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Acta Crystallogr Sect E Struct Rep Online. 2008 October 1; 64(Pt 10): m1310.
Published online 2008 September 24. doi:  10.1107/S1600536808029681
PMCID: PMC2959480

Hexa-μ2-acetato-κ12 O:O′-μ3-oxido-tris­[aqua­chromium(III)] nitrate acetic acid solvate

Abstract

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

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

An external file that holds a picture, illustration, etc.
Object name is e-64-m1310-scheme1.jpg

Experimental

Crystal data

  • [Cr3(C2H3O2)6O(H2O)3]NO3·C2H4O2
  • M r = 702.37
  • Monoclinic, An external file that holds a picture, illustration, etc.
Object name is e-64-m1310-efi1.jpg
  • a = 11.7034 (1) Å
  • b = 14.5102 (2) Å
  • c = 15.0427 (2) Å
  • β = 91.532 (1)°
  • V = 2553.62 (5) Å3
  • Z = 4
  • Mo Kα radiation
  • μ = 1.35 mm−1
  • T = 100 (2) K
  • 0.20 × 0.10 × 0.05 mm

Data collection

  • Bruker SMART APEX diffractometer
  • Absorption correction: multi-scan (SADABS; Sheldrick, 1996 [triangle]) T min = 0.774, T max = 0.936
  • 22819 measured reflections
  • 5836 independent reflections
  • 5092 reflections with I > 2σ(I)
  • R int = 0.046

Refinement

  • R[F 2 > 2σ(F 2)] = 0.067
  • wR(F 2) = 0.224
  • S = 1.38
  • 5836 reflections
  • 359 parameters
  • H-atom parameters constrained
  • Δρmax = 1.77 e Å−3
  • Δρmin = −1.33 e Å−3

Data collection: APEX2 (Bruker, 2007 [triangle]); cell refinement: SAINT (Bruker, 2007 [triangle]); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 [triangle]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 [triangle]); molecular graphics: X-SEED (Barbour, 2001 [triangle]); software used to prepare material for publication: publCIF (Westrip, 2008 [triangle]).

Table 1
Hydrogen-bond geometry (Å, °)

Supplementary Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536808029681/tk2306sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808029681/tk2306Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Acknowledgments

We thank the University of Malaya (JPJ Vote) for supporting this sudy.

supplementary crystallographic information

Experimental

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

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.

Figures

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.

Crystal data

[Cr3(C2H3O2)6O(H2O)3]NO3·C2H4O2F(000) = 1436
Mr = 702.37Dx = 1.827 Mg m3
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 mm1
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

Bruker SMART APEX diffractometer5836 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

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 = 1.38w = 1/[σ2(Fo2) + (0.1P)2 + 1P] where P = (Fo2 + 2Fc2)/3
5836 reflections(Δ/σ)max = 0.001
359 parametersΔρmax = 1.77 e Å3
0 restraintsΔρmin = −1.33 e Å3

Special details

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)

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)

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, °)

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, °)

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.

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: TK2306).

References

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