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ISSN: 2056-9890

Tetra-μ-acetato-κ8O:O′-bis­­[(3-cyano­pyridine-κN1)ruthenium(II,III)](RuRu) hexa­fluoridophosphate 1,2-di­chloro­ethane monosolvate

aDepartment of Chemistry, St Francis Xavier University, PO Box 5000, Antigonish, Nova Scotia, Canada B2G 2W5, and bDepartment of Chemistry, Queen's University, Kingston, Ontario, Canada K7L 3N6
*Correspondence e-mail: maquino@stfx.ca

(Received 14 September 2011; accepted 11 October 2011; online 22 October 2011)

The title compound, [Ru2(CH3CO2)4(C6H4N2)2]PF6·C2H4Cl2, was obtained via a rapid substitution reaction in 2-propanol whereby 3-cyano­pyridine replaces the axial water mol­ecules in the diaquatetra-μ-acetato-diruthenium(II,III) hexa­fluorido­phosphate starting material. The product rapidly precipated and crystals were grown from 1,2-dichloro­ethane. The 1,2-dichloro­ethane mol­ecule of solvation exhibits disorder with two different orientations [occupancy ratio 0.51 (6):0.49 (6)]. All three parts, the cation, the anion and the disordered solvent mol­ecule lie on crystallographic inversion centers. The Ru—Ru bond length of 2.2702 (6) Å fits nicely into the range seen for similar complexes and correlates well with the reduction potential of the complex and donor strength of the axial ligand, 3-cyano­pyridine, as postulated in a previous study [Vamvounis et al. (2000[Vamvounis, G., Caplan, J. F., Cameron, T. S., Robertson, K. N. & Aquino, M. A. S. (2000). Inorg. Chim. Acta, 305, 87-98.]). Inorg. Chim. Acta, 305, 87–98]. The 3-cyano­pyridine ligands orient themselves in an anti configuration with respect to each other and the Ru—Ru—N angle [174.27 (7)°] is close to being linear.

Related literature

For related structures and physical measurements, see: Vamvounis et al. (2000[Vamvounis, G., Caplan, J. F., Cameron, T. S., Robertson, K. N. & Aquino, M. A. S. (2000). Inorg. Chim. Acta, 305, 87-98.]).

[Scheme 1]

Experimental

Crystal data
  • [Ru2(C2H3O2)4(C6H4N2)2]PF6·C2H4Cl2

  • Mr = 890.46

  • Triclinic, [P \overline 1]

  • a = 8.1743 (6) Å

  • b = 10.3955 (10) Å

  • c = 11.397 (1) Å

  • α = 105.860 (6)°

  • β = 108.929 (5)°

  • γ = 104.099 (5)°

  • V = 820.38 (14) Å3

  • Z = 1

  • Mo Kα radiation

  • μ = 1.21 mm−1

  • T = 180 K

  • 0.20 × 0.20 × 0.15 mm

Data collection
  • Bruker APEXII CCD diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2010)[Bruker (2010). APEX2, SADABS and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.] Tmin = 0.793, Tmax = 0.839

  • 6133 measured reflections

  • 3175 independent reflections

  • 2784 reflections with I > 2σ(I)

  • Rint = 0.027

Refinement
  • R[F2 > 2σ(F2)] = 0.028

  • wR(F2) = 0.078

  • S = 1.09

  • 3175 reflections

  • 226 parameters

  • H-atom parameters constrained

  • Δρmax = 0.85 e Å−3

  • Δρmin = −0.76 e Å−3

Data collection: APEX2 (Bruker, 2010[Bruker (2010). APEX2, SADABS and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2010[Bruker (2010). APEX2, SADABS and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Supporting information


Comment top

A number of years ago our lab synthesized and structurally characterized a series of diruthenium(II,III) tetraacetate complexes with different axial donor ligands of varying donor strengths (Vamvounis et al., 2000). One reason to study these was to synthesize dimers with asymmetric bidendate axial donors that could act as bridges for mixed-metal metallopolymers and extended arrays (i.e. in the case of cyanopyridine adducts the pyridine end could be coordinated to a harder metal than the cyano end). The other reason was to correlate axial donor strength (as well as redox potential) with the Ru—Ru bond length. These ligands ranged from weak donors such as water and methanol to relatively strong donors such as dimethylformamide, dimethylsulfoxide and various pyridine derivatives. Unfortunately while we were able to structurally characterize the 4-cyanopyridine adduct in the earlier paper we were unable to obtain the 3-cyanopyridine adduct. This structure is now finally reported here.

