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The synthesis of 1'-phenyl­thio-1-ferroceneboronic acid resulted in its trimerization with the loss of three mol­ecules of water to form crystalline 2,4,6-tris(1'-phenyl­thio-1-ferro­cen­yl)­boroxin, C48H39B3Fe3O3S3 or [Fe3(C15H12B3O3)(C11H9S)3]. The asymmetric unit contains two boroxin mol­ecules conjugated with the attached cyclo­penta­dienyl rings to form an aromatic ring. The cyclo­penta­dienyl rings of five of the six ferrocenes are in an eclipsed conformation; the cyclo­penta­dienyl rings of the other ferrocene are in the gauche form. Hydro­lysis of the boroxin ring with aqueous base apparently is needed to produce the corresponding boronic acid required in a Suzuki coupling reaction.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536801013988/om6042sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536801013988/om6042Isup2.hkl
Contains datablock I

CCDC reference: 172196

Key indicators

  • Single-crystal X-ray study
  • T = 296 K
  • Mean [sigma](C-C) = 0.016 Å
  • R factor = 0.047
  • wR factor = 0.158
  • Data-to-parameter ratio = 14.3

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry








Comment top

In contrast to the identification of 2-(N,N-dimethylaminoalkyl)ferroceneboronic acids by their crystal structures (Norrild & Sotofte, 2001), our attempt to characterize 1'-phenylthio-1-ferroceneboronic acid, (II), by X-ray analysis showed that its structure was exclusively that of the corresponding boroxin, i.e the title compound, (I). In our studies of chiral ferrocenyl phosphine ligands (Hua et al., 2001), (I) was synthesized from the metallation of 1,1'-bis(tri-n-butylstannyl)ferrocene with n-butyllithium, followed by treatment with diphenyl disulfide, and a subsequent second metallation with n-butyllithium, followed by borination with trimethyl borate and acid hydrolysis. The fact that we found that water is needed in the Suzuki coupling reaction (Miyaura, 1998) when we used (I) as a substrate, and that insufficient structural characterization was afforded by spectroscopic methods, made us unsure of the unequivocal identity of the product, and we turned to X-ray analysis. Indeed, the X-ray structure of (I), shown with atom numbering in Fig. 1, indicates that the initial boronic acid product derived from the aforementioned reactions underwent complete dehydration to form the boroxin.

Although ferroceneboronic acid underwent partial dehydration in vacuo after several days to give triferrocenylboroxin (Post et al., 1970), 1'-phenylthio-1-ferroceneboronic acid, (II), apparently exists, at least in its crystalline state, exclusively as the boroxin (I). This anhydro structure explains the need to use water and base (such as sodium carbonate) in Suzuki reactions of (I), i.e. in order to hydrolyze it into boronic acid (II) so that a coupling reaction with an aryl halide may take place in the presence of palladium(0). X-ray structures of triferrocenylboroxins have not been reported previously.

The asymmetric unit of (I) contains two chemically identical but conformationally slightly different molecules, the largest conformational variation involving the ferrocene moieties containing Fe3 and Fe3a, respectively. In molecule 1, the ferrocene moiety containing Fe3 is essentially eclipsed, while in molecule 2 the corresponding ferrocene moiety, Fe3a, is nearly perfectly staggered. In fact, all of the other ferrocene moieties are essentially eclipsed; the actual rotational values for each ferrocene moiety is tabulated in the CIF. A second significant conformational difference involves the dihedral angle between the boroxin ring and the lower cyclopentadienyl ring of the Fe3/Fe3a ferrocene moieties, the values being 16.4 (5) and 6.6 (6)°, respectively. Of course both of these differences produce several associated torsional differences. Other dihedral angles between the boroxin rings and their bonded cyclopentadienyl rings are 3.6 (5), 3.6 (5), 7.3 (5) and 5.9 (5)° for the Fe1, Fe1a, Fe2, and Fe2a ferrocene moieties, respectively. Stabilization from the aromaticity of the boroxin ring (Jug, 1983) is likely the driving force for the formation of (I). Indeed, the boroxin-ring atoms are reasonably coplanar in both molecules, the deviations from planarity ranging from -0.020 (5) to 0.020 (10) Å and -0.027 (6) to 0.021 (12) Å, respectively, for molecules 1 and 2. The sp2-hybridized B—O bond lengths of (I) range from 1.369 (10) to 1.387 (10) Å in molecule 1 and from 1.368 (11) to 1.390 (12) Å in molecule 2. These bond lengths are in marked contrast to that of the sp3-hybridized B—O single bond of 1.505 Å reported by Voloshin et al. (1997), and are consistent with an aromatic ring structure. Selected geometric parameters are listed in Table 1.

Experimental top

2,4,6-Tris(1'-phenylthio-1-ferrocenyl)boroxin, (I), was prepared by treating a cold (195 K) tetrahydrofuran (10 ml) solution of 1,1'-bis(tri-n-butylstannyl)ferrocene (1.56 g, 2.0 mmol) (Wright, 1990) under argon with n-BuLi (in hexane, 2.0 mmol) for 30 min, followed by the addition of diphenyl disulfide (0.436 g, 2.0 mmol). After the solution was stirred at 195 K for 1 h and 273 K for 3 h, the reaction was quenched with aqueous ammonium chloride, and extracted with diethyl ether, and the ether extract was dried (MgSO4), concentrated, and column chromatographed on silica gel to give an 89% yield of 1-(tri-n-butylstannyl)-1'-(phenylthio)ferrocene. The resulting sulfenylferrocene (0.60 g, 1.0 mmol) in 10 ml of tetrahydrofuran under argon was treated with n-BuLi (in hexane, 1.2 mmol) at 195 K for 30 min, followed by trimethyl borate (0.13 ml, 1.2 mmol). After the solution was stirred at 195 K for 1 h and 273 K for 1 h, 0.5 N HCl (10 ml) was added, and the solution was stirred at 248 K for 1 h and extracted with ether. The ether extract was dried (MgSO4), concentrated, and triturated with cold hexane twice, and the remaining yellow solids were dried under vacuo to give (I) (74% yield). Recrystallization of (I) from ether gave yellow crystals (m.p. 404–406 K) suitable for X-ray analysis.

Refinement top

Although the crystal diffracted strongly at low angle and was of good quality judging by its peak shapes, it diffracted poorly at higher angles. Thus only about 30% of the approximately 15 000 possible diffraction maxima were observed at the 2σ level, despite three weeks of data collection. Certainly low-temperature data would have improved the data set considerably but our laboratory does not currently have that capability.

Computing details top

Data collection: MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1996); cell refinement: MSC/AFC Diffractometer Control Software; data reduction: PROCESS in TEXSAN (Molecular Structure Corporation, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: LS in TEXSAN and SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP (Johnson, 1965) in TEXSAN; software used to prepare material for publication: TEXSAN, SHELXL97 and PLATON (Spek, 2000).

Figures top
[Figure 1] Fig. 1. The molecular structure and atom-numbering scheme for (I) with displacement ellipsoids at the 30% probablilty level. The relative orientation of the two molecules in the asymmetric unit has been changed so that they can be more easily compared.
2,4,6-Tris(1'-phenylthio-1-ferrocenyl)boroxin top
Crystal data top
[Fe3(C15H12B3O3)(C11H9S)3]F(000) = 1968
Mr = 959.98Dx = 1.463 Mg m3
Triclinic, P1Melting point = 404–406 K
a = 17.501 (4) ÅMo Kα radiation, λ = 0.71069 Å
b = 18.875 (5) ÅCell parameters from 25 reflections
c = 14.999 (4) Åθ = 10.1–13.1°
α = 113.137 (19)°µ = 1.17 mm1
β = 101.89 (2)°T = 296 K
γ = 74.30 (2)°Prism, brown
V = 4358.4 (19) Å30.43 × 0.17 × 0.13 mm
Z = 4
Data collection top
Rigaku AFC-5S
diffractometer
4619 reflections with I > 2σ(I)
Radiation source: sealed tubeRint = 0.079
Graphite monochromatorθmax = 25.1°, θmin = 1.8°
ω scansh = 020
Absorption correction: ψ scan
(North et al., 1968)
k = 2122
Tmin = 0.791, Tmax = 0.859l = 1717
16062 measured reflections3 standard reflections every 100 reflections
15452 independent reflections intensity decay: 0.9%
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.047Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.158H-atom parameters constrained
S = 0.93 w = 1/[σ2(Fo2) + (0.0438P)2]
where P = (Fo2 + 2Fc2)/3
15452 reflections(Δ/σ)max = 0.001
1081 parametersΔρmax = 0.40 e Å3
0 restraintsΔρmin = 0.49 e Å3
Crystal data top
[Fe3(C15H12B3O3)(C11H9S)3]γ = 74.30 (2)°
Mr = 959.98V = 4358.4 (19) Å3
Triclinic, P1Z = 4
a = 17.501 (4) ÅMo Kα radiation
b = 18.875 (5) ŵ = 1.17 mm1
c = 14.999 (4) ÅT = 296 K
α = 113.137 (19)°0.43 × 0.17 × 0.13 mm
β = 101.89 (2)°
Data collection top
Rigaku AFC-5S
diffractometer
4619 reflections with I > 2σ(I)
Absorption correction: ψ scan
(North et al., 1968)
Rint = 0.079
Tmin = 0.791, Tmax = 0.8593 standard reflections every 100 reflections
16062 measured reflections intensity decay: 0.9%
15452 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0470 restraints
wR(F2) = 0.158H-atom parameters constrained
S = 0.93Δρmax = 0.40 e Å3
15452 reflectionsΔρmin = 0.49 e Å3
1081 parameters
Special details top

