Literature DB >> 22219738

Hexa-μ(2)-acetato-κO:O'-(azido-κN)bis-(methanol-κO)-μ(3)-oxido-trichromium(III) methanol monosolvate.

Guo-Qing Jiang1, Jian-Hua Li, Miao Wang, Yu-Jun Shi.   

Abstract

In the crystal structure of the title complex, [Cr(3)(CH(3)CO(2))(6)(N(3))O(CH(3)OH)(2)]·CH(3)OH, the trinuclear core has a central O atom; two methanol mol-ecules and an azide ion are coordinated to the Cr(III) atoms in the core. The three Cr(III) atoms form vertices of a nearly equilateral triangle. Each of the six acetate carboxyl-ate groups bridges a Cr-O-Cr fragment. In the crystal, the molecules inter-act with methanol solvent mol-ecules through O-H⋯O and O-H⋯N hydrogen bonds, forming a two-dimensional hydrogen-bonded network parallel to (100).

Entities:  

Year:  2011        PMID： 22219738      PMCID： PMC3246918          DOI： 10.1107/S1600536811039699

Source DB:  PubMed          Journal:  Acta Crystallogr Sect E Struct Rep Online        ISSN： 1600-5368


Related literature

The design and synthesis of bioactive organic metal complexes have attracted attention since the deficiency of certain trace metals can cause diseases and disorders, see: Farrel (1999 ▶). For the supplementation of animal diets with chromium, see: Vincent (2000 ▶). For chromium carboxyl­ate complexes, see: Anson et al. (1997 ▶); Chang & Jeffrey (1970 ▶); Fujihara et al. (1998 ▶). For the synthesis of the starting material, [Cr3O(CH3CO2)6(H2O)3]Cl·6H2O, see: Earnshaw et al. (1966 ▶).

Experimental

Crystal data

[Cr3(C2H3O2)6(N3)O(CH4O)2]·CH4O M = 664.42 Monoclinic, a = 21.165 (5) Å b = 10.609 (3) Å c = 15.641 (4) Å β = 130.484 (4)° V = 2671.2 (12) Å3 Z = 4 Mo Kα radiation μ = 1.27 mm−1 T = 153 K 0.20 × 0.16 × 0.12 mm

Data collection

Bruker SMART APEX CCD area-detector diffractometer Absorption correction: multi-scan (SADABS; Bruker, 2000 ▶) T min = 0.776, T max = 0.859 6800 measured reflections 3692 independent reflections 3155 reflections with I > 2σ(I) R int = 0.034

