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Acta Cryst. (2008). E64, m1175    [ doi:10.1107/S1600536808025798 ]

Diaqua-[mu]3-oxido-hexakis([mu]2-trichloroacetato-[kappa]2O:O')(trichloroacetato-[kappa]O)trichromium(III) acetonitrile trisolvate

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

Abstract top

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 CrIII 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).

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.

Refinement top

One of the seven trichloroacetate groups was found to be disordered over two sites. The six C—Cl distances were restrained to within 0.01 Å of each other, as were the Cl···Cl distances. The anisotropic displacement parameters of the disordered Cl atoms were restrained to be nearly isotropic. The disorder refined to a 0.636 (12):0.364 (12) site occupancy ratio. The water hydrogen atoms were located in a difference Fourier map, and were refined with a distance restraint of O—H 0.84 (1) Å; their temperature factors were freely refined. The methyl-H atoms were generated geometrically (C—H = 0.98 Å), and were included in the refinement in the riding model approximation with Uiso(H) = 1.5Ueq(C). The final difference Fourier map had a large peak in the vicinity of the disordered Cl atoms, but was otherwise featureless.

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 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]·3C2H3NF000 = 2876
Mr = 1467.78Dx = 1.883 Mg m−3
Monoclinic, P21/nMo Kα radiation
λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 9535 reflections
a = 11.6307 (6) Åθ = 2.2–28.2º
b = 19.481 (1) ŵ = 1.76 mm−1
c = 22.949 (1) ÅT = 100 (2) K
β = 95.355 (1)ºBlock, green
V = 5177.0 (5) Å30.25 × 0.20 × 0.15 mm
Z = 4
Data collection top
Bruker SMART APEX
diffractometer		9590 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.029
Monochromator: graphiteθmax = 27.5º
ω scansθmin = 1.4º
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)		h = −15→11
Tmin = 0.667, Tmax = 0.778k = −25→25
29504 measured reflectionsl = −29→29
11718 independent reflections
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.041H atoms treated by a mixture of
independent and constrained refinement
wR(F2) = 0.118  w = 1/[σ2(Fo2) + (0.0626P)2 + 7.2035P]
where P = (Fo2 + 2Fc2)/3
S = 1.04(Δ/σ)max = 0.001
11718 reflectionsΔρmax = 1.42 e Å−3
624 parametersΔρmin = −0.74 e Å−3
72 restraintsExtinction correction: none
