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The title compound, [Co2(C2H4NO)2(OH)2(C5H5N)4](ClO4)2·2C2H3N, consists of two octa­hedral CoIII centers arranged around an inversion point in which two cis hydroxide and two trans acetyl­amidate ligands link the two centers together, forming a dimeric cationic complex. Each CoIII center has two cis pyridine ligands which coordinate in the same plane as the cis hydroxide ligands. Two acetonitrile solvent mol­ecules and two perchlorate anions are hydrogen bonded to the H atoms on the bridging hydroxide and acetyl­amidate (N atom) ligands, respectively.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270112031964/fg3263sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270112031964/fg3263Isup2.hkl
Contains datablock I

CCDC reference: 899062

Comment top

In the process of studying cobalt phosphinate compounds, we isolated and crystallized di-µ-acetylamido-di-µ-hydroxido-bis[dipyridinecobalt(III)] bis(perchlorate) acetonitrile disolvate, (I). Related dihydroxide- and acetate-bridged cobalt(III) dimers were first produced by Werner (1910) and later characterized crystallographically by Mandel et al. (1977). These types of compounds have been studied as model metal centers for different enzymes. Lee et al. (2002) stabilized the dimeric core using sterically hindered carbocyclic acid derivatives to study the active site in metallohydrolases. Williams et al. (1999) used 1,4,7-triazacyclononane to stabilize a related cobalt dimer in order to study the hydrolyses of phosphate esters in metallophosphatase enzymes. The fact that (I) has bridging acetylamidate ligands is significant since relatively few transition metal compounds containing this ligand have been structurally characterized. Fedotova et al. (2008) synthesized a platinum(II) dimer with acetylamidate ligands, Chavan et al. (1986) used acetamide to make rhodium(II) dimers, Mironov (1999) stabilized rhenium chalcolgen clusters with acetylamidate ligands and Fuma & Ebihara (2006) used acetamide to make dirhodium paddle-wheel units that were bridged by perrhenate.

Two formula units of (I) constitute the unit cell, with the asymmetric unit consisting of half a complex cation lying about an inversion center, one perchlorate anion and one acetonitrile solvent molecule, both linked to the half cation by hydrogen bonds. The two CoIII centers are bridged by two trans-acetylamidate, through one O from one acetylamidate and one N from the other, and two cis-hydroxide ligands (Fig. 1). The Co1—O2 bond length is 1.9374 (12) Å, whereas that for Co1—N1 is 1.9059 (14) Å. The O2—Co—N1 angle is bent towards the adjacent CoIII center away from ideality, 180 to 169.26 (6)°. Interestingly, the C—O bond length [C11—O2 = 1.2973 (19) Å] is shorter than N—C [C11—N1 = 1.313 (2) Å] on the acetylamidate ligands. There are two pyridine molecules coordinated cis to each CoIII center in the same plane as the hydroxide ligands with pyridine torsion angles of 47.0 (1) and 45.8 (1)° for the N2 and N3 pyridine (py) ligands, respectively, against the metal–hydroxide plane. The two Npy—Co bond lengths are 1.9418 (14) and 1.9374 (12) Å for Co1—N2 and Co1—N3, respectively, and the N2—Co1—N3 angle is slightly larger than 90° at 94.08 (6)°. The Co1—O1 and Co1—O1i bond lengths are 1.8777 (12) Å and the O1—Co—O1i angle is 88.73 (5)° [symmetry code: (i) -x+1, -y+1, -z+1]; thus, this bridging arrangement constitutes a crystallographically imposed planar but slightly distorted square geometry.

The Co···Co distance in the dimer is 2.6847 (4) Å and is longer than the equivalent Co···Co distance in three other complexes containing the [Co2(OH)2(O2CCR)2]4+ core as evident in a search of the Cambridge Structural Database (CSD, Version 5.33 [OK?]; Allen, 2002): (i) 2.655 (2) ° in a tetrahydrofuran solvate of [Co2(OH)2(O2CR)2L4]2+ (R = tBu and L = 3,5-dimethylpyrazole) (Denisova et al., 2003), (ii) 2.669 (2) Å in the analogous benzene solvate (Denisova et al., 2006) and (iii) 2.6802 (5) Å in [Co2(OH)2(O2CR)2L2L'2]2+ (κ2-O2CR = κ1-L = 2,6-di-p-tolylbenzoate and L' = pyridine; Lee et al., 2002).