Refinement

R[F 2 > 2σ(F 2)] = 0.059 wR(F 2) = 0.130 S = 1.08 3692 reflections 343 parameters 986 restraints H-atom parameters constrained Δρmax = 0.49 e Å−3 Δρmin = −0.47 e Å−3 Absolute structure: Flack (1983 ▶), 1110 Friedel pairs Flack parameter: 0.05 (3) Data collection: SMART (Bruker, 2000 ▶); cell refinement: SAINT (Bruker, 2000 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: SHELXTL (Sheldrick, 2008 ▶); software used to prepare material for publication: SHELXTL. Crystal structure: contains datablock(s) global, I. DOI: 10.1107/S1600536811039699/ds2137sup1.cif Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536811039699/ds2137Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Cr3(C2H3O2)6(N3)O(CH4O)2]·CH4OZ = 4
Mr = 664.42F(000) = 1364
Monoclinic, CcDx = 1.652 Mg m−3
Hall symbol: C -2ycMo Kα radiation, λ = 0.71073 Å
a = 21.165 (5) Åθ = 2.3–28.5°
b = 10.609 (3) ŵ = 1.27 mm−1
c = 15.641 (4) ÅT = 153 K
β = 130.484 (4)°Prism, green
V = 2671.2 (12) Å30.2 × 0.16 × 0.12 mm
Bruker SMART APEX CCD area-detector diffractometer3692 independent reflections
Radiation source: fine-focus sealed tube3155 reflections with I > 2σ(I)
graphiteRint = 0.034
φ and ω scansθmax = 25.9°, θmin = 2.3°
Absorption correction: multi-scan (SADABS; Bruker, 2000)h = −23→23
Tmin = 0.776, Tmax = 0.859k = −12→13
6800 measured reflectionsl = −18→19
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.059H-atom parameters constrained
wR(F2) = 0.130w = 1/[σ2(Fo2) + (0.0594P)2 + 7.9006P] where P = (Fo2 + 2Fc2)/3
S = 1.08(Δ/σ)max < 0.001
3692 reflectionsΔρmax = 0.49 e Å−3
343 parametersΔρmin = −0.47 e Å−3
986 restraintsAbsolute structure: Flack (1983), 1110 Friedel pairs
Primary atom site location: structure-invariant direct methodsFlack parameter: 0.05 (3)
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > 2sigma(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.
xyzUiso*/Ueq
C10.30660 (19)0.3957 (4)0.2755 (3)0.0348 (7)
C20.3497 (2)0.4770 (4)0.2475 (3)0.0456 (11)
H2A0.31620.54980.20630.068*
H2B0.35740.42950.20270.068*
H2C0.40270.50330.31580.068*
C30.31584 (19)−0.0377 (3)0.3313 (3)0.0333 (10)
C40.36487 (16)−0.1389 (3)0.3277 (2)0.0270 (8)
H4A0.3272−0.19580.26680.041*
H4B0.3983−0.18470.39740.041*
H4C0.4001−0.10020.31670.041*
C50.39185 (18)0.2443 (4)0.6047 (3)0.0320 (9)
C60.4793 (2)0.2640 (4)0.7168 (3)0.0409 (11)
H6A0.51200.30960.70450.061*
