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Acta Cryst. (2008). E64, m1310    [ doi:10.1107/S1600536808029681 ]

Hexa-[mu]2-acetato-[kappa]12O:O'-[mu]3-oxido-tris[aquachromium(III)] nitrate acetic acid solvate

M. J. Maah, C. I. Abdullah, S. N. Gan, A. Mohd Jelan and S. W. Ng

Abstract top

In the crystal structure of the title salt, [Cr3(C2H3O2)6O(H2O)3]NO3·CH3CO2H, the trinuclear [Cr3(CH3CO2)6O(H2O)3] cluster cation has an oxide O atom that is connected to three water-coordinated CrIII atoms, the three metal atoms forming the points of an equilateral triangle. Each of the six acetate carboxylate groups bridges a Cr-O-Cr fragment. The cluster cation interacts with the nitrate counter-ion and solvent molecules through O-H...O hydrogen bonds, forming a three-dimensional hydrogen-bonded network.

Related literature top

For crystal structure reports of [Cr3(C2H3O2)6O(H2O)3]+ salts; see: Anson et al. (1997); Fujihara et al. (1998); Glowiak et al. (1996); Karu et al. (1993); Winpenny et al. (2005).

Experimental top

Chromium(III) nitrate nonahydrate (10.06 g, 0.025 mol) was heated in acetic acid (24 ml, 0.42 mol) for 10 h. The solution was filtered and the acetic acid allowed to evaporate slowly. The dark-green crystals that separated were washed with chloroform and then dried at 433 K for 24 h. Yield: 70%.

Refinement top

The O- and C-bound H-atoms were placed in calculated positions with O—H = 0.84 Å and C—H 0.98 Å, and were included in the refinement in the riding model approximation, with U(H) set to 1.5 U(O, C). The final difference Fourier map had a large peak/deep hole at about 1 Å from the Cr3 atom.

Computing details top

Data collection: APEX2 (Bruker, 2007); cell refinement: SAINT (Bruker, 2007); 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: X-SEED (Barbour, 2001); software used to prepare material for publication: publCIF (Westrip, 2008).