Primary atom site location: structure-invariant direct methods
Crystal data top
[Cr3(C2Cl3O2)7O(H2O)2]·3C2H3NV = 5177.0 (5) Å3
Mr = 1467.78Z = 4
Monoclinic, P21/nMo Kα
a = 11.6307 (6) ŵ = 1.76 mm−1
b = 19.481 (1) ÅT = 100 (2) K
c = 22.949 (1) Å0.25 × 0.20 × 0.15 mm
β = 95.355 (1)º
Data collection top
Bruker SMART APEX
diffractometer		11718 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)		9590 reflections with I > 2σ(I)
Tmin = 0.667, Tmax = 0.778Rint = 0.029
29504 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.04172 restraints
wR(F2) = 0.118H atoms treated by a mixture of
independent and constrained refinement
S = 1.04Δρmax = 1.42 e Å−3
11718 reflectionsΔρmin = −0.74 e Å−3
624 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Cr10.74255 (4)0.76778 (3)0.70072 (2)0.01404 (12)
Cr20.68641 (4)0.73747 (3)0.83719 (2)0.01277 (11)
Cr30.72390 (4)0.60693 (3)0.74830 (2)0.01179 (11)
Cl10.96872 (8)0.85657 (6)0.56393 (4)0.0333 (2)
Cl20.89615 (9)0.99687 (5)0.57400 (4)0.0345 (2)
Cl30.73830 (8)0.89677 (4)0.52068 (3)0.02158 (18)
Cl40.36046 (10)0.88419 (6)0.80350 (5)0.0431 (3)
Cl50.35756 (9)0.81589 (5)0.69151 (5)0.0430 (3)
Cl60.46821 (8)0.94801 (4)0.70989 (4)0.02438 (19)
Cl70.98178 (10)0.88074 (7)0.90381 (5)0.0451 (3)
Cl81.09295 (9)0.78569 (5)0.83228 (5)0.0346 (2)
Cl91.03479 (9)0.92225 (5)0.78947 (5)0.0356 (2)
Cl100.44418 (9)0.70978 (5)0.55064 (4)0.0322 (2)
Cl110.38086 (9)0.61375 (7)0.63683 (5)0.0399 (3)
Cl120.53908 (9)0.57331 (5)0.55303 (4)0.0336 (2)
Cl130.9998 (4)0.6385 (3)0.58065 (14)0.0556 (10)0.636 (12)
Cl141.1108 (2)0.71821 (13)0.67552 (16)0.0352 (8)0.636 (12)
Cl151.0981 (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)
Cl160.31914 (8)0.66992 (5)0.78820 (4)0.0287 (2)
Cl170.35454 (8)0.52405 (5)0.79999 (4)0.0292 (2)
Cl180.37880 (7)0.61005 (4)0.90215 (3)0.01931 (17)
Cl190.93022 (8)0.51554 (5)0.92623 (4)0.0272 (2)
Cl200.99064 (8)0.65247 (6)0.96451 (4)0.0344 (2)
Cl211.07222 (7)0.60054 (5)0.85829 (4)0.02607 (19)
O10.7710 (2)0.82999 (12)0.63619 (10)0.0187 (5)
O20.8135 (3)0.93428 (14)0.67484 (11)0.0281 (6)
O30.6252 (2)0.83313 (12)0.72363 (10)0.0179 (5)
O40.55621 (19)0.79526 (12)0.80588 (10)0.0163 (5)
O50.8720 (2)0.81086 (13)0.74973 (10)0.0197 (5)
O60.8001 (2)0.81248 (12)0.83713 (10)0.0184 (5)
O70.6175 (2)0.72533 (12)0.64643 (10)0.0178 (5)
O80.6429 (2)0.61373 (12)0.66921 (9)0.0160 (5)
O90.8600 (2)0.71060 (12)0.66684 (10)0.0184 (5)
O100.8769 (2)0.61126 (12)0.71653 (10)0.0168 (5)