Geometry. FERROCENE GROUP CENTROIDS

Ferrocene Name Fractional Coordinates

Fe1 (bottom) Cg1 0.3659 (2) 1.0827 (2) 0.9680 (3) Fe1 (top) Cg2 0.2254 (2) 1.0619 (2) 0.7820 (3) Fe2 (bottom) Cg3 0.5496 (2) 0.6678 (2) 0.8118 (3) Fe2 (top) Cg4 0.3964 (2) 0.6438 (3) 0.6434 (3) Fe3 (bottom) Cg5 0.6717 (2) 0.9288 (2) 0.6565 (3) Fe3 (top) Cg6 0.5741 (3) 0.8381 (2) 0.4475 (3) Fe1a (bottom) Cg7 0.1365 (2) 0.9727 (2) 0.0910 (3) Fe1a (top) Cg8 0.2946 (2) 0.8243 (2) 0.0582 (3) Fe2a (bottom) Cg9 - 0.0175 (2) 0.8674 (3) -0.4184 (3) Fe2a (top) Cg10 0.1456 (3) 0.7296 (2) -0.4633 (4) Fe3a (bottom) Cg11 - 0.1489 (3) 0.7239 (3) -0.1176 (4) Fe3a (top) Cg12 - 0.0181 (3) 0.5559 (3) -0.1879 (5)

FERROCENE TORSION ANGLES

Fe1 Ferrocene

C1—Cg1—Cg2—C6 - 6.5 (7) C2—Cg1—Cg2—C7 - 6.9 (7) C3—Cg1—Cg2—C8 - 7.1 (7) C4—Cg1—Cg2—C9 - 6.9 (8) C5—Cg1—Cg2—C10 - 6.5 (6) —————————

Fe2 Ferrocene

C11—Cg3—Cg4—C16 - 7.0 (6) C12—Cg3—Cg4—C17 - 6.4 (8) C13—Cg3—Cg4—C18 - 6.0 (8) C14—Cg3—Cg4—C19 - 6.1 (7) C15—Cg3—Cg4—C20 - 6.8 (7) —————————

Fe3 Ferrocene

C21—Cg5—Cg6—C26 2.2 (8) C22—Cg5—Cg6—C27 4.0 (7) C23—Cg5—Cg6—C28 3.6 (8) C24—Cg5—Cg6—C29 2.5 (8) C25—Cg5—Cg6—C30 2.6 (7) —————————

Fe1a Ferrocene

C1a—Cg7—Cg8—C6a -5.1 (7) C2a—Cg7—Cg8—C7a -5.4 (6) C3a—Cg7—Cg8—C8a -5.7 (7) C4a—Cg7—Cg8—C9a -5.7 (7) C5a—Cg7—Cg8—C10a - 4.9 (7) —————————-

Fe2a Ferrocene

C11aCg9—Cg10—C16a - 12.2 (7) C12aCg9—Cg10—C17a - 11.5 (8) C13aCg9—Cg10—C18a - 10.4 (9) C14aCg9—Cg10—C19a - 12.3 (9) C15aCg9—Cg10—C20a - 11.2 (7) ——————————

Fe3a

C21aCg11—Cg12—C26a - 41.8 (11) C22aCg11—Cg12—C27a - 40.9 (9) C23aCg11—Cg12—C28a - 41.6 (9) C24aCg11—Cg12—C29a - 42.2 (9) C25aCg11—Cg12—C30a - 41.3 (11) ———————————