Figures top
[Figure 1] Fig. 1. Thermal ellipsoid (Barbour, 2001) plot of [Cr3(C2H3O2)6O(H2O)3].[NO3].CH3CO2H at the 70% probability level. Hydrogen atoms are drawn as spheres of arbitrary radius.
Hexa-µ2-acetato-κ12O:O'-µ3-oxido-\ tris[aquachromium(III)] nitrate acetic acid solvate top
Crystal data top
[Cr3(C2H3O2)6O(H2O)3]NO3·C2H4O2F(000) = 1436
Mr = 702.37Dx = 1.827 Mg m−3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 9927 reflections
a = 11.7034 (1) Åθ = 2.2–28.2°
b = 14.5102 (2) ŵ = 1.35 mm−1
c = 15.0427 (2) ÅT = 100 K
β = 91.532 (1)°Chip, green
V = 2553.62 (5) Å30.20 × 0.10 × 0.05 mm
Z = 4
Data collection top
Bruker SMART APEX
diffractometer		5836 independent reflections
Radiation source: fine-focus sealed tube5092 reflections with I > 2σ(I)
graphiteRint = 0.046
ω scansθmax = 27.5°, θmin = 2.0°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)		h = −15→15
Tmin = 0.774, Tmax = 0.936k = −18→18
22819 measured reflectionsl = −19→19
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)] = 0.067Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.224H-atom parameters constrained
S = 1.38 w = 1/[σ2(Fo2) + (0.1P)2 + 1P]
where P = (Fo2 + 2Fc2)/3
5836 reflections(Δ/σ)max = 0.001
359 parametersΔρmax = 1.77 e Å−3
0 restraintsΔρmin = −1.33 e Å−3
Crystal data top
[Cr3(C2H3O2)6O(H2O)3]NO3·C2H4O2V = 2553.62 (5) Å3
Mr = 702.37Z = 4
Monoclinic, P21/cMo Kα radiation
a = 11.7034 (1) ŵ = 1.35 mm−1
b = 14.5102 (2) ÅT = 100 K
c = 15.0427 (2) Å0.20 × 0.10 × 0.05 mm
β = 91.532 (1)°
Data collection top
Bruker SMART APEX
diffractometer		5836 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)		5092 reflections with I > 2σ(I)
Tmin = 0.774, Tmax = 0.936Rint = 0.046
22819 measured reflectionsθmax = 27.5°
Refinement top
R[F2 > 2σ(F2)] = 0.067H-atom parameters constrained
wR(F2) = 0.224Δρmax = 1.77 e Å−3
S = 1.38Δρmin = −1.33 e Å−3
5836 reflectionsAbsolute structure: ?
359 parametersFlack parameter: ?
0 restraintsRogers parameter: ?
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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Cr10.40542 (6)0.60336 (5)0.62841 (5)0.0131 (2)
Cr20.17034 (6)0.56625 (5)0.73703 (5)0.0135 (2)
Cr30.18005 (6)0.73269 (6)0.58877 (5)0.0140 (2)
O10.4536 (3)0.6151 (3)0.7549 (2)0.0198 (8)
O20.2966 (3)0.5724 (3)0.8261 (3)0.0205 (8)
O30.3914 (3)0.4689 (3)0.6374 (3)0.0184 (7)
O40.2208 (3)0.4442 (3)0.6949 (3)0.0198 (8)
