Hexa-μ2-acetato-κ12O:O′-μ3-oxido-tris­[aqua­chromium(III)] nitrate acetic acid solvate

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

doi:10.1107/S1600536808029681

metal-organic compounds

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ISSN: 2056-9890

Volume 64| Part 10| October 2008| Page m1310

doi:10.1107/S1600536808029681

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Hexa-μ₂-acetato-κ¹²O:O′-μ₃-oxido-tris[aquachromium(III)] nitrate acetic acid solvate

Mohd Jamil Maah,^a ^* Che Ibrahim Abdullah,^a Seng Neon Gan,^a Aishah Mohd Jelan ^b and Seik Weng Ng ^a

^aDepartment of Chemistry, University of Malaya, 50603 Kuala Lumpur, Malaysia, and ^bCentre for Foundation Studies in Science, University of Malaya, 50603 Kuala Lumpur, Malaysia
^*Correspondence e-mail: mjamil@um.edu.my

(Received 15 September 2008; accepted 16 September 2008; online 24 September 2008)

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 Cr^III 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 ); Fujihara et al. (1998 ); Glowiak et al. (1996 ); Karu et al. (1993 ); Winpenny et al. (2005 ).

Experimental

Crystal data

[Cr₃(C₂H₃O₂)₆O(H₂O)₃]NO₃·C₂H₄O₂
M_r = 702.37
Monoclinic, P 2₁ /c
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 ) 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[F² > 2σ(F²)] = 0.067
wR(F²) = 0.224
S = 1.38
5836 reflections
359 parameters
H-atom parameters constrained
Δρ_max = 1.77 e Å⁻³
Δρ_min = −1.33 e Å⁻³

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1w—H11⋯O16	0.84	1.96	2.769 (6)	162
O1w—H12⋯O12ⁱ	0.84	2.06	2.873 (5)	162
O2w—H21⋯O14	0.84	1.92	2.668 (6)	147
O2w—H22⋯O18ⁱⁱ	0.84	1.93	2.725 (6)	157
O3w—H31⋯O14ⁱⁱⁱ	0.84	2.28	2.781 (5)	118
O3w—H32⋯O5ⁱⁱⁱ	0.84	2.42	3.244 (6)	165
O15—H15⋯O18^iv	0.84	1.81	2.624 (6)	163
Symmetry codes: (i) -x+1, -y+1, -z+1; (ii) $[-x+1, y-{\script{1\over 2}}, -z+{\script{3\over 2}}]$ ; (iii) $[x, -y+{\script{3\over 2}}, z-{\script{1\over 2}}]$ ; (iv) $[x-1, -y+{\script{3\over 2}}, z+{\script{1\over 2}}]$ .

Data collection: APEX2 (Bruker, 2007 ); cell refinement: SAINT (Bruker, 2007); data reduction: SAINT; 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 ).

Supporting information

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

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

checkCIF report

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%.

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

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·C₂H₄O₂	F(000) = 1436
M_r = 702.37	D_x = 1.827 Mg m⁻³
Monoclinic, P2₁/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 9927 reflections
a = 11.7034 (1) Å	θ = 2.2–28.2°
b = 14.5102 (2) Å	µ = 1.35 mm⁻¹
c = 15.0427 (2) Å	T = 100 K
β = 91.532 (1)°	Chip, green
V = 2553.62 (5) Å³	0.20 × 0.10 × 0.05 mm
Z = 4

Data collection top

Bruker SMART APEX diffractometer	5836 independent reflections
Radiation source: fine-focus sealed tube	5092 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.046
ω scans	θ_max = 27.5°, θ_min = 2.0°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −15→15
T_min = 0.774, T_max = 0.936	k = −18→18
22819 measured reflections	l = −19→19

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.067	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.224	H-atom parameters constrained
S = 1.38	w = 1/[σ²(F_o²) + (0.1P)² + 1P] where P = (F_o² + 2F_c²)/3
5836 reflections	(Δ/σ)_max = 0.001
359 parameters	Δρ_max = 1.77 e Å⁻³
0 restraints	Δρ_min = −1.33 e Å⁻³

Crystal data top

[Cr₃(C₂H₃O₂)₆O(H₂O)₃]NO₃·C₂H₄O₂	V = 2553.62 (5) Å³
M_r = 702.37	Z = 4
Monoclinic, P2₁/c	Mo Kα radiation
a = 11.7034 (1) Å	µ = 1.35 mm⁻¹
b = 14.5102 (2) Å	T = 100 K
c = 15.0427 (2) Å	0.20 × 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)
T_min = 0.774, T_max = 0.936	R_int = 0.046
22819 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.067	0 restraints
wR(F²) = 0.224	H-atom parameters constrained
S = 1.38	Δρ_max = 1.77 e Å⁻³
5836 reflections	Δρ_min = −1.33 e Å⁻³
359 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.

