B17—B18—B13	59.9 (3)
B9—B4—B10	60.8 (3)	B15—B18—B13	107.7 (3)
B9—B4—B3	60.7 (3)	B16—B18—B14	106.9 (4)
B10—B4—B3	109.0 (4)	B17—B18—B14	106.9 (3)
B9—B4—B6	108.8 (3)	B15—B18—B14	59.6 (3)
B10—B4—B6	107.9 (4)	B13—B18—B14	59.5 (3)
B3—B4—B6	60.1 (3)	B16—B18—Br12	122.8 (3)
B9—B4—B5	108.9 (4)	B17—B18—Br12	121.6 (3)
B10—B4—B5	59.9 (3)	B15—B18—Br12	122.7 (3)
B3—B4—B5	108.2 (4)	B13—B18—Br12	120.7 (3)
B6—B4—B5	59.6 (3)	B14—B18—Br12	122.4 (3)
B9—B4—Br4	121.5 (3)	C1AA—B19—B14	104.4 (4)
B10—B4—Br4	122.0 (3)	C1AA—B19—B23	58.6 (3)
B3—B4—Br4	121.1 (3)	B14—B19—B23	108.5 (4)
B6—B4—Br4	121.1 (3)	C1AA—B19—B13	105.1 (4)
B5—B4—Br4	121.4 (3)	B14—B19—B13	60.5 (3)
B11—B5—B1	60.0 (3)	B23—B19—B13	60.6 (3)
B11—B5—B10	60.3 (3)	C1AA—B19—B20	58.2 (3)
B1—B5—B10	108.2 (4)	B14—B19—B20	60.1 (3)
B11—B5—B6	108.0 (3)	B23—B19—B20	107.9 (4)
B1—B5—B6	60.1 (3)	B13—B19—B20	108.6 (4)
B10—B5—B6	107.7 (4)	C1AA—B19—H19	125.1
B11—B5—B4	107.5 (4)	B14—B19—H19	122.2
B1—B5—B4	107.9 (3)	B23—B19—H19	121.3
B10—B5—B4	59.2 (3)	B13—B19—H19	121.7
B6—B5—B4	60.1 (3)	B20—B19—H19	121.5
B11—B5—Br5	122.3 (3)	C1AA—B20—B14	103.9 (4)
B1—B5—Br5	123.0 (3)	C1AA—B20—B15	104.8 (4)
B10—B5—Br5	120.8 (3)	B14—B20—B15	60.1 (3)
B6—B5—Br5	122.0 (3)	C1AA—B20—B21	59.2 (3)
B4—B5—Br5	120.9 (3)	B14—B20—B21	108.4 (4)
B1—B6—B5	59.8 (3)	B15—B20—B21	60.4 (3)
B1—B6—B2	60.5 (3)	C1AA—B20—B19	58.3 (3)
B5—B6—B2	107.8 (3)	B14—B20—B19	59.3 (3)
B1—B6—B3	108.6 (3)	B15—B20—B19	107.6 (4)
B5—B6—B3	108.2 (3)	B21—B20—B19	108.3 (4)
B2—B6—B3	59.7 (3)	C1AA—B20—H20	125.0
B1—B6—B4	107.8 (3)	B14—B20—H20	122.8
B5—B6—B4	60.3 (3)	B15—B20—H20	122.3
B2—B6—B4	106.8 (3)	B21—B20—H20	120.8
B3—B6—B4	59.4 (3)	B19—B20—H20	121.8
B1—B6—Br6	122.2 (3)	C1AA—B21—B16	103.4 (4)
B5—B6—Br6	122.3 (3)	C1AA—B21—B20	57.9 (3)
B2—B6—Br6	122.0 (3)	B16—B21—B20	107.4 (4)
B3—B6—Br6	120.7 (3)	C1AA—B21—B15	103.4 (4)
B4—B6—Br6	121.9 (3)	B16—B21—B15	60.0 (3)