The title compound (I) (Fig. 1) can be compared to the 4-cyanopyridine adduct reported previously (Vamvounis et al., 2000). The Ru—Ru bond lengths are 2.2702 (6) Å and 2.2741 (7) Å respectively which fits well into correlation of Ru—Ru bond length with axial ligand donor strength as outlined in the earlier paper. (i.e. the 3-cyanopyridine being the slightly weaker donor as measured electrochemically manifests a shorter Ru—Ru bond length structurally in the complex because less electron density is being donated into the metal-metal antibonding HOMO). The 3-cyanopyridine ligands are situated anti with respect to each other and the pyridine planes essentially bifurcate the planes formed by the perpendicular carboxylate groups (O—C—O), e.g. the O1—Ru1—N1—C5 torsion angle is -48.5 °.

Related literature top

For related structures and physical measurements, see: Vamvounis et al. (2000).

Experimental top

The method of preparation of the title compound (I) was similar to the method used by (Vamvounis et al., 2000) in preparing the earlier pyridine adducts of diruthenium(II,III) tetraacetate except that a 2.1:1 ligand to metal ratio was used instead of a 4:1 ratio. For example, [Ru2(µ-O2CCH3)4(H2O)2](PF6) (0.100 g, 0.161 mmol) was dissolved in 10 ml of 2-propanol. A 2.1-fold access of 3-cyanopyridine (0.037 g, 0.338 mmol) was added with stirring and a green precipitate formed immediately. The solution was stirred for another 5 minutes and the olive-green product collected via suction filtration, washed with 50 ml of 2-propanol and dried in vacuo. (Yield = 0.101 g, 79%). Crystals were grown by slow evaporation from 1,2-dichloroethane.

Refinement top

The structure was solved by direct methods. All non-hydrogen atoms were refined anisotropically. All H atoms were placed in geometrically calculated positions, with C—H = 0.95 (aromatic), 0.99(CH2) and 0.98 (methyl) Å, and refined as riding atoms, with Uiso(H) = 1.5 Ueq(C) (methyl), and 1.2 Ueq(other C). In addition, the methyl groups were refined with AFIX 137, which allowed the rotation of the methyl groups whilst keeping the C—H distances and X—C—H angles fixed. The solvent molecule C2H4Cl2 in the structure is disordered. It was split and refined into two parts with different orientations and with nearly equal occupancies.

Computing details top

Data collection: APEX2 (Bruker, 2010); cell refinement: SAINT (Bruker, 2010); data reduction: SAINT (Bruker, 2010); 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).