O50.1056 (3)0.6751 (3)0.7966 (3)0.0195 (7)
O60.0969 (3)0.7819 (3)0.6894 (3)0.0195 (8)
O70.0316 (3)0.5543 (3)0.6608 (3)0.0189 (7)
O80.0452 (3)0.6588 (3)0.5512 (3)0.0192 (7)
O90.3030 (3)0.8221 (3)0.6195 (2)0.0174 (7)
O100.4560 (3)0.7309 (3)0.6132 (3)0.0193 (8)
O110.2517 (3)0.7039 (3)0.4743 (2)0.0176 (7)
O120.3748 (3)0.5871 (3)0.4972 (2)0.0172 (7)
O130.2517 (3)0.6341 (2)0.6511 (2)0.0147 (7)
O14−0.0709 (3)0.5678 (3)0.9306 (3)0.0256 (9)
O15−0.2549 (4)0.5997 (3)0.9442 (3)0.0299 (10)
H15−0.24330.62210.99510.045*
O160.7058 (3)0.7280 (3)0.5673 (3)0.0267 (9)
O170.8176 (4)0.7184 (3)0.6842 (3)0.0290 (9)
O180.8263 (4)0.8364 (3)0.5964 (3)0.0358 (11)
O1W0.5731 (3)0.5752 (3)0.6032 (2)0.0172 (7)
H110.60420.62240.58250.026*
H120.57650.53210.56620.026*
O2W0.0843 (3)0.4914 (3)0.8268 (3)0.0200 (8)
H210.05920.52660.86610.030*
H220.12850.45240.85050.030*
O3W0.1111 (3)0.8387 (3)0.5119 (3)0.0222 (8)
H310.04240.84650.52470.033*
H320.11520.82500.45780.033*
N10.7827 (4)0.7597 (3)0.6176 (3)0.0214 (9)
C10.3976 (4)0.6011 (3)0.8241 (3)0.0161 (9)
C20.4557 (5)0.6207 (4)0.9128 (4)0.0213 (10)
H2A0.44040.68450.93020.032*
H2B0.53830.61160.90810.032*
H2C0.42600.57870.95770.032*
C30.3122 (4)0.4166 (4)0.6615 (3)0.0163 (9)
C40.3268 (5)0.3144 (4)0.6485 (4)0.0233 (11)
H4A0.30050.28160.70110.035*
H4B0.40770.30050.63980.035*
H4C0.28180.29460.59610.035*
C50.0764 (4)0.7537 (4)0.7646 (4)0.0175 (10)
C60.0117 (5)0.8165 (4)0.8254 (4)0.0213 (11)
H6A−0.07030.80350.81940.032*
H6B0.02590.88090.80920.032*
H6C0.03750.80600.88710.032*
C7−0.0024 (4)0.5925 (4)0.5887 (3)0.0173 (10)
C8−0.1111 (4)0.5551 (4)0.5464 (4)0.0217 (11)
H8A−0.11160.56720.48230.033*
H8B−0.17710.58540.57270.033*
H8C−0.11540.48860.55670.033*
C90.4087 (4)0.8085 (4)0.6238 (3)0.0163 (9)
C100.4856 (5)0.8895 (4)0.6411 (4)0.0214 (11)
H10A0.44170.94660.63360.032*
H10B0.54800.88870.59910.032*
H10C0.51720.88620.70200.032*
C110.3182 (4)0.6420 (3)0.4472 (3)0.0154 (9)
C120.3291 (5)0.6330 (4)0.3480 (3)0.0213 (10)
H12A0.26930.59180.32440.032*
H12B0.40440.60760.33490.032*
H12C0.32080.69390.32030.032*
C13−0.1699 (4)0.5671 (4)0.9000 (4)0.0196 (10)
C14−0.2012 (5)0.5280 (4)0.8109 (4)0.0220 (11)
H14A−0.14390.54630.76790.033*
H14B−0.27630.55150.79140.033*
H14C−0.20400.46060.81480.033*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cr10.0129 (4)0.0149 (4)0.0115 (4)0.0003 (3)0.0011 (3)0.0001 (3)