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

	x	y	z	U_iso*/U_eq
Cr1	0.40542 (6)	0.60336 (5)	0.62841 (5)	0.0131 (2)
Cr2	0.17034 (6)	0.56625 (5)	0.73703 (5)	0.0135 (2)
Cr3	0.18005 (6)	0.73269 (6)	0.58877 (5)	0.0140 (2)
O1	0.4536 (3)	0.6151 (3)	0.7549 (2)	0.0198 (8)
O2	0.2966 (3)	0.5724 (3)	0.8261 (3)	0.0205 (8)
O3	0.3914 (3)	0.4689 (3)	0.6374 (3)	0.0184 (7)
O4	0.2208 (3)	0.4442 (3)	0.6949 (3)	0.0198 (8)
O5	0.1056 (3)	0.6751 (3)	0.7966 (3)	0.0195 (7)
O6	0.0969 (3)	0.7819 (3)	0.6894 (3)	0.0195 (8)
O7	0.0316 (3)	0.5543 (3)	0.6608 (3)	0.0189 (7)
O8	0.0452 (3)	0.6588 (3)	0.5512 (3)	0.0192 (7)
O9	0.3030 (3)	0.8221 (3)	0.6195 (2)	0.0174 (7)
O10	0.4560 (3)	0.7309 (3)	0.6132 (3)	0.0193 (8)
O11	0.2517 (3)	0.7039 (3)	0.4743 (2)	0.0176 (7)
O12	0.3748 (3)	0.5871 (3)	0.4972 (2)	0.0172 (7)
O13	0.2517 (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	−0.2433	0.6221	0.9951	0.045*
O16	0.7058 (3)	0.7280 (3)	0.5673 (3)	0.0267 (9)
O17	0.8176 (4)	0.7184 (3)	0.6842 (3)	0.0290 (9)
O18	0.8263 (4)	0.8364 (3)	0.5964 (3)	0.0358 (11)
O1W	0.5731 (3)	0.5752 (3)	0.6032 (2)	0.0172 (7)
H11	0.6042	0.6224	0.5825	0.026*
H12	0.5765	0.5321	0.5662	0.026*
O2W	0.0843 (3)	0.4914 (3)	0.8268 (3)	0.0200 (8)
H21	0.0592	0.5266	0.8661	0.030*
H22	0.1285	0.4524	0.8505	0.030*
O3W	0.1111 (3)	0.8387 (3)	0.5119 (3)	0.0222 (8)
H31	0.0424	0.8465	0.5247	0.033*
H32	0.1152	0.8250	0.4578	0.033*
N1	0.7827 (4)	0.7597 (3)	0.6176 (3)	0.0214 (9)
C1	0.3976 (4)	0.6011 (3)	0.8241 (3)	0.0161 (9)
C2	0.4557 (5)	0.6207 (4)	0.9128 (4)	0.0213 (10)
H2A	0.4404	0.6845	0.9302	0.032*
H2B	0.5383	0.6116	0.9081	0.032*
H2C	0.4260	0.5787	0.9577	0.032*
C3	0.3122 (4)	0.4166 (4)	0.6615 (3)	0.0163 (9)
C4	0.3268 (5)	0.3144 (4)	0.6485 (4)	0.0233 (11)
H4A	0.3005	0.2816	0.7011	0.035*
H4B	0.4077	0.3005	0.6398	0.035*
H4C	0.2818	0.2946	0.5961	0.035*
C5	0.0764 (4)	0.7537 (4)	0.7646 (4)	0.0175 (10)
C6	0.0117 (5)	0.8165 (4)	0.8254 (4)	0.0213 (11)
H6A	−0.0703	0.8035	0.8194	0.032*
H6B	0.0259	0.8809	0.8092	0.032*
H6C	0.0375	0.8060	0.8871	0.032*
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	−0.1116	0.5672	0.4823	0.033*
H8B	−0.1771	0.5854	0.5727	0.033*
H8C	−0.1154	0.4886	0.5567	0.033*
C9	0.4087 (4)	0.8085 (4)	0.6238 (3)	0.0163 (9)
C10	0.4856 (5)	0.8895 (4)	0.6411 (4)	0.0214 (11)
H10A	0.4417	0.9466	0.6336	0.032*
H10B	0.5480	0.8887	0.5991	0.032*
H10C	0.5172	0.8862	0.7020	0.032*
C11	0.3182 (4)	0.6420 (3)	0.4472 (3)	0.0154 (9)
C12	0.3291 (5)	0.6330 (4)	0.3480 (3)	0.0213 (10)
H12A	0.2693	0.5918	0.3244	0.032*
H12B	0.4044	0.6076	0.3349	0.032*
H12C	0.3208	0.6939	0.3203	0.032*
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	−0.1439	0.5463	0.7679	0.033*
H14B	−0.2763	0.5515	0.7914	0.033*
H14C	−0.2040	0.4606	0.8148	0.033*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Cr1	0.0129 (4)	0.0149 (4)	0.0115 (4)	0.0003 (3)	0.0011 (3)	0.0001 (3)