C0AA—B7—B2	104.0 (4)	B20—B21—B15	59.8 (3)
C0AA—B7—B8	59.0 (3)	C1AA—B21—B22	58.4 (3)
B2—B7—B8	59.6 (3)	B16—B21—B22	59.5 (3)
C0AA—B7—B11	58.9 (3)	B20—B21—B22	107.4 (4)
B2—B7—B11	107.3 (3)	B15—B21—B22	107.5 (4)
B8—B7—B11	108.5 (4)	C1AA—B21—H21	125.7
C0AA—B7—B1	104.2 (4)	B16—B21—H21	122.8
B2—B7—B1	60.3 (3)	B20—B21—H21	121.8
B8—B7—B1	108.4 (4)	B15—B21—H21	122.7
B11—B7—B1	59.1 (3)	B22—B21—H21	121.8
C0AA—B7—H7	125.0	C1AA—B22—B17	104.0 (4)
B2—B7—H7	122.8	C1AA—B22—B16	103.9 (4)
B8—B7—H7	121.0	B17—B22—B16	60.3 (3)
B11—B7—H7	121.7	C1AA—B22—B23	58.2 (3)
B1—B7—H7	122.5	B17—B22—B23	60.0 (3)
C0AA—B8—B2	103.7 (4)	B16—B22—B23	108.0 (4)
C0AA—B8—B7	58.0 (3)	C1AA—B22—B21	58.7 (3)
B2—B8—B7	60.1 (3)	B17—B22—B21	108.3 (4)
C0AA—B8—B9	58.6 (3)	B16—B22—B21	59.8 (3)
B2—B8—B9	107.6 (4)	B23—B22—B21	108.1 (4)
B7—B8—B9	107.8 (4)	C1AA—B22—H22	125.5
C0AA—B8—B3	103.8 (3)	B17—B22—H22	122.3
B2—B8—B3	59.7 (3)	B16—B22—H22	122.6
B7—B8—B3	107.8 (4)	B23—B22—H22	121.5
B9—B8—B3	59.8 (3)	B21—B22—H22	121.2
C0AA—B8—H8	125.6	C1AA—B23—B19	58.5 (3)
B2—B8—H8	122.7	C1AA—B23—B17	104.4 (4)
B7—B8—H8	121.5	B19—B23—B17	107.9 (4)
B9—B8—H8	121.5	C1AA—B23—B22	59.1 (3)
B3—B8—H8	122.7	B19—B23—B22	108.3 (4)
C0AA—B9—B4	103.5 (4)	B17—B23—B22	59.7 (3)
C0AA—B9—B10	58.0 (3)	C1AA—B23—B13	104.5 (4)
B4—B9—B10	59.7 (3)	B19—B23—B13	59.8 (3)
C0AA—B9—B3	103.9 (4)	B17—B23—B13	60.2 (3)
B4—B9—B3	59.9 (3)	B22—B23—B13	108.3 (4)
B10—B9—B3	107.4 (4)	C1AA—B23—H23	124.9
C0AA—B9—B8	58.4 (3)	B19—B23—H23	121.5
B4—B9—B8	107.9 (4)	B17—B23—H23	122.6
B10—B9—B8	107.5 (4)	B22—B23—H23	121.2
B3—B9—B8	60.2 (3)	B13—B23—H23	122.3
C0AA—B9—H9	125.6	N1S—C1S—C2S	179.4 (10)
B4—B9—H9	122.7	C1S—C2S—H2SC	109.5
B10—B9—H9	122.0	C1S—C2S—H2SB	109.5
B3—B9—H9	122.5	H2SC—C2S—H2SB	109.5
B8—B9—H9	121.4	C1S—C2S—H2SA	109.5
C0AA—B10—B4	104.2 (3)	H2SC—C2S—H2SA	109.5
C0AA—B10—B11	59.1 (3)	H2SB—C2S—H2SA	109.5

