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Acta Cryst. (2007). E63, m2505    [ doi:10.1107/S1600536807043346 ]

Bis([mu]-{(1,3-phenylene)[tert-butyl(pyrazol-1-yl)borato][tert-butyl(dipyrazol-1-yl)borato]})dihydroxydiiron(II) tetrahydrofuran disolvate

F. Zhang, H.-W. Lerner and M. Bolte

Abstract top

The title compound, [Fe2(C23H32B2N6O)2]·2C4H8O, features a dinuclear complex located on a centre of inversion. It crystallizes with two molecules of tetrahydrofuran in the asymmetric unit. The molecular conformation of a pseudopolymorph of the title complex with two molecules of toluene in the asymmetric unit is almost identical. It is noteworthy that the hydroxyl H atom is shielded from any classical hydrogen-bond acceptor and there is only a short contact to the centre of an aromatic ring (centroid...H = 2.48 Å).

Comment top

Careful hydrolysis of the homoditopic phenylene-bridged Li and K scorpionates [m-(pz2BtBu)2C6H4]2− leads to the corresponding heteroditopic derivative [m-(pz(HO)BtBu)(pz2BtBu)C6H4]2−. We report here the X-ray crystal structure analysis of the macrocyclic complex (I). Very recently we have described the synthesis of the metallomacrocycle (I) (Zhang et al., 2007). X-ray quality crystals of the macrocycle (I) were grown from a tetrahydrofuran solution at ambient temperature.

Now we present a pseudopolymorph of this complex crystallized from tetrahydrofuran (Fig. 1). Both structures feature dinuclear complexes located on a centre of inversion. The title complex crystallizes with two molecules of tetrahydrofuran in the unit cell. It is noteworthy, that the hydroxyl H atom is shielded from any classical hydrogen bond acceptor. There is just a short contact to the centre of an aromatic ring [O1—H1 0.72 (5) Å, H1···cog(C41i—C46i) 2.48 Å, O1—H1···cog 132.4°; symmetry operator (i): 1 − x, 1 − y, 1 − z]. A least-squares of the complexes of the two pseudopolymorphs fitting all non-H atoms (r.m.s. deviation 0.091 Å) (Fig. 2) shows that the molecular conformations are almost identical. Thus, the solvent molecules in both crystal structures have no influence on the conformation of the complex.

Related literature top

For a related compound and synthesis, see: Zhang et al. (2007). Please provide figure 1; current figure 1 is same as figure 2.

Experimental top

The title compound (I) was synthesized according to the method described by Zhang et al. (2007). X-ray quality crystals of (I) (0.2 mmol) were grown from a tetrahydrofuran solution (10 ml) at ambient temperature.

Refinement top

H atoms were geometrically positioned and refined using a riding model with fixed individual displacement parameters [Uiso(H) = 1.2 Ueq(C,O) or Uiso(H) = 1.5 Ueq(Cmethyl)] and C—H ranging from 0.95Å to 0.99 Å. The coordinates of the hydroxyl H atom were refined. The C—C distance of the the molecules were refined with a distance restraint of 1.50 (1) Å.

Computing details top

Data collection: X-AREA (Stoe & Cie, 2001); cell refinement: X-AREA (Stoe & Cie, 2001); data reduction: X-AREA (Stoe & Cie, 2001); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP in SHELXTL-Plus (Sheldrick, 1991); software used to prepare material for publication: SHELXL97 (Sheldrick, 1997) and PLATON (Spek, 2003).