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Fe10.29685 (7)1.06919 (6)0.87315 (8)0.0471 (3)
Fe20.47392 (7)0.65657 (6)0.72540 (9)0.0492 (3)
Fe30.62170 (7)0.88341 (7)0.55256 (9)0.0497 (3)
S10.33682 (15)0.93442 (14)0.65159 (16)0.0696 (7)
S20.49139 (14)0.65204 (14)0.50676 (18)0.0638 (7)
S30.73295 (16)0.77355 (15)0.37595 (18)0.0737 (7)
O10.5161 (3)0.9637 (3)0.8049 (4)0.0507 (14)
O20.4739 (3)0.8787 (3)0.8586 (3)0.0491 (14)
O30.5778 (3)0.8279 (3)0.7552 (4)0.0519 (15)
B10.4684 (6)0.9526 (6)0.8588 (7)0.044 (2)
B20.5312 (6)0.8160 (5)0.8096 (7)0.046 (3)
B30.5721 (6)0.9014 (6)0.7544 (7)0.048 (3)
C10.4118 (5)1.0249 (5)0.9210 (5)0.046 (2)
C20.4030 (5)1.1039 (5)0.9291 (6)0.054 (2)
C30.3443 (5)1.1524 (5)0.9898 (6)0.061 (3)
C40.3147 (5)1.1056 (5)1.0217 (6)0.062 (3)
C50.3559 (5)1.0269 (5)0.9783 (5)0.052 (2)
C60.2704 (5)1.0093 (5)0.7288 (5)0.050 (2)
C70.2581 (5)1.0910 (5)0.7472 (6)0.061 (3)
C80.2011 (5)1.1319 (5)0.8138 (6)0.064 (3)
C90.1777 (5)1.0766 (6)0.8359 (6)0.066 (3)
C100.2195 (5)1.0006 (5)0.7844 (6)0.057 (2)
C110.5439 (5)0.7343 (5)0.8138 (6)0.049 (2)
C120.5046 (5)0.7108 (5)0.8694 (6)0.058 (2)
C130.5274 (5)0.6289 (6)0.8462 (7)0.067 (3)
C140.5804 (6)0.6010 (5)0.7745 (7)0.071 (3)
C150.5917 (5)0.6638 (5)0.7550 (6)0.061 (3)
C160.3848 (5)0.7114 (5)0.6521 (6)0.063 (3)
C170.3520 (5)0.6808 (7)0.7042 (7)0.071 (3)
C180.3811 (6)0.6008 (6)0.6733 (7)0.076 (3)
C190.4308 (5)0.5782 (5)0.6004 (6)0.061 (2)
C200.4333 (5)0.6477 (5)0.5870 (6)0.050 (2)
C210.6291 (5)0.9165 (5)0.7024 (6)0.048 (2)
C220.7025 (5)0.8660 (5)0.6638 (6)0.058 (2)
C230.7320 (5)0.9029 (6)0.6177 (7)0.073 (3)
C240.6787 (6)0.9750 (6)0.6230 (7)0.068 (3)
C250.6163 (5)0.9834 (5)0.6754 (6)0.056 (2)
C260.5291 (6)0.8267 (6)0.4877 (7)0.071 (3)
C270.6018 (6)0.7765 (5)0.4592 (6)0.063 (3)
C280.6372 (5)0.8107 (5)0.4149 (6)0.060 (3)
C290.5849 (6)0.8836 (5)0.4148 (6)0.061 (2)
C300.5177 (5)0.8929 (5)0.4609 (7)0.066 (3)
C310.2800 (5)0.9146 (5)0.5358 (5)0.044 (2)
C320.2083 (5)0.9625 (5)0.5155 (6)0.060 (2)
C330.1703 (5)0.9420 (5)0.4225 (7)0.065 (3)
C340.2012 (6)0.8764 (5)0.3485 (6)0.061 (3)
C350.2715 (6)0.8285 (5)0.3683 (6)0.058 (2)
C360.3098 (5)0.8478 (5)0.4615 (7)0.054 (2)
C370.4305 (6)0.6323 (5)0.3932 (7)0.059 (2)
C380.3526 (6)0.6268 (5)0.3835 (7)0.070 (3)
C390.3072 (6)0.6124 (6)0.2929 (10)0.085 (3)
C400.3407 (9)0.6035 (6)0.2138 (9)0.103 (4)
C410.4155 (8)0.6105 (7)0.2232 (9)0.104 (4)
C420.4625 (7)0.6238 (6)0.3127 (9)0.093 (4)
C430.7170 (8)0.7175 (6)0.2492 (7)0.073 (3)
C440.6455 (9)0.7292 (6)0.1949 (8)0.101 (4)
C450.6370 (10)0.6869 (8)0.0938 (10)0.127 (5)
C460.6988 (14)0.6334 (10)0.0525 (12)0.144 (8)
C470.7687 (12)0.6188 (10)0.1065 (13)0.145 (7)
C480.7792 (8)0.6616 (7)0.2061 (10)0.106 (4)
H20.43191.12080.89870.065*
H30.32771.20671.00630.074*
H40.27541.12291.06340.075*
H50.34750.98330.98630.062*
H70.28351.11370.71990.074*
H80.18231.18620.83850.077*
H90.14031.08790.87820.079*
H100.21460.95340.78640.068*
H120.46930.74480.91430.070*
H130.51100.59920.87260.081*
H140.60430.54830.74460.085*
H150.62470.66010.71130.074*
H160.37600.76420.65950.075*
H170.31700.70970.75110.086*
H180.36960.56680.69720.091*
H190.45710.52720.56710.073*
H220.72610.81710.66890.070*
H230.77900.88320.58840.087*
H240.68371.01060.59680.082*
H250.57331.02620.68990.068*
H260.49390.81790.51910.086*
H270.62300.72870.46810.076*
H290.59330.91820.38930.073*
H300.47410.93520.47150.080*
H320.18651.00790.56450.072*
H330.12190.97380.40920.078*
H340.17480.86430.28550.073*
H350.29320.78330.31890.069*
H360.35720.81480.47460.064*
H380.33000.63270.43760.084*
H390.25420.60880.28630.101*
H400.31080.59250.15280.123*
H410.43690.60640.16910.125*
H420.51540.62700.31790.112*
H440.60200.76540.22480.121*
H450.58860.69610.05630.152*
H460.69370.60580.01440.173*
H470.81060.57950.07690.174*
H480.82810.65220.24260.127*
Fe1a0.21424 (7)0.89679 (7)0.07239 (8)0.0534 (4)
Fe2a0.06336 (7)0.79691 (7)0.44042 (9)0.0537 (4)
Fe3a0.08267 (8)0.64032 (8)0.15273 (9)0.0637 (4)
S1a0.19960 (15)0.72321 (14)0.10513 (18)0.0751 (8)
S2a0.07081 (15)0.61748 (15)0.4399 (2)0.0797 (8)
S3a0.12791 (17)0.48871 (17)0.1357 (2)0.1007 (10)
O1a0.0028 (3)0.8410 (3)0.0604 (4)0.0597 (16)
O2a0.0468 (3)0.8913 (3)0.1604 (4)0.0583 (16)
O3a0.0458 (3)0.8063 (3)0.2291 (4)0.0612 (16)
B1a0.0488 (6)0.8856 (6)0.0709 (8)0.056 (3)
B2a0.0015 (7)0.8533 (6)0.2389 (8)0.058 (3)
B3a0.0469 (6)0.8024 (6)0.1388 (9)0.059 (3)
C1a0.0971 (5)0.9348 (5)0.0193 (6)0.054 (2)
C2a0.1016 (5)0.9393 (5)0.1176 (6)0.056 (2)
C3a0.1536 (6)0.9886 (5)0.1778 (6)0.064 (3)
C4a0.1824 (5)1.0170 (5)0.1196 (7)0.065 (3)
C5a0.1477 (5)0.9838 (5)0.0209 (6)0.061 (3)
C6a0.2568 (5)0.7813 (5)0.0092 (6)0.052 (2)
C7a0.2635 (5)0.7925 (5)0.0925 (6)0.062 (3)
C8a0.3134 (5)0.8465 (5)0.1451 (6)0.061 (2)
C9a0.3370 (5)0.8702 (5)0.0788 (7)0.060 (2)
C10a0.3025 (5)0.8312 (5)0.0161 (7)0.064 (3)
C11a0.0144 (5)0.8648 (5)0.3380 (6)0.050 (2)
C12a0.0232 (5)0.9123 (5)0.3624 (7)0.062 (3)
C13a0.0036 (6)0.8972 (6)0.4631 (8)0.080 (3)
C14a0.0450 (6)0.8426 (7)0.5024 (7)0.076 (3)
C15a0.0551 (5)0.8203 (5)0.4260 (7)0.065 (3)
C16a0.1589 (5)0.7358 (5)0.3798 (7)0.063 (3)
C17a0.1842 (5)0.7786 (5)0.4213 (9)0.072 (3)
C18a0.1570 (7)0.7544 (6)0.5191 (9)0.088 (4)
C19a0.1139 (6)0.6952 (6)0.5416 (7)0.067 (3)
C20a0.1139 (5)0.6840 (5)0.4547 (7)0.051 (2)
C21a0.1035 (5)0.7593 (5)0.1258 (7)0.060 (2)
C22a0.1625 (7)0.7241 (5)0.1984 (8)0.082 (3)
C23a0.2021 (6)0.6890 (7)0.1594 (11)0.099 (4)
C24a0.1686 (7)0.7015 (6)0.0622 (10)0.097 (4)
C25a0.1079 (6)0.7454 (5)0.0420 (7)0.072 (3)
C26a0.0020 (11)0.5721 (9)0.2494 (13)0.133 (6)
C27a0.0621 (8)0.5334 (6)0.2595 (8)0.095 (4)
C28a0.0619 (5)0.5257 (5)0.1695 (7)0.059 (2)
C29a0.0002 (6)0.5593 (6)0.1063 (8)0.083 (3)
C30a0.0358 (7)0.5891 (8)0.1549 (13)0.120 (5)
C31a0.2615 (6)0.6279 (5)0.1316 (7)0.066 (3)
C32a0.3302 (7)0.6100 (6)0.0753 (7)0.082 (3)
C33a0.3732 (7)0.5315 (7)0.1019 (9)0.102 (4)
C34a0.3475 (8)0.4737 (7)0.1823 (10)0.097 (4)
C35a0.2785 (8)0.4929 (6)0.2394 (9)0.093 (4)
C36a0.2362 (6)0.5702 (6)0.2138 (7)0.071 (3)
C37a0.1431 (6)0.5295 (5)0.4759 (6)0.061 (2)
C38a0.2161 (6)0.5239 (5)0.5024 (7)0.073 (3)
C39a0.2694 (7)0.4529 (8)0.5316 (8)0.103 (4)
C40a0.2489 (10)0.3857 (8)0.5382 (10)0.124 (6)