H6B0.50460.18360.74990.061*
H6C0.47640.31110.76650.061*
C70.09410 (16)0.3896 (3)0.1609 (2)0.0290 (8)
C80.01608 (18)0.4630 (3)0.0702 (3)0.0315 (9)
H8A−0.01520.47870.09390.047*
H8B−0.01710.41490.00190.047*
H8C0.03110.54170.05750.047*
C90.10500 (15)−0.0215 (3)0.2246 (2)0.0254 (7)
C100.02352 (17)−0.0967 (3)0.1558 (3)0.0336 (9)
H10A0.0228−0.14870.20530.050*
H10B0.0195−0.14880.10230.050*
H10C−0.0226−0.03940.11680.050*
C110.1791 (2)0.2515 (4)0.4951 (3)0.0357 (10)
C120.1373 (2)0.2719 (4)0.5457 (3)0.0425 (11)
H12A0.15770.34850.58880.064*
H12B0.14990.20220.59380.064*
H12C0.07830.27780.48630.064*
C130.2572 (2)0.6577 (4)0.3982 (3)0.0376 (11)
H13A0.27270.63250.35520.056*
H13B0.29690.71730.45460.056*
H13C0.20310.69580.34940.056*
C140.3548 (2)−0.1309 (4)0.6294 (3)0.0441 (12)
H14A0.3815−0.15800.60100.066*
H14B0.3481−0.20160.66120.066*
H14C0.3883−0.06790.68620.066*
C160.0674 (3)0.6046 (5)0.3771 (4)0.0615 (15)
H16A0.03400.66480.37810.092*
H16B0.04730.52110.37090.092*
H16C0.06410.62110.31390.092*
Cr10.24501 (3)0.37094 (6)0.39698 (4)0.03574 (16)
Cr20.19595 (3)0.16932 (5)0.20163 (5)0.03655 (17)
Cr30.25541 (3)0.06601 (6)0.44353 (4)0.03542 (16)
N10.16124 (17)0.1451 (3)0.0481 (3)0.0411 (10)
N20.09146 (19)0.0877 (4)−0.0301 (3)0.0486 (11)
N30.04438 (17)0.0238 (3)−0.0905 (3)0.0415 (9)
O10.23315 (13)0.2032 (2)0.3494 (2)0.0366 (6)
O20.30800 (13)0.4304 (2)0.3528 (2)0.0381 (6)
O30.26887 (12)0.2994 (2)0.21374 (18)0.0318 (5)
O40.28633 (13)0.0431 (2)0.25849 (19)0.0351 (6)
O50.31318 (13)−0.0395 (2)0.40820 (19)0.0341 (6)
O60.36588 (13)0.1342 (2)0.57644 (19)0.0341 (6)
O70.35263 (15)0.3426 (2)0.5511 (2)0.0414 (7)
O80.14220 (14)0.4327 (2)0.2559 (2)0.0364 (7)
O90.10370 (13)0.2883 (2)0.12721 (19)0.0331 (6)
O100.12087 (14)0.0348 (3)0.16931 (19)0.0378 (6)
O110.14884 (12)−0.0185 (2)0.32863 (18)0.0324 (6)
O120.20495 (13)0.1442 (2)0.5015 (2)0.0378 (7)
O130.18466 (13)0.3474 (2)0.4524 (2)0.0364 (6)
O140.25539 (16)0.5504 (2)0.4508 (2)0.0397 (7)
O150.27862 (14)−0.0813 (3)0.5434 (2)0.0417 (7)
O160.14976 (14)0.6145 (3)0.4761 (2)0.0399 (8)
H16F0.15480.68360.51980.060*
H14D0.25350.56940.49980.060*
H15A0.2419−0.06690.54700.060*
U11U22U33U12U13U23
C10.0278 (9)0.0326 (15)0.0316 (7)0.0037 (10)0.0137 (6)0.0048 (9)
C20.0432 (12)0.0458 (19)0.0370 (13)−0.0092 (13)0.0213 (9)−0.0077 (13)
C30.0290 (11)0.0250 (14)0.0300 (12)0.0024 (11)0.0121 (8)0.0045 (11)