Figures top
[Figure 1] Fig. 1. Perspective view of the title compound with the atom numbering; displacement ellipsoids are at the 50% probability level. H atoms bonded to C and the solvent molecules omitted for clarity. Symmetry operator for generating equivalent atoms: −x + 1, −y + 1, −z + 1.
[Figure 2] Fig. 2. Least-squares fit of the title complex (open bonds) with its pseudopolymorph crystallized with toluene (full bonds).
top
Crystal data top
[Fe2(C23H32B2N6O)2]·2C4H8OZ = 1
Mr = 1116.24F000 = 592
Triclinic, P1Dx = 1.273 Mg m−3
Hall symbol: -P 1Mo Kα radiation
λ = 0.71073 Å
a = 11.645 (2) ÅCell parameters from 10281 reflections
b = 12.363 (2) Åθ = 3.4–25.8º
c = 12.507 (2) ŵ = 0.55 mm−1
α = 71.619 (12)ºT = 173 (2) K
β = 63.139 (12)ºBlock, colourless
γ = 66.862 (13)º0.32 × 0.24 × 0.13 mm
V = 1456.1 (5) Å3
Data collection top
STOE IPDS II two-circle
diffractometer		5438 independent reflections
Radiation source: fine-focus sealed tube3411 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.079
T = 173(2) Kθmax = 25.7º
ω scansθmin = 3.5º
Absorption correction: multi-scan
(MULABS; Spek, 2003; Blessing, 1995)		h = −14→14
Tmin = 0.843, Tmax = 0.932k = −14→15
12022 measured reflectionsl = −15→15
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)] = 0.063H atoms treated by a mixture of
independent and constrained refinement
wR(F2) = 0.155  w = 1/[σ2(Fo2) + (0.0841P)2]
where P = (Fo2 + 2Fc2)/3
S = 0.89(Δ/σ)max = 0.006
5438 reflectionsΔρmax = 0.71 e Å−3
346 parametersΔρmin = −0.48 e Å−3
3 restraintsExtinction correction: none
Primary atom site location: structure-invariant direct methods
Crystal data top
[Fe2(C23H32B2N6O)2]·2C4H8Oγ = 66.862 (13)º
Mr = 1116.24V = 1456.1 (5) Å3
Triclinic, P1Z = 1
a = 11.645 (2) ÅMo Kα
b = 12.363 (2) ŵ = 0.55 mm−1
c = 12.507 (2) ÅT = 173 (2) K
α = 71.619 (12)º0.32 × 0.24 × 0.13 mm
β = 63.139 (12)º
Data collection top
STOE IPDS II two-circle
diffractometer		5438 independent reflections
Absorption correction: multi-scan
(MULABS; Spek, 2003; Blessing, 1995)		3411 reflections with I > 2σ(I)
Tmin = 0.843, Tmax = 0.932Rint = 0.079
12022 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0633 restraints
wR(F2) = 0.155H atoms treated by a mixture of
independent and constrained refinement
S = 0.89Δρmax = 0.71 e Å−3
5438 reflectionsΔρmin = −0.48 e Å−3
346 parameters
Special details top

Experimental.