C41a0.1785 (11)0.3897 (9)0.5104 (10)0.121 (5)
C42a0.1252 (8)0.4614 (7)0.4796 (8)0.099 (4)
C43a0.0796 (6)0.3872 (6)0.1592 (7)0.073 (3)
C44a0.0130 (7)0.3513 (7)0.2068 (7)0.091 (3)
C45a0.0185 (8)0.2727 (8)0.2232 (8)0.112 (4)
C46a0.0146 (9)0.2291 (8)0.1954 (11)0.118 (5)
C47a0.0805 (9)0.2673 (9)0.1431 (12)0.126 (5)
C48a0.1146 (6)0.3452 (8)0.1260 (9)0.105 (4)
H2a0.07440.91350.13840.067*
H3a0.16681.00060.24460.076*
H4a0.21751.05110.14140.078*
H5a0.15650.99250.03270.073*
H7a0.23910.76830.11900.074*
H8a0.32810.86350.21210.073*
H9a0.36990.90580.09480.072*
H10a0.30840.83690.07310.077*
H12a0.05480.94690.31950.075*
H13a0.02060.92030.49800.096*
H14a0.06690.82380.56710.091*
H15a0.08350.78310.43250.078*
H16a0.16960.74020.31460.076*
H17a0.21420.81700.38850.086*
H18a0.16570.77390.56340.106*
H19a0.08990.66850.60280.081*
H22a0.17330.72430.26170.098*
H23a0.24300.66230.19210.119*
H24a0.18310.68450.01900.116*
H25a0.07650.76200.01720.087*
H26a0.01080.58460.29790.159*
H27a0.09650.51560.31580.114*
H29a0.01450.56150.04220.100*
H30a0.07760.61550.12860.144*
H32a0.34830.64910.02030.098*
H33a0.42010.51880.06390.123*
H34a0.37610.42190.19850.116*
H35a0.26060.45410.29480.111*
H36a0.19000.58320.25280.086*
H38a0.22950.56900.50040.087*
H39a0.31910.45040.54700.124*
H40a0.28350.33710.56180.149*
H41a0.16600.34430.51200.145*
H42a0.07680.46370.46110.119*
H44a0.01070.37960.22780.109*
H45a0.06440.24880.25480.134*
H46a0.00580.17540.21060.141*
H47a0.10190.23910.11920.152*
H48a0.15980.36950.09310.126*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe10.0559 (8)0.0412 (7)0.0398 (7)0.0057 (6)0.0064 (6)0.0124 (6)
Fe20.0457 (8)0.0422 (7)0.0564 (8)0.0077 (6)0.0063 (6)0.0148 (6)
Fe30.0428 (8)0.0503 (8)0.0567 (8)0.0127 (6)0.0033 (6)0.0192 (7)
S10.0683 (17)0.0643 (16)0.0463 (15)0.0032 (13)0.0060 (13)0.0060 (12)
S20.0603 (16)0.0706 (17)0.0690 (17)0.0254 (13)0.0076 (13)0.0262 (14)
S30.0779 (19)0.0713 (17)0.0688 (18)0.0087 (14)0.0163 (15)0.0226 (14)
O10.052 (4)0.044 (3)0.055 (4)0.006 (3)0.002 (3)0.021 (3)
O20.059 (4)0.041 (3)0.045 (3)0.004 (3)0.009 (3)0.016 (3)
O30.068 (4)0.040 (4)0.048 (4)0.013 (3)0.012 (3)0.013 (3)
B10.042 (6)0.044 (6)0.044 (6)0.012 (5)0.011 (5)0.020 (5)
B20.063 (7)0.039 (6)0.030 (6)0.016 (6)0.010 (5)0.011 (5)
B30.050 (7)0.046 (7)0.039 (6)0.006 (5)0.017 (5)0.020 (5)
C10.054 (6)0.051 (6)0.036 (5)0.010 (5)0.010 (4)0.017 (4)
C20.056 (6)0.045 (6)0.062 (6)0.009 (5)0.007 (5)0.021 (5)
C30.067 (7)0.046 (6)0.056 (6)0.011 (5)0.001 (5)0.007 (5)
C40.068 (7)0.069 (7)0.040 (6)0.012 (6)0.007 (5)0.010 (5)
C50.083 (7)0.039 (5)0.035 (5)0.018 (5)0.007 (5)0.018 (4)
C60.058 (6)0.051 (6)0.036 (5)0.012 (5)0.003 (4)0.016 (4)
C70.078 (7)0.062 (7)0.041 (6)0.003 (5)0.001 (5)0.026 (5)
C80.066 (7)0.047 (6)0.058 (7)0.011 (5)0.003 (5)0.015 (5)
C90.054 (6)0.076 (7)0.054 (6)0.006 (6)0.009 (5)0.013 (6)
C100.072 (7)0.063 (7)0.043 (6)0.031 (6)0.012 (5)0.024 (5)
C110.048 (6)0.049 (6)0.046 (5)0.015 (5)0.006 (4)0.014 (5)
C120.072 (7)0.042 (6)0.055 (6)0.006 (5)0.001 (5)0.020 (5)
C130.059 (7)0.076 (8)0.073 (7)0.014 (6)0.005 (6)0.034 (6)
C140.075 (7)0.023 (5)0.103 (8)0.000 (5)0.013 (6)0.027 (5)
C150.041 (6)0.055 (6)0.074 (7)0.001 (5)0.002 (5)0.017 (5)
C160.045 (6)0.060 (6)0.059 (6)0.001 (5)0.007 (5)0.010 (5)
C170.034 (6)0.118 (10)0.056 (7)0.006 (6)0.007 (5)0.030 (7)
C180.082 (8)0.080 (8)0.072 (8)0.036 (7)0.008 (6)0.022 (7)
C190.071 (7)0.052 (6)0.054 (6)0.020 (5)0.015 (5)0.004 (5)
C200.053 (6)0.053 (6)0.044 (5)0.020 (5)0.002 (4)0.014 (5)
C210.055 (6)0.038 (5)0.043 (5)0.011 (5)0.002 (4)0.009 (4)
C220.043 (6)0.046 (6)0.066 (6)0.005 (5)0.006 (5)0.010 (5)
C230.042 (6)0.088 (8)0.072 (7)0.030 (6)0.004 (5)0.002 (6)
C240.060 (7)0.062 (7)0.086 (8)0.029 (6)0.014 (6)0.016 (6)
C250.052 (6)0.053 (6)0.062 (6)0.012 (5)0.003 (5)0.018 (5)
C260.057 (7)0.072 (7)0.097 (8)0.034 (6)0.014 (6)0.041 (6)
C270.066 (7)0.061 (6)0.070 (7)0.022 (6)0.013 (5)0.035 (5)
C280.071 (7)0.058 (6)0.056 (6)0.021 (6)0.007 (5)0.028 (5)
C290.068 (7)0.058 (6)0.063 (6)0.020 (5)0.004 (5)0.029 (5)
C300.049 (6)0.063 (7)0.076 (7)0.005 (5)0.010 (5)0.027 (6)
C310.051 (6)0.041 (5)0.040 (5)0.004 (4)0.014 (4)0.014 (4)
C320.064 (7)0.051 (6)0.048 (6)0.004 (5)0.009 (5)0.010 (5)
C330.053 (6)0.074 (7)0.055 (6)0.009 (5)0.002 (5)0.026 (6)
C340.073 (7)0.066 (7)0.045 (6)0.017 (6)0.002 (5)0.024 (5)
C350.084 (8)0.049 (6)0.043 (6)0.021 (6)0.017 (5)0.010 (5)
C360.050 (6)0.044 (6)0.065 (7)0.006 (5)0.007 (5)0.020 (5)
C370.062 (7)0.038 (5)0.074 (7)0.012 (5)0.005 (6)0.016 (5)
C380.075 (8)0.058 (6)0.069 (8)0.005 (6)0.005 (6)0.021 (6)
C390.074 (8)0.065 (7)0.109 (10)0.003 (6)0.002 (8)0.038 (7)
C400.123 (12)0.090 (9)0.069 (9)0.010 (9)0.002 (9)0.017 (7)
C410.090 (10)0.142 (12)0.082 (10)0.014 (9)0.020 (8)0.044 (8)
C420.075 (8)0.144 (11)0.076 (8)0.036 (7)0.018 (7)0.040 (8)
C430.122 (10)0.053 (7)0.058 (7)0.031 (7)0.011 (7)0.024 (6)
C440.178 (14)0.062 (7)0.057 (8)0.020 (8)0.001 (8)0.024 (7)
C450.213 (18)0.093 (11)0.071 (11)0.049 (11)0.002 (10)0.021 (8)
C460.28 (3)0.099 (13)0.066 (12)0.078 (17)0.033 (13)0.012 (10)
C470.22 (2)0.120 (13)0.113 (15)0.046 (14)0.113 (14)0.010 (12)
C480.132 (11)0.077 (9)0.118 (12)0.026 (8)0.074 (9)0.011 (8)
Fe1a0.0607 (9)0.0521 (8)0.0439 (8)0.0121 (7)0.0069 (7)0.0128 (6)
Fe2a0.0447 (8)0.0607 (8)0.0546 (8)0.0019 (6)0.0104 (6)0.0257 (7)
Fe3a0.0587 (9)0.0677 (9)0.0637 (9)0.0080 (7)0.0161 (7)0.0216 (7)
S1a0.0721 (18)0.0639 (17)0.0622 (17)0.0081 (14)0.0031 (14)0.0005 (13)
S2a0.0637 (17)0.0685 (18)0.117 (2)0.0134 (14)0.0320 (16)0.0330 (17)
S3a0.082 (2)0.084 (2)0.142 (3)0.0203 (17)0.035 (2)0.034 (2)
O1a0.059 (4)0.074 (4)0.051 (4)0.022 (3)0.002 (3)0.025 (3)
O2a0.061 (4)0.068 (4)0.044 (4)0.015 (3)0.002 (3)0.022 (3)
O3a0.067 (4)0.071 (4)0.044 (4)0.013 (3)0.005 (3)0.019 (3)
B1a0.046 (7)0.052 (7)0.060 (8)0.004 (6)0.007 (6)0.018 (6)
B2a0.052 (7)0.057 (7)0.058 (8)0.005 (6)0.011 (6)0.022 (6)
B3a0.046 (7)0.048 (7)0.070 (9)0.007 (6)0.012 (6)0.016 (6)
C1a0.066 (6)0.052 (6)0.041 (6)0.015 (5)0.001 (5)0.014 (5)
C2a0.048 (6)0.052 (6)0.059 (6)0.005 (5)0.011 (5)0.012 (5)
C3a0.082 (7)0.061 (6)0.042 (6)0.018 (6)0.006 (5)0.010 (5)
C4a0.059 (6)0.056 (6)0.068 (7)0.012 (5)0.000 (5)0.012 (6)