Cr2	0.0135 (4)	0.0149 (4)	0.0123 (4)	0.0005 (3)	0.0018 (3)	−0.0001 (3)
Cr3	0.0134 (4)	0.0149 (4)	0.0136 (4)	0.0010 (3)	0.0001 (3)	−0.0013 (3)
O1	0.0163 (16)	0.029 (2)	0.0142 (17)	−0.0013 (14)	0.0007 (13)	0.0001 (15)
O2	0.0194 (18)	0.027 (2)	0.0154 (17)	−0.0023 (15)	0.0007 (14)	0.0032 (15)
O3	0.0155 (16)	0.0158 (17)	0.0241 (19)	0.0014 (13)	0.0044 (14)	0.0029 (14)
O4	0.0209 (18)	0.0149 (17)	0.0239 (19)	−0.0013 (14)	0.0088 (15)	−0.0018 (14)
O5	0.0207 (17)	0.0184 (18)	0.0194 (18)	0.0023 (14)	0.0033 (14)	−0.0001 (15)
O6	0.0187 (17)	0.0204 (18)	0.0196 (19)	0.0021 (14)	0.0020 (14)	−0.0027 (15)
O7	0.0152 (16)	0.0233 (19)	0.0182 (18)	−0.0021 (14)	0.0017 (13)	0.0031 (15)
O8	0.0177 (17)	0.0194 (18)	0.0205 (18)	0.0000 (14)	−0.0014 (14)	−0.0024 (15)
O9	0.0172 (17)	0.0167 (17)	0.0182 (17)	−0.0009 (13)	−0.0010 (13)	0.0004 (14)
O10	0.0164 (17)	0.0166 (17)	0.025 (2)	0.0004 (13)	0.0038 (14)	0.0010 (15)
O11	0.0204 (17)	0.0190 (18)	0.0136 (17)	0.0005 (14)	0.0010 (13)	0.0003 (14)
O12	0.0171 (17)	0.0208 (18)	0.0136 (16)	0.0012 (14)	0.0011 (13)	−0.0022 (14)
O13	0.0131 (15)	0.0175 (17)	0.0135 (16)	0.0007 (13)	0.0020 (12)	−0.0006 (13)
O14	0.0195 (18)	0.029 (2)	0.029 (2)	−0.0017 (16)	0.0010 (16)	−0.0053 (17)
O15	0.022 (2)	0.042 (3)	0.025 (2)	0.0091 (18)	−0.0012 (16)	−0.0096 (19)
O16	0.0219 (19)	0.026 (2)	0.032 (2)	−0.0049 (16)	−0.0010 (17)	0.0024 (18)
O17	0.043 (2)	0.028 (2)	0.0164 (19)	0.0016 (18)	0.0006 (17)	0.0017 (16)
O18	0.051 (3)	0.026 (2)	0.030 (2)	−0.017 (2)	−0.010 (2)	0.0036 (19)
O1W	0.0153 (16)	0.0180 (17)	0.0184 (18)	−0.0002 (13)	0.0038 (13)	−0.0010 (14)
O2W	0.0204 (17)	0.0196 (18)	0.0205 (18)	0.0039 (14)	0.0079 (14)	0.0009 (15)
O3W	0.0213 (18)	0.0214 (19)	0.024 (2)	0.0047 (15)	−0.0029 (15)	−0.0008 (16)
N1	0.028 (2)	0.021 (2)	0.016 (2)	−0.0016 (18)	0.0057 (18)	−0.0024 (18)
C1	0.018 (2)	0.017 (2)	0.013 (2)	0.0040 (18)	−0.0013 (18)	−0.0018 (18)
C2	0.020 (2)	0.025 (3)	0.018 (3)	0.001 (2)	−0.0008 (19)	−0.005 (2)
C3	0.017 (2)	0.018 (2)	0.013 (2)	0.0020 (18)	−0.0011 (18)	−0.0007 (18)
C4	0.023 (3)	0.016 (2)	0.032 (3)	−0.001 (2)	0.008 (2)	−0.004 (2)
C5	0.013 (2)	0.019 (2)	0.020 (2)	−0.0014 (18)	−0.0020 (18)	−0.005 (2)
C6	0.025 (3)	0.023 (3)	0.016 (2)	0.007 (2)	0.002 (2)	−0.006 (2)
C7	0.013 (2)	0.022 (2)	0.017 (2)	0.0019 (18)	0.0024 (18)	−0.0037 (19)
C8	0.018 (2)	0.023 (3)	0.024 (3)	0.0000 (19)	−0.001 (2)	−0.003 (2)
C9	0.018 (2)	0.021 (2)	0.010 (2)	−0.0031 (18)	0.0006 (17)	0.0007 (18)
C10	0.020 (2)	0.021 (3)	0.023 (3)	−0.004 (2)	0.001 (2)	−0.002 (2)
C11	0.014 (2)	0.016 (2)	0.016 (2)	−0.0016 (17)	0.0007 (17)	−0.0026 (18)
C12	0.026 (3)	0.027 (3)	0.011 (2)	0.004 (2)	0.0006 (19)	−0.001 (2)
C13	0.019 (2)	0.018 (2)	0.022 (3)	−0.0010 (18)	−0.002 (2)	0.001 (2)
C14	0.024 (3)	0.027 (3)	0.015 (2)	−0.002 (2)	−0.001 (2)	−0.002 (2)