The unique perchlorate anion is hydrogen bonded to the H atom of the acetylamidate ligand and the unique acetonitrile ligand is hydrogen bonded to the bridging hydroxide H atoms (Fig. 1 and Table 1).

Related literature top

For related literature, see: Allen (2002); Chavan et al. (1986); Denisova et al. (2003, 2006); Fedotova et al. (2008); Fuma & Ebihara (2006); Lee et al. (2002); Mandel et al. (1977); Mironov (1999); Werner (1910); Williams et al. (1999).

Experimental top

Co(ClO4)2.6H2O (0.203 g) and pyridine (0.5 ml) were dissolved in acetonitrile (15 ml) and heated to 333 K. To this solution was added dropwise 30% by weight H2O2 (0.6 ml) which resulted in a change in color of the solution from pink to dark red. The resulting solution was heated under reflux for 1 h, allowed to cool to room temperature and diethyl ether added until the solution became cloudy. After 1 d, large, red, needle-shaped crystals (yield 0.073 g, 33.6%) were obtained.

Refinement top

Two H atoms involved in hydrogen bonding were refined freely. The other H atoms were placed at calculated positions, with C—H = 0.95 (aromatic) or 0.98 Å (methyl) and refined using a riding model, with Uiso(H) = 1.5Ueq(C) for methyl groups and 1.2Ueq(C) otherwise.

Computing details top

Data collection: SAINT [or APEX2?] (Bruker, 2009); cell refinement: SAINT (Bruker, 2009); data reduction: SORTAV (Blessing, 1995); program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999) and publCIF (Westrip, 2010).

Figures top
[Figure 1] Fig. 1. The molecular structure of (I), with hydrogen bonds illustrated with dashed lines. H atoms are represented by spheres of arbitrary radii and displacement ellipsoids are drawn at the 30% probability level. [Symmetry code: (i) -x+1, -y+1, -z+1.]
di-µ-acetylamido-κ2O:N;κ2N:O- di-µ-hydroxido-κ4O:O-bis[bis(pyridine-κN)cobalt(III)] bis(perchlorate) acetonitrile disolvate top
Crystal data top
[Co2(C2H4NO)2(OH)2(C5H5N)4](ClO4)2·2C2H3NF(000) = 888
Mr = 865.41Dx = 1.602 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 4635 reflections
a = 10.6198 (7) Åθ = 2.3–29.2°
b = 10.2440 (7) ŵ = 1.15 mm1
c = 16.503 (1) ÅT = 100 K
β = 92.167 (1)°Prism, red
V = 1794.1 (2) Å30.46 × 0.22 × 0.17 mm
Z = 2
Data collection top
Bruker APEXII CCD
diffractometer
5809 independent reflections
Radiation source: sealed x-ray tube4796 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.037
ϕ or ω oscillation scansθmax = 31.9°, θmin = 2.3°
Absorption correction: multi-scan
(SADABS; Bruker, 2008)
h = 1515
Tmin = 0.652, Tmax = 0.746k = 1515
21140 measured reflectionsl = 2424
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)] = 0.037Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.085H atoms treated by a mixture of independent and constrained refinement
S = 1.04 w = 1/[σ2(Fo2) + (0.0329P)2 + 1.1062P]
where P = (Fo2 + 2Fc2)/3
5809 reflections(Δ/σ)max = 0.001
245 parametersΔρmax = 0.73 e Å3
0 restraintsΔρmin = 0.45 e Å3
Crystal data top
[Co2(C2H4NO)2(OH)2(C5H5N)4](ClO4)2·2C2H3NV = 1794.1 (2) Å3
Mr = 865.41Z = 2
Monoclinic, P21/nMo Kα radiation
a = 10.6198 (7) ŵ = 1.15 mm1
b = 10.2440 (7) ÅT = 100 K
c = 16.503 (1) Å0.46 × 0.22 × 0.17 mm
β = 92.167 (1)°
Data collection top
Bruker APEXII CCD
diffractometer
5809 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2008)
4796 reflections with I > 2σ(I)
Tmin = 0.652, Tmax = 0.746Rint = 0.037
21140 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0370 restraints
wR(F2) = 0.085H atoms treated by a mixture of independent and constrained refinement
S = 1.04Δρmax = 0.73 e Å3
5809 reflectionsΔρmin = 0.45 e Å3
245 parameters
Special details top