C40.0308 (9)0.0293 (15)0.0256 (10)−0.0053 (10)0.0204 (7)−0.0066 (11)
C50.0272 (10)0.0348 (16)0.0326 (12)0.0012 (12)0.0188 (8)−0.0020 (12)
C60.0338 (12)0.0416 (18)0.0363 (14)−0.0018 (14)0.0179 (10)0.0014 (14)
C70.0255 (9)0.0349 (16)0.0303 (10)0.0058 (11)0.0198 (7)0.0067 (11)
C80.0308 (11)0.0261 (15)0.0309 (12)0.0075 (12)0.0170 (8)−0.0005 (11)
C90.0261 (8)0.0277 (15)0.0341 (8)0.0003 (9)0.0247 (6)−0.0053 (9)
C100.0372 (10)0.0294 (16)0.0389 (12)−0.0152 (11)0.0268 (8)−0.0164 (11)
C110.0319 (11)0.0310 (15)0.0283 (12)0.0020 (12)0.0125 (8)−0.0036 (12)
C120.0353 (12)0.0362 (18)0.0385 (14)0.0067 (14)0.0161 (9)−0.0006 (14)
C130.0359 (13)0.0311 (17)0.0316 (13)−0.0065 (13)0.0156 (10)−0.0092 (13)
C140.0360 (13)0.0302 (17)0.0481 (16)−0.0055 (13)0.0192 (10)0.0020 (14)
C160.0601 (18)0.042 (2)0.0531 (19)0.0028 (18)0.0239 (13)−0.0114 (17)
Cr10.03062 (18)0.0319 (3)0.0343 (2)−0.0015 (2)0.01643 (14)−0.0020 (2)
Cr20.0327 (2)0.0252 (2)0.0313 (2)−0.0022 (2)0.01160 (16)−0.0014 (2)
Cr30.03091 (18)0.0307 (3)0.0328 (2)−0.0003 (2)0.01535 (15)−0.0001 (2)
N10.0346 (12)0.0321 (15)0.0345 (12)−0.0021 (12)0.0125 (9)0.0019 (12)
N20.0338 (12)0.0470 (17)0.0418 (14)−0.0075 (13)0.0142 (10)−0.0084 (13)
N30.0349 (11)0.0421 (16)0.0385 (12)−0.0112 (12)0.0198 (8)−0.0107 (12)
O10.0333 (7)0.0309 (9)0.0317 (6)−0.0027 (8)0.0149 (5)0.0006 (7)
O20.0335 (6)0.0320 (9)0.0355 (6)−0.0059 (8)0.0165 (5)−0.0047 (7)
O30.0332 (6)0.0327 (9)0.0284 (7)−0.0041 (6)0.0195 (5)−0.0006 (7)
O40.0372 (7)0.0300 (9)0.0292 (7)0.0077 (7)0.0176 (6)0.0013 (7)
O50.0329 (7)0.0278 (9)0.0303 (8)0.0021 (7)0.0155 (6)0.0022 (7)
O60.0336 (7)0.0285 (9)0.0296 (8)−0.0017 (8)0.0158 (6)−0.0012 (8)
O70.0365 (8)0.0293 (9)0.0323 (8)−0.0001 (8)0.0107 (6)−0.0012 (8)
O80.0358 (8)0.0286 (9)0.0312 (8)0.0040 (8)0.0156 (6)0.0009 (8)
O90.0314 (7)0.0325 (9)0.0280 (7)0.0044 (7)0.0160 (5)−0.0011 (7)
O100.0378 (6)0.0356 (8)0.0287 (7)−0.0088 (5)0.0166 (5)0.0026 (7)
O110.0288 (7)0.0299 (9)0.0337 (7)−0.0056 (7)0.0181 (5)0.0023 (7)
O120.0316 (7)0.0329 (10)0.0367 (8)−0.0005 (8)0.0168 (6)−0.0027 (8)
O130.0370 (7)0.0281 (9)0.0345 (8)0.0016 (8)0.0189 (6)−0.0010 (7)
O140.0392 (7)0.0316 (9)0.0305 (8)0.0013 (8)0.0146 (6)−0.0029 (8)
O150.0376 (8)0.0313 (10)0.0339 (9)0.0031 (8)0.0133 (6)0.0023 (8)
O160.0378 (9)0.0369 (12)0.0277 (9)−0.0048 (10)0.0135 (7)−0.0136 (9)
C1—O21.245 (5)C13—O141.419 (5)
C1—O31.270 (4)C13—H13A0.9600
C1—C21.511 (7)C13—H13B0.9600
C2—H2A0.9600C13—H13C0.9600