Figures top
[Figure 1] Fig. 1. The molecular structure of (I), with atom labels and 50% probability ellipsoids for the non-H atoms. Solvent molecule omitted for clarity. Symmetry operator A = -x + 1, -y + 1, -z + 1; B = -x, -y + 1, -z.
Tetra-µ-acetato-κ8O:O'-bis[(3-cyanopyridine- κN1)ruthenium(II,III)](RuRu) hexafluoridophosphate 1,2-dichloroethane monosolvate top
Crystal data top
[Ru2(C2H3O2)4(C6H4N2)2]PF6·C2H4Cl2Z = 1
Mr = 890.46F(000) = 439
Triclinic, P1Dx = 1.802 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 8.1743 (6) ÅCell parameters from 4068 reflections
b = 10.3955 (10) Åθ = 2.4–27.1°
c = 11.397 (1) ŵ = 1.21 mm1
α = 105.860 (6)°T = 180 K
β = 108.929 (5)°Block, brown
γ = 104.099 (5)°0.20 × 0.20 × 0.15 mm
V = 820.38 (14) Å3
Data collection top
Bruker APEXII CCD
diffractometer
3175 independent reflections
Radiation source: fine-focus sealed tube2784 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.027
ϕ and ω scansθmax = 26.0°, θmin = 2.1°
Absorption correction: multi-scan
(SADABS; Bruker, 2010)
h = 1010
Tmin = 0.793, Tmax = 0.839k = 1212
6133 measured reflectionsl = 1412
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.028Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.078H-atom parameters constrained
S = 1.09 w = 1/[σ2(Fo2) + (0.0226P)2 + 1.188P]
where P = (Fo2 + 2Fc2)/3
3175 reflections(Δ/σ)max < 0.001
226 parametersΔρmax = 0.85 e Å3
0 restraintsΔρmin = 0.76 e Å3
Crystal data top
[Ru2(C2H3O2)4(C6H4N2)2]PF6·C2H4Cl2γ = 104.099 (5)°
Mr = 890.46V = 820.38 (14) Å3
Triclinic, P1Z = 1
a = 8.1743 (6) ÅMo Kα radiation
b = 10.3955 (10) ŵ = 1.21 mm1
c = 11.397 (1) ÅT = 180 K
α = 105.860 (6)°0.20 × 0.20 × 0.15 mm
β = 108.929 (5)°
Data collection top
Bruker APEXII CCD
diffractometer
3175 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2010)
2784 reflections with I > 2σ(I)
Tmin = 0.793, Tmax = 0.839Rint = 0.027
6133 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0280 restraints
wR(F2) = 0.078H-atom parameters constrained
S = 1.09Δρmax = 0.85 e Å3
3175 reflectionsΔρmin = 0.76 e Å3
226 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 > 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
xyzUiso*/UeqOcc. (<1)
P10.00000.50000.00000.0346 (3)
Ru10.47865 (3)0.38173 (3)0.45928 (2)0.02328 (10)
O10.7543 (3)0.4309 (2)0.5531 (2)0.0269 (5)
O20.7964 (3)0.6638 (2)0.6343 (2)0.0270 (5)
O30.5095 (3)0.3989 (2)0.2954 (2)0.0271 (5)
O40.5481 (3)0.6314 (2)0.3736 (2)0.0270 (5)
N10.4058 (4)0.1379 (3)0.3754 (3)0.0256 (6)
N20.0128 (5)0.2151 (4)0.4373 (4)0.0600 (10)
C10.8583 (4)0.5624 (4)0.6211 (3)0.0274 (7)
C21.0631 (4)0.6004 (4)0.6875 (4)0.0359 (8)
H2A1.11260.67170.77920.054*
H2B1.12180.64050.63640.054*
H2C1.08930.51400.69060.054*
C30.5368 (4)0.5203 (4)0.2848 (3)0.0272 (7)
C40.5549 (5)0.5324 (4)0.1623 (4)0.0373 (8)
H4A0.66690.61460.18840.056*
H4B0.44570.54630.10730.056*