O110.57304 (19)0.66600 (12)0.85012 (10)0.0155 (5)
O120.56962 (19)0.58956 (12)0.77652 (9)0.0147 (5)
O130.81379 (19)0.68469 (12)0.87790 (10)0.0169 (5)
O140.81080 (19)0.58767 (12)0.82463 (9)0.0151 (5)
O150.71611 (19)0.70351 (11)0.76204 (9)0.0136 (4)
O1W0.6544 (2)0.77209 (13)0.91690 (10)0.0190 (5)
H1W10.684 (3)0.747 (2)0.9440 (15)0.059 (17)*
H1W20.5872 (17)0.783 (2)0.9250 (17)0.034 (13)*
O2W0.7303 (2)0.50636 (12)0.73377 (10)0.0171 (5)
H2W10.759 (4)0.4871 (18)0.7053 (11)0.032 (12)*
H2W20.726 (4)0.4790 (17)0.7610 (12)0.050 (15)*
N10.7157 (3)0.67991 (19)1.00764 (16)0.0338 (8)
N20.4284 (4)0.7968 (3)0.9455 (2)0.0556 (12)
N30.8447 (5)0.4523 (3)0.6464 (2)0.0685 (15)
C10.8074 (3)0.89117 (17)0.63661 (14)0.0157 (6)
C20.8515 (3)0.91082 (17)0.57647 (14)0.0172 (7)
C30.5520 (3)0.82935 (16)0.75960 (14)0.0158 (6)
C40.4390 (3)0.86978 (19)0.74313 (17)0.0229 (7)
C50.8757 (3)0.82309 (17)0.80318 (15)0.0173 (7)
C60.9912 (3)0.85391 (19)0.83110 (15)0.0215 (7)
C70.5957 (3)0.66336 (18)0.64181 (13)0.0156 (6)
C80.4943 (3)0.64175 (18)0.59620 (15)0.0196 (7)
C90.9091 (3)0.65627 (17)0.68302 (14)0.0161 (6)
C101.0241 (3)0.64354 (16)0.65623 (14)0.0254 (8)
C110.5281 (3)0.62049 (17)0.81711 (14)0.0142 (6)
C120.3999 (3)0.60421 (18)0.82725 (14)0.0177 (7)
C130.8484 (3)0.62681 (17)0.86503 (14)0.0144 (6)
C140.9565 (3)0.59973 (18)0.90309 (15)0.0187 (7)
C150.7356 (3)0.6309 (2)1.03291 (16)0.0255 (8)
C160.7599 (4)0.5680 (2)1.06581 (18)0.0342 (9)
H16A0.80740.57851.10230.051*
H16B0.80160.53601.04240.051*
H16C0.68720.54701.07500.051*
C170.3472 (4)0.7913 (2)0.9685 (2)0.0423 (11)
C180.2451 (4)0.7862 (3)0.9985 (3)0.0504 (13)
H18A0.26300.76201.03560.076*
H18B0.18580.76090.97420.076*
H18C0.21670.83241.00620.076*
C190.8283 (8)0.4449 (4)0.5933 (4)0.091 (2)
C200.8044 (9)0.4336 (6)0.5267 (3)0.126 (4)
H20A0.87040.41020.51190.189*
H20B0.79250.47810.50710.189*
H20C0.73500.40530.51870.189*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cr10.0128 (3)0.0158 (3)0.0139 (2)0.0004 (2)0.00299 (19)0.00348 (19)
Cr20.0104 (2)0.0147 (3)0.0134 (2)−0.00009 (19)0.00208 (18)0.00052 (19)
Cr30.0095 (2)0.0149 (3)0.0112 (2)0.00076 (19)0.00208 (18)0.00201 (18)
Cl10.0189 (5)0.0495 (6)0.0329 (5)0.0045 (4)0.0097 (4)−0.0016 (4)
Cl20.0441 (6)0.0272 (5)0.0306 (5)−0.0214 (4)−0.0047 (4)0.0062 (4)
Cl30.0244 (4)0.0247 (4)0.0147 (4)−0.0056 (3)−0.0031 (3)−0.0002 (3)
Cl40.0320 (6)0.0450 (6)0.0567 (7)0.0210 (5)0.0277 (5)0.0231 (5)
Cl50.0313 (6)0.0279 (5)0.0645 (7)−0.0076 (4)−0.0240 (5)0.0102 (5)