Geometric parameters (Å, º) top

Cr1—O13	1.893 (3)	O18—N1	1.268 (7)
Cr1—O10	1.959 (4)	O1W—H11	0.8400
Cr1—O3	1.962 (4)	O1W—H12	0.8400
Cr1—O1	1.978 (4)	O2W—H21	0.8400
Cr1—O12	2.010 (4)	O2W—H22	0.8400
Cr1—O1W	2.049 (4)	O3W—H31	0.8400
Cr2—O13	1.901 (4)	O3W—H32	0.8400
Cr2—O2	1.969 (4)	C1—C2	1.509 (7)
Cr2—O7	1.970 (4)	C2—H2A	0.9800
Cr2—O5	1.976 (4)	C2—H2B	0.9800
Cr2—O4	1.977 (4)	C2—H2C	0.9800
Cr2—O2W	2.022 (4)	C3—C4	1.506 (7)
Cr3—O13	1.894 (4)	C4—H4A	0.9800
Cr3—O6	1.956 (4)	C4—H4B	0.9800
Cr3—O8	1.978 (4)	C4—H4C	0.9800
Cr3—O11	1.980 (4)	C5—C6	1.511 (7)
Cr3—O9	1.982 (4)	C6—H6A	0.9800
Cr3—O3W	2.075 (4)	C6—H6B	0.9800
O1—C1	1.260 (6)	C6—H6C	0.9800
O2—C1	1.255 (7)	C7—C8	1.508 (7)
O3—C3	1.259 (6)	C8—H8A	0.9800
O4—C3	1.259 (6)	C8—H8B	0.9800
O5—C5	1.281 (7)	C8—H8C	0.9800
O6—C5	1.233 (7)	C9—C10	1.498 (7)
O7—C7	1.272 (6)	C10—H10A	0.9800
O8—C7	1.254 (7)	C10—H10B	0.9800
O9—C9	1.254 (6)	C10—H10C	0.9800
O10—C9	1.267 (7)	C11—C12	1.507 (7)
O11—C11	1.263 (6)	C12—H12A	0.9800
O12—C11	1.269 (6)	C12—H12B	0.9800
O14—C13	1.236 (7)	C12—H12C	0.9800
O15—C13	1.300 (7)	C13—C14	1.492 (7)
O15—H15	0.8400	C14—H14A	0.9800
O16—N1	1.247 (6)	C14—H14B	0.9800
O17—N1	1.228 (6)	C14—H14C	0.9800