C5a0.081 (7)0.056 (6)0.051 (6)0.011 (5)0.007 (5)0.027 (5)
C6a0.060 (6)0.056 (6)0.041 (6)0.015 (5)0.005 (4)0.016 (5)
C7a0.071 (7)0.065 (6)0.053 (6)0.015 (5)0.017 (5)0.019 (5)
C8a0.058 (6)0.065 (7)0.053 (6)0.011 (5)0.001 (5)0.019 (5)
C9a0.052 (6)0.067 (6)0.066 (7)0.025 (5)0.007 (5)0.021 (6)
C10a0.063 (7)0.072 (7)0.054 (7)0.015 (5)0.015 (5)0.014 (5)
C11a0.034 (5)0.057 (6)0.059 (6)0.002 (4)0.013 (5)0.023 (5)
C12a0.056 (6)0.047 (6)0.071 (7)0.005 (5)0.005 (5)0.018 (5)
C13a0.074 (8)0.080 (8)0.083 (9)0.023 (6)0.026 (7)0.042 (7)
C14a0.057 (7)0.108 (9)0.056 (7)0.010 (6)0.003 (6)0.042 (7)
C15a0.044 (6)0.078 (7)0.066 (7)0.008 (5)0.009 (5)0.023 (6)
C16a0.049 (6)0.061 (6)0.075 (7)0.007 (5)0.005 (6)0.034 (6)
C17a0.061 (7)0.055 (7)0.103 (9)0.015 (5)0.015 (7)0.030 (7)
C18a0.088 (9)0.081 (8)0.113 (10)0.026 (7)0.063 (8)0.057 (8)
C19a0.076 (7)0.068 (7)0.046 (6)0.001 (6)0.018 (5)0.013 (5)
C20a0.033 (5)0.060 (6)0.057 (6)0.001 (4)0.013 (5)0.021 (5)
C21a0.056 (6)0.073 (7)0.046 (6)0.024 (5)0.004 (5)0.012 (5)
C22a0.099 (9)0.057 (7)0.078 (8)0.017 (6)0.018 (7)0.026 (6)
C23a0.056 (8)0.084 (9)0.151 (13)0.006 (6)0.006 (8)0.044 (9)
C24a0.068 (9)0.087 (9)0.136 (12)0.013 (7)0.058 (8)0.037 (8)
C25a0.065 (7)0.074 (7)0.076 (8)0.009 (6)0.020 (6)0.024 (6)
C26a0.162 (17)0.100 (12)0.160 (16)0.018 (11)0.105 (14)0.058 (12)
C27a0.143 (12)0.071 (8)0.055 (8)0.002 (8)0.016 (8)0.019 (6)
C28a0.050 (6)0.062 (6)0.059 (6)0.012 (5)0.006 (5)0.022 (5)
C29a0.055 (7)0.099 (9)0.099 (9)0.013 (6)0.003 (7)0.047 (7)
C30a0.061 (9)0.093 (10)0.213 (17)0.005 (7)0.064 (11)0.052 (12)
C31a0.075 (8)0.065 (7)0.054 (7)0.024 (6)0.019 (6)0.007 (6)
C32a0.087 (8)0.074 (8)0.071 (8)0.002 (7)0.022 (7)0.015 (6)
C33a0.108 (10)0.078 (9)0.113 (11)0.003 (8)0.016 (8)0.035 (8)
C34a0.107 (11)0.061 (8)0.130 (12)0.007 (8)0.051 (9)0.030 (9)
C35a0.134 (12)0.055 (8)0.093 (9)0.029 (8)0.045 (9)0.008 (7)
C36a0.079 (7)0.067 (7)0.068 (7)0.023 (6)0.025 (6)0.011 (6)
C37a0.072 (7)0.061 (7)0.055 (6)0.025 (6)0.006 (5)0.026 (5)
C38a0.069 (7)0.052 (7)0.085 (8)0.001 (6)0.008 (6)0.020 (6)
C39a0.079 (9)0.096 (10)0.094 (9)0.007 (8)0.004 (7)0.010 (8)
C40a0.152 (15)0.065 (10)0.100 (11)0.002 (11)0.035 (11)0.012 (8)
C41a0.180 (17)0.069 (10)0.114 (12)0.051 (12)0.030 (12)0.039 (9)
C42a0.122 (11)0.079 (9)0.100 (9)0.045 (9)0.014 (8)0.033 (8)
C43a0.060 (7)0.062 (7)0.070 (7)0.015 (6)0.015 (6)0.007 (6)
C44a0.102 (10)0.093 (10)0.067 (8)0.006 (8)0.005 (7)0.037 (7)
C45a0.139 (13)0.084 (10)0.088 (9)0.002 (10)0.012 (8)0.032 (8)
C46a0.097 (12)0.080 (10)0.147 (13)0.020 (9)0.033 (10)0.032 (10)
C47a0.096 (11)0.092 (11)0.214 (17)0.042 (9)0.044 (11)0.095 (11)
C48a0.061 (8)0.123 (12)0.145 (11)0.047 (8)0.026 (7)0.063 (10)
Geometric parameters (Å, º) top
O1—B11.378 (10)C23—C241.409 (11)
O1a—B1a1.380 (11)C24—C251.413 (11)
B1—O21.372 (10)C21—C251.420 (10)
B1a—O2a1.381 (11)C26—C271.398 (11)
O2—B21.387 (10)C27—C281.401 (11)
O2a—B2a1.368 (11)C28—C291.432 (11)
B2—O31.377 (10)C29—C301.420 (11)
B2a—O3a1.390 (12)C26—C301.411 (11)
O3—B31.369 (10)C21a—C22a1.427 (11)
O3a—B3a1.390 (12)C22a—C23a1.406 (13)
B3—O11.378 (10)C23a—C24a1.406 (14)
B3a—O1a1.385 (11)C24a—C25a1.432 (13)
B1—C11.537 (12)C21a—C25a1.401 (11)
B1a—C1a1.542 (12)C26a—C27a1.388 (16)
B2—C111.521 (12)C27a—C28a1.413 (12)
B2a—C11a1.548 (13)C28a—C29a1.393 (11)
B3—C211.529 (12)C29a—C30a1.395 (15)
B3a—C21a1.523 (13)C26a—C30a1.386 (17)
S1—C61.752 (8)C31—C321.389 (10)
S1a—C6a1.742 (8)C32—C331.368 (10)
S1—C311.768 (8)C33—C341.365 (10)
S1a—C31a1.768 (10)C34—C351.371 (11)
S2—C201.765 (8)C35—C361.371 (10)
S2a—C20a1.731 (9)C31—C361.372 (10)
S2—C371.773 (9)C31a—C32a1.364 (12)
S2a—C37a1.758 (10)C32a—C33a1.406 (13)
S3—C281.758 (9)C33a—C34a1.361 (14)
S3a—C28a1.743 (9)C34a—C35a1.379 (14)
S3—C431.782 (10)C35a—C36a1.385 (12)
S3a—C43a1.796 (10)C31a—C36a1.372 (11)
Fe1—C12.055 (8)C37—C381.368 (11)
Fe1—C22.042 (8)C38—C391.391 (12)
Fe1—C32.041 (8)C39—C401.363 (13)
Fe1—C42.039 (8)C40—C411.324 (14)
Fe1—C52.016 (7)C41—C421.391 (13)
Fe1—C62.031 (8)C37—C421.370 (12)
Fe1—C72.032 (8)C37a—C38a1.380 (11)
Fe1—C82.036 (8)C38a—C39a1.374 (12)
Fe1—C92.025 (9)C39a—C40a1.372 (16)
Fe1—C102.033 (8)C40a—C41a1.354 (17)
Fe1a—C1a2.081 (8)C41a—C42a1.385 (16)
Fe1a—C2a2.064 (8)C37a—C42a1.382 (12)
Fe1a—C3a2.043 (8)C43—C441.361 (13)
Fe1a—C4a2.044 (8)C44—C451.407 (14)
Fe1a—C5a2.059 (8)C45—C461.329 (19)
Fe1a—C6a2.051 (8)C46—C471.347 (19)
Fe1a—C7a2.038 (9)C47—C481.392 (17)
Fe1a—C8a2.060 (8)C43—C481.359 (13)
Fe1a—C9a2.060 (8)C43a—C44a1.364 (12)
Fe1a—C10a2.049 (8)C44a—C45a1.375 (13)
Fe2—C112.046 (8)C45a—C46a1.347 (15)
Fe2—C122.021 (8)C46a—C47a1.395 (16)
Fe2—C132.052 (9)C47a—C48a1.370 (14)
Fe2—C142.024 (8)C43a—C48a1.397 (13)
Fe2—C152.047 (8)C2—H20.9300
Fe2—C162.007 (8)C2a—H2a0.9300
Fe2—C172.041 (8)C3—H30.9300
Fe2—C182.027 (9)C3a—H3a0.9300
Fe2—C192.029 (8)C4—H40.9300
Fe2—C202.007 (8)C4a—H4a0.9300
Fe2a—C11a2.055 (8)C5—H50.9300
Fe2a—C12a2.029 (8)C5a—H5a0.9300
Fe2a—C13a2.020 (9)C7—H70.9300
Fe2a—C14a2.054 (9)C7a—H7a0.9300
Fe2a—C15a2.038 (8)C8—H80.9300
Fe2a—C16a2.028 (8)C8a—H8a0.9300
Fe2a—C17a2.026 (9)C9—H90.9300
Fe2a—C18a2.016 (9)C9a—H9a0.9300
Fe2a—C19a2.029 (8)C10—H100.9300
Fe2a—C20a2.018 (8)C10a—H10a0.9300
Fe3—C212.068 (8)C12—H120.9300
Fe3—C222.024 (8)C12a—H12a0.9300
Fe3—C232.034 (9)C13—H130.9300
Fe3—C242.040 (8)C13a—H13a0.9300
Fe3—C252.051 (8)C14—H140.9300
Fe3—C262.047 (8)C14a—H14a0.9300
Fe3—C272.028 (9)C15—H150.9300
Fe3—C282.006 (9)C15a—H15a0.9300
Fe3—C292.035 (8)C16—H160.9300
Fe3—C302.054 (8)C16a—H16a0.9300
Fe3a—C21a2.060 (9)C17—H170.9300
Fe3a—C22a2.046 (9)C17a—H17a0.9300
Fe3a—C23a2.042 (10)C18—H180.9300
Fe3a—C24a2.027 (10)C18a—H18a0.9300
Fe3a—C25a2.031 (9)C19—H190.9300
Fe3a—C26a2.036 (13)C19a—H19a0.9300
Fe3a—C27a2.018 (10)C22—H220.9300
Fe3a—C28a2.015 (8)C22a—H22a0.9300
Fe3a—C29a2.033 (9)C23—H230.9300
Fe3a—C30a2.038 (12)C23a—H23a0.9300
C1—C21.414 (10)C24—H240.9300
C2—C31.394 (10)C24a—H24a0.9300
C3—C41.400 (11)C25—H250.9300
C4—C51.415 (10)C25a—H25a0.9300
C1—C51.413 (10)C26—H260.9300
C6—C71.419 (10)C26a—H26a0.9300
C7—C81.406 (11)C27—H270.9300
C8—C91.388 (11)C27a—H27a0.9300
C9—C101.409 (11)C29—H290.9300
C6—C101.417 (10)C29a—H29a0.9300
C1a—C2a1.431 (10)C30—H300.9300