Cl60.0246 (4)0.0168 (4)0.0320 (5)0.0038 (3)0.0037 (3)0.0075 (3)
Cl70.0338 (6)0.0700 (8)0.0317 (5)−0.0181 (5)0.0043 (4)−0.0204 (5)
Cl80.0231 (5)0.0291 (5)0.0492 (6)0.0034 (4)−0.0098 (4)0.0042 (4)
Cl90.0253 (5)0.0303 (5)0.0495 (6)−0.0113 (4)−0.0057 (4)0.0172 (4)
Cl100.0359 (5)0.0282 (5)0.0291 (5)0.0015 (4)−0.0152 (4)0.0076 (4)
Cl110.0192 (5)0.0669 (8)0.0334 (5)−0.0113 (5)0.0016 (4)0.0109 (5)
Cl120.0399 (6)0.0328 (5)0.0258 (5)0.0067 (4)−0.0081 (4)−0.0095 (4)
Cl130.0395 (16)0.112 (3)0.0170 (11)0.0297 (15)0.0124 (9)0.0041 (11)
Cl140.0124 (10)0.0279 (10)0.0660 (18)−0.0058 (7)0.0066 (10)0.0156 (10)
Cl150.0214 (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)
Cl160.0158 (4)0.0420 (6)0.0283 (5)0.0072 (4)0.0009 (3)0.0121 (4)
Cl170.0231 (5)0.0326 (5)0.0336 (5)−0.0133 (4)0.0119 (4)−0.0121 (4)
Cl180.0165 (4)0.0251 (4)0.0174 (4)−0.0001 (3)0.0070 (3)0.0011 (3)
Cl190.0242 (5)0.0303 (5)0.0259 (4)0.0024 (4)−0.0043 (3)0.0115 (4)
Cl200.0232 (5)0.0452 (6)0.0318 (5)0.0122 (4)−0.0136 (4)−0.0189 (4)
Cl210.0117 (4)0.0285 (5)0.0387 (5)0.0009 (3)0.0060 (3)−0.0024 (4)
O10.0216 (13)0.0186 (12)0.0162 (11)−0.0034 (10)0.0031 (9)0.0034 (9)
O20.0416 (17)0.0240 (14)0.0190 (13)0.0025 (12)0.0051 (11)−0.0055 (10)
O30.0166 (12)0.0177 (12)0.0201 (12)0.0016 (9)0.0046 (9)0.0038 (9)
O40.0140 (12)0.0170 (12)0.0182 (11)0.0018 (9)0.0027 (9)0.0030 (9)
O50.0162 (12)0.0244 (13)0.0186 (12)−0.0050 (10)0.0022 (9)0.0053 (10)
O60.0168 (12)0.0189 (12)0.0201 (12)−0.0048 (9)0.0053 (9)−0.0020 (9)
O70.0180 (12)0.0196 (12)0.0156 (11)0.0002 (9)0.0007 (9)0.0041 (9)
O80.0174 (12)0.0169 (12)0.0135 (11)0.0015 (9)0.0003 (9)0.0011 (9)
O90.0163 (12)0.0211 (12)0.0186 (12)0.0029 (10)0.0064 (9)0.0052 (9)
O100.0132 (11)0.0190 (12)0.0188 (11)0.0022 (9)0.0049 (9)0.0041 (9)
O110.0138 (11)0.0172 (12)0.0158 (11)−0.0017 (9)0.0039 (9)0.0000 (9)
O120.0114 (11)0.0182 (12)0.0148 (11)−0.0002 (9)0.0032 (8)0.0013 (9)
O130.0129 (11)0.0203 (12)0.0172 (11)0.0032 (9)−0.0001 (9)−0.0012 (9)
O140.0132 (11)0.0164 (11)0.0154 (11)0.0001 (9)−0.0001 (9)0.0023 (9)
O150.0124 (11)0.0150 (11)0.0138 (11)0.0027 (9)0.0035 (8)0.0023 (8)
O1W0.0174 (13)0.0230 (13)0.0173 (12)0.0018 (10)0.0050 (10)−0.0007 (10)
O2W0.0216 (13)0.0163 (12)0.0140 (11)0.0016 (10)0.0046 (9)0.0022 (9)
N10.0257 (18)0.038 (2)0.038 (2)0.0025 (15)0.0060 (15)0.0135 (16)
N20.047 (3)0.076 (3)0.046 (3)0.011 (2)0.013 (2)0.000 (2)
N30.089 (4)0.057 (3)0.067 (3)−0.005 (3)0.046 (3)−0.022 (3)
C10.0133 (16)0.0204 (17)0.0135 (15)0.0014 (13)0.0016 (12)0.0020 (12)
