Diaqua-μ3-oxido-hexa­kis(μ2-trichloro­acetato-κ2O:O′)(trichloro­acetato-κO)trichromium(III) acetonitrile tris­olvate

Soume, B.B.M.D.; Yahya, R.; Gan, S.N.; Ng, S.W.

doi:10.1107/S1600536808025798

metal-organic compounds

CRYSTALLOGRAPHIC
COMMUNICATIONS

ISSN: 2056-9890

Volume 64| Part 9| September 2008| Page m1175

doi:10.1107/S1600536808025798

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Diaqua-μ₃-oxido-hexakis(μ₂-trichloroacetato-κ²O:O′)(trichloroacetato-κO)trichromium(III) acetonitrile trisolvate

B. B. Mougang D. Soume,^a Rosiyah Yahya,^a Seng Neon Gan ^a and Seik Weng Ng ^a ^*

^aDepartment of Chemistry, University of Malaya, 50603 Kuala Lumpur, Malaysia
^*Correspondence e-mail: seikweng@um.edu.my

(Received 8 August 2008; accepted 11 August 2008; online 16 August 2008)

In the crystal structure of the title compound, [Cr₃(C₂Cl₃O₂)₇O(H₂O)₂]·3CH₃CN, the trinuclear [Cr₃O(H₂O)₂(Cl₃CCO₂)₇] molecule has an oxide O atom that is connected to one monodentate trichloroacetate-coordinated and two water-coordinated Cr^III atoms, the three metal atoms forming the points of an equilateral triangle. Each of the six remaining carboxylate groups bridges a Cr–O–Cr fragment. The cluster interacts with the three solvent molecules through water–acetonitrile O—H⋯N hydrogen bonds. Adjacent clusters are linked by a water–carboxylate O—H⋯O hydrogen bond to give a helical chain. One of the CCl₃ groups was found to be disordered over two positions, with the major component having a site-occupancy factor of 0.64 (1).

Related literature

Oxo-centred chromium(III) chloroacetates form an efficient class of Zigler–Natta catalysts for the polymerization of olefins; see: Gan et al. (2000 ).

Experimental

Crystal data

[Cr₃(C₂Cl₃O₂)₇O(H₂O)₂]·3C₂H₃N
M_r = 1467.78
Monoclinic, P 2₁ /n
a = 11.6307 (6) Å
b = 19.481 (1) Å
c = 22.949 (1) Å
β = 95.355 (1)°
V = 5177.0 (5) Å³
Z = 4
Mo Kα radiation
μ = 1.76 mm⁻¹
T = 100 (2) K
0.25 × 0.20 × 0.15 mm

Data collection

Bruker SMART APEX diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ) T_min = 0.667, T_max = 0.778
29504 measured reflections
11718 independent reflections
9590 reflections with I > 2σ(I)
R_int = 0.029

Refinement

R[F² > 2σ(F²)] = 0.041
wR(F²) = 0.118
S = 1.04
11718 reflections
624 parameters
72 restraints
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 1.42 e Å⁻³
Δρ_min = −0.74 e Å⁻³

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1w—H1w1⋯N1	0.84 (1)	1.97 (2)	2.791 (4)	166 (5)
O1w—H1w2⋯N2	0.85 (1)	1.97 (1)	2.810 (5)	173 (4)
O2w—H2w1⋯N3	0.85 (1)	1.88 (1)	2.719 (5)	171 (4)
O2w—H2w2⋯O2ⁱ	0.83 (1)	1.81 (1)	2.613 (3)	165 (4)
Symmetry code: (i) $[-x+{\script{3\over 2}}, y-{\script{1\over 2}}, -z+{\script{3\over 2}}]$ .

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 global, I. DOI: 10.1107/S1600536808025798/tk2293sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536808025798/tk2293Isup2.hkl

checkCIF report

Comment top

Oxo-centered chromium(III) chloroacetates form an efficient class of Zigler–Natta catalysts for the polymerization of olefins (Gan et al., 2000). The title trichloroacetate oxo-cluster crystallizes with acetonitrile (Scheme I, Fig. 1). In the crystal structure, the oxo-O atom is connected to one monodentate trichloroacetate-coordinated and two water-coordinated chromium(III) atoms, the three metal atoms forming the points of an equilateral triangle. Each of the six remaining carboxylate groups chelates a Cr–O–Cr fragment. The cluster interacts with the three solvate molecules through hydrogen bonds; hydrogen bonds involving the water molecule as a donor give rise to a helical chain that runs along the b-axis.

Related literature top

Oxo-centred chromium(III) chloroacetates form an efficient class of Zigler–Natta catalysts for the polymerization of olefins; see: Gan et al. (2000).

Experimental top

Chromium(III) chloride hexahydrate (10 g) was refluxed with trichloroacetic acid in a molar ratio of 1:6 for 6 h. The solution was filtered hot; the cooled solution yielded a green product that was washed with chloroform (90% yield). Analysis found: Cr, 11.13, C, 11.98, H, 0.72; Cr₃Cl₂₁C₁₄O₂₀H₁₀ requires: Cr, 11.15, C, 12.02, H, 0.72. Dark-green crystals of the acetonitrile solvate were obtained by recrystallization from an acetonitrile solution.

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 plot (Barbour, 2001) plot of [Cr₃O(H₂O)₂(Cl₃CCO₂)₇].3CH₃CN at the 70% probability level. Hydrogen atoms are drawn as spheres of arbitrary radius. For clarity, the minor disorder component is not shown. Hydrogen bonds are denoted by dashed lines.