Experimental. IR (cm-1): 3393.0 (w), 3314.4 (m), 2251.7 (w), 1606.8 (m), 1549.7 (br), 1476.2 (m), 1449.0 (s), 1238.1 (m), 1214.2 (s), 1154.9 (w), 1092.7 (sh), 1064.7 (vs), 941.4 (m), 898.0 (m), 771.2 (sh), 760.8 (s), 693.5 (vs).

Geometry. All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Co10.46912 (2)0.55025 (2)0.426797 (13)0.01179 (6)
O10.38651 (11)0.45010 (11)0.50391 (7)0.0131 (2)
H1A0.336 (2)0.488 (3)0.5203 (16)0.033 (7)*
N10.42416 (13)0.70022 (13)0.48763 (8)0.0135 (3)
H1B0.399 (2)0.772 (2)0.4665 (13)0.021 (5)*
O20.47517 (11)0.61555 (11)0.61550 (7)0.0145 (2)
N20.31450 (13)0.54632 (13)0.36017 (8)0.0135 (3)
C10.25497 (16)0.43048 (16)0.35255 (10)0.0163 (3)
H10.29460.35460.37460.02*
C20.13793 (17)0.41899 (17)0.31358 (11)0.0190 (3)
H20.09720.33660.30970.023*
C30.08103 (17)0.52900 (18)0.28036 (11)0.0217 (4)
H30.00040.52330.25360.026*
C40.14303 (17)0.64758 (18)0.28664 (11)0.0209 (3)
H40.10630.72410.26340.025*
C50.25940 (16)0.65295 (16)0.32729 (10)0.0167 (3)
H50.30160.73450.33210.02*
N30.56135 (13)0.64926 (14)0.34850 (8)0.0147 (3)
C60.55776 (16)0.61638 (17)0.26919 (10)0.0186 (3)
H60.50880.54320.25190.022*
C70.62304 (18)0.68584 (19)0.21237 (11)0.0230 (4)
H70.61840.6610.15690.028*
C80.69538 (18)0.79237 (19)0.23758 (12)0.0249 (4)
H80.740.84220.19950.03*
C90.70130 (18)0.82470 (18)0.31919 (12)0.0234 (4)
H90.75140.89610.33810.028*
C100.63306 (16)0.75143 (17)0.37290 (11)0.0189 (3)
H100.6370.7740.42880.023*
C110.44008 (14)0.70913 (16)0.56673 (10)0.0140 (3)
C120.41864 (17)0.83912 (16)0.60668 (11)0.0187 (3)
H12A0.49720.88950.60810.028*
H12B0.39160.82510.66210.028*
H12C0.35320.88730.57580.028*
N40.15243 (16)0.58853 (18)0.54242 (11)0.0284 (4)
C410.07223 (18)0.64581 (19)0.51135 (12)0.0243 (4)
C420.0309 (2)0.7190 (2)0.47192 (14)0.0314 (4)
H42A0.06680.66830.42630.047*
H42B0.0010.80230.4520.047*
H42C0.09630.73550.5110.047*
Cl10.21490 (4)1.00646 (4)0.41599 (3)0.02444 (10)
O30.12447 (17)0.94963 (19)0.35856 (11)0.0484 (5)
O40.33574 (13)0.94539 (13)0.40484 (9)0.0255 (3)
O50.2253 (2)1.14318 (15)0.40122 (13)0.0582 (6)
O60.17453 (14)0.98297 (16)0.49681 (9)0.0336 (3)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co10.01319 (10)0.01015 (10)0.01196 (10)0.00040 (8)0.00044 (7)0.00032 (8)
O10.0135 (5)0.0121 (5)0.0137 (5)0.0004 (4)0.0006 (4)0.0008 (4)
N10.0147 (6)0.0103 (6)0.0154 (6)0.0006 (5)0.0007 (5)0.0002 (5)
O20.0165 (5)0.0128 (5)0.0142 (5)0.0006 (4)0.0003 (4)0.0007 (4)
N20.0149 (6)0.0128 (6)0.0127 (6)0.0009 (5)0.0004 (5)0.0002 (5)
C10.0182 (8)0.0138 (7)0.0167 (7)0.0012 (6)0.0006 (6)0.0003 (6)