C2—H2B0.9600C14—O151.367 (4)
C2—H2C0.9600C14—H14A0.9600
C3—O41.224 (4)C14—H14B0.9600
C3—O51.241 (5)C14—H14C0.9600
C3—C41.519 (5)C16—O161.394 (4)
C4—H4A0.9600C16—H16A0.9600
C4—H4B0.9600C16—H16B0.9600
C4—H4C0.9600C16—H16C0.9600
C5—O61.243 (4)Cr1—O11.881 (3)
C5—O71.256 (4)Cr1—O81.949 (2)
C5—C61.527 (4)Cr1—O21.961 (3)
C6—H6A0.9600Cr1—O131.970 (3)
C6—H6B0.9600Cr1—O71.990 (2)
C6—H6C0.9600Cr1—O142.035 (3)
C7—O81.220 (4)Cr2—O11.931 (3)
C7—O91.270 (5)Cr2—O101.943 (3)
C7—C81.517 (4)Cr2—O91.952 (2)
C8—H8A0.9600Cr2—O31.986 (3)
C8—H8B0.9600Cr2—O42.009 (3)
C8—H8C0.9600Cr2—N12.021 (4)
C9—O111.245 (4)Cr3—O11.900 (3)
C9—O101.262 (5)Cr3—O111.964 (2)
C9—C101.536 (4)Cr3—O121.976 (3)
C10—H10A0.9600Cr3—O51.983 (3)
C10—H10B0.9600Cr3—O62.000 (2)
C10—H10C0.9600Cr3—O152.032 (3)
C11—O121.239 (5)N1—N21.305 (4)
C11—O131.264 (5)N2—N31.059 (4)
C11—C121.538 (7)O14—H14D0.8179
C12—H12A0.9600O15—H15A0.8296
C12—H12B0.9600O16—H16F0.9601
C12—H12C0.9600
O2—C1—O3125.7 (4)H16B—C16—H16C109.5
O2—C1—C2118.3 (3)O1—Cr1—O896.06 (10)
O3—C1—C2116.0 (4)O1—Cr1—O296.40 (13)
C1—C2—H2A109.5O8—Cr1—O290.44 (12)
C1—C2—H2B109.5O1—Cr1—O1395.49 (13)
H2A—C2—H2B109.5O8—Cr1—O1388.55 (12)
C1—C2—H2C109.5O2—Cr1—O13168.11 (11)
H2A—C2—H2C109.5O1—Cr1—O795.18 (10)
H2B—C2—H2C109.5O8—Cr1—O7168.75 (11)
O4—C3—O5126.6 (4)O2—Cr1—O788.29 (12)
O4—C3—C4114.2 (4)O13—Cr1—O790.40 (13)
O5—C3—C4119.1 (3)O1—Cr1—O14177.65 (16)
C3—C4—H4A109.5O8—Cr1—O1483.99 (10)
C3—C4—H4B109.5O2—Cr1—O1485.95 (13)
H4A—C4—H4B109.5O13—Cr1—O1482.16 (13)
C3—C4—H4C109.5O7—Cr1—O1484.77 (10)
H4A—C4—H4C109.5O1—Cr2—O1094.44 (12)
H4B—C4—H4C109.5O1—Cr2—O993.78 (11)
O6—C5—O7126.5 (3)O10—Cr2—O989.29 (11)
O6—C5—C6117.6 (3)O1—Cr2—O393.94 (11)
O7—C5—C6115.8 (3)O10—Cr2—O3171.55 (13)
C5—C6—H6A109.5O9—Cr2—O391.26 (11)
C5—C6—H6B109.5O1—Cr2—O493.63 (11)
H6A—C6—H6B109.5O10—Cr2—O490.47 (11)
C5—C6—H6C109.5O9—Cr2—O4172.58 (12)
H6A—C6—H6C109.5O3—Cr2—O487.90 (11)
H6B—C6—H6C109.5O1—Cr2—N1175.94 (14)
O8—C7—O9126.2 (3)O10—Cr2—N189.56 (13)
O8—C7—C8119.2 (3)O9—Cr2—N185.55 (12)
O9—C7—C8114.6 (3)O3—Cr2—N182.08 (13)
C7—C8—H8A109.5O4—Cr2—N187.03 (12)
C7—C8—H8B109.5O1—Cr3—O1194.65 (10)
H8A—C8—H8B109.5O1—Cr3—O1295.62 (13)
C7—C8—H8C109.5O11—Cr3—O1288.27 (11)
H8A—C8—H8C109.5O1—Cr3—O595.98 (13)
H8B—C8—H8C109.5O11—Cr3—O592.11 (11)
O11—C9—O10125.4 (3)O12—Cr3—O5168.32 (11)
O11—C9—C10118.3 (3)O1—Cr3—O693.59 (10)
O10—C9—C10116.3 (3)O11—Cr3—O6171.59 (12)