H4C0.56400.44430.11040.056*
C50.2756 (5)0.0610 (4)0.4029 (4)0.0345 (8)
H5A0.21300.10830.44630.041*
C60.2307 (4)0.0857 (4)0.3693 (4)0.0324 (7)
C70.3223 (5)0.1549 (4)0.3063 (4)0.0347 (8)
H7A0.29670.25470.28490.042*
C80.4511 (5)0.0752 (4)0.2759 (4)0.0391 (8)
H8A0.51400.11970.23070.047*
C90.4882 (5)0.0701 (4)0.3115 (4)0.0341 (8)
H9A0.57680.12390.28910.041*
C100.0933 (5)0.1605 (4)0.4058 (4)0.0411 (9)
F10.0541 (3)0.6132 (3)0.0917 (2)0.0518 (6)
F20.1696 (3)0.6283 (3)0.0146 (2)0.0474 (6)
F30.1334 (3)0.4879 (3)0.1314 (2)0.0485 (6)
Cl1A0.242 (4)0.032 (3)0.9565 (15)0.163 (4)0.51 (6)
C11A0.056 (5)0.077 (4)1.010 (4)0.108 (10)0.51 (6)
H11A0.10940.14571.10400.129*0.51 (6)
H11B0.01930.11420.94960.129*0.51 (6)
Cl1B0.191 (4)0.0453 (18)0.914 (4)0.152 (7)0.49 (6)
C11B0.013 (10)0.052 (7)0.969 (5)0.21 (3)0.49 (6)
H11C0.10200.12250.89120.246*0.49 (6)
H11D0.06630.09951.02770.246*0.49 (6)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
P10.0257 (6)0.0448 (8)0.0286 (7)0.0091 (6)0.0114 (5)0.0107 (6)
Ru10.02188 (14)0.02672 (16)0.02337 (15)0.00927 (11)0.01160 (11)0.00975 (11)
O10.0250 (11)0.0321 (13)0.0288 (12)0.0144 (10)0.0142 (10)0.0121 (10)
O20.0245 (11)0.0280 (12)0.0279 (12)0.0087 (9)0.0122 (9)0.0093 (10)
O30.0275 (11)0.0353 (13)0.0221 (11)0.0143 (10)0.0128 (9)0.0108 (10)
O40.0256 (11)0.0331 (13)0.0282 (12)0.0126 (10)0.0137 (10)0.0157 (10)
N10.0284 (14)0.0222 (13)0.0245 (14)0.0091 (11)0.0094 (11)0.0086 (11)
N20.056 (2)0.047 (2)0.086 (3)0.0132 (18)0.044 (2)0.027 (2)
C10.0251 (16)0.0387 (19)0.0245 (16)0.0123 (15)0.0148 (13)0.0150 (15)
C20.0217 (16)0.044 (2)0.039 (2)0.0108 (15)0.0114 (15)0.0139 (17)
C30.0192 (15)0.0380 (19)0.0258 (16)0.0125 (14)0.0101 (13)0.0117 (15)
C40.0389 (19)0.055 (2)0.0297 (19)0.0225 (18)0.0203 (16)0.0222 (18)
C50.0313 (18)0.0354 (19)0.037 (2)0.0124 (15)0.0161 (16)0.0123 (16)
C60.0256 (16)0.0301 (18)0.0351 (19)0.0069 (14)0.0086 (15)0.0111 (15)
C70.0350 (19)0.0246 (17)0.0357 (19)0.0116 (15)0.0093 (15)0.0049 (15)
C80.041 (2)0.036 (2)0.042 (2)0.0174 (17)0.0242 (18)0.0055 (17)
C90.0359 (19)0.0325 (19)0.0364 (19)0.0144 (15)0.0200 (16)0.0094 (16)
C100.035 (2)0.033 (2)0.052 (2)0.0089 (16)0.0180 (18)0.0144 (18)
F10.0460 (13)0.0548 (15)0.0486 (14)0.0190 (11)0.0235 (11)0.0064 (12)
F20.0361 (12)0.0529 (14)0.0419 (13)0.0030 (10)0.0152 (10)0.0151 (11)
F30.0350 (12)0.0666 (16)0.0383 (13)0.0138 (11)0.0092 (10)0.0239 (12)
Cl1A0.185 (10)0.204 (9)0.091 (6)0.089 (8)0.039 (6)0.050 (5)
C11A0.15 (2)0.068 (16)0.075 (12)0.049 (13)0.014 (13)0.018 (11)
Cl1B0.132 (9)0.179 (7)0.158 (15)0.066 (6)0.068 (9)0.067 (8)
C11B0.20 (5)0.18 (5)0.11 (3)0.06 (4)0.00 (3)0.03 (2)
Geometric parameters (Å, º) top
P1—F1i1.598 (2)C2—H2B0.9800
P1—F11.598 (2)C2—H2C0.9800
P1—F21.599 (2)C3—C41.485 (4)
P1—F2i1.599 (2)C4—H4A0.9800
P1—F31.600 (2)C4—H4B0.9800
P1—F3i1.600 (2)C4—H4C0.9800
Ru1—O32.012 (2)C5—C61.387 (5)