O13—Cr1—O10	95.17 (16)	Cr3—O3W—H32	109.5
O13—Cr1—O3	98.06 (15)	H31—O3W—H32	109.5
O10—Cr1—O3	166.77 (16)	O17—N1—O16	122.2 (5)
O13—Cr1—O1	93.10 (15)	O17—N1—O18	120.4 (5)
O10—Cr1—O1	87.24 (17)	O16—N1—O18	117.4 (5)
O3—Cr1—O1	92.37 (17)	O2—C1—O1	125.7 (5)
O13—Cr1—O12	93.38 (15)	O2—C1—C2	116.4 (5)
O10—Cr1—O12	92.45 (16)	O1—C1—C2	117.9 (5)
O3—Cr1—O12	86.44 (16)	C1—C2—H2A	109.5
O1—Cr1—O12	173.51 (15)	C1—C2—H2B	109.5
O13—Cr1—O1W	177.86 (16)	H2A—C2—H2B	109.5
O10—Cr1—O1W	82.69 (15)	C1—C2—H2C	109.5
O3—Cr1—O1W	84.09 (15)	H2A—C2—H2C	109.5
O1—Cr1—O1W	86.87 (15)	H2B—C2—H2C	109.5
O12—Cr1—O1W	86.66 (15)	O4—C3—O3	124.2 (5)
O13—Cr2—O2	93.38 (15)	O4—C3—C4	117.7 (5)
O13—Cr2—O7	93.98 (15)	O3—C3—C4	118.0 (5)
O2—Cr2—O7	172.47 (16)	C3—C4—H4A	109.5
O13—Cr2—O5	95.72 (16)	C3—C4—H4B	109.5
O2—Cr2—O5	86.87 (17)	H4A—C4—H4B	109.5
O7—Cr2—O5	90.83 (16)	C3—C4—H4C	109.5
O13—Cr2—O4	94.97 (16)	H4A—C4—H4C	109.5
O2—Cr2—O4	91.88 (17)	H4B—C4—H4C	109.5
O7—Cr2—O4	89.05 (17)	O6—C5—O5	125.8 (5)
O5—Cr2—O4	169.29 (17)	O6—C5—C6	117.9 (5)
O13—Cr2—O2W	178.67 (16)	O5—C5—C6	116.3 (5)
O2—Cr2—O2W	87.02 (16)	C5—C6—H6A	109.5
O7—Cr2—O2W	85.66 (16)	C5—C6—H6B	109.5
O5—Cr2—O2W	85.56 (16)	H6A—C6—H6B	109.5
O4—Cr2—O2W	83.75 (16)	C5—C6—H6C	109.5
O13—Cr3—O6	96.66 (16)	H6A—C6—H6C	109.5
O13—Cr3—O8	94.10 (15)	H6B—C6—H6C	109.5
O6—Cr3—O8	90.55 (16)	O8—C7—O7	125.8 (5)
O13—Cr3—O11	94.52 (15)	O8—C7—C8	117.8 (5)
O6—Cr3—O11	168.79 (16)	O7—C7—C8	116.4 (5)
O8—Cr3—O11	89.43 (16)	C7—C8—H8A	109.5
O13—Cr3—O9	94.02 (15)	C7—C8—H8B	109.5
O6—Cr3—O9	87.33 (16)	H8A—C8—H8B	109.5
O8—Cr3—O9	171.80 (16)	C7—C8—H8C	109.5
O11—Cr3—O9	91.12 (16)	H8A—C8—H8C	109.5
O13—Cr3—O3W	175.13 (16)	H8B—C8—H8C	109.5
O6—Cr3—O3W	88.07 (16)	O9—C9—O10	124.6 (5)
O8—Cr3—O3W	86.97 (16)	O9—C9—C10	118.2 (5)
O11—Cr3—O3W	80.73 (16)	O10—C9—C10	117.2 (4)
O9—Cr3—O3W	85.05 (16)	C9—C10—H10A	109.5
C1—O1—Cr1	129.8 (3)	C9—C10—H10B	109.5
C1—O2—Cr2	133.6 (3)	H10A—C10—H10B	109.5
C3—O3—Cr1	133.1 (3)	C9—C10—H10C	109.5
C3—O4—Cr2	132.6 (3)	H10A—C10—H10C	109.5
C5—O5—Cr2	130.0 (4)	H10B—C10—H10C	109.5
C5—O6—Cr3	134.5 (4)	O11—C11—O12	124.9 (5)
C7—O7—Cr2	133.8 (3)	O11—C11—C12	116.7 (5)
C7—O8—Cr3	130.4 (3)	O12—C11—C12	118.4 (4)
C9—O9—Cr3	128.2 (3)	C11—C12—H12A	109.5
C9—O10—Cr1	133.7 (3)	C11—C12—H12B	109.5
C11—O11—Cr3	135.2 (3)	H12A—C12—H12B	109.5
C11—O12—Cr1	125.8 (3)	C11—C12—H12C	109.5
Cr1—O13—Cr3	119.96 (19)	H12A—C12—H12C	109.5
Cr1—O13—Cr2	119.74 (18)	H12B—C12—H12C	109.5
Cr3—O13—Cr2	120.30 (18)	O14—C13—O15	121.9 (5)
C13—O15—H15	120.0	O14—C13—C14	122.9 (5)
Cr1—O1W—H11	109.5	O15—C13—C14	115.2 (5)
Cr1—O1W—H12	109.5	C13—C14—H14A	109.5
H11—O1W—H12	109.5	C13—C14—H14B	109.5
Cr2—O2W—H21	109.5	H14A—C14—H14B	109.5
Cr2—O2W—H22	109.5	C13—C14—H14C	109.5
H21—O2W—H22	109.5	H14A—C14—H14C	109.5
Cr3—O3W—H31	109.5	H14B—C14—H14C	109.5