C9—C10—H10A109.5O12—Cr3—O689.24 (11)
C9—C10—H10B109.5O5—Cr3—O688.72 (11)
H10A—C10—H10B109.5O1—Cr3—O15179.66 (11)
C9—C10—H10C109.5O11—Cr3—O1585.02 (10)
H10A—C10—H10C109.5O12—Cr3—O1584.44 (13)
H10B—C10—H10C109.5O5—Cr3—O1583.97 (12)
O12—C11—O13126.4 (5)O6—Cr3—O1586.74 (10)
O12—C11—C12117.4 (4)N2—N1—Cr2119.4 (3)
O13—C11—C12116.2 (4)N3—N2—N1166.3 (4)
C11—C12—H12A109.5Cr1—O1—Cr3121.05 (16)
C11—C12—H12B109.5Cr1—O1—Cr2119.72 (15)
H12A—C12—H12B109.5Cr3—O1—Cr2119.22 (14)
C11—C12—H12C109.5C1—O2—Cr1130.8 (2)
H12A—C12—H12C109.5C1—O3—Cr2134.2 (3)
H12B—C12—H12C109.5C3—O4—Cr2130.0 (3)
O14—C13—H13A109.5C3—O5—Cr3133.3 (2)
O14—C13—H13B109.5C5—O6—Cr3131.1 (2)
H13A—C13—H13B109.5C5—O7—Cr1132.4 (2)
O14—C13—H13C109.5C7—O8—Cr1133.5 (2)
H13A—C13—H13C109.5C7—O9—Cr2131.88 (17)
H13B—C13—H13C109.5C9—O10—Cr2134.9 (2)
O15—C14—H14A109.5C9—O11—Cr3130.3 (3)
O15—C14—H14B109.5C11—O12—Cr3133.7 (3)
H14A—C14—H14B109.5C11—O13—Cr1130.1 (3)
O15—C14—H14C109.5C13—O14—Cr1123.2 (3)
H14A—C14—H14C109.5C13—O14—H14D112.4
H14B—C14—H14C109.5Cr1—O14—H14D124.1
O16—C16—H16A109.5C14—O15—Cr3126.4 (3)
O16—C16—H16B109.5C14—O15—H15A124.3
H16A—C16—H16B109.5Cr3—O15—H15A98.1
O16—C16—H16C109.5C16—O16—H16F109.2
H16A—C16—H16C109.5
O1—Cr2—N1—N2−150.2 (17)C6—C5—O6—Cr3176.4 (3)
O10—Cr2—N1—N219.8 (3)O1—Cr3—O6—C529.2 (4)
O9—Cr2—N1—N2−69.5 (3)O11—Cr3—O6—C5−139.1 (8)
O3—Cr2—N1—N2−161.4 (3)O12—Cr3—O6—C5−66.3 (4)
O4—Cr2—N1—N2110.3 (3)O5—Cr3—O6—C5125.2 (4)
Cr2—N1—N2—N3−110 (2)O15—Cr3—O6—C5−150.8 (4)
O8—Cr1—O1—Cr3−136.06 (16)O6—C5—O7—Cr1−9.9 (8)
O2—Cr1—O1—Cr3132.82 (15)C6—C5—O7—Cr1171.7 (3)
O13—Cr1—O1—Cr3−46.94 (15)O1—Cr1—O7—C5−10.8 (4)
O7—Cr1—O1—Cr343.96 (18)O8—Cr1—O7—C5169.4 (7)
O14—Cr1—O1—Cr3−45 (2)O2—Cr1—O7—C5−107.0 (4)
O8—Cr1—O1—Cr242.87 (18)O13—Cr1—O7—C584.8 (4)
O2—Cr1—O1—Cr2−48.26 (15)O14—Cr1—O7—C5166.9 (4)
O13—Cr1—O1—Cr2131.98 (15)O9—C7—O8—Cr1−5.3 (7)
O7—Cr1—O1—Cr2−137.11 (17)C8—C7—O8—Cr1177.1 (3)
O14—Cr1—O1—Cr2134 (2)O1—Cr1—O8—C7−13.9 (4)
O11—Cr3—O1—Cr1128.45 (16)O2—Cr1—O8—C782.6 (4)
O12—Cr3—O1—Cr139.74 (16)O13—Cr1—O8—C7−109.3 (4)
O5—Cr3—O1—Cr1−138.94 (15)O7—Cr1—O8—C7166.0 (7)
O6—Cr3—O1—Cr1−49.85 (17)O14—Cr1—O8—C7168.5 (4)
O15—Cr3—O1—Cr1140 (50)O8—C7—O9—Cr2−5.1 (6)
O11—Cr3—O1—Cr2−50.48 (17)C8—C7—O9—Cr2172.6 (3)
O12—Cr3—O1—Cr2−139.20 (14)O1—Cr2—O9—C729.4 (4)
O5—Cr3—O1—Cr242.13 (15)O10—Cr2—O9—C7123.8 (4)
O6—Cr3—O1—Cr2131.22 (16)O3—Cr2—O9—C7−64.6 (4)
O15—Cr3—O1—Cr2−39 (26)O4—Cr2—O9—C7−148.0 (8)