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
B10—H10···Br8ⁱ	1.12	2.85	3.612 (5)	125
C1AA—H1A···Br4ⁱⁱ	1.12	2.77	3.547 (5)	126

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

Experimental details

Crystal data
Chemical formula	[Ru(C₂H₃N)₆](CH₆B₁₁Br₆)₂·C₂H₃N
M_r	1621.30
Crystal system, space group	Orthorhombic, Pna2₁
Temperature (K)	173
a, b, c (Å)	21.332 (2), 11.7577 (10), 20.2620 (17)
V (Å³)	5082.1 (8)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	9.77
Crystal size (mm)	0.20 × 0.15 × 0.10

Data collection
Diffractometer	Bruker CCD-1000 area-detector diffractometer
Absorption correction	Multi-scan (SADABS; Bruker, 2007)
T_min, T_max	0.245, 0.442
No. of measured, independent and observed [I > 2σ(I)] reflections	36328, 13481, 10985
R_int	0.042
(sin θ/λ)_max (Å⁻¹)	0.689

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.033, 0.062, 0.97
No. of reflections	13481
No. of parameters	531
No. of restraints	1
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.83, −0.73
Absolute structure	Flack (1983), 6319 Friedel pairs
Absolute structure parameter	0.000 (5)

Computer programs: SMART (Bruker, 2000), SAINT (Bruker, 2007), SHELXTL (Sheldrick, 2008) and publCIF (Westrip, 2010).

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
B10—H10···Br8ⁱ	1.12	2.85	3.612 (5)	125.3
C1AA—H1A···Br4ⁱⁱ	1.12	2.77	3.547 (5)	125.9

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

Acknowledgements

We thank the National Science Foundation for financial support. Support of this research via the PRF 44692.01-GB award by the American Chemical Society and the Cottrell College Award CC6755 from Research Corporation is gratefully acknowledged. We are grateful to Dr Ilia A. Guzei (University of Wisconsin, Madison) for his help in the preparation of this submission.

References

Bergman, R. G. & Chang, J. (1987). J. Am. Chem. Soc. 109, 4298–4304. CrossRef Web of Science Google Scholar
Brookhart, M., Grant, B. & Volpe, A. F. Jr (1992). Organometallics, 11, 3920–3922. CrossRef CAS Web of Science Google Scholar
Bruker (2000). SMART. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Bruker (2007). SADABS and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Burns, R. M. & Hubbard, J. L. (1994). J. Am. Chem. Soc. 116, 9514–9520. CSD CrossRef CAS Web of Science Google Scholar
Flack, H. D. (1983). Acta Cryst. A39, 876–881. CrossRef CAS Web of Science IUCr Journals Google Scholar
Pearsal, M., Gembicky, M., Dominiak, P., Larsen, A. & Coppens, P. (2007). Acta Cryst. E63, m2596. 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
Stasko, D., Hoffmann, S. P., Kim, K.-C., Fackler, N. L. P., Larsen, A. S., Drovetskaya, T., Tham, F. S., Reed, C. A., Rickard, C. E. F. & Boyd, P. D. W. (2002). J. Am. Chem. Soc. 124, 13869–13876. Web of Science CSD CrossRef PubMed CAS Google Scholar
Westrip, S. P. (2010). publCIF. In preparation. 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.

CRYSTALLOGRAPHIC
COMMUNICATIONS

ISSN: 2056-9890

Volume 66| Part 3| March 2010| Pages m325-m326

doi:10.1107/S1600536810006252

Open

access

Format		BIBTeX
		EndNote
		RefMan
		Refer
		Medline
		CIF
		SGML
		Plain Text

Format		BIBTeX
		EndNote
		RefMan
		Refer
		Medline
		CIF
		SGML
		Plain Text

Search IUCr Journals		doi		Advanced search
Author		volume	page

metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

Hexa­kis­(aceto­nitrile-κN)ruthenium(II) bis­­(hexa­bromo­carbadodeca­borate) aceto­nitrile solvate

Related literature

Experimental

Crystal data

Data collection

Refinement

Supporting information

Acknowledgements

References

metal-organic compounds

Hexakis(acetonitrile-κN)ruthenium(II) bis(hexabromocarbadodecaborate) acetonitrile solvate