C20.0203 (8)0.0166 (8)0.0199 (8)0.0052 (6)0.0028 (6)0.0001 (6)
C30.0178 (8)0.0248 (9)0.0221 (9)0.0017 (7)0.0055 (7)0.0030 (7)
C40.0219 (8)0.0189 (8)0.0215 (8)0.0020 (7)0.0044 (7)0.0037 (7)
C50.0196 (8)0.0141 (7)0.0163 (7)0.0001 (6)0.0000 (6)0.0012 (6)
N30.0150 (6)0.0135 (6)0.0157 (6)0.0011 (5)0.0005 (5)0.0027 (5)
C60.0189 (8)0.0190 (8)0.0181 (8)0.0027 (6)0.0007 (6)0.0011 (6)
C70.0239 (9)0.0278 (9)0.0176 (8)0.0063 (7)0.0047 (7)0.0055 (7)
C80.0240 (9)0.0218 (9)0.0295 (10)0.0047 (7)0.0110 (7)0.0096 (7)
C90.0226 (9)0.0175 (8)0.0304 (10)0.0016 (7)0.0064 (7)0.0033 (7)
C100.0193 (8)0.0162 (8)0.0212 (8)0.0008 (6)0.0023 (6)0.0017 (6)
C110.0113 (7)0.0127 (7)0.0180 (7)0.0005 (5)0.0009 (6)0.0008 (6)
C120.0207 (8)0.0138 (7)0.0216 (8)0.0014 (6)0.0000 (6)0.0046 (6)
N40.0230 (8)0.0286 (9)0.0338 (9)0.0015 (7)0.0035 (7)0.0061 (7)
C410.0233 (9)0.0211 (9)0.0290 (10)0.0030 (7)0.0078 (7)0.0067 (7)
C420.0283 (10)0.0259 (10)0.0402 (12)0.0043 (8)0.0037 (9)0.0023 (9)
Cl10.0294 (2)0.01517 (19)0.0289 (2)0.00356 (16)0.00293 (18)0.00678 (16)
O30.0392 (10)0.0630 (13)0.0417 (10)0.0070 (9)0.0158 (8)0.0016 (9)
O40.0263 (7)0.0184 (6)0.0320 (7)0.0024 (5)0.0031 (6)0.0036 (5)
O50.0781 (14)0.0132 (7)0.0863 (15)0.0087 (8)0.0437 (12)0.0129 (8)
O60.0324 (8)0.0392 (9)0.0296 (8)0.0022 (7)0.0051 (6)0.0089 (7)
Geometric parameters (Å, º) top
Co1—O11.8777 (12)C6—C71.384 (2)
Co1—N11.9059 (14)C6—H60.95
Co1—O2i1.9374 (12)C7—C81.389 (3)
Co1—N31.9374 (14)C7—H70.95
Co1—N21.9418 (14)C8—C91.386 (3)
Co1—Co1i2.6847 (4)C8—H80.95
O1—H1A0.72 (3)C9—C101.387 (2)
N1—C111.313 (2)C9—H90.95
N1—H1B0.85 (2)C10—H100.95
O2—C111.2973 (19)C11—C121.507 (2)
N2—C51.344 (2)C12—H12A0.98
N2—C11.348 (2)C12—H12B0.98
C1—C21.383 (2)C12—H12C0.98
C1—H10.95N4—C411.140 (3)
C2—C31.382 (2)C41—C421.460 (3)
C2—H20.95C42—H42A0.98
C3—C41.384 (3)C42—H42B0.98
C3—H30.95C42—H42C0.98
C4—C51.385 (2)Cl1—O51.4265 (16)
C4—H40.95Cl1—O61.4367 (16)
C5—H50.95Cl1—O41.4456 (14)
N3—C101.347 (2)Cl1—O31.4459 (18)
N3—C61.351 (2)
O1—Co1—O1i88.73 (5)N2—C5—H5119
O1—Co1—N187.17 (6)C4—C5—H5119
O1i—Co1—N184.02 (6)C10—N3—C6118.58 (15)
O1—Co1—O2i85.53 (5)C10—N3—Co1120.12 (12)
O1i—Co1—O2i87.96 (5)C6—N3—Co1121.28 (12)
N1—Co1—O2i169.26 (6)N3—C6—C7122.13 (17)
O1—Co1—N3177.39 (6)N3—C6—H6118.9
O1i—Co1—N389.17 (5)C7—C6—H6118.9
N1—Co1—N394.15 (6)C6—C7—C8119.11 (17)
O2i—Co1—N392.85 (5)C6—C7—H7120.4
O1—Co1—N288.03 (5)C8—C7—H7120.4
O1i—Co1—N2176.71 (5)C9—C8—C7118.87 (17)
N1—Co1—N295.26 (6)C9—C8—H8120.6
O2i—Co1—N292.35 (5)C7—C8—H8120.6
N3—Co1—N294.08 (6)C8—C9—C10119.09 (18)
O1—Co1—Co1i44.37 (4)C8—C9—H9120.5
N1—Co1—Co1i83.83 (4)C10—C9—H9120.5