Cr20.0135 (4)0.0149 (4)0.0123 (4)0.0005 (3)0.0018 (3)−0.0001 (3)
Cr30.0134 (4)0.0149 (4)0.0136 (4)0.0010 (3)0.0001 (3)−0.0013 (3)
O10.0163 (16)0.029 (2)0.0142 (17)−0.0013 (14)0.0007 (13)0.0001 (15)
O20.0194 (18)0.027 (2)0.0154 (17)−0.0023 (15)0.0007 (14)0.0032 (15)
O30.0155 (16)0.0158 (17)0.0241 (19)0.0014 (13)0.0044 (14)0.0029 (14)
O40.0209 (18)0.0149 (17)0.0239 (19)−0.0013 (14)0.0088 (15)−0.0018 (14)
O50.0207 (17)0.0184 (18)0.0194 (18)0.0023 (14)0.0033 (14)−0.0001 (15)
O60.0187 (17)0.0204 (18)0.0196 (19)0.0021 (14)0.0020 (14)−0.0027 (15)
O70.0152 (16)0.0233 (19)0.0182 (18)−0.0021 (14)0.0017 (13)0.0031 (15)
O80.0177 (17)0.0194 (18)0.0205 (18)0.0000 (14)−0.0014 (14)−0.0024 (15)
O90.0172 (17)0.0167 (17)0.0182 (17)−0.0009 (13)−0.0010 (13)0.0004 (14)
O100.0164 (17)0.0166 (17)0.025 (2)0.0004 (13)0.0038 (14)0.0010 (15)
O110.0204 (17)0.0190 (18)0.0136 (17)0.0005 (14)0.0010 (13)0.0003 (14)
O120.0171 (17)0.0208 (18)0.0136 (16)0.0012 (14)0.0011 (13)−0.0022 (14)
O130.0131 (15)0.0175 (17)0.0135 (16)0.0007 (13)0.0020 (12)−0.0006 (13)
O140.0195 (18)0.029 (2)0.029 (2)−0.0017 (16)0.0010 (16)−0.0053 (17)
O150.022 (2)0.042 (3)0.025 (2)0.0091 (18)−0.0012 (16)−0.0096 (19)
O160.0219 (19)0.026 (2)0.032 (2)−0.0049 (16)−0.0010 (17)0.0024 (18)
O170.043 (2)0.028 (2)0.0164 (19)0.0016 (18)0.0006 (17)0.0017 (16)
O180.051 (3)0.026 (2)0.030 (2)−0.017 (2)−0.010 (2)0.0036 (19)
O1W0.0153 (16)0.0180 (17)0.0184 (18)−0.0002 (13)0.0038 (13)−0.0010 (14)
O2W0.0204 (17)0.0196 (18)0.0205 (18)0.0039 (14)0.0079 (14)0.0009 (15)
O3W0.0213 (18)0.0214 (19)0.024 (2)0.0047 (15)−0.0029 (15)−0.0008 (16)
N10.028 (2)0.021 (2)0.016 (2)−0.0016 (18)0.0057 (18)−0.0024 (18)
C10.018 (2)0.017 (2)0.013 (2)0.0040 (18)−0.0013 (18)−0.0018 (18)
C20.020 (2)0.025 (3)0.018 (3)0.001 (2)−0.0008 (19)−0.005 (2)
C30.017 (2)0.018 (2)0.013 (2)0.0020 (18)−0.0011 (18)−0.0007 (18)
C40.023 (3)0.016 (2)0.032 (3)−0.001 (2)0.008 (2)−0.004 (2)
C50.013 (2)0.019 (2)0.020 (2)−0.0014 (18)−0.0020 (18)−0.005 (2)
C60.025 (3)0.023 (3)0.016 (2)0.007 (2)0.002 (2)−0.006 (2)
C70.013 (2)0.022 (2)0.017 (2)0.0019 (18)0.0024 (18)−0.0037 (19)
C80.018 (2)0.023 (3)0.024 (3)0.0000 (19)−0.001 (2)−0.003 (2)
C90.018 (2)0.021 (2)0.010 (2)−0.0031 (18)0.0006 (17)0.0007 (18)
C100.020 (2)0.021 (3)0.023 (3)−0.004 (2)0.001 (2)−0.002 (2)
C110.014 (2)0.016 (2)0.016 (2)−0.0016 (17)0.0007 (17)−0.0026 (18)
C120.026 (3)0.027 (3)0.011 (2)0.004 (2)0.0006 (19)−0.001 (2)