Diaqua-µ₃-oxido-hexakis(µ₂-trichloroacetato- κ²O:O')(trichloroacetato-κO)trichromium(III) acetonitrile trisolvate top

Crystal data top

[Cr₃(C₂Cl₃O₂)₇O(H₂O)₂]·3C₂H₃N	F(000) = 2876
M_r = 1467.78	D_x = 1.883 Mg m⁻³
Monoclinic, P2₁/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 9535 reflections
a = 11.6307 (6) Å	θ = 2.2–28.2°
b = 19.481 (1) Å	µ = 1.76 mm⁻¹
c = 22.949 (1) Å	T = 100 K
β = 95.355 (1)°	Block, green
V = 5177.0 (5) Å³	0.25 × 0.20 × 0.15 mm
Z = 4

Data collection top

Bruker SMART APEX diffractometer	11718 independent reflections
Radiation source: fine-focus sealed tube	9590 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.029
ω scans	θ_max = 27.5°, θ_min = 1.4°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −15→11
T_min = 0.667, T_max = 0.778	k = −25→25
29504 measured reflections	l = −29→29

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)] = 0.041	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.118	H atoms treated by a mixture of independent and constrained refinement
S = 1.04	w = 1/[σ²(F_o²) + (0.0626P)² + 7.2035P] where P = (F_o² + 2F_c²)/3
11718 reflections	(Δ/σ)_max = 0.001
624 parameters	Δρ_max = 1.42 e Å⁻³
72 restraints	Δρ_min = −0.74 e Å⁻³

Crystal data top

[Cr₃(C₂Cl₃O₂)₇O(H₂O)₂]·3C₂H₃N	V = 5177.0 (5) Å³
M_r = 1467.78	Z = 4
Monoclinic, P2₁/n	Mo Kα radiation
a = 11.6307 (6) Å	µ = 1.76 mm⁻¹
b = 19.481 (1) Å	T = 100 K
c = 22.949 (1) Å	0.25 × 0.20 × 0.15 mm
β = 95.355 (1)°

Data collection top

Bruker SMART APEX diffractometer	11718 independent reflections
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	9590 reflections with I > 2σ(I)
T_min = 0.667, T_max = 0.778	R_int = 0.029
29504 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.041	72 restraints
wR(F²) = 0.118	H atoms treated by a mixture of independent and constrained refinement
S = 1.04	Δρ_max = 1.42 e Å⁻³
11718 reflections	Δρ_min = −0.74 e Å⁻³
624 parameters