C2a—C3a1.403 (10)C30a—H30a0.9300
C3a—C4a1.413 (11)C32—H320.9300
C4a—C5a1.435 (11)C32a—H32a0.9300
C1a—C5a1.433 (11)C33—H330.9300
C6a—C7a1.439 (10)C33a—H33a0.9300
C7a—C8a1.410 (11)C34—H340.9300
C8a—C9a1.408 (10)C34a—H34a0.9300
C9a—C10a1.412 (11)C35—H350.9300
C6a—C10a1.435 (10)C35a—H35a0.9300
C11—C121.434 (10)C36—H360.9300
C12—C131.404 (11)C36a—H36a0.9300
C13—C141.413 (11)C38—H380.9300
C14—C151.398 (11)C38a—H38a0.9300
C11—C151.425 (10)C39—H390.9300
C16—C171.411 (11)C39a—H39a0.9300
C17—C181.373 (12)C40—H400.9300
C18—C191.398 (11)C40a—H40a0.9300
C19—C201.417 (10)C41—H410.9300
C16—C201.409 (10)C41a—H41a0.9300
C11a—C12a1.431 (11)C42—H420.9300
C12a—C13a1.408 (11)C42a—H42a0.9300
C13a—C14a1.386 (12)C44—H440.9300
C14a—C15a1.422 (11)C44a—H44a0.9300
C11a—C15a1.421 (11)C45—H450.9300
C16a—C17a1.393 (11)C45a—H45a0.9300
C17a—C18a1.376 (12)C46—H460.9300
C18a—C19a1.409 (12)C46a—H46a0.9300
C19a—C20a1.399 (11)C47—H470.9300
C16a—C20a1.424 (11)C47a—H47a0.9300
C21—C221.451 (10)C48—H480.9300
C22—C231.396 (11)C48a—H48a0.9300
O1—B1—O2120.0 (8)C29a—C28a—S3a124.2 (8)
O1a—B1a—O2a120.3 (9)C48a—C43a—S3a115.9 (10)
B1—O2—B2120.0 (7)C44a—C43a—S3a123.6 (10)
B1a—O2a—B2a120.0 (8)C3—C2—H2125.2
O2—B2—O3119.2 (7)C1—C2—H2125.2
O2a—B2a—O3a119.6 (9)C3a—C2a—H2a125.4
B2—O3—B3121.0 (7)C1a—C2a—H2a125.4
B2a—O3a—B3a121.0 (8)C2—C3—H3125.8
O3—B3—O1119.4 (8)C4—C3—H3125.8
O3a—B3a—O1a118.2 (9)C2a—C3a—H3a125.7
B3—O1—B1120.3 (7)C4a—C3a—H3a125.7
B3a—O1a—B1a120.7 (8)C3—C4—H4126.5
O2—B1—C1121.4 (8)C5—C4—H4126.5
O2a—B1a—C1a119.6 (9)C3a—C4a—H4a126.1
O1—B1—C1118.6 (8)C5a—C4a—H4a126.1
O1a—B1a—C1a119.9 (9)C1—C5—H5125.2
O2—B2—C11121.9 (9)C4—C5—H5125.2
O2a—B2a—C11a122.8 (10)C8—C7—H7125.8
O3—B2—C11119.0 (8)C6—C7—H7125.8
O3a—B2a—C11a117.4 (9)C1a—C5a—H5a126.0
O1—B3—C21119.2 (8)C4a—C5a—H5a126.0
O1a—B3a—C21a121.0 (10)C8a—C7a—H7a125.9
O3—B3—C21121.3 (8)C6a—C7a—H7a125.9
O3a—B3a—C21a120.8 (9)C9—C8—H8126.2
C2—C1—B1126.3 (8)C7—C8—H8126.2
C2a—C1a—B1a126.6 (9)C9a—C8a—H8a125.8
C5—C1—B1128.1 (8)C7a—C8a—H8a125.8
C5a—C1a—B1a126.8 (9)C8—C9—H9125.3
C12—C11—B2127.6 (8)C10—C9—H9125.3
C12a—C11a—B2a126.4 (9)C8a—C9a—H9a125.6
C15—C11—B2126.3 (9)C10a—C9a—H9a125.6
C15a—C11a—B2a126.0 (9)C9—C10—H10126.3
C22—C21—B3129.2 (8)C6—C10—H10126.3
C22a—C21a—B3a126.1 (10)C9a—C10a—H10a126.1
C25—C21—B3125.3 (8)C6a—C10a—H10a126.1
C25a—C21a—B3a127.6 (9)C13—C12—H12125.0
C6—S1—C31102.9 (4)C11—C12—H12125.0
C6a—S1a—C31a102.7 (5)C13a—C12a—H12a126.2
C20—S2—C37104.4 (4)C11a—C12a—H12a126.2
C20a—S2a—C37a102.4 (4)C12—C13—H13127.0
C28—S3—C43105.1 (5)C14—C13—H13127.0
C28a—S3a—C43a103.5 (5)C14a—C13a—H13a125.2
C3—C2—C1109.6 (8)C12a—C13a—H13a125.2
C2—C3—C4108.4 (8)C15—C14—H14124.9
C3—C4—C5106.9 (8)C13—C14—H14124.9
C1—C5—C4109.5 (7)C15a—C14a—H14a126.1
C5—C1—C2105.6 (7)C14—C15—H15126.0
C3a—C2a—C1a109.2 (8)C11—C15—H15126.0
C2a—C3a—C4a108.5 (8)C11a—C15a—H15a125.9
C3a—C4a—C5a107.7 (8)C14a—C15a—H15a125.9
C1a—C5a—C4a108.0 (8)C20—C16—H16126.1
C2a—C1a—C5a106.6 (7)C17—C16—H16126.1
C8—C7—C6108.5 (8)C17a—C16a—H16a126.1
C9—C8—C7107.6 (8)C20a—C16a—H16a126.1
C8—C9—C10109.4 (8)C18—C17—H17126.1
C9—C10—C6107.3 (8)C16—C17—H17126.1
C10—C6—C7107.2 (7)C17—C18—H18125.1
C8a—C7a—C6a108.2 (8)C19—C18—H18125.1
C9a—C8a—C7a108.3 (8)C17a—C18a—H18a125.4
C8a—C9a—C10a108.8 (8)C19a—C18a—H18a125.4
C9a—C10a—C6a107.9 (8)C13a—C14a—H14a126.1
C10a—C6a—C7a106.8 (7)C18a—C17a—H17a125.8
C13—C12—C11110.1 (8)C16a—C17a—H17a125.8
C12—C13—C14105.9 (8)C18—C19—H19126.5
C15—C14—C13110.2 (8)C20—C19—H19126.5
C14—C15—C11107.9 (8)C20a—C19a—H19a126.3
C15—C11—C12105.9 (7)C18a—C19a—H19a126.3
C13a—C12a—C11a107.5 (9)C23—C22—H22125.6
C14a—C13a—C12a109.6 (10)C21—C22—H22125.6
C13a—C14a—C15a107.7 (9)C23a—C22a—H22a125.3
C11a—C15a—C14a108.2 (9)C21a—C22a—H22a125.3
C15a—C11a—C12a106.9 (8)C22—C23—H23125.6
C18—C17—C16107.8 (8)C24—C23—H23125.6
C17—C18—C19109.9 (9)C24a—C23a—H23a126.1
C18—C19—C20106.9 (8)C22a—C23a—H23a126.1
C16—C20—C19107.6 (8)C23—C24—H24126.3
C20—C16—C17107.7 (8)C25—C24—H24126.3
C18a—C17a—C16a108.3 (9)C23a—C24a—H24a126.3
C17a—C18a—C19a109.2 (9)C25a—C24a—H24a126.3
C20a—C19a—C18a107.3 (9)C24—C25—H25125.2
C19a—C20a—C16a107.4 (8)C21—C25—H25125.2
C17a—C16a—C20a107.9 (9)C21a—C25a—H25a125.4
C23—C22—C21108.8 (8)C24a—C25a—H25a125.4
C22—C23—C24108.8 (8)C27—C26—H26125.6
C23—C24—C25107.5 (9)C30—C26—H26125.6
C24—C25—C21109.7 (8)C30a—C26a—H26a125.7
C25—C21—C22105.3 (8)C27a—C26a—H26a125.7
C23a—C22a—C21a109.4 (10)C26—C27—H27125.9
C24a—C23a—C22a107.8 (11)C28—C27—H27125.9
C23a—C24a—C25a107.3 (11)C26a—C27a—H27a125.9
C21a—C25a—C24a109.2 (10)C28a—C27a—H27a125.9
C25a—C21a—C22a106.3 (9)C28—C29—H29126.5
C26—C27—C28108.3 (8)C28a—C29a—H29a125.5
C27—C28—C29108.2 (8)C30a—C29a—H29a125.5
C30—C29—C28106.9 (8)C26—C30—H30126.1
C26—C30—C29107.8 (8)C29—C30—H30126.1
C27—C26—C30108.8 (9)C26a—C30a—H30a126.2
C26a—C27a—C28a108.1 (12)C29a—C30a—H30a126.2
C29a—C28a—C27a106.7 (9)C33—C32—H32120.4
C28a—C29a—C30a108.9 (11)C31—C32—H32120.4
C26a—C30a—C29a107.7 (14)C34—C33—H33119.0
C30a—C26a—C27a108.6 (14)C32—C33—H33119.0
C33—C32—C31119.1 (8)C34a—C33a—H33a119.4
C34—C33—C32122.0 (8)C32a—C33a—H33a119.4
C33—C34—C35119.1 (8)C31a—C32a—H32a120.6
C36—C35—C34119.5 (8)C33a—C32a—H32a120.6
C35—C36—C31121.7 (8)C33—C34—H34120.5
C36—C31—C32118.5 (8)C35—C34—H34120.5
C31a—C32a—C33a118.8 (11)C36—C35—H35120.2
C34a—C33a—C32a121.3 (12)C34—C35—H35120.2
C33a—C34a—C35a119.3 (12)C33a—C34a—H34a120.4
C34a—C35a—C36a119.7 (11)C35a—C34a—H34a120.4
C31a—C36a—C35a120.8 (10)C34a—C35a—H35a120.2
C32a—C31a—C36a120.1 (10)C36a—C35a—H35a120.2
C37—C38—C39120.1 (10)C31a—C36a—H36a119.6
C40—C39—C38119.7 (11)C35a—C36a—H36a119.6
C41—C40—C39120.4 (12)C35—C36—H36119.1
C40—C41—C42121.0 (12)C31—C36—H36119.1
C37—C42—C41119.7 (10)C37—C38—H38119.9
C38—C37—C42119.0 (10)C39—C38—H38119.9
C39a—C38a—C37a121.1 (10)C30—C29—H29126.5
C40a—C39a—C38a119.8 (13)C39a—C38a—H38a119.4
C41a—C40a—C39a120.3 (15)C37a—C38a—H38a119.4
C40a—C41a—C42a120.0 (14)C40—C39—H39120.2
C37a—C42a—C41a120.8 (12)C38—C39—H39120.2
C38a—C37a—C42a117.9 (10)C40a—C39a—H39a120.1
C43—C44—C45120.3 (13)C38a—C39a—H39a120.1
C46—C45—C44119.3 (17)C41—C40—H40119.8
C45—C46—C47120.8 (19)C39—C40—H40119.8
C46—C47—C48120.9 (18)C41a—C40a—H40a119.9