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

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 > σ(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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Fe10.67506 (6)0.23657 (5)0.43545 (5)0.03806 (19)
B10.6272 (4)0.6466 (4)0.4266 (4)0.0347 (9)
C10.7258 (4)0.6458 (4)0.4873 (4)0.0446 (10)
C160.6609 (5)0.7524 (5)0.5551 (5)0.0614 (13)
H16A0.64510.82690.49820.092*
H16B0.72150.75250.58980.092*
H16C0.57500.74580.62060.092*
C170.8641 (5)0.6558 (4)0.3918 (5)0.0584 (12)
H17A0.85170.72780.33110.088*
H17B0.91150.58540.35170.088*
H17C0.91720.66060.43160.088*
C180.7467 (5)0.5330 (4)0.5815 (4)0.0534 (11)
H18A0.78840.46250.54210.080*
H18B0.65940.52890.64610.080*
H18C0.80550.53540.61670.080*
O10.4944 (3)0.6315 (2)0.5255 (3)0.0378 (6)
H10.486 (5)0.577 (4)0.568 (4)0.045*
B20.9482 (4)0.2460 (4)0.2463 (4)0.0372 (10)
C21.0880 (4)0.2689 (4)0.1373 (4)0.0451 (10)
C261.2155 (4)0.1607 (4)0.1204 (5)0.0588 (12)
H26A1.20040.09550.10500.088*
H26B1.23580.13460.19420.088*
H26C1.29160.18330.05120.088*
C271.0681 (5)0.3157 (4)0.0148 (4)0.0559 (12)
H27A1.05000.2550−0.00510.084*
H27B1.14980.3333−0.04950.084*
H27C0.99170.38860.02130.084*
C281.1163 (5)0.3695 (4)0.1599 (5)0.0547 (11)
H28A1.03630.43940.17160.082*
H28B1.19240.39090.08980.082*
H28C1.13820.34230.23290.082*
N110.8418 (3)0.1957 (3)0.4743 (3)0.0384 (7)
N120.9571 (3)0.2016 (3)0.3765 (3)0.0363 (7)
C131.0580 (4)0.1641 (4)0.4176 (4)0.0451 (10)
H131.14920.16070.36760.054*
C141.0105 (5)0.1319 (4)0.5403 (4)0.0510 (11)
H141.05970.10200.59210.061*
C150.8726 (5)0.1526 (4)0.5735 (4)0.0472 (10)
H150.81040.13840.65420.057*
N210.7824 (3)0.1335 (3)0.3015 (3)0.0377 (7)
N220.9084 (3)0.1441 (3)0.2278 (3)0.0374 (7)
C230.9705 (5)0.0626 (4)0.1544 (4)0.0466 (10)
H231.05940.05070.09460.056*
C240.8853 (5)−0.0011 (4)0.1795 (4)0.0496 (11)
H240.9026−0.06420.14130.060*
C250.7695 (5)0.0458 (4)0.2716 (4)0.0456 (10)
H250.69150.01950.30860.055*
N310.5511 (3)0.1507 (3)0.5870 (3)0.0409 (8)
N320.4261 (3)0.2227 (3)0.6412 (3)0.0357 (7)
C330.3659 (5)0.1651 (4)0.7500 (4)0.0456 (10)
H330.27770.19660.80570.055*
C340.4508 (5)0.0533 (4)0.7695 (4)0.0548 (11)
H340.4346−0.00740.83880.066*
C350.5645 (5)0.0494 (4)0.6655 (4)0.0512 (11)
H350.6431−0.01740.65130.061*
C410.8185 (4)0.3640 (3)0.2563 (3)0.0344 (8)
C420.7845 (4)0.4487 (3)0.3267 (3)0.0337 (8)
H420.83670.43230.37350.040*
C430.6796 (3)0.5553 (3)0.3330 (3)0.0328 (8)
C440.6057 (4)0.5772 (3)0.2612 (4)0.0368 (8)
H440.53300.64840.26270.044*
C450.6361 (4)0.4975 (4)0.1885 (4)0.0394 (9)
H450.58510.51510.14030.047*
C460.7406 (4)0.3923 (4)0.1858 (3)0.0382 (9)
H460.76020.33830.13580.046*
O510.2229 (15)0.7421 (11)0.1334 (15)0.305 (8)
C520.2894 (18)0.8316 (14)0.0926 (15)0.203 (7)
H52A0.28830.85530.16170.244*
H52B0.24810.90310.04360.244*
C530.4281 (17)0.7680 (13)0.0174 (15)0.332 (19)
H53A0.48750.73640.06410.399*
H53B0.46650.8225−0.05660.399*
C540.4151 (11)0.6687 (18)−0.0155 (10)0.273 (14)
H54A0.39750.6960−0.09150.327*
H54B0.49910.6011−0.02770.327*
C550.3015 (14)0.6316 (10)0.0861 (10)0.158 (5)
H55A0.33150.56680.14710.189*
H55B0.25110.60590.05760.189*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe10.0325 (3)0.0385 (3)0.0401 (3)−0.0055 (2)−0.0123 (2)−0.0112 (3)