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

	x	y	z	U_iso*/U_eq	Occ. (<1)
Cr1	0.74255 (4)	0.76778 (3)	0.70072 (2)	0.01404 (12)
Cr2	0.68641 (4)	0.73747 (3)	0.83719 (2)	0.01277 (11)
Cr3	0.72390 (4)	0.60693 (3)	0.74830 (2)	0.01179 (11)
Cl1	0.96872 (8)	0.85657 (6)	0.56393 (4)	0.0333 (2)
Cl2	0.89615 (9)	0.99687 (5)	0.57400 (4)	0.0345 (2)
Cl3	0.73830 (8)	0.89677 (4)	0.52068 (3)	0.02158 (18)
Cl4	0.36046 (10)	0.88419 (6)	0.80350 (5)	0.0431 (3)
Cl5	0.35756 (9)	0.81589 (5)	0.69151 (5)	0.0430 (3)
Cl6	0.46821 (8)	0.94801 (4)	0.70989 (4)	0.02438 (19)
Cl7	0.98178 (10)	0.88074 (7)	0.90381 (5)	0.0451 (3)
Cl8	1.09295 (9)	0.78569 (5)	0.83228 (5)	0.0346 (2)
Cl9	1.03479 (9)	0.92225 (5)	0.78947 (5)	0.0356 (2)
Cl10	0.44418 (9)	0.70978 (5)	0.55064 (4)	0.0322 (2)
Cl11	0.38086 (9)	0.61375 (7)	0.63683 (5)	0.0399 (3)
Cl12	0.53908 (9)	0.57331 (5)	0.55303 (4)	0.0336 (2)
Cl13	0.9998 (4)	0.6385 (3)	0.58065 (14)	0.0556 (10)	0.636 (12)
Cl14	1.1108 (2)	0.71821 (13)	0.67552 (16)	0.0352 (8)	0.636 (12)
Cl15	1.0981 (8)	0.5711 (3)	0.6842 (4)	0.0316 (13)	0.636 (12)
Cl3'	0.9729 (10)	0.6101 (9)	0.5847 (3)	0.105 (5)	0.364 (12)
Cl4'	1.1068 (6)	0.7141 (3)	0.6463 (8)	0.103 (3)	0.364 (12)
Cl5'	1.1046 (14)	0.5774 (5)	0.6926 (7)	0.0252 (17)	0.364 (12)
Cl16	0.31914 (8)	0.66992 (5)	0.78820 (4)	0.0287 (2)
Cl17	0.35454 (8)	0.52405 (5)	0.79999 (4)	0.0292 (2)
Cl18	0.37880 (7)	0.61005 (4)	0.90215 (3)	0.01931 (17)
Cl19	0.93022 (8)	0.51554 (5)	0.92623 (4)	0.0272 (2)
Cl20	0.99064 (8)	0.65247 (6)	0.96451 (4)	0.0344 (2)
Cl21	1.07222 (7)	0.60054 (5)	0.85829 (4)	0.02607 (19)
O1	0.7710 (2)	0.82999 (12)	0.63619 (10)	0.0187 (5)
O2	0.8135 (3)	0.93428 (14)	0.67484 (11)	0.0281 (6)
O3	0.6252 (2)	0.83313 (12)	0.72363 (10)	0.0179 (5)
O4	0.55621 (19)	0.79526 (12)	0.80588 (10)	0.0163 (5)
O5	0.8720 (2)	0.81086 (13)	0.74973 (10)	0.0197 (5)
O6	0.8001 (2)	0.81248 (12)	0.83713 (10)	0.0184 (5)
O7	0.6175 (2)	0.72533 (12)	0.64643 (10)	0.0178 (5)
O8	0.6429 (2)	0.61373 (12)	0.66921 (9)	0.0160 (5)
O9	0.8600 (2)	0.71060 (12)	0.66684 (10)	0.0184 (5)
O10	0.8769 (2)	0.61126 (12)	0.71653 (10)	0.0168 (5)
O11	0.57304 (19)	0.66600 (12)	0.85012 (10)	0.0155 (5)
O12	0.56962 (19)	0.58956 (12)	0.77652 (9)	0.0147 (5)
O13	0.81379 (19)	0.68469 (12)	0.87790 (10)	0.0169 (5)
O14	0.81080 (19)	0.58767 (12)	0.82463 (9)	0.0151 (5)
O15	0.71611 (19)	0.70351 (11)	0.76204 (9)	0.0136 (4)
O1W	0.6544 (2)	0.77209 (13)	0.91690 (10)	0.0190 (5)
H1W1	0.684 (3)	0.747 (2)	0.9440 (15)	0.059 (17)*
H1W2	0.5872 (17)	0.783 (2)	0.9250 (17)	0.034 (13)*
O2W	0.7303 (2)	0.50636 (12)	0.73377 (10)	0.0171 (5)
H2W1	0.759 (4)	0.4871 (18)	0.7053 (11)	0.032 (12)*
H2W2	0.726 (4)	0.4790 (17)	0.7610 (12)	0.050 (15)*
N1	0.7157 (3)	0.67991 (19)	1.00764 (16)	0.0338 (8)
N2	0.4284 (4)	0.7968 (3)	0.9455 (2)	0.0556 (12)
N3	0.8447 (5)	0.4523 (3)	0.6464 (2)	0.0685 (15)
C1	0.8074 (3)	0.89117 (17)	0.63661 (14)	0.0157 (6)
C2	0.8515 (3)	0.91082 (17)	0.57647 (14)	0.0172 (7)
C3	0.5520 (3)	0.82935 (16)	0.75960 (14)	0.0158 (6)
C4	0.4390 (3)	0.86978 (19)	0.74313 (17)	0.0229 (7)
C5	0.8757 (3)	0.82309 (17)	0.80318 (15)	0.0173 (7)
C6	0.9912 (3)	0.85391 (19)	0.83110 (15)	0.0215 (7)
C7	0.5957 (3)	0.66336 (18)	0.64181 (13)	0.0156 (6)
C8	0.4943 (3)	0.64175 (18)	0.59620 (15)	0.0196 (7)
C9	0.9091 (3)	0.65627 (17)	0.68302 (14)	0.0161 (6)
C10	1.0241 (3)	0.64354 (16)	0.65623 (14)	0.0254 (8)
C11	0.5281 (3)	0.62049 (17)	0.81711 (14)	0.0142 (6)
C12	0.3999 (3)	0.60421 (18)	0.82725 (14)	0.0177 (7)
C13	0.8484 (3)	0.62681 (17)	0.86503 (14)	0.0144 (6)
C14	0.9565 (3)	0.59973 (18)	0.90309 (15)	0.0187 (7)
C15	0.7356 (3)	0.6309 (2)	1.03291 (16)	0.0255 (8)
C16	0.7599 (4)	0.5680 (2)	1.06581 (18)	0.0342 (9)
H16A	0.8074	0.5785	1.1023	0.051*
H16B	0.8016	0.5360	1.0424	0.051*
H16C	0.6872	0.5470	1.0750	0.051*
C17	0.3472 (4)	0.7913 (2)	0.9685 (2)	0.0423 (11)
C18	0.2451 (4)	0.7862 (3)	0.9985 (3)	0.0504 (13)
H18A	0.2630	0.7620	1.0356	0.076*
H18B	0.1858	0.7609	0.9742	0.076*
H18C	0.2167	0.8324	1.0062	0.076*
C19	0.8283 (8)	0.4449 (4)	0.5933 (4)	0.091 (2)
C20	0.8044 (9)	0.4336 (6)	0.5267 (3)	0.126 (4)
H20A	0.8704	0.4102	0.5119	0.189*
H20B	0.7925	0.4781	0.5071	0.189*
H20C	0.7350	0.4053	0.5187	0.189*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Cr1	0.0128 (3)	0.0158 (3)	0.0139 (2)	0.0004 (2)	0.00299 (19)	0.00348 (19)
Cr2	0.0104 (2)	0.0147 (3)	0.0134 (2)	−0.00009 (19)	0.00208 (18)	0.00052 (19)
Cr3	0.0095 (2)	0.0149 (3)	0.0112 (2)	0.00076 (19)	0.00208 (18)	0.00201 (18)
Cl1	0.0189 (5)	0.0495 (6)	0.0329 (5)	0.0045 (4)	0.0097 (4)	−0.0016 (4)
Cl2	0.0441 (6)	0.0272 (5)	0.0306 (5)	−0.0214 (4)	−0.0047 (4)	0.0062 (4)