Ru1—O12.015 (2)C5—H5A0.9500
Ru1—O2ii2.016 (2)C6—C71.387 (5)
Ru1—O4ii2.023 (2)C6—C101.447 (5)
Ru1—Ru1ii2.2702 (6)C7—C81.373 (5)
Ru1—N12.295 (3)C7—H7A0.9500
O1—C11.273 (4)C8—C91.378 (5)
O2—C11.270 (4)C8—H8A0.9500
O2—Ru1ii2.016 (2)C9—H9A0.9500
O3—C31.273 (4)Cl1A—C11A1.93 (4)
O4—C31.272 (4)C11A—C11Aiii1.56 (7)
O4—Ru1ii2.023 (2)C11A—H11A0.9900
N1—C91.323 (4)C11A—H11B0.9900
N1—C51.345 (4)Cl1B—C11B1.93 (8)
N2—C101.130 (5)C11B—C11Biii1.22 (11)
C1—C21.491 (4)C11B—H11C0.9900
C2—H2A0.9800C11B—H11D0.9900
F1i—P1—F1180.00 (16)H2A—C2—H2B109.5
F1i—P1—F289.90 (12)C1—C2—H2C109.5
F1—P1—F290.10 (12)H2A—C2—H2C109.5
F1i—P1—F2i90.11 (12)H2B—C2—H2C109.5
F1—P1—F2i89.89 (12)O4—C3—O3123.1 (3)
F2—P1—F2i180.0O4—C3—C4118.5 (3)
F1i—P1—F390.18 (13)O3—C3—C4118.5 (3)
F1—P1—F389.82 (13)C3—C4—H4A109.5
F2—P1—F389.81 (12)C3—C4—H4B109.5
F2i—P1—F390.19 (12)H4A—C4—H4B109.5
F1i—P1—F3i89.82 (13)C3—C4—H4C109.5
F1—P1—F3i90.18 (13)H4A—C4—H4C109.5
F2—P1—F3i90.19 (12)H4B—C4—H4C109.5
F2i—P1—F3i89.81 (12)N1—C5—C6121.5 (3)
F3—P1—F3i180.0N1—C5—H5A119.3
O3—Ru1—O189.72 (9)C6—C5—H5A119.3
O3—Ru1—O2ii89.97 (9)C7—C6—C5119.4 (3)
O1—Ru1—O2ii178.99 (9)C7—C6—C10122.2 (3)
O3—Ru1—O4ii178.79 (9)C5—C6—C10118.4 (3)
O1—Ru1—O4ii89.53 (9)C8—C7—C6118.1 (3)
O2ii—Ru1—O4ii90.77 (8)C8—C7—H7A120.9
O3—Ru1—Ru1ii90.35 (7)C6—C7—H7A120.9
O1—Ru1—Ru1ii90.07 (7)C7—C8—C9119.4 (3)
O2ii—Ru1—Ru1ii88.97 (6)C7—C8—H8A120.3
O4ii—Ru1—Ru1ii88.71 (7)C9—C8—H8A120.3
O3—Ru1—N192.05 (9)N1—C9—C8122.8 (3)
O1—Ru1—N195.14 (9)N1—C9—H9A118.6
O2ii—Ru1—N185.83 (9)C8—C9—H9A118.6
O4ii—Ru1—N188.95 (9)N2—C10—C6177.9 (4)
Ru1ii—Ru1—N1174.27 (7)C11Aiii—C11A—Cl1A97 (3)
C1—O1—Ru1118.3 (2)C11Aiii—C11A—H11A112.3
C1—O2—Ru1ii119.4 (2)Cl1A—C11A—H11A112.3
C3—O3—Ru1118.4 (2)C11Aiii—C11A—H11B112.3
C3—O4—Ru1ii119.5 (2)Cl1A—C11A—H11B112.3
C9—N1—C5118.7 (3)H11A—C11A—H11B109.9
C9—N1—Ru1125.8 (2)C11Biii—C11B—Cl1B99 (9)
C5—N1—Ru1115.4 (2)C11Biii—C11B—H11C111.9
O2—C1—O1123.2 (3)Cl1B—C11B—H11C111.9
O2—C1—C2118.0 (3)C11Biii—C11B—H11D111.9
O1—C1—C2118.8 (3)Cl1B—C11B—H11D111.9
C1—C2—H2A109.5H11C—C11B—H11D109.6
C1—C2—H2B109.5
O3—Ru1—O1—C190.1 (2)Ru1ii—O2—C1—C2177.8 (2)
O4ii—Ru1—O1—C188.9 (2)Ru1—O1—C1—O21.0 (4)
Ru1ii—Ru1—O1—C10.2 (2)Ru1—O1—C1—C2178.2 (2)
N1—Ru1—O1—C1177.8 (2)Ru1ii—O4—C3—O30.1 (4)
O1—Ru1—O3—C391.2 (2)Ru1ii—O4—C3—C4179.3 (2)
O2ii—Ru1—O3—C387.8 (2)Ru1—O3—C3—O41.0 (4)
Ru1ii—Ru1—O3—C31.2 (2)Ru1—O3—C3—C4178.5 (2)
N1—Ru1—O3—C3173.6 (2)C9—N1—C5—C61.9 (5)
O3—Ru1—N1—C941.4 (3)Ru1—N1—C5—C6173.9 (3)
O1—Ru1—N1—C948.5 (3)N1—C5—C6—C70.2 (5)
O2ii—Ru1—N1—C9131.3 (3)N1—C5—C6—C10178.1 (3)
O4ii—Ru1—N1—C9137.9 (3)C5—C6—C7—C82.0 (5)
O3—Ru1—N1—C5143.1 (2)C10—C6—C7—C8179.8 (4)
O1—Ru1—N1—C5127.0 (2)C6—C7—C8—C91.6 (5)
O2ii—Ru1—N1—C553.3 (2)C5—N1—C9—C82.3 (5)
O4ii—Ru1—N1—C537.6 (2)Ru1—N1—C9—C8173.0 (3)
Ru1ii—O2—C1—O11.4 (4)C7—C8—C9—N10.5 (6)
Symmetry codes: (i) x, y+1, z; (ii) x+1, y+1, z+1; (iii) x, y, z+2.