O2i—Co1—Co1i85.44 (3)N3—C10—C9122.19 (17)
N3—Co1—Co1i133.51 (4)N3—C10—H10118.9
N2—Co1—Co1i132.39 (4)C9—C10—H10118.9
Co1—O1—Co1i91.27 (5)O2—C11—N1126.06 (15)
Co1—O1—H1A109 (2)O2—C11—C12115.22 (14)
Co1i—O1—H1A112 (2)N1—C11—C12118.71 (15)
C11—N1—Co1123.66 (11)C11—C12—H12A109.5
C11—N1—H1B111.9 (14)C11—C12—H12B109.5
Co1—N1—H1B124.1 (14)H12A—C12—H12B109.5
C11—O2—Co1i120.58 (10)C11—C12—H12C109.5
C5—N2—C1118.84 (14)H12A—C12—H12C109.5
C5—N2—Co1123.90 (11)H12B—C12—H12C109.5
C1—N2—Co1117.04 (11)N4—C41—C42179.7 (2)
N2—C1—C2121.90 (16)C41—C42—H42A109.5
N2—C1—H1119.1C41—C42—H42B109.5
C2—C1—H1119.1H42A—C42—H42B109.5
C3—C2—C1119.13 (16)C41—C42—H42C109.5
C3—C2—H2120.4H42A—C42—H42C109.5
C1—C2—H2120.4H42B—C42—H42C109.5
C2—C3—C4119.11 (16)O5—Cl1—O6110.53 (11)
C2—C3—H3120.4O5—Cl1—O4109.18 (10)
C4—C3—H3120.4O6—Cl1—O4110.07 (9)
C3—C4—C5118.98 (16)O5—Cl1—O3109.69 (13)
C3—C4—H4120.5O6—Cl1—O3109.08 (11)
C5—C4—H4120.5O4—Cl1—O3108.25 (10)
N2—C5—C4122.02 (16)
O1i—Co1—O1—Co1i0C1—N2—C5—C40.7 (2)
N1—Co1—O1—Co1i84.07 (6)Co1—N2—C5—C4173.72 (13)
O2i—Co1—O1—Co1i88.05 (5)C3—C4—C5—N20.6 (3)
N2—Co1—O1—Co1i179.44 (6)O1i—Co1—N3—C1044.90 (13)
O1—Co1—N1—C1147.42 (13)N1—Co1—N3—C1039.04 (13)
O1i—Co1—N1—C1141.60 (13)O2i—Co1—N3—C10132.81 (13)
O2i—Co1—N1—C110.2 (4)N2—Co1—N3—C10134.63 (13)
N3—Co1—N1—C11130.33 (13)Co1i—Co1—N3—C1046.39 (15)
N2—Co1—N1—C11135.18 (13)O1i—Co1—N3—C6133.65 (13)
Co1i—Co1—N1—C113.03 (13)N1—Co1—N3—C6142.42 (13)
O1—Co1—N2—C5129.66 (14)O2i—Co1—N3—C645.73 (13)
N1—Co1—N2—C542.69 (14)N2—Co1—N3—C646.83 (13)
O2i—Co1—N2—C5144.89 (13)Co1i—Co1—N3—C6132.15 (11)
N3—Co1—N2—C551.87 (14)C10—N3—C6—C71.4 (2)
Co1i—Co1—N2—C5129.13 (12)Co1—N3—C6—C7179.96 (13)
O1—Co1—N2—C144.81 (12)N3—C6—C7—C80.4 (3)
N1—Co1—N2—C1131.79 (12)C6—C7—C8—C90.9 (3)
O2i—Co1—N2—C140.63 (12)C7—C8—C9—C101.2 (3)
N3—Co1—N2—C1133.66 (12)C6—N3—C10—C91.0 (3)
Co1i—Co1—N2—C145.34 (14)Co1—N3—C10—C9179.62 (13)
C5—N2—C1—C21.5 (2)C8—C9—C10—N30.3 (3)
Co1—N2—C1—C2173.27 (13)Co1i—O2—C11—N18.1 (2)
N2—C1—C2—C31.0 (3)Co1i—O2—C11—C12170.77 (11)
C1—C2—C3—C40.3 (3)Co1—N1—C11—O27.7 (2)
C2—C3—C4—C51.1 (3)Co1—N1—C11—C12171.23 (12)
Symmetry code: (i) x+1, y+1, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H1A···N40.72 (2)2.25 (2)2.952 (2)165 (3)
N1—H1B···O40.85 (2)2.14 (2)2.993 (2)176 (2)
C1—H1···O5ii0.952.333.070 (2)134
C5—H5···O40.952.493.345 (2)150
C6—H6···O3iii0.952.463.286 (3)145
C12—H12A···O4iv0.982.473.428 (2)167
C12—H12C···O60.982.463.439 (2)173
C42—H42B···O30.982.553.470 (3)155
C42—H42C···O5v0.982.383.311 (3)158
Symmetry codes: (ii) x, y1, z; (iii) x+1/2, y1/2, z+1/2; (iv) x+1, y+2, z+1; (v) x, y+2, z+1.