Cl3	0.0244 (4)	0.0247 (4)	0.0147 (4)	−0.0056 (3)	−0.0031 (3)	−0.0002 (3)
Cl4	0.0320 (6)	0.0450 (6)	0.0567 (7)	0.0210 (5)	0.0277 (5)	0.0231 (5)
Cl5	0.0313 (6)	0.0279 (5)	0.0645 (7)	−0.0076 (4)	−0.0240 (5)	0.0102 (5)
Cl6	0.0246 (4)	0.0168 (4)	0.0320 (5)	0.0038 (3)	0.0037 (3)	0.0075 (3)
Cl7	0.0338 (6)	0.0700 (8)	0.0317 (5)	−0.0181 (5)	0.0043 (4)	−0.0204 (5)
Cl8	0.0231 (5)	0.0291 (5)	0.0492 (6)	0.0034 (4)	−0.0098 (4)	0.0042 (4)
Cl9	0.0253 (5)	0.0303 (5)	0.0495 (6)	−0.0113 (4)	−0.0057 (4)	0.0172 (4)
Cl10	0.0359 (5)	0.0282 (5)	0.0291 (5)	0.0015 (4)	−0.0152 (4)	0.0076 (4)
Cl11	0.0192 (5)	0.0669 (8)	0.0334 (5)	−0.0113 (5)	0.0016 (4)	0.0109 (5)
Cl12	0.0399 (6)	0.0328 (5)	0.0258 (5)	0.0067 (4)	−0.0081 (4)	−0.0095 (4)
Cl13	0.0395 (16)	0.112 (3)	0.0170 (11)	0.0297 (15)	0.0124 (9)	0.0041 (11)
Cl14	0.0124 (10)	0.0279 (10)	0.0660 (18)	−0.0058 (7)	0.0066 (10)	0.0156 (10)
Cl15	0.0214 (19)	0.0290 (15)	0.047 (3)	0.0084 (12)	0.0165 (17)	0.0106 (15)
Cl3'	0.076 (6)	0.221 (13)	0.020 (2)	0.086 (7)	0.014 (3)	−0.001 (5)
Cl4'	0.050 (3)	0.058 (3)	0.214 (9)	0.025 (2)	0.084 (5)	0.081 (4)
Cl5'	0.017 (2)	0.030 (3)	0.029 (3)	0.012 (2)	0.0058 (17)	0.008 (2)
Cl16	0.0158 (4)	0.0420 (6)	0.0283 (5)	0.0072 (4)	0.0009 (3)	0.0121 (4)
Cl17	0.0231 (5)	0.0326 (5)	0.0336 (5)	−0.0133 (4)	0.0119 (4)	−0.0121 (4)
Cl18	0.0165 (4)	0.0251 (4)	0.0174 (4)	−0.0001 (3)	0.0070 (3)	0.0011 (3)
Cl19	0.0242 (5)	0.0303 (5)	0.0259 (4)	0.0024 (4)	−0.0043 (3)	0.0115 (4)
Cl20	0.0232 (5)	0.0452 (6)	0.0318 (5)	0.0122 (4)	−0.0136 (4)	−0.0189 (4)
Cl21	0.0117 (4)	0.0285 (5)	0.0387 (5)	0.0009 (3)	0.0060 (3)	−0.0024 (4)
O1	0.0216 (13)	0.0186 (12)	0.0162 (11)	−0.0034 (10)	0.0031 (9)	0.0034 (9)
O2	0.0416 (17)	0.0240 (14)	0.0190 (13)	0.0025 (12)	0.0051 (11)	−0.0055 (10)
O3	0.0166 (12)	0.0177 (12)	0.0201 (12)	0.0016 (9)	0.0046 (9)	0.0038 (9)
O4	0.0140 (12)	0.0170 (12)	0.0182 (11)	0.0018 (9)	0.0027 (9)	0.0030 (9)
O5	0.0162 (12)	0.0244 (13)	0.0186 (12)	−0.0050 (10)	0.0022 (9)	0.0053 (10)
O6	0.0168 (12)	0.0189 (12)	0.0201 (12)	−0.0048 (9)	0.0053 (9)	−0.0020 (9)
O7	0.0180 (12)	0.0196 (12)	0.0156 (11)	0.0002 (9)	0.0007 (9)	0.0041 (9)
O8	0.0174 (12)	0.0169 (12)	0.0135 (11)	0.0015 (9)	0.0003 (9)	0.0011 (9)
O9	0.0163 (12)	0.0211 (12)	0.0186 (12)	0.0029 (10)	0.0064 (9)	0.0052 (9)
O10	0.0132 (11)	0.0190 (12)	0.0188 (11)	0.0022 (9)	0.0049 (9)	0.0041 (9)
O11	0.0138 (11)	0.0172 (12)	0.0158 (11)	−0.0017 (9)	0.0039 (9)	0.0000 (9)
O12	0.0114 (11)	0.0182 (12)	0.0148 (11)	−0.0002 (9)	0.0032 (8)	0.0013 (9)
O13	0.0129 (11)	0.0203 (12)	0.0172 (11)	0.0032 (9)	−0.0001 (9)	−0.0012 (9)
O14	0.0132 (11)	0.0164 (11)	0.0154 (11)	0.0001 (9)	−0.0001 (9)	0.0023 (9)
O15	0.0124 (11)	0.0150 (11)	0.0138 (11)	0.0027 (9)	0.0035 (8)	0.0023 (8)
O1W	0.0174 (13)	0.0230 (13)	0.0173 (12)	0.0018 (10)	0.0050 (10)	−0.0007 (10)
O2W	0.0216 (13)	0.0163 (12)	0.0140 (11)	0.0016 (10)	0.0046 (9)	0.0022 (9)
N1	0.0257 (18)	0.038 (2)	0.038 (2)	0.0025 (15)	0.0060 (15)	0.0135 (16)
N2	0.047 (3)	0.076 (3)	0.046 (3)	0.011 (2)	0.013 (2)	0.000 (2)
N3	0.089 (4)	0.057 (3)	0.067 (3)	−0.005 (3)	0.046 (3)	−0.022 (3)
C1	0.0133 (16)	0.0204 (17)	0.0135 (15)	0.0014 (13)	0.0016 (12)	0.0020 (12)
C2	0.0181 (17)	0.0179 (16)	0.0154 (15)	−0.0046 (13)	0.0001 (13)	0.0015 (12)
C3	0.0132 (16)	0.0124 (15)	0.0217 (16)	0.0001 (12)	0.0014 (12)	0.0016 (12)
C4	0.0183 (18)	0.0192 (18)	0.031 (2)	0.0029 (14)	0.0032 (14)	0.0066 (14)
C5	0.0150 (16)	0.0137 (15)	0.0234 (17)	−0.0021 (12)	0.0023 (13)	0.0028 (13)
C6	0.0162 (17)	0.0268 (19)	0.0212 (17)	−0.0045 (14)	0.0004 (13)	0.0014 (14)
C7	0.0144 (16)	0.0225 (17)	0.0106 (14)	0.0022 (13)	0.0040 (12)	0.0026 (12)
C8	0.0195 (17)	0.0212 (17)	0.0177 (16)	0.0015 (14)	0.0005 (13)	0.0033 (13)
C9	0.0112 (15)	0.0218 (17)	0.0152 (15)	0.0011 (13)	0.0013 (12)	−0.0005 (12)
C10	0.0178 (18)	0.031 (2)	0.0286 (19)	0.0065 (15)	0.0093 (14)	0.0119 (15)
C11	0.0100 (15)	0.0182 (16)	0.0145 (15)	0.0012 (12)	0.0022 (11)	0.0065 (12)
C12	0.0139 (16)	0.0223 (17)	0.0175 (16)	0.0006 (13)	0.0049 (12)	0.0013 (13)
C13	0.0083 (15)	0.0206 (17)	0.0146 (15)	−0.0007 (12)	0.0022 (11)	0.0023 (12)
C14	0.0129 (16)	0.0236 (18)	0.0191 (16)	0.0021 (13)	−0.0012 (13)	−0.0023 (13)
C15	0.0207 (19)	0.032 (2)	0.0237 (18)	−0.0009 (16)	0.0027 (14)	0.0001 (16)
C16	0.046 (3)	0.028 (2)	0.028 (2)	0.0033 (18)	−0.0004 (18)	0.0012 (16)
C17	0.036 (3)	0.039 (3)	0.052 (3)	0.008 (2)	0.005 (2)	−0.004 (2)
C18	0.035 (3)	0.036 (3)	0.082 (4)	0.002 (2)	0.018 (3)	0.008 (2)
C19	0.110 (6)	0.059 (4)	0.112 (7)	0.002 (4)	0.052 (5)	−0.005 (4)
C20	0.133 (9)	0.177 (10)	0.073 (6)	0.024 (7)	0.036 (5)	−0.032 (6)