O10—Cr2—O1—Cr1−137.26 (15)N1—Cr2—O9—C7−146.6 (4)
O9—Cr2—O1—Cr1−47.68 (16)O11—C9—O10—Cr2−15.3 (6)
O3—Cr2—O1—Cr143.85 (16)C10—C9—O10—Cr2163.1 (2)
O4—Cr2—O1—Cr1131.99 (15)O1—Cr2—O10—C9−5.6 (3)
N1—Cr2—O1—Cr132.8 (19)O9—Cr2—O10—C9−99.3 (3)
O10—Cr2—O1—Cr341.69 (16)O3—Cr2—O10—C9166.9 (6)
O9—Cr2—O1—Cr3131.27 (15)O4—Cr2—O10—C988.1 (3)
O3—Cr2—O1—Cr3−137.21 (15)N1—Cr2—O10—C9175.1 (3)
O4—Cr2—O1—Cr3−49.07 (16)O10—C9—O11—Cr3−1.6 (5)
N1—Cr2—O1—Cr3−148.3 (17)C10—C9—O11—Cr3−180.0 (2)
O3—C1—O2—Cr1−9.1 (5)O1—Cr3—O11—C932.0 (3)
C2—C1—O2—Cr1167.7 (2)O12—Cr3—O11—C9127.5 (3)
O1—Cr1—O2—C130.3 (3)O5—Cr3—O11—C9−64.2 (3)
O8—Cr1—O2—C1−65.8 (3)O6—Cr3—O11—C9−159.7 (8)
O13—Cr1—O2—C1−150.8 (4)O15—Cr3—O11—C9−148.0 (3)
O7—Cr1—O2—C1125.4 (3)O13—C11—O12—Cr3−5.7 (5)
O14—Cr1—O2—C1−149.8 (3)C12—C11—O12—Cr3175.46 (19)
O2—C1—O3—Cr22.7 (5)O1—Cr3—O12—C11−10.1 (3)
C2—C1—O3—Cr2−174.2 (2)O11—Cr3—O12—C11−104.6 (3)
O1—Cr2—O3—C1−19.3 (3)O5—Cr3—O12—C11163.4 (4)
O10—Cr2—O3—C1168.2 (6)O6—Cr3—O12—C1183.5 (3)
O9—Cr2—O3—C174.6 (3)O15—Cr3—O12—C11170.3 (3)
O4—Cr2—O3—C1−112.8 (3)O12—C11—O13—Cr1−7.8 (5)
N1—Cr2—O3—C1159.9 (3)C12—C11—O13—Cr1171.06 (19)
O5—C3—O4—Cr2−21.2 (5)O1—Cr1—O13—C1131.7 (3)
C4—C3—O4—Cr2163.1 (2)O8—Cr1—O13—C11127.6 (3)
O1—Cr2—O4—C339.6 (3)O2—Cr1—O13—C11−147.2 (4)
O10—Cr2—O4—C3−54.9 (3)O7—Cr1—O13—C11−63.6 (3)
O9—Cr2—O4—C3−143.0 (8)O14—Cr1—O13—C11−148.2 (3)
O3—Cr2—O4—C3133.4 (3)O1—Cr1—O14—C13−150 (2)
N1—Cr2—O4—C3−144.4 (3)O8—Cr1—O14—C13−58.2 (3)
O4—C3—O5—Cr37.1 (5)O2—Cr1—O14—C1332.6 (2)
C4—C3—O5—Cr3−177.4 (2)O13—Cr1—O14—C13−147.6 (3)
O1—Cr3—O5—C3−17.4 (3)O7—Cr1—O14—C13121.3 (3)
O11—Cr3—O5—C377.5 (3)O1—Cr3—O15—C14139 (26)
O12—Cr3—O5—C3169.1 (4)O11—Cr3—O15—C14150.3 (4)
O6—Cr3—O5—C3−110.9 (3)O12—Cr3—O15—C14−121.0 (4)
O15—Cr3—O5—C3162.3 (3)O5—Cr3—O15—C1457.7 (3)
O7—C5—O6—Cr3−2.0 (7)O6—Cr3—O15—C14−31.4 (4)
D—H···AD—HH···AD···AD—H···A
O16—H16F···N1i0.961.852.734 (4)151.
O16—H16F···O3i0.962.362.972 (3)122.
O16—H16F···O9i0.962.543.254 (5)132.
O16—H16F···N2i0.962.633.370 (5)134.
O15—H15A···N1ii0.831.912.621 (5)144.
O15—H15A···N2ii0.832.583.332 (5)152.
O14—H14D···O160.822.032.602 (5)126.
Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯AD⋯AD—H⋯A
O16—H16F⋯N1i0.961.852.734 (4)151
O16—H16F⋯O3i0.962.362.972 (3)122
O16—H16F⋯O9i0.962.543.254 (5)132
O16—H16F⋯N2i0.962.633.370 (5)134
O15—H15A⋯N1ii0.831.912.621 (5)144
O15—H15A⋯N2ii0.832.583.332 (5)152
O14—H14D⋯O160.822.032.602 (5)126