C43—C48—C47119.1 (14)C39a—C40a—H40a119.9
C48—C43—C44119.6 (11)C40—C41—H41119.5
C43a—C44a—C45a119.2 (12)C42—C41—H41119.5
C46a—C45a—C44a122.4 (14)C40a—C41a—H41a120.0
C45a—C46a—C47a117.8 (14)C42a—C41a—H41a120.0
C48a—C47a—C46a121.7 (14)C37—C42—H42120.1
C47a—C48a—C43a118.1 (12)C41—C42—H42120.1
C44a—C43a—C48a120.6 (10)C37a—C42a—H42a119.6
C10—C6—S1127.3 (7)C41a—C42a—H42a119.6
C7—C6—S1125.5 (7)C43—C44—H44119.9
C36—C31—S1117.2 (7)C45—C44—H44119.9
C32—C31—S1124.3 (6)C43a—C44a—H44a120.4
C10a—C6a—S1a126.1 (7)C45a—C44a—H44a120.4
C7a—C6a—S1a127.0 (7)C46—C45—H45120.4
C36a—C31a—S1a116.0 (9)C44—C45—H45120.4
C32a—C31a—S1a123.9 (8)C46a—C45a—H45a118.8
C16—C20—S2127.3 (7)C44a—C45a—H45a118.8
C19—C20—S2125.0 (7)C45—C46—H46119.6
C38—C37—S2122.6 (8)C47—C46—H46119.6
C42—C37—S2118.4 (9)C45a—C46a—H46a121.1
C16a—C20a—S2a125.5 (7)C47a—C46a—H46a121.1
C19a—C20a—S2a127.1 (8)C46—C47—H47119.6
C38a—C37a—S2a124.1 (8)C48—C47—H47119.6
C42a—C37a—S2a117.9 (9)C48a—C47a—H47a119.1
C27—C28—S3125.2 (7)C46a—C47a—H47a119.1
C29—C28—S3126.4 (7)C43—C48—H48120.5
C48—C43—S3118.1 (11)C47—C48—H48120.5
C44—C43—S3122.2 (10)C47a—C48a—H48a120.9
C27a—C28a—S3a128.9 (9)C43a—C48a—H48a120.9
C5—C1—C2—C30.4 (9)S1—C31—C32—C33178.7 (7)
C5a—C1a—C2a—C3a0.5 (9)S1a—C31a—C32a—C33a177.9 (8)
B1—C1—C2—C3178.2 (7)C31—C32—C33—C340.9 (14)
B1a—C1a—C2a—C3a178.3 (8)C31a—C32a—C33a—C34a0.1 (16)
C1—C2—C3—C40.1 (10)C32—C33—C34—C351.5 (14)
C1a—C2a—C3a—C4a0.6 (10)C32a—C33a—C34a—C35a1.0 (18)
C2—C3—C4—C50.6 (9)C33—C34—C35—C360.6 (13)
C2a—C3a—C4a—C5a0.4 (10)C33a—C34a—C35a—C36a0.6 (17)
C2—C1—C5—C40.8 (9)C34—C35—C36—C310.8 (12)
C2a—C1a—C5a—C4a0.2 (9)C34a—C35a—C36a—C31a0.8 (15)
B1—C1—C5—C4178.5 (7)C32—C31—C36—C351.3 (12)
B1a—C1a—C5a—C4a178.6 (8)C32a—C31a—C36a—C35a1.8 (14)
C3—C4—C5—C10.9 (9)S1—C31—C36—C35177.9 (6)
C3a—C4a—C5a—C1a0.1 (10)S1a—C31a—C36a—C35a177.6 (7)
C31—S1—C6—C1094.9 (8)C20—S2—C37—C387.6 (8)
C31a—S1a—C6a—C10a101.8 (8)C20a—S2a—C37a—C38a3.4 (9)
C31—S1—C6—C785.4 (7)C20—S2—C37—C42173.7 (8)
C31a—S1a—C6a—C7a82.4 (8)C20a—S2a—C37a—C42a175.5 (8)
C10—C6—C7—C80.5 (9)C42—C37—C38—C390.3 (14)
C10a—C6a—C7a—C8a1.2 (9)C42a—C37a—C38a—C39a0.1 (14)
S1—C6—C7—C8179.3 (6)S2—C37—C38—C39179.0 (7)
S1a—C6a—C7a—C8a177.7 (6)S2a—C37a—C38a—C39a178.8 (7)
C6—C7—C8—C90.4 (10)C37—C38—C39—C400.2 (15)
C6a—C7a—C8a—C9a0.9 (10)C37a—C38a—C39a—C40a2.3 (16)
C7—C8—C9—C100.2 (10)C38—C39—C40—C411.7 (17)
C7a—C8a—C9a—C10a0.3 (10)C38a—C39a—C40a—C41a4 (2)
C8—C9—C10—C60.1 (10)C39—C40—C41—C423 (2)
C8a—C9a—C10a—C6a0.5 (10)C39a—C40a—C41a—C42a3 (2)
C7—C6—C10—C90.4 (9)C38—C37—C42—C410.5 (15)
C7a—C6a—C10a—C9a1.1 (9)C38a—C37a—C42a—C41a1.0 (16)
S1—C6—C10—C9179.4 (6)S2—C37—C42—C41178.2 (9)
S1a—C6a—C10a—C9a177.6 (6)S2a—C37a—C42a—C41a177.9 (9)
C15—C11—C12—C130.1 (9)C40—C41—C42—C372.0 (19)
C15a—C11a—C12a—C13a1.1 (9)C40a—C41a—C42a—C37a1 (2)
B2—C11—C12—C13174.4 (8)C28—S3—C43—C48158.9 (8)
B2a—C11a—C12a—C13a171.7 (8)C28a—S3a—C43a—C48a171.6 (8)
C11—C12—C13—C140.8 (10)C28—S3—C43—C4421.5 (10)
C11a—C12a—C13a—C14a0.3 (10)C28a—S3a—C43a—C44a8.7 (10)
C12—C13—C14—C151.2 (10)C48—C43—C44—C453.4 (16)
C12a—C13a—C14a—C15a1.6 (11)C48a—C43a—C44a—C45a1.2 (15)
C13—C14—C15—C111.2 (10)S3—C43—C44—C45176.2 (8)
C13a—C14a—C15a—C11a2.3 (10)S3a—C43a—C44a—C45a178.5 (8)
C12—C11—C15—C140.6 (9)C43—C44—C45—C462.2 (19)
C12a—C11a—C15a—C14a2.1 (9)C43a—C44a—C45a—C46a1.0 (18)
B2—C11—C15—C14173.8 (8)C44—C45—C46—C471 (3)
B2a—C11a—C15a—C14a172.7 (8)C44a—C45a—C46a—C47a4 (2)
C20—C16—C17—C181.3 (10)C45—C46—C47—C483 (3)
C20a—C16a—C17a—C18a0.6 (10)C45a—C46a—C47a—C48a5 (2)
C16—C17—C18—C191.4 (11)C44—C43—C48—C471.5 (16)
C16a—C17a—C18a—C19a0.1 (11)C44a—C43a—C48a—C47a0.4 (16)
C17—C18—C19—C200.9 (11)S3—C43—C48—C47178.1 (9)
C17a—C18a—C19a—C20a0.9 (11)S3a—C43a—C48a—C47a179.3 (9)
C17—C16—C20—C190.7 (9)C46—C47—C48—C432 (2)
C17a—C16a—C20a—C19a1.1 (9)C46a—C47a—C48a—C43a2.5 (19)
C17—C16—C20—S2177.8 (6)B2—O2—B1—O14.4 (11)
C17a—C16a—C20a—S2a179.1 (6)B2a—O2a—B1a—O1a0.7 (12)
C18—C19—C20—C160.1 (10)B2—O2—B1—C1173.5 (7)
C18a—C19a—C20a—C16a1.2 (9)B2a—O2a—B1a—C1a174.2 (8)
C18—C19—C20—S2177.0 (6)B3—O1—B1—O23.0 (11)
C18a—C19a—C20a—S2a179.1 (6)B3a—O1a—B1a—O2a1.1 (12)
C37—S2—C20—C1696.7 (8)B3—O1—B1—C1174.8 (7)
C37a—S2a—C20a—C16a95.9 (7)B3a—O1a—B1a—C1a173.8 (7)
C37—S2—C20—C1986.6 (8)C5—C1—B1—O24.8 (13)
C37a—S2a—C20a—C19a81.6 (8)C5a—C1a—B1a—O2a5.3 (13)
C25—C21—C22—C231.1 (9)C2—C1—B1—O2177.9 (7)
C25a—C21a—C22a—C23a0.3 (11)C2a—C1a—B1a—O2a176.1 (7)
B3—C21—C22—C23176.8 (8)C5—C1—B1—O1177.3 (7)
B3a—C21a—C22a—C23a179.2 (9)C5a—C1a—B1a—O1a179.8 (8)
C21—C22—C23—C241.5 (10)C2—C1—B1—O10.1 (12)
C21a—C22a—C23a—C24a0.0 (12)C2a—C1a—B1a—O1a1.2 (13)
C22—C23—C24—C251.4 (10)B3—O3—B2—O24.6 (11)
C22a—C23a—C24a—C25a0.3 (12)B3a—O3a—B2a—O2a5.5 (12)
C23—C24—C25—C210.7 (10)B3—O3—B2—C11175.8 (7)
C23a—C24a—C25a—C21a0.5 (11)B3a—O3a—B2a—C11a170.2 (7)
C22—C21—C25—C240.2 (9)B1—O2—B2—O35.1 (11)
C22a—C21a—C25a—C24a0.4 (10)B1a—O2a—B2a—O3a2.9 (12)
B3—C21—C25—C24176.1 (7)B1—O2—B2—C11175.3 (7)
B3a—C21a—C25a—C24a179.0 (8)B1a—O2a—B2a—C11a172.6 (8)
C30—C26—C27—C280.4 (10)C15—C11—B2—O310.0 (12)
C30a—C26a—C27a—C28a0.1 (15)C15a—C11a—B2a—O3a13.0 (12)
C26—C27—C28—C290.6 (10)C12—C11—B2—O3176.8 (7)
C26a—C27a—C28a—C29a0.8 (12)C12a—C11a—B2a—O3a178.1 (7)
C26—C27—C28—S3174.6 (6)C15—C11—B2—O2169.6 (7)
C26a—C27a—C28a—S3a174.9 (8)C15a—C11a—B2a—O2a171.4 (8)
C43—S3—C28—C2796.4 (8)C12—C11—B2—O23.6 (13)
C43a—S3a—C28a—C27a94.7 (9)C12a—C11a—B2a—O2a2.5 (13)
C43—S3—C28—C2989.3 (8)B2—O3—B3—O13.3 (11)
C43a—S3a—C28a—C29a90.2 (8)B2a—O3a—B3a—O1a5.7 (12)
C27—C28—C29—C300.6 (10)B2—O3—B3—C21173.9 (7)
C27a—C28a—C29a—C30a1.5 (11)B2a—O3a—B3a—C21a172.2 (8)
S3—C28—C29—C30174.5 (6)B1—O1—B3—O32.5 (11)
S3a—C28a—C29a—C30a174.5 (7)B1a—O1a—B3a—O3a3.5 (12)
C27—C26—C30—C290.0 (10)B1—O1—B3—C21174.8 (7)
C27a—C26a—C30a—C29a1.1 (16)B1a—O1a—B3a—C21a174.4 (8)
C28—C29—C30—C260.4 (10)C25—C21—B3—O3162.7 (7)
C28a—C29a—C30a—C26a1.6 (14)C25a—C21a—B3a—O3a175.1 (8)
C6—S1—C31—C36167.7 (6)C22—C21—B3—O312.2 (13)
C6a—S1a—C31a—C36a171.8 (7)C22a—C21a—B3a—O3a4.3 (14)
C6—S1—C31—C3213.1 (8)C25—C21—B3—O120.1 (12)
C6a—S1a—C31a—C32a8.8 (9)C25a—C21a—B3a—O1a7.0 (14)
C36—C31—C32—C330.5 (12)C22—C21—B3—O1165.0 (7)
C36a—C31a—C32a—C33a1.4 (15)C22a—C21a—B3a—O1a173.6 (8)