C130.019 (2)0.018 (2)0.022 (3)−0.0010 (18)−0.002 (2)0.001 (2)
C140.024 (3)0.027 (3)0.015 (2)−0.002 (2)−0.001 (2)−0.002 (2)
Geometric parameters (Å, °) top
Cr1—O131.893 (3)O18—N11.268 (7)
Cr1—O101.959 (4)O1W—H110.8400
Cr1—O31.962 (4)O1W—H120.8400
Cr1—O11.978 (4)O2W—H210.8400
Cr1—O122.010 (4)O2W—H220.8400
Cr1—O1W2.049 (4)O3W—H310.8400
Cr2—O131.901 (4)O3W—H320.8400
Cr2—O21.969 (4)C1—C21.509 (7)
Cr2—O71.970 (4)C2—H2A0.9800
Cr2—O51.976 (4)C2—H2B0.9800
Cr2—O41.977 (4)C2—H2C0.9800
Cr2—O2W2.022 (4)C3—C41.506 (7)
Cr3—O131.894 (4)C4—H4A0.9800
Cr3—O61.956 (4)C4—H4B0.9800
Cr3—O81.978 (4)C4—H4C0.9800
Cr3—O111.980 (4)C5—C61.511 (7)
Cr3—O91.982 (4)C6—H6A0.9800
Cr3—O3W2.075 (4)C6—H6B0.9800
O1—C11.260 (6)C6—H6C0.9800
O2—C11.255 (7)C7—C81.508 (7)
O3—C31.259 (6)C8—H8A0.9800
O4—C31.259 (6)C8—H8B0.9800
O5—C51.281 (7)C8—H8C0.9800
O6—C51.233 (7)C9—C101.498 (7)
O7—C71.272 (6)C10—H10A0.9800
O8—C71.254 (7)C10—H10B0.9800
O9—C91.254 (6)C10—H10C0.9800
O10—C91.267 (7)C11—C121.507 (7)
O11—C111.263 (6)C12—H12A0.9800
O12—C111.269 (6)C12—H12B0.9800
O14—C131.236 (7)C12—H12C0.9800
O15—C131.300 (7)C13—C141.492 (7)
O15—H150.8400C14—H14A0.9800
O16—N11.247 (6)C14—H14B0.9800
O17—N11.228 (6)C14—H14C0.9800
O13—Cr1—O1095.17 (16)Cr3—O3W—H32109.5
O13—Cr1—O398.06 (15)H31—O3W—H32109.5
O10—Cr1—O3166.77 (16)O17—N1—O16122.2 (5)
O13—Cr1—O193.10 (15)O17—N1—O18120.4 (5)
O10—Cr1—O187.24 (17)O16—N1—O18117.4 (5)
O3—Cr1—O192.37 (17)O2—C1—O1125.7 (5)
O13—Cr1—O1293.38 (15)O2—C1—C2116.4 (5)
O10—Cr1—O1292.45 (16)O1—C1—C2117.9 (5)
O3—Cr1—O1286.44 (16)C1—C2—H2A109.5
O1—Cr1—O12173.51 (15)C1—C2—H2B109.5
O13—Cr1—O1W177.86 (16)H2A—C2—H2B109.5
O10—Cr1—O1W82.69 (15)C1—C2—H2C109.5
O3—Cr1—O1W84.09 (15)H2A—C2—H2C109.5
O1—Cr1—O1W86.87 (15)H2B—C2—H2C109.5
O12—Cr1—O1W86.66 (15)O4—C3—O3124.2 (5)
O13—Cr2—O293.38 (15)O4—C3—C4117.7 (5)
O13—Cr2—O793.98 (15)O3—C3—C4118.0 (5)
O2—Cr2—O7172.47 (16)C3—C4—H4A109.5
O13—Cr2—O595.72 (16)C3—C4—H4B109.5
O2—Cr2—O586.87 (17)H4A—C4—H4B109.5
O7—Cr2—O590.83 (16)C3—C4—H4C109.5
O13—Cr2—O494.97 (16)H4A—C4—H4C109.5
O2—Cr2—O491.88 (17)H4B—C4—H4C109.5
O7—Cr2—O489.05 (17)O6—C5—O5125.8 (5)
O5—Cr2—O4169.29 (17)O6—C5—C6117.9 (5)
O13—Cr2—O2W178.67 (16)O5—C5—C6116.3 (5)
O2—Cr2—O2W87.02 (16)C5—C6—H6A109.5
O7—Cr2—O2W85.66 (16)C5—C6—H6B109.5
O5—Cr2—O2W85.56 (16)H6A—C6—H6B109.5
O4—Cr2—O2W83.75 (16)C5—C6—H6C109.5
O13—Cr3—O696.66 (16)H6A—C6—H6C109.5