C20.0181 (17)0.0179 (16)0.0154 (15)−0.0046 (13)0.0001 (13)0.0015 (12)
C30.0132 (16)0.0124 (15)0.0217 (16)0.0001 (12)0.0014 (12)0.0016 (12)
C40.0183 (18)0.0192 (18)0.031 (2)0.0029 (14)0.0032 (14)0.0066 (14)
C50.0150 (16)0.0137 (15)0.0234 (17)−0.0021 (12)0.0023 (13)0.0028 (13)
C60.0162 (17)0.0268 (19)0.0212 (17)−0.0045 (14)0.0004 (13)0.0014 (14)
C70.0144 (16)0.0225 (17)0.0106 (14)0.0022 (13)0.0040 (12)0.0026 (12)
C80.0195 (17)0.0212 (17)0.0177 (16)0.0015 (14)0.0005 (13)0.0033 (13)
C90.0112 (15)0.0218 (17)0.0152 (15)0.0011 (13)0.0013 (12)−0.0005 (12)
C100.0178 (18)0.031 (2)0.0286 (19)0.0065 (15)0.0093 (14)0.0119 (15)
C110.0100 (15)0.0182 (16)0.0145 (15)0.0012 (12)0.0022 (11)0.0065 (12)
C120.0139 (16)0.0223 (17)0.0175 (16)0.0006 (13)0.0049 (12)0.0013 (13)
C130.0083 (15)0.0206 (17)0.0146 (15)−0.0007 (12)0.0022 (11)0.0023 (12)
C140.0129 (16)0.0236 (18)0.0191 (16)0.0021 (13)−0.0012 (13)−0.0023 (13)
C150.0207 (19)0.032 (2)0.0237 (18)−0.0009 (16)0.0027 (14)0.0001 (16)
C160.046 (3)0.028 (2)0.028 (2)0.0033 (18)−0.0004 (18)0.0012 (16)
C170.036 (3)0.039 (3)0.052 (3)0.008 (2)0.005 (2)−0.004 (2)
C180.035 (3)0.036 (3)0.082 (4)0.002 (2)0.018 (3)0.008 (2)
C190.110 (6)0.059 (4)0.112 (7)0.002 (4)0.052 (5)−0.005 (4)
C200.133 (9)0.177 (10)0.073 (6)0.024 (7)0.036 (5)−0.032 (6)
Geometric parameters (Å, °) top
Cr1—O151.930 (2)Cl21—C141.768 (4)
Cr1—O11.965 (2)O1—C11.264 (4)
Cr1—O31.973 (2)O2—C11.212 (4)
Cr1—O91.978 (2)O3—C31.242 (4)
Cr1—O51.980 (2)O4—C31.250 (4)
Cr1—O72.003 (2)O5—C51.246 (4)
Cr2—O151.909 (2)O6—C51.246 (4)
Cr2—O111.959 (2)O7—C71.236 (4)
Cr2—O131.966 (2)O8—C71.252 (4)
Cr2—O41.968 (2)O9—C91.243 (4)
Cr2—O61.971 (2)O10—C91.247 (4)
Cr2—O1W2.017 (2)O11—C111.249 (4)
Cr3—O151.911 (2)O12—C111.244 (4)
Cr3—O81.970 (2)O13—C131.242 (4)
Cr3—O141.975 (2)O14—C131.248 (4)
Cr3—O101.986 (2)O1W—H1W10.839 (10)
Cr3—O2W1.990 (2)O1W—H1W20.849 (10)
Cr3—O121.993 (2)O2W—H2W10.850 (10)
Cl1—C21.769 (4)O2W—H2W20.826 (10)
Cl2—C21.757 (3)N1—C151.131 (5)
Cl3—C21.770 (3)N2—C171.130 (6)
Cl4—C41.752 (4)N3—C191.225 (10)
Cl5—C41.787 (4)C1—C21.564 (4)
Cl6—C41.752 (4)C3—C41.549 (5)
Cl7—C61.762 (4)C5—C61.554 (5)
Cl8—C61.778 (4)C7—C81.560 (5)
Cl9—C61.741 (4)C9—C101.543 (5)
Cl10—C81.754 (3)C11—C121.562 (4)
Cl11—C81.772 (4)C13—C141.555 (4)
Cl12—C81.768 (4)C15—C161.453 (5)
Cl13—C101.734 (4)C16—H16A0.9800
Cl14—C101.802 (4)C16—H16B0.9800
Cl15—C101.744 (5)C16—H16C0.9800
Cl3'—C101.813 (6)C17—C181.429 (7)
Cl4'—C101.705 (5)C18—H18A0.9800