O13—Cr1—O1—C1	30.3 (5)	O10—Cr1—O12—C11	−49.0 (4)
O10—Cr1—O1—C1	125.3 (5)	O3—Cr1—O12—C11	144.2 (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—Cr3	37.4 (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—Cr3	124.9 (2)
O4—Cr2—O2—C1	88.3 (5)	O12—Cr1—O13—Cr3	−55.4 (2)
O2W—Cr2—O2—C1	171.9 (5)	O10—Cr1—O13—Cr2	−142.1 (2)
O13—Cr1—O3—C3	−8.3 (5)	O3—Cr1—O13—Cr2	38.2 (2)
O10—Cr1—O3—C3	173.3 (6)	O1—Cr1—O13—Cr2	−54.6 (2)
O1—Cr1—O3—C3	85.2 (5)	O12—Cr1—O13—Cr2	125.1 (2)
O12—Cr1—O3—C3	−101.2 (5)	O6—Cr3—O13—Cr1	−140.3 (2)
O1W—Cr1—O3—C3	171.8 (5)	O8—Cr3—O13—Cr1	128.7 (2)
O13—Cr2—O4—C3	33.4 (5)	O11—Cr3—O13—Cr1	38.9 (2)
O2—Cr2—O4—C3	−60.2 (5)	O9—Cr3—O13—Cr1	−52.5 (2)
O7—Cr2—O4—C3	127.3 (5)	O6—Cr3—O13—Cr2	39.2 (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—C5	31.9 (4)	O9—Cr3—O13—Cr2	127.0 (2)
O2—Cr2—O5—C5	125.0 (4)	O2—Cr2—O13—Cr1	46.6 (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—Cr1	133.8 (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—C5	82.1 (5)	O7—Cr2—O13—Cr3	45.5 (2)
O11—Cr3—O6—C5	171.9 (7)	O5—Cr2—O13—Cr3	−45.7 (2)
O9—Cr3—O6—C5	−105.9 (5)	O4—Cr2—O13—Cr3	134.9 (2)
O3W—Cr3—O6—C5	169.0 (5)	Cr2—O2—C1—O1	−18.2 (8)
O13—Cr2—O7—C7	−12.7 (5)	Cr2—O2—C1—C2	161.6 (4)
O5—Cr2—O7—C7	83.1 (5)	Cr1—O1—C1—O2	3.0 (8)
O4—Cr2—O7—C7	−107.6 (5)	Cr1—O1—C1—C2	−176.8 (4)
O2W—Cr2—O7—C7	168.6 (5)	Cr2—O4—C3—O3	−9.0 (8)
O13—Cr3—O8—C7	30.7 (5)	Cr2—O4—C3—C4	171.8 (4)
O6—Cr3—O8—C7	−66.0 (5)	Cr1—O3—C3—O4	−6.9 (8)
O11—Cr3—O8—C7	125.2 (5)	Cr1—O3—C3—C4	172.3 (4)
O3W—Cr3—O8—C7	−154.0 (5)	Cr3—O6—C5—O5	−2.5 (8)
O13—Cr3—O9—C9	38.7 (4)	Cr3—O6—C5—C6	177.2 (4)
O6—Cr3—O9—C9	135.2 (4)	Cr2—O5—C5—O6	−10.0 (8)
O11—Cr3—O9—C9	−55.9 (4)	Cr2—O5—C5—C6	170.3 (3)
O3W—Cr3—O9—C9	−136.5 (4)	Cr3—O8—C7—O7	−3.7 (8)
O13—Cr1—O10—C9	6.9 (5)	Cr3—O8—C7—C8	174.9 (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—C8	173.6 (4)
O12—Cr1—O10—C9	100.5 (5)	Cr3—O9—C9—O10	−3.9 (7)
O1W—Cr1—O10—C9	−173.2 (5)	Cr3—O9—C9—C10	174.9 (3)
O13—Cr3—O11—C11	2.2 (5)	Cr1—O10—C9—O9	−25.2 (8)
O6—Cr3—O11—C11	178.1 (7)	Cr1—O10—C9—C10	155.9 (4)
O8—Cr3—O11—C11	−91.9 (5)	Cr3—O11—C11—O12	−13.8 (8)
O9—Cr3—O11—C11	96.3 (5)	Cr3—O11—C11—C12	165.6 (4)
O3W—Cr3—O11—C11	−178.9 (5)	Cr1—O12—C11—O11	−16.4 (7)
O13—Cr1—O12—C11	46.3 (4)	Cr1—O12—C11—C12	164.2 (4)