Geometric parameters (Å, º) top

Cr1—O15	1.930 (2)	Cl21—C14	1.768 (4)
Cr1—O1	1.965 (2)	O1—C1	1.264 (4)
Cr1—O3	1.973 (2)	O2—C1	1.212 (4)
Cr1—O9	1.978 (2)	O3—C3	1.242 (4)
Cr1—O5	1.980 (2)	O4—C3	1.250 (4)
Cr1—O7	2.003 (2)	O5—C5	1.246 (4)
Cr2—O15	1.909 (2)	O6—C5	1.246 (4)
Cr2—O11	1.959 (2)	O7—C7	1.236 (4)
Cr2—O13	1.966 (2)	O8—C7	1.252 (4)
Cr2—O4	1.968 (2)	O9—C9	1.243 (4)
Cr2—O6	1.971 (2)	O10—C9	1.247 (4)
Cr2—O1W	2.017 (2)	O11—C11	1.249 (4)
Cr3—O15	1.911 (2)	O12—C11	1.244 (4)
Cr3—O8	1.970 (2)	O13—C13	1.242 (4)
Cr3—O14	1.975 (2)	O14—C13	1.248 (4)
Cr3—O10	1.986 (2)	O1W—H1W1	0.839 (10)
Cr3—O2W	1.990 (2)	O1W—H1W2	0.849 (10)
Cr3—O12	1.993 (2)	O2W—H2W1	0.850 (10)
Cl1—C2	1.769 (4)	O2W—H2W2	0.826 (10)
Cl2—C2	1.757 (3)	N1—C15	1.131 (5)
Cl3—C2	1.770 (3)	N2—C17	1.130 (6)
Cl4—C4	1.752 (4)	N3—C19	1.225 (10)
Cl5—C4	1.787 (4)	C1—C2	1.564 (4)
Cl6—C4	1.752 (4)	C3—C4	1.549 (5)
Cl7—C6	1.762 (4)	C5—C6	1.554 (5)
Cl8—C6	1.778 (4)	C7—C8	1.560 (5)
Cl9—C6	1.741 (4)	C9—C10	1.543 (5)
Cl10—C8	1.754 (3)	C11—C12	1.562 (4)
Cl11—C8	1.772 (4)	C13—C14	1.555 (4)
Cl12—C8	1.768 (4)	C15—C16	1.453 (5)
Cl13—C10	1.734 (4)	C16—H16A	0.9800
Cl14—C10	1.802 (4)	C16—H16B	0.9800
Cl15—C10	1.744 (5)	C16—H16C	0.9800
Cl3'—C10	1.813 (6)	C17—C18	1.429 (7)
Cl4'—C10	1.705 (5)	C18—H18A	0.9800
Cl5'—C10	1.757 (6)	C18—H18B	0.9800
Cl16—C12	1.780 (4)	C18—H18C	0.9800
Cl17—C12	1.745 (4)	C19—C20	1.544 (11)
Cl18—C12	1.762 (3)	C20—H20A	0.9800
Cl19—C14	1.759 (4)	C20—H20B	0.9800
Cl20—C14	1.759 (3)	C20—H20C	0.9800