Cl5'—C101.757 (6)C18—H18B0.9800
Cl16—C121.780 (4)C18—H18C0.9800
Cl17—C121.745 (4)C19—C201.544 (11)
Cl18—C121.762 (3)C20—H20A0.9800
Cl19—C141.759 (4)C20—H20B0.9800
Cl20—C141.759 (3)C20—H20C0.9800
O15—Cr1—O1177.60 (10)C3—C4—Cl6110.7 (2)
O15—Cr1—O393.62 (9)Cl4—C4—Cl6110.0 (2)
O1—Cr1—O388.40 (10)C3—C4—Cl5104.4 (2)
O15—Cr1—O994.83 (9)Cl4—C4—Cl5109.6 (2)
O1—Cr1—O983.11 (10)Cl6—C4—Cl5109.6 (2)
O3—Cr1—O9171.35 (10)O6—C5—O5128.5 (3)
O15—Cr1—O591.45 (10)O6—C5—C6116.1 (3)
O1—Cr1—O589.66 (10)O5—C5—C6115.4 (3)
O3—Cr1—O594.78 (10)C5—C6—Cl9110.7 (2)
O9—Cr1—O586.86 (10)C5—C6—Cl7112.2 (2)
O15—Cr1—O791.71 (9)Cl9—C6—Cl7109.9 (2)
O1—Cr1—O787.10 (10)C5—C6—Cl8105.4 (2)
O3—Cr1—O787.27 (10)Cl9—C6—Cl8110.6 (2)
O9—Cr1—O790.63 (10)Cl7—C6—Cl8107.91 (19)
O5—Cr1—O7176.12 (10)O7—C7—O8129.4 (3)
O15—Cr2—O1194.11 (10)O7—C7—C8117.2 (3)
O15—Cr2—O1393.23 (9)O8—C7—C8113.4 (3)
O11—Cr2—O1392.54 (10)C7—C8—Cl10112.6 (2)
O15—Cr2—O493.81 (9)C7—C8—Cl12109.6 (2)
O11—Cr2—O487.48 (10)Cl10—C8—Cl12109.56 (19)
O13—Cr2—O4172.95 (10)C7—C8—Cl11106.5 (2)
O15—Cr2—O694.50 (10)Cl10—C8—Cl11108.88 (19)
O11—Cr2—O6171.16 (10)Cl12—C8—Cl11109.6 (2)
O13—Cr2—O684.97 (10)O9—C9—O10128.8 (3)
O4—Cr2—O693.95 (10)O9—C9—C10114.1 (3)
O15—Cr2—O1W179.24 (10)C9—C10—Cl4'116.4 (4)
O11—Cr2—O1W85.21 (10)C9—C10—Cl13110.0 (3)
O13—Cr2—O1W86.47 (10)C9—C10—Cl15113.5 (4)
O4—Cr2—O1W86.50 (10)Cl4'—C10—Cl15115.9 (5)
O6—Cr2—O1W86.17 (10)Cl13—C10—Cl15110.6 (4)
O15—Cr3—O893.43 (9)C9—C10—Cl5'111.8 (7)
O15—Cr3—O1493.95 (9)Cl4'—C10—Cl5'111.8 (5)
O8—Cr3—O14172.40 (10)Cl13—C10—Cl5'117.6 (7)
O15—Cr3—O1094.39 (10)C9—C10—Cl14105.0 (2)
O8—Cr3—O1091.54 (10)Cl13—C10—Cl14109.1 (2)
O14—Cr3—O1086.09 (10)Cl15—C10—Cl14108.5 (3)
O15—Cr3—O2W179.43 (10)Cl5'—C10—Cl14102.3 (5)
O8—Cr3—O2W86.22 (10)C9—C10—Cl3'101.2 (4)
O14—Cr3—O2W86.41 (10)Cl4'—C10—Cl3'108.1 (4)
O10—Cr3—O2W86.07 (10)Cl5'—C10—Cl3'106.4 (5)
O15—Cr3—O1293.18 (9)Cl14—C10—Cl3'129.9 (5)
O8—Cr3—O1286.73 (9)O12—C11—O11128.9 (3)
O14—Cr3—O1294.66 (9)O12—C11—C12117.1 (3)
O10—Cr3—O12172.32 (10)O11—C11—C12113.9 (3)
O2W—Cr3—O1286.35 (10)C11—C12—Cl17112.9 (2)
C1—O1—Cr1130.9 (2)C11—C12—Cl18110.7 (2)
C3—O3—Cr1132.3 (2)Cl17—C12—Cl18110.02 (18)
C3—O4—Cr2125.6 (2)C11—C12—Cl16104.2 (2)
C5—O5—Cr1126.5 (2)Cl17—C12—Cl16109.59 (19)
C5—O6—Cr2129.5 (2)Cl18—C12—Cl16109.25 (18)
C7—O7—Cr1126.0 (2)O13—C13—O14129.3 (3)
C7—O8—Cr3131.6 (2)O13—C13—C14115.9 (3)
C9—O9—Cr1132.6 (2)O14—C13—C14114.8 (3)
C9—O10—Cr3126.0 (2)C13—C14—Cl19109.4 (2)
C11—O11—Cr2131.5 (2)C13—C14—Cl20111.2 (2)