Symmetry codes: (i) ; (ii) .

  4 in total

Review 1.  Elucidating a biological role for chromium at a molecular level.

Authors:  J B Vincent
Journal:  Acc Chem Res       Date:  2000-07       Impact factor: 22.384

2.  Crystal Structures of the Isomorphous Prototypic Oxo-Centered Trinuclear Complexes [Cr(3)O(OOCCH(3))(6)(H(2)O)(3)]Cl.6H(2)O and [Fe(3)O(OOCCH(3))(6)(H(2)O)(3)]Cl.6H(2)O.

Authors:  C. E. Anson; J. P. Bourke; R. D. Cannon; U. A. Jayasooriya; M. Molinier; A. K. Powell
Journal:  Inorg Chem       Date:  1997-03-12       Impact factor: 5.165

3.  A short history of SHELX.

Authors:  George M Sheldrick
Journal:  Acta Crystallogr A       Date:  2007-12-21       Impact factor: 2.290

4.  Kinetic Study on the Substitution of Dimethylacetamide for the Terminal Aqua Ligands in the Trinuclear Chromium(III) Complexes [Cr(3)(&mgr;(3)-O)(&mgr;-RCO(2))(6)(H(2)O)(3)](+) (R = H, CH(3), CH(3)CH(2), CH(2)Cl, CHCl(2), CH(3)OCH(2), (CH(3))(3)C, CH(2)ClCH(2), (CH(3)CH(2))(2)CH). Elucidation of the Mechanism from the Activation Volumes and the Substituent Effects of Bridging Carboxylate Ligands.

Authors:  Takashi Fujihara; Jun Aonahata; Shigekazu Kumakura; Akira Nagasawa; Kazuhiro Murakami; Tasuku Ito
Journal:  Inorg Chem       Date:  1998-07-27       Impact factor: 5.165
  4 in total

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