O15—Cr1—O1	177.60 (10)	C3—C4—Cl6	110.7 (2)
O15—Cr1—O3	93.62 (9)	Cl4—C4—Cl6	110.0 (2)
O1—Cr1—O3	88.40 (10)	C3—C4—Cl5	104.4 (2)
O15—Cr1—O9	94.83 (9)	Cl4—C4—Cl5	109.6 (2)
O1—Cr1—O9	83.11 (10)	Cl6—C4—Cl5	109.6 (2)
O3—Cr1—O9	171.35 (10)	O6—C5—O5	128.5 (3)
O15—Cr1—O5	91.45 (10)	O6—C5—C6	116.1 (3)
O1—Cr1—O5	89.66 (10)	O5—C5—C6	115.4 (3)
O3—Cr1—O5	94.78 (10)	C5—C6—Cl9	110.7 (2)
O9—Cr1—O5	86.86 (10)	C5—C6—Cl7	112.2 (2)
O15—Cr1—O7	91.71 (9)	Cl9—C6—Cl7	109.9 (2)
O1—Cr1—O7	87.10 (10)	C5—C6—Cl8	105.4 (2)
O3—Cr1—O7	87.27 (10)	Cl9—C6—Cl8	110.6 (2)
O9—Cr1—O7	90.63 (10)	Cl7—C6—Cl8	107.91 (19)
O5—Cr1—O7	176.12 (10)	O7—C7—O8	129.4 (3)
O15—Cr2—O11	94.11 (10)	O7—C7—C8	117.2 (3)
O15—Cr2—O13	93.23 (9)	O8—C7—C8	113.4 (3)
O11—Cr2—O13	92.54 (10)	C7—C8—Cl10	112.6 (2)
O15—Cr2—O4	93.81 (9)	C7—C8—Cl12	109.6 (2)
O11—Cr2—O4	87.48 (10)	Cl10—C8—Cl12	109.56 (19)
O13—Cr2—O4	172.95 (10)	C7—C8—Cl11	106.5 (2)
O15—Cr2—O6	94.50 (10)	Cl10—C8—Cl11	108.88 (19)
O11—Cr2—O6	171.16 (10)	Cl12—C8—Cl11	109.6 (2)
O13—Cr2—O6	84.97 (10)	O9—C9—O10	128.8 (3)
O4—Cr2—O6	93.95 (10)	O9—C9—C10	114.1 (3)
O15—Cr2—O1W	179.24 (10)	C9—C10—Cl4'	116.4 (4)
O11—Cr2—O1W	85.21 (10)	C9—C10—Cl13	110.0 (3)
O13—Cr2—O1W	86.47 (10)	C9—C10—Cl15	113.5 (4)
O4—Cr2—O1W	86.50 (10)	Cl4'—C10—Cl15	115.9 (5)
O6—Cr2—O1W	86.17 (10)	Cl13—C10—Cl15	110.6 (4)
O15—Cr3—O8	93.43 (9)	C9—C10—Cl5'	111.8 (7)
O15—Cr3—O14	93.95 (9)	Cl4'—C10—Cl5'	111.8 (5)
O8—Cr3—O14	172.40 (10)	Cl13—C10—Cl5'	117.6 (7)
O15—Cr3—O10	94.39 (10)	C9—C10—Cl14	105.0 (2)
O8—Cr3—O10	91.54 (10)	Cl13—C10—Cl14	109.1 (2)
O14—Cr3—O10	86.09 (10)	Cl15—C10—Cl14	108.5 (3)
O15—Cr3—O2W	179.43 (10)	Cl5'—C10—Cl14	102.3 (5)
O8—Cr3—O2W	86.22 (10)	C9—C10—Cl3'	101.2 (4)
O14—Cr3—O2W	86.41 (10)	Cl4'—C10—Cl3'	108.1 (4)
O10—Cr3—O2W	86.07 (10)	Cl5'—C10—Cl3'	106.4 (5)
O15—Cr3—O12	93.18 (9)	Cl14—C10—Cl3'	129.9 (5)
O8—Cr3—O12	86.73 (9)	O12—C11—O11	128.9 (3)
O14—Cr3—O12	94.66 (9)	O12—C11—C12	117.1 (3)
O10—Cr3—O12	172.32 (10)	O11—C11—C12	113.9 (3)
O2W—Cr3—O12	86.35 (10)	C11—C12—Cl17	112.9 (2)
C1—O1—Cr1	130.9 (2)	C11—C12—Cl18	110.7 (2)
C3—O3—Cr1	132.3 (2)	Cl17—C12—Cl18	110.02 (18)
C3—O4—Cr2	125.6 (2)	C11—C12—Cl16	104.2 (2)
C5—O5—Cr1	126.5 (2)	Cl17—C12—Cl16	109.59 (19)
C5—O6—Cr2	129.5 (2)	Cl18—C12—Cl16	109.25 (18)
C7—O7—Cr1	126.0 (2)	O13—C13—O14	129.3 (3)
C7—O8—Cr3	131.6 (2)	O13—C13—C14	115.9 (3)
C9—O9—Cr1	132.6 (2)	O14—C13—C14	114.8 (3)
C9—O10—Cr3	126.0 (2)	C13—C14—Cl19	109.4 (2)
C11—O11—Cr2	131.5 (2)	C13—C14—Cl20	111.2 (2)
C11—O12—Cr3	125.8 (2)	Cl19—C14—Cl20	109.58 (19)
C13—O13—Cr2	127.4 (2)	C13—C14—Cl21	106.9 (2)
C13—O14—Cr3	131.1 (2)	Cl19—C14—Cl21	110.30 (19)
Cr2—O15—Cr3	120.38 (11)	Cl20—C14—Cl21	109.49 (19)
Cr2—O15—Cr1	119.25 (12)	N1—C15—C16	179.3 (5)
Cr3—O15—Cr1	120.35 (11)	C15—C16—H16A	109.5
Cr2—O1W—H1W1	112 (3)	C15—C16—H16B	109.5
Cr2—O1W—H1W2	122 (3)	H16A—C16—H16B	109.5
H1W1—O1W—H1W2	108.1 (17)	C15—C16—H16C	109.5
Cr3—O2W—H2W1	126 (3)	H16A—C16—H16C	109.5
Cr3—O2W—H2W2	120 (3)	H16B—C16—H16C	109.5
H2W1—O2W—H2W2	110.6 (18)	N2—C17—C18	178.2 (6)
O2—C1—O1	131.0 (3)	C17—C18—H18A	109.5
O2—C1—C2	117.9 (3)	C17—C18—H18B	109.5
O1—C1—C2	111.2 (3)	H18A—C18—H18B	109.5
C1—C2—Cl2	112.6 (2)	C17—C18—H18C	109.5
C1—C2—Cl3	108.5 (2)	H18A—C18—H18C	109.5
Cl2—C2—Cl3	109.03 (18)	H18B—C18—H18C	109.5
C1—C2—Cl1	108.6 (2)	N3—C19—C20	178.0 (9)
Cl2—C2—Cl1	109.29 (19)	C19—C20—H20A	109.5
Cl3—C2—Cl1	108.81 (18)	C19—C20—H20B	109.5
O3—C3—O4	128.4 (3)	H20A—C20—H20B	109.5
O3—C3—C4	115.3 (3)	C19—C20—H20C	109.5
O4—C3—C4	116.3 (3)	H20A—C20—H20C	109.5
C3—C4—Cl4	112.4 (2)	H20B—C20—H20C	109.5