C11—O12—Cr3125.8 (2)Cl19—C14—Cl20109.58 (19)
C13—O13—Cr2127.4 (2)C13—C14—Cl21106.9 (2)
C13—O14—Cr3131.1 (2)Cl19—C14—Cl21110.30 (19)
Cr2—O15—Cr3120.38 (11)Cl20—C14—Cl21109.49 (19)
Cr2—O15—Cr1119.25 (12)N1—C15—C16179.3 (5)
Cr3—O15—Cr1120.35 (11)C15—C16—H16A109.5
Cr2—O1W—H1W1112 (3)C15—C16—H16B109.5
Cr2—O1W—H1W2122 (3)H16A—C16—H16B109.5
H1W1—O1W—H1W2108.1 (17)C15—C16—H16C109.5
Cr3—O2W—H2W1126 (3)H16A—C16—H16C109.5
Cr3—O2W—H2W2120 (3)H16B—C16—H16C109.5
H2W1—O2W—H2W2110.6 (18)N2—C17—C18178.2 (6)
O2—C1—O1131.0 (3)C17—C18—H18A109.5
O2—C1—C2117.9 (3)C17—C18—H18B109.5
O1—C1—C2111.2 (3)H18A—C18—H18B109.5
C1—C2—Cl2112.6 (2)C17—C18—H18C109.5
C1—C2—Cl3108.5 (2)H18A—C18—H18C109.5
Cl2—C2—Cl3109.03 (18)H18B—C18—H18C109.5
C1—C2—Cl1108.6 (2)N3—C19—C20178.0 (9)
Cl2—C2—Cl1109.29 (19)C19—C20—H20A109.5
Cl3—C2—Cl1108.81 (18)C19—C20—H20B109.5
O3—C3—O4128.4 (3)H20A—C20—H20B109.5
O3—C3—C4115.3 (3)C19—C20—H20C109.5
O4—C3—C4116.3 (3)H20A—C20—H20C109.5
C3—C4—Cl4112.4 (2)H20B—C20—H20C109.5
O3—Cr1—O1—C162.2 (3)O7—Cr1—O15—Cr356.08 (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—C2162.3 (2)
O7—Cr1—O1—C1149.5 (3)O2—C1—C2—Cl2−3.5 (4)
O15—Cr1—O3—C3−7.9 (3)O1—C1—C2—Cl2177.0 (2)
O1—Cr1—O3—C3170.8 (3)O2—C1—C2—Cl3−124.3 (3)
O5—Cr1—O3—C3−99.7 (3)O1—C1—C2—Cl356.2 (3)
O7—Cr1—O3—C383.6 (3)O2—C1—C2—Cl1117.6 (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—O428.9 (5)
O6—Cr2—O4—C355.3 (3)Cr1—O3—C3—C4−148.2 (2)
O1W—Cr2—O4—C3141.2 (3)Cr2—O4—C3—O31.6 (5)
O15—Cr1—O5—C5−40.0 (3)Cr2—O4—C3—C4178.7 (2)
O1—Cr1—O5—C5142.1 (3)O3—C3—C4—Cl4−161.7 (3)
O3—Cr1—O5—C553.7 (3)O4—C3—C4—Cl420.9 (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—Cl6144.4 (3)
O13—Cr2—O6—C582.2 (3)O3—C3—C4—Cl579.6 (3)
O4—Cr2—O6—C5−104.8 (3)O4—C3—C4—Cl5−97.8 (3)
O1W—Cr2—O6—C5168.9 (3)Cr2—O6—C5—O534.3 (5)
O15—Cr1—O7—C7−38.4 (3)Cr2—O6—C5—C6−144.0 (3)
O1—Cr1—O7—C7139.6 (3)Cr1—O5—C5—O6−1.4 (5)
O3—Cr1—O7—C7−131.9 (3)Cr1—O5—C5—C6176.9 (2)
O9—Cr1—O7—C756.5 (3)O6—C5—C6—Cl9−133.0 (3)
O15—Cr3—O8—C7−5.6 (3)O5—C5—C6—Cl948.5 (4)
O10—Cr3—O8—C7−100.0 (3)O6—C5—C6—Cl7−9.9 (4)
O2W—Cr3—O8—C7174.0 (3)O5—C5—C6—Cl7171.6 (3)
O12—Cr3—O8—C787.4 (3)O6—C5—C6—Cl8107.3 (3)
O15—Cr1—O9—C9−7.1 (3)O5—C5—C6—Cl8−71.2 (3)
O1—Cr1—O9—C9174.1 (3)Cr1—O7—C7—O81.2 (5)
O5—Cr1—O9—C984.1 (3)Cr1—O7—C7—C8−179.7 (2)
O7—Cr1—O9—C9−98.9 (3)Cr3—O8—C7—O727.7 (5)
O15—Cr3—O10—C9−40.5 (3)Cr3—O8—C7—C8−151.5 (2)
O8—Cr3—O10—C953.1 (3)O7—C7—C8—Cl109.9 (4)
O14—Cr3—O10—C9−134.1 (3)O8—C7—C8—Cl10−170.8 (2)