O13—Cr3—O894.10 (15)H6B—C6—H6C109.5
O6—Cr3—O890.55 (16)O8—C7—O7125.8 (5)
O13—Cr3—O1194.52 (15)O8—C7—C8117.8 (5)
O6—Cr3—O11168.79 (16)O7—C7—C8116.4 (5)
O8—Cr3—O1189.43 (16)C7—C8—H8A109.5
O13—Cr3—O994.02 (15)C7—C8—H8B109.5
O6—Cr3—O987.33 (16)H8A—C8—H8B109.5
O8—Cr3—O9171.80 (16)C7—C8—H8C109.5
O11—Cr3—O991.12 (16)H8A—C8—H8C109.5
O13—Cr3—O3W175.13 (16)H8B—C8—H8C109.5
O6—Cr3—O3W88.07 (16)O9—C9—O10124.6 (5)
O8—Cr3—O3W86.97 (16)O9—C9—C10118.2 (5)
O11—Cr3—O3W80.73 (16)O10—C9—C10117.2 (4)
O9—Cr3—O3W85.05 (16)C9—C10—H10A109.5
C1—O1—Cr1129.8 (3)C9—C10—H10B109.5
C1—O2—Cr2133.6 (3)H10A—C10—H10B109.5
C3—O3—Cr1133.1 (3)C9—C10—H10C109.5
C3—O4—Cr2132.6 (3)H10A—C10—H10C109.5
C5—O5—Cr2130.0 (4)H10B—C10—H10C109.5
C5—O6—Cr3134.5 (4)O11—C11—O12124.9 (5)
C7—O7—Cr2133.8 (3)O11—C11—C12116.7 (5)
C7—O8—Cr3130.4 (3)O12—C11—C12118.4 (4)
C9—O9—Cr3128.2 (3)C11—C12—H12A109.5
C9—O10—Cr1133.7 (3)C11—C12—H12B109.5
C11—O11—Cr3135.2 (3)H12A—C12—H12B109.5
C11—O12—Cr1125.8 (3)C11—C12—H12C109.5
Cr1—O13—Cr3119.96 (19)H12A—C12—H12C109.5
Cr1—O13—Cr2119.74 (18)H12B—C12—H12C109.5
Cr3—O13—Cr2120.30 (18)O14—C13—O15121.9 (5)
C13—O15—H15120.0O14—C13—C14122.9 (5)
Cr1—O1W—H11109.5O15—C13—C14115.2 (5)
Cr1—O1W—H12109.5C13—C14—H14A109.5
H11—O1W—H12109.5C13—C14—H14B109.5
Cr2—O2W—H21109.5H14A—C14—H14B109.5
Cr2—O2W—H22109.5C13—C14—H14C109.5
H21—O2W—H22109.5H14A—C14—H14C109.5
Cr3—O3W—H31109.5H14B—C14—H14C109.5
O13—Cr1—O1—C130.3 (5)O10—Cr1—O12—C11−49.0 (4)
O10—Cr1—O1—C1125.3 (5)O3—Cr1—O12—C11144.2 (4)
O3—Cr1—O1—C1−67.9 (5)O1W—Cr1—O12—C11−131.5 (4)
O1W—Cr1—O1—C1−151.8 (5)O10—Cr1—O13—Cr337.4 (2)
O13—Cr2—O2—C1−6.8 (5)O3—Cr1—O13—Cr3−142.2 (2)
O5—Cr2—O2—C1−102.4 (5)O1—Cr1—O13—Cr3124.9 (2)
O4—Cr2—O2—C188.3 (5)O12—Cr1—O13—Cr3−55.4 (2)
O2W—Cr2—O2—C1171.9 (5)O10—Cr1—O13—Cr2−142.1 (2)
O13—Cr1—O3—C3−8.3 (5)O3—Cr1—O13—Cr238.2 (2)
O10—Cr1—O3—C3173.3 (6)O1—Cr1—O13—Cr2−54.6 (2)
O1—Cr1—O3—C385.2 (5)O12—Cr1—O13—Cr2125.1 (2)
O12—Cr1—O3—C3−101.2 (5)O6—Cr3—O13—Cr1−140.3 (2)
O1W—Cr1—O3—C3171.8 (5)O8—Cr3—O13—Cr1128.7 (2)
O13—Cr2—O4—C333.4 (5)O11—Cr3—O13—Cr138.9 (2)
O2—Cr2—O4—C3−60.2 (5)O9—Cr3—O13—Cr1−52.5 (2)
O7—Cr2—O4—C3127.3 (5)O6—Cr3—O13—Cr239.2 (2)
O5—Cr2—O4—C3−143.3 (8)O8—Cr3—O13—Cr2−51.8 (2)
O2W—Cr2—O4—C3−146.9 (5)O11—Cr3—O13—Cr2−141.5 (2)
O13—Cr2—O5—C531.9 (4)O9—Cr3—O13—Cr2127.0 (2)
O2—Cr2—O5—C5125.0 (4)O2—Cr2—O13—Cr146.6 (2)
O7—Cr2—O5—C5−62.2 (4)O7—Cr2—O13—Cr1−135.0 (2)