O3—Cr1—O1—C1	62.2 (3)	O7—Cr1—O15—Cr3	56.08 (14)
O9—Cr1—O1—C1	−119.5 (3)	Cr1—O1—C1—O2	−17.1 (6)
O5—Cr1—O1—C1	−32.6 (3)	Cr1—O1—C1—C2	162.3 (2)
O7—Cr1—O1—C1	149.5 (3)	O2—C1—C2—Cl2	−3.5 (4)
O15—Cr1—O3—C3	−7.9 (3)	O1—C1—C2—Cl2	177.0 (2)
O1—Cr1—O3—C3	170.8 (3)	O2—C1—C2—Cl3	−124.3 (3)
O5—Cr1—O3—C3	−99.7 (3)	O1—C1—C2—Cl3	56.2 (3)
O7—Cr1—O3—C3	83.6 (3)	O2—C1—C2—Cl1	117.6 (3)
O15—Cr2—O4—C3	−39.5 (3)	O1—C1—C2—Cl1	−61.9 (3)
O11—Cr2—O4—C3	−133.4 (3)	Cr1—O3—C3—O4	28.9 (5)
O6—Cr2—O4—C3	55.3 (3)	Cr1—O3—C3—C4	−148.2 (2)
O1W—Cr2—O4—C3	141.2 (3)	Cr2—O4—C3—O3	1.6 (5)
O15—Cr1—O5—C5	−40.0 (3)	Cr2—O4—C3—C4	178.7 (2)
O1—Cr1—O5—C5	142.1 (3)	O3—C3—C4—Cl4	−161.7 (3)
O3—Cr1—O5—C5	53.7 (3)	O4—C3—C4—Cl4	20.9 (4)
O9—Cr1—O5—C5	−134.8 (3)	O3—C3—C4—Cl6	−38.2 (4)
O15—Cr2—O6—C5	−10.7 (3)	O4—C3—C4—Cl6	144.4 (3)
O13—Cr2—O6—C5	82.2 (3)	O3—C3—C4—Cl5	79.6 (3)
O4—Cr2—O6—C5	−104.8 (3)	O4—C3—C4—Cl5	−97.8 (3)
O1W—Cr2—O6—C5	168.9 (3)	Cr2—O6—C5—O5	34.3 (5)
O15—Cr1—O7—C7	−38.4 (3)	Cr2—O6—C5—C6	−144.0 (3)
O1—Cr1—O7—C7	139.6 (3)	Cr1—O5—C5—O6	−1.4 (5)
O3—Cr1—O7—C7	−131.9 (3)	Cr1—O5—C5—C6	176.9 (2)
O9—Cr1—O7—C7	56.5 (3)	O6—C5—C6—Cl9	−133.0 (3)
O15—Cr3—O8—C7	−5.6 (3)	O5—C5—C6—Cl9	48.5 (4)
O10—Cr3—O8—C7	−100.0 (3)	O6—C5—C6—Cl7	−9.9 (4)
O2W—Cr3—O8—C7	174.0 (3)	O5—C5—C6—Cl7	171.6 (3)
O12—Cr3—O8—C7	87.4 (3)	O6—C5—C6—Cl8	107.3 (3)
O15—Cr1—O9—C9	−7.1 (3)	O5—C5—C6—Cl8	−71.2 (3)
O1—Cr1—O9—C9	174.1 (3)	Cr1—O7—C7—O8	1.2 (5)
O5—Cr1—O9—C9	84.1 (3)	Cr1—O7—C7—C8	−179.7 (2)
O7—Cr1—O9—C9	−98.9 (3)	Cr3—O8—C7—O7	27.7 (5)
O15—Cr3—O10—C9	−40.5 (3)	Cr3—O8—C7—C8	−151.5 (2)
O8—Cr3—O10—C9	53.1 (3)	O7—C7—C8—Cl10	9.9 (4)
O14—Cr3—O10—C9	−134.1 (3)	O8—C7—C8—Cl10	−170.8 (2)
O2W—Cr3—O10—C9	139.2 (3)	O7—C7—C8—Cl12	132.2 (3)
O15—Cr2—O11—C11	−7.5 (3)	O8—C7—C8—Cl12	−48.5 (3)
O13—Cr2—O11—C11	−100.9 (3)	O7—C7—C8—Cl11	−109.4 (3)
O4—Cr2—O11—C11	86.1 (3)	O8—C7—C8—Cl11	69.9 (3)
O1W—Cr2—O11—C11	172.8 (3)	Cr1—O9—C9—O10	22.5 (5)
O15—Cr3—O12—C11	−35.3 (3)	Cr1—O9—C9—C10	−158.9 (2)
O8—Cr3—O12—C11	−128.6 (3)	Cr3—O10—C9—O9	7.7 (5)
O14—Cr3—O12—C11	58.9 (3)	Cr3—O10—C9—C10	−170.8 (2)
O2W—Cr3—O12—C11	145.0 (3)	O9—C9—C10—Cl4'	36.3 (7)
O15—Cr2—O13—C13	−34.4 (3)	O10—C9—C10—Cl4'	−145.0 (7)
O11—Cr2—O13—C13	59.8 (3)	O9—C9—C10—Cl13	−60.9 (4)
O6—Cr2—O13—C13	−128.7 (3)	O10—C9—C10—Cl13	117.9 (3)
O1W—Cr2—O13—C13	144.9 (3)	O9—C9—C10—Cl15	174.7 (4)
O15—Cr3—O14—C13	−2.0 (3)	O10—C9—C10—Cl15	−6.6 (5)
O10—Cr3—O14—C13	92.1 (3)	O9—C9—C10—Cl5'	166.5 (5)
O2W—Cr3—O14—C13	178.4 (3)	O10—C9—C10—Cl5'	−14.7 (6)
O12—Cr3—O14—C13	−95.5 (3)	O9—C9—C10—Cl14	56.3 (3)
O11—Cr2—O15—Cr3	−39.09 (14)	O10—C9—C10—Cl14	−124.9 (3)
O13—Cr2—O15—Cr3	53.69 (14)	O9—C9—C10—Cl3'	−80.5 (6)
O4—Cr2—O15—Cr3	−126.83 (13)	O10—C9—C10—Cl3'	98.2 (6)
O6—Cr2—O15—Cr3	138.90 (13)	Cr3—O12—C11—O11	−3.2 (5)
O11—Cr2—O15—Cr1	142.66 (13)	Cr3—O12—C11—C12	173.2 (2)
O13—Cr2—O15—Cr1	−124.55 (13)	Cr2—O11—C11—O12	31.1 (5)
O4—Cr2—O15—Cr1	54.92 (13)	Cr2—O11—C11—C12	−145.3 (2)
O6—Cr2—O15—Cr1	−39.35 (14)	O12—C11—C12—Cl17	23.3 (4)
O8—Cr3—O15—Cr2	140.83 (13)	O11—C11—C12—Cl17	−159.8 (2)
O14—Cr3—O15—Cr2	−40.99 (14)	O12—C11—C12—Cl18	147.1 (2)
O10—Cr3—O15—Cr2	−127.36 (13)	O11—C11—C12—Cl18	−36.0 (3)
O12—Cr3—O15—Cr2	53.92 (13)	O12—C11—C12—Cl16	−95.5 (3)
O8—Cr3—O15—Cr1	−40.94 (14)	O11—C11—C12—Cl16	81.4 (3)
O14—Cr3—O15—Cr1	137.24 (13)	Cr2—O13—C13—O14	−1.5 (5)
O10—Cr3—O15—Cr1	50.87 (14)	Cr2—O13—C13—C14	176.2 (2)
O12—Cr3—O15—Cr1	−127.86 (13)	Cr3—O14—C13—O13	25.1 (5)
O3—Cr1—O15—Cr2	−38.30 (14)	Cr3—O14—C13—C14	−152.6 (2)
O9—Cr1—O15—Cr2	143.55 (13)	O13—C13—C14—Cl19	131.3 (3)
O5—Cr1—O15—Cr2	56.58 (14)	O14—C13—C14—Cl19	−50.7 (3)
O7—Cr1—O15—Cr2	−125.67 (13)	O13—C13—C14—Cl20	10.2 (4)
O3—Cr1—O15—Cr3	143.45 (13)	O14—C13—C14—Cl20	−171.8 (2)
O9—Cr1—O15—Cr3	−34.69 (14)	O13—C13—C14—Cl21	−109.3 (3)
O5—Cr1—O15—Cr3	−121.66 (14)	O14—C13—C14—Cl21	68.7 (3)