O2W—Cr3—O10—C9139.2 (3)O7—C7—C8—Cl12132.2 (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—C1186.1 (3)O8—C7—C8—Cl1169.9 (3)
O1W—Cr2—O11—C11172.8 (3)Cr1—O9—C9—O1022.5 (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—O97.7 (5)
O14—Cr3—O12—C1158.9 (3)Cr3—O10—C9—C10−170.8 (2)
O2W—Cr3—O12—C11145.0 (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—C1359.8 (3)O9—C9—C10—Cl13−60.9 (4)
O6—Cr2—O13—C13−128.7 (3)O10—C9—C10—Cl13117.9 (3)
O1W—Cr2—O13—C13144.9 (3)O9—C9—C10—Cl15174.7 (4)
O15—Cr3—O14—C13−2.0 (3)O10—C9—C10—Cl15−6.6 (5)
O10—Cr3—O14—C1392.1 (3)O9—C9—C10—Cl5'166.5 (5)
O2W—Cr3—O14—C13178.4 (3)O10—C9—C10—Cl5'−14.7 (6)
O12—Cr3—O14—C13−95.5 (3)O9—C9—C10—Cl1456.3 (3)
O11—Cr2—O15—Cr3−39.09 (14)O10—C9—C10—Cl14−124.9 (3)
O13—Cr2—O15—Cr353.69 (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—Cr3138.90 (13)Cr3—O12—C11—O11−3.2 (5)
O11—Cr2—O15—Cr1142.66 (13)Cr3—O12—C11—C12173.2 (2)
O13—Cr2—O15—Cr1−124.55 (13)Cr2—O11—C11—O1231.1 (5)
O4—Cr2—O15—Cr154.92 (13)Cr2—O11—C11—C12−145.3 (2)
O6—Cr2—O15—Cr1−39.35 (14)O12—C11—C12—Cl1723.3 (4)
O8—Cr3—O15—Cr2140.83 (13)O11—C11—C12—Cl17−159.8 (2)
O14—Cr3—O15—Cr2−40.99 (14)O12—C11—C12—Cl18147.1 (2)
O10—Cr3—O15—Cr2−127.36 (13)O11—C11—C12—Cl18−36.0 (3)
O12—Cr3—O15—Cr253.92 (13)O12—C11—C12—Cl16−95.5 (3)
O8—Cr3—O15—Cr1−40.94 (14)O11—C11—C12—Cl1681.4 (3)
O14—Cr3—O15—Cr1137.24 (13)Cr2—O13—C13—O14−1.5 (5)
O10—Cr3—O15—Cr150.87 (14)Cr2—O13—C13—C14176.2 (2)
O12—Cr3—O15—Cr1−127.86 (13)Cr3—O14—C13—O1325.1 (5)
O3—Cr1—O15—Cr2−38.30 (14)Cr3—O14—C13—C14−152.6 (2)
O9—Cr1—O15—Cr2143.55 (13)O13—C13—C14—Cl19131.3 (3)
O5—Cr1—O15—Cr256.58 (14)O14—C13—C14—Cl19−50.7 (3)
O7—Cr1—O15—Cr2−125.67 (13)O13—C13—C14—Cl2010.2 (4)
O3—Cr1—O15—Cr3143.45 (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—Cl2168.7 (3)
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
O1W—H1W1···N10.84 (1)1.97 (2)2.791 (4)166 (5)
O1W—H1W2···N20.85 (1)1.97 (1)2.810 (5)173 (4)
O2W—H2W1···N30.85 (1)1.88 (1)2.719 (5)171 (4)
O2W—H2W2···O2i0.83 (1)1.81 (1)2.613 (3)165 (4)
Symmetry codes: (i) −x+3/2, y−1/2, −z+3/2.
Table 1
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
O1W—H1W1···N10.84 (1)1.97 (2)2.791 (4)166 (5)
O1W—H1W2···N20.85 (1)1.97 (1)2.810 (5)173 (4)
O2W—H2W1···N30.85 (1)1.88 (1)2.719 (5)171 (4)
O2W—H2W2···O2i0.83 (1)1.81 (1)2.613 (3)165 (4)
Symmetry codes: (i) −x+3/2, y−1/2, −z+3/2.
Acknowledgements top

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

references
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