Experimental details

Crystal data
Chemical formula[Co2(C2H4NO)2(OH)2(C5H5N)4](ClO4)2·2C2H3N
Mr865.41
Crystal system, space groupMonoclinic, P21/n
Temperature (K)100
a, b, c (Å)10.6198 (7), 10.2440 (7), 16.503 (1)
β (°) 92.167 (1)
V3)1794.1 (2)
Z2
Radiation typeMo Kα
µ (mm1)1.15
Crystal size (mm)0.46 × 0.22 × 0.17
Data collection
DiffractometerBruker APEXII CCD
diffractometer
Absorption correctionMulti-scan
(SADABS; Bruker, 2008)
Tmin, Tmax0.652, 0.746
No. of measured, independent and
observed [I > 2σ(I)] reflections
21140, 5809, 4796
Rint0.037
(sin θ/λ)max1)0.743
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.037, 0.085, 1.04
No. of reflections5809
No. of parameters245
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)0.73, 0.45

Computer programs: SAINT [or APEX2?] (Bruker, 2009), SAINT (Bruker, 2009), SORTAV (Blessing, 1995), SIR97 (Altomare et al., 1999), SHELXL97 (Sheldrick, 2008), ORTEP-3 for Windows (Farrugia, 1997), WinGX (Farrugia, 1999) and publCIF (Westrip, 2010).

Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H1A···N40.72 (2)2.25 (2)2.952 (2)165 (3)
N1—H1B···O40.85 (2)2.14 (2)2.993 (2)176 (2)
 

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