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1W—H1W1···N1	0.84 (1)	1.97 (2)	2.791 (4)	166 (5)
O1W—H1W2···N2	0.85 (1)	1.97 (1)	2.810 (5)	173 (4)
O2W—H2W1···N3	0.85 (1)	1.88 (1)	2.719 (5)	171 (4)
O2W—H2W2···O2ⁱ	0.83 (1)	1.81 (1)	2.613 (3)	165 (4)

Symmetry code: (i) −x+3/2, y−1/2, −z+3/2.

Experimental details

Crystal data
Chemical formula	[Cr₃(C₂Cl₃O₂)₇O(H₂O)₂]·3C₂H₃N
M_r	1467.78
Crystal system, space group	Monoclinic, P2₁/n
Temperature (K)	100
a, b, c (Å)	11.6307 (6), 19.481 (1), 22.949 (1)
β (°)	95.355 (1)
V (Å³)	5177.0 (5)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	1.76
Crystal size (mm)	0.25 × 0.20 × 0.15

Data collection
Diffractometer	Bruker SMART APEX diffractometer
Absorption correction	Multi-scan (SADABS; Sheldrick, 1996)
T_min, T_max	0.667, 0.778
No. of measured, independent and observed [I > 2σ(I)] reflections	29504, 11718, 9590
R_int	0.029
(sin θ/λ)_max (Å⁻¹)	0.650

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.041, 0.118, 1.04
No. of reflections	11718
No. of parameters	624
No. of restraints	72
H-atom treatment	H atoms treated by a mixture of independent and constrained refinement
Δρ_max, Δρ_min (e Å⁻³)	1.42, −0.74

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—H1W1···N1	0.84 (1)	1.97 (2)	2.791 (4)	166 (5)
O1W—H1W2···N2	0.85 (1)	1.97 (1)	2.810 (5)	173 (4)
O2W—H2W1···N3	0.85 (1)	1.88 (1)	2.719 (5)	171 (4)
O2W—H2W2···O2ⁱ	0.83 (1)	1.81 (1)	2.613 (3)	165 (4)

Symmetry code: (i) −x+3/2, y−1/2, −z+3/2.

Acknowledgements

The authors thank the University of Malaya for supporting this study (grant Nos. PS078-2007C and PS208-2008A).

References

Barbour, L. J. (2001). J. Supramol. Chem. 1, 189–191. CrossRef CAS Google Scholar
Bruker (2007). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Gan, S.-N., Jelan, A. M. & Ooi, C. P. (2000). Trinuclear oxo-centered chromium(III) carboxylate complexes as Ziegler–Natta catalysts for ethylene polymerization in Progress and Development of Catalytic Olefin Polymerization, edited by T. Sano, T. Uozumi, H. Nakatani & M. Terano, pp. 25–32. Tokyo: Technology and Education Publishers. Google Scholar
Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany. Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Westrip, S. P. (2008). publCIF. In preparation. Google Scholar

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