Experimental details

Crystal data
Chemical formula[Ru2(C2H3O2)4(C6H4N2)2]PF6·C2H4Cl2
Mr890.46
Crystal system, space groupTriclinic, P1
Temperature (K)180
a, b, c (Å)8.1743 (6), 10.3955 (10), 11.397 (1)
α, β, γ (°)105.860 (6), 108.929 (5), 104.099 (5)
V3)820.38 (14)
Z1
Radiation typeMo Kα
µ (mm1)1.21
Crystal size (mm)0.20 × 0.20 × 0.15
Data collection
DiffractometerBruker APEXII CCD
diffractometer
Absorption correctionMulti-scan
(SADABS; Bruker, 2010)
Tmin, Tmax0.793, 0.839
No. of measured, independent and
observed [I > 2σ(I)] reflections
6133, 3175, 2784
Rint0.027
(sin θ/λ)max1)0.617
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.028, 0.078, 1.09
No. of reflections3175
No. of parameters226
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.85, 0.76

Computer programs: APEX2 (Bruker, 2010), SAINT (Bruker, 2010), SHELXTL (Sheldrick, 2008).

 

Acknowledgements

The authors thank the NSERC (Canada) for financial support.

References

First citationBruker (2010). APEX2, SADABS and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.  Google Scholar
First citationSheldrick, G. M. (2008). Acta Cryst. A64, 112–122.  Web of Science CrossRef CAS IUCr Journals Google Scholar
First citationVamvounis, G., Caplan, J. F., Cameron, T. S., Robertson, K. N. & Aquino, M. A. S. (2000). Inorg. Chim. Acta, 305, 87–98.  Web of Science CSD CrossRef Google Scholar

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