O4—Cr2—O5—C5−151.5 (8)O5—Cr2—O13—Cr1133.8 (2)
O2W—Cr2—O5—C5−147.8 (4)O4—Cr2—O13—Cr1−45.6 (2)
O13—Cr3—O6—C5−12.1 (5)O2—Cr2—O13—Cr3−132.9 (2)
O8—Cr3—O6—C582.1 (5)O7—Cr2—O13—Cr345.5 (2)
O11—Cr3—O6—C5171.9 (7)O5—Cr2—O13—Cr3−45.7 (2)
O9—Cr3—O6—C5−105.9 (5)O4—Cr2—O13—Cr3134.9 (2)
O3W—Cr3—O6—C5169.0 (5)Cr2—O2—C1—O1−18.2 (8)
O13—Cr2—O7—C7−12.7 (5)Cr2—O2—C1—C2161.6 (4)
O5—Cr2—O7—C783.1 (5)Cr1—O1—C1—O23.0 (8)
O4—Cr2—O7—C7−107.6 (5)Cr1—O1—C1—C2−176.8 (4)
O2W—Cr2—O7—C7168.6 (5)Cr2—O4—C3—O3−9.0 (8)
O13—Cr3—O8—C730.7 (5)Cr2—O4—C3—C4171.8 (4)
O6—Cr3—O8—C7−66.0 (5)Cr1—O3—C3—O4−6.9 (8)
O11—Cr3—O8—C7125.2 (5)Cr1—O3—C3—C4172.3 (4)
O3W—Cr3—O8—C7−154.0 (5)Cr3—O6—C5—O5−2.5 (8)
O13—Cr3—O9—C938.7 (4)Cr3—O6—C5—C6177.2 (4)
O6—Cr3—O9—C9135.2 (4)Cr2—O5—C5—O6−10.0 (8)
O11—Cr3—O9—C9−55.9 (4)Cr2—O5—C5—C6170.3 (3)
O3W—Cr3—O9—C9−136.5 (4)Cr3—O8—C7—O7−3.7 (8)
O13—Cr1—O10—C96.9 (5)Cr3—O8—C7—C8174.9 (3)
O3—Cr1—O10—C9−174.6 (6)Cr2—O7—C7—O8−7.8 (8)
O1—Cr1—O10—C9−86.0 (5)Cr2—O7—C7—C8173.6 (4)
O12—Cr1—O10—C9100.5 (5)Cr3—O9—C9—O10−3.9 (7)
O1W—Cr1—O10—C9−173.2 (5)Cr3—O9—C9—C10174.9 (3)
O13—Cr3—O11—C112.2 (5)Cr1—O10—C9—O9−25.2 (8)
O6—Cr3—O11—C11178.1 (7)Cr1—O10—C9—C10155.9 (4)
O8—Cr3—O11—C11−91.9 (5)Cr3—O11—C11—O12−13.8 (8)
O9—Cr3—O11—C1196.3 (5)Cr3—O11—C11—C12165.6 (4)
O3W—Cr3—O11—C11−178.9 (5)Cr1—O12—C11—O11−16.4 (7)
O13—Cr1—O12—C1146.3 (4)Cr1—O12—C11—C12164.2 (4)
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
O1w—H11···O160.841.962.769 (6)162
O1w—H12···O12i0.842.062.873 (5)162
O2w—H21···O140.841.922.668 (6)147
O2w—H22···O18ii0.841.932.725 (6)157
O3w—H31···O14iii0.842.282.781 (5)118
O3w—H32···O5iii0.842.423.244 (6)165
O15—H15···O18iv0.841.812.624 (6)163
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) −x+1, y−1/2, −z+3/2; (iii) x, −y+3/2, z−1/2; (iv) x−1, −y+3/2, z+1/2.
Table 1
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
O1w—H11···O160.841.962.769 (6)162
O1w—H12···O12i0.842.062.873 (5)162
O2w—H21···O140.841.922.668 (6)147
O2w—H22···O18ii0.841.932.725 (6)157
O3w—H31···O14iii0.842.282.781 (5)118
O3w—H32···O5iii0.842.423.244 (6)165
O15—H15···O18iv0.841.812.624 (6)163
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) −x+1, y−1/2, −z+3/2; (iii) x, −y+3/2, z−1/2; (iv) x−1, −y+3/2, z+1/2.
Acknowledgements top

We thank MOSTE (eSc project No. 02–02-11-SF0033) for supporting this study.

references
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