Experimental details

Crystal data
Chemical formula[Fe3(C15H12B3O3)(C11H9S)3]
Mr959.98
Crystal system, space groupTriclinic, P1
Temperature (K)296
a, b, c (Å)17.501 (4), 18.875 (5), 14.999 (4)
α, β, γ (°)113.137 (19), 101.89 (2), 74.30 (2)
V3)4358.4 (19)
Z4
Radiation typeMo Kα
µ (mm1)1.17
Crystal size (mm)0.43 × 0.17 × 0.13
Data collection
DiffractometerRigaku AFC-5S
diffractometer
Absorption correctionψ scan
(North et al., 1968)
Tmin, Tmax0.791, 0.859
No. of measured, independent and
observed [I > 2σ(I)] reflections
16062, 15452, 4619
Rint0.079
(sin θ/λ)max1)0.596
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.047, 0.158, 0.93
No. of reflections15452
No. of parameters1081
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.40, 0.49

Computer programs: MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1996), MSC/AFC Diffractometer Control Software, PROCESS in TEXSAN (Molecular Structure Corporation, 1997), SHELXS97 (Sheldrick, 1990), LS in TEXSAN and SHELXL97 (Sheldrick, 1997), ORTEP (Johnson, 1965) in TEXSAN, TEXSAN, SHELXL97 and PLATON (Spek, 2000).

Selected geometric parameters (Å, º) top
O1—B11.378 (10)B2a—C11a1.548 (13)
O1a—B1a1.380 (11)B3—C211.529 (12)
B1—O21.372 (10)B3a—C21a1.523 (13)
B1a—O2a1.381 (11)S1—C61.752 (8)
O2—B21.387 (10)S1a—C6a1.742 (8)
O2a—B2a1.368 (11)S1—C311.768 (8)
B2—O31.377 (10)S1a—C31a1.768 (10)
B2a—O3a1.390 (12)S2—C201.765 (8)
O3—B31.369 (10)S2a—C20a1.731 (9)
O3a—B3a1.390 (12)S2—C371.773 (9)
B3—O11.378 (10)S2a—C37a1.758 (10)
B3a—O1a1.385 (11)S3—C281.758 (9)
B1—C11.537 (12)S3a—C28a1.743 (9)
B1a—C1a1.542 (12)S3—C431.782 (10)
B2—C111.521 (12)S3a—C43a1.796 (10)
O1—B1—O2120.0 (8)O1a—B3a—C21a121.0 (10)
O1a—B1a—O2a120.3 (9)O3—B3—C21121.3 (8)
B1—O2—B2120.0 (7)O3a—B3a—C21a120.8 (9)
B1a—O2a—B2a120.0 (8)C2—C1—B1126.3 (8)
O2—B2—O3119.2 (7)C2a—C1a—B1a126.6 (9)
O2a—B2a—O3a119.6 (9)C5—C1—B1128.1 (8)
B2—O3—B3121.0 (7)C5a—C1a—B1a126.8 (9)
B2a—O3a—B3a121.0 (8)C12—C11—B2127.6 (8)
O3—B3—O1119.4 (8)C12a—C11a—B2a126.4 (9)
O3a—B3a—O1a118.2 (9)C15—C11—B2126.3 (9)
B3—O1—B1120.3 (7)C15a—C11a—B2a126.0 (9)
B3a—O1a—B1a120.7 (8)C22—C21—B3129.2 (8)
O2—B1—C1121.4 (8)C22a—C21a—B3a126.1 (10)
O2a—B1a—C1a119.6 (9)C25—C21—B3125.3 (8)
O1—B1—C1118.6 (8)C25a—C21a—B3a127.6 (9)
O1a—B1a—C1a119.9 (9)C6—S1—C31102.9 (4)
O2—B2—C11121.9 (9)C6a—S1a—C31a102.7 (5)
O2a—B2a—C11a122.8 (10)C20—S2—C37104.4 (4)
O3—B2—C11119.0 (8)C20a—S2a—C37a102.4 (4)
O3a—B2a—C11a117.4 (9)C28—S3—C43105.1 (5)
O1—B3—C21119.2 (8)C28a—S3a—C43a103.5 (5)
 

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