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1w—H11···O16	0.84	1.96	2.769 (6)	162
O1w—H12···O12ⁱ	0.84	2.06	2.873 (5)	162
O2w—H21···O14	0.84	1.92	2.668 (6)	147
O2w—H22···O18ⁱⁱ	0.84	1.93	2.725 (6)	157
O3w—H31···O14ⁱⁱⁱ	0.84	2.28	2.781 (5)	118
O3w—H32···O5ⁱⁱⁱ	0.84	2.42	3.244 (6)	165
O15—H15···O18^iv	0.84	1.81	2.624 (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.

Experimental details

Crystal data
Chemical formula	[Cr₃(C₂H₃O₂)₆O(H₂O)₃]NO₃·C₂H₄O₂
M_r	702.37
Crystal system, space group	Monoclinic, P2₁/c
Temperature (K)	100
a, b, c (Å)	11.7034 (1), 14.5102 (2), 15.0427 (2)
β (°)	91.532 (1)
V (Å³)	2553.62 (5)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	1.35
Crystal size (mm)	0.20 × 0.10 × 0.05

Data collection
Diffractometer	Bruker SMART APEX diffractometer
Absorption correction	Multi-scan (SADABS; Sheldrick, 1996)
T_min, T_max	0.774, 0.936
No. of measured, independent and observed [I > 2σ(I)] reflections	22819, 5836, 5092
R_int	0.046
(sin θ/λ)_max (Å⁻¹)	0.650

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.067, 0.224, 1.38
No. of reflections	5836
No. of parameters	359
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	1.77, −1.33

Computer programs: APEX2 (Bruker, 2007), SAINT (Bruker, 2007), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), X-SEED (Barbour, 2001), publCIF (Westrip, 2008).

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1w—H11···O16	0.84	1.96	2.769 (6)	162
O1w—H12···O12ⁱ	0.84	2.06	2.873 (5)	162
O2w—H21···O14	0.84	1.92	2.668 (6)	147
O2w—H22···O18ⁱⁱ	0.84	1.93	2.725 (6)	157
O3w—H31···O14ⁱⁱⁱ	0.84	2.28	2.781 (5)	118
O3w—H32···O5ⁱⁱⁱ	0.84	2.42	3.244 (6)	165
O15—H15···O18^iv	0.84	1.81	2.624 (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

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

References

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