B10.030 (2)0.031 (2)0.036 (2)−0.0068 (17)−0.0083 (17)−0.0065 (18)
C10.043 (2)0.041 (2)0.055 (3)−0.0087 (18)−0.023 (2)−0.012 (2)
C160.065 (3)0.057 (3)0.079 (3)−0.005 (2)−0.041 (3)−0.028 (3)
C170.045 (2)0.054 (3)0.083 (3)−0.015 (2)−0.025 (2)−0.017 (3)
C180.061 (3)0.050 (3)0.056 (3)−0.007 (2)−0.035 (2)−0.009 (2)
O10.0384 (14)0.0317 (15)0.0375 (16)−0.0121 (12)−0.0104 (12)−0.0022 (12)
B20.039 (2)0.033 (2)0.038 (2)−0.0060 (18)−0.0158 (19)−0.0088 (19)
C20.041 (2)0.038 (2)0.046 (2)−0.0076 (17)−0.0095 (18)−0.0093 (19)
C260.039 (2)0.055 (3)0.068 (3)−0.006 (2)−0.008 (2)−0.022 (2)
C270.055 (3)0.055 (3)0.042 (2)−0.016 (2)−0.006 (2)−0.006 (2)
C280.046 (2)0.052 (3)0.062 (3)−0.019 (2)−0.012 (2)−0.010 (2)
N110.0416 (17)0.0377 (18)0.0355 (18)−0.0098 (14)−0.0173 (15)−0.0038 (14)
N120.0354 (16)0.0326 (16)0.0384 (18)−0.0056 (13)−0.0151 (14)−0.0067 (14)
C130.041 (2)0.042 (2)0.058 (3)−0.0080 (18)−0.027 (2)−0.008 (2)
C140.056 (3)0.046 (2)0.061 (3)−0.009 (2)−0.039 (2)−0.004 (2)
C150.058 (3)0.040 (2)0.044 (2)−0.012 (2)−0.024 (2)−0.0037 (19)
N210.0368 (16)0.0390 (18)0.0372 (17)−0.0112 (14)−0.0125 (14)−0.0085 (14)
N220.0375 (17)0.0334 (17)0.0361 (17)−0.0052 (13)−0.0123 (14)−0.0083 (14)
C230.055 (2)0.039 (2)0.042 (2)−0.0086 (19)−0.015 (2)−0.0126 (19)
C240.067 (3)0.039 (2)0.051 (3)−0.015 (2)−0.025 (2)−0.016 (2)
C250.053 (2)0.042 (2)0.049 (2)−0.0166 (19)−0.025 (2)−0.005 (2)
N310.0376 (17)0.0328 (17)0.051 (2)−0.0016 (14)−0.0199 (15)−0.0112 (16)
N320.0355 (16)0.0327 (17)0.0368 (18)−0.0100 (14)−0.0108 (14)−0.0074 (14)
C330.052 (2)0.042 (2)0.042 (2)−0.0207 (19)−0.0134 (19)−0.0037 (19)
C340.070 (3)0.041 (2)0.054 (3)−0.019 (2)−0.031 (2)0.007 (2)
C350.055 (3)0.030 (2)0.063 (3)−0.0039 (19)−0.028 (2)−0.004 (2)
C410.0351 (19)0.034 (2)0.0326 (19)−0.0124 (16)−0.0110 (16)−0.0041 (16)
C420.0333 (18)0.0298 (19)0.038 (2)−0.0080 (15)−0.0138 (16)−0.0072 (16)
C430.0302 (18)0.0296 (18)0.0341 (19)−0.0093 (14)−0.0091 (15)−0.0034 (16)
C440.0361 (19)0.0302 (19)0.041 (2)−0.0052 (15)−0.0169 (17)−0.0036 (17)
C450.043 (2)0.040 (2)0.037 (2)−0.0107 (17)−0.0211 (17)−0.0025 (17)
C460.044 (2)0.039 (2)0.0308 (19)−0.0134 (17)−0.0128 (17)−0.0057 (17)
O510.276 (14)0.186 (10)0.390 (19)−0.067 (10)−0.006 (13)−0.154 (12)
C520.28 (2)0.162 (12)0.262 (18)−0.106 (14)−0.177 (17)0.019 (12)
C530.173 (14)0.34 (3)0.35 (3)−0.134 (17)−0.159 (18)0.27 (2)
C540.086 (7)0.60 (4)0.111 (8)0.005 (13)−0.031 (6)−0.185 (16)
C550.229 (14)0.142 (9)0.146 (9)−0.029 (9)−0.132 (10)−0.020 (7)
Geometric parameters (Å, °) top
Fe1—O1i1.973 (3)C14—C151.399 (6)
Fe1—N112.046 (3)C14—H140.9500
Fe1—N212.048 (3)C15—H150.9500
Fe1—N312.065 (4)N21—C251.331 (5)
B1—O11.520 (5)N21—N221.369 (5)
B1—N32i1.593 (5)N22—C231.339 (5)
B1—C431.632 (5)C23—C241.371 (7)
B1—C11.633 (6)C23—H230.9500
C1—C181.533 (6)C24—C251.372 (6)
C1—C171.536 (7)C24—H240.9500
C1—C161.540 (6)C25—H250.9500
C16—H16A0.9800N31—C351.329 (6)
C16—H16B0.9800N31—N321.357 (4)
C16—H16C0.9800N32—C331.330 (5)
C17—H17A0.9800N32—B1i1.593 (5)
C17—H17B0.9800C33—C341.370 (6)
C17—H17C0.9800C33—H330.9500
C18—H18A0.9800C34—C351.371 (7)
C18—H18B0.9800C34—H340.9500
C18—H18C0.9800C35—H350.9500
O1—Fe1i1.973 (3)C41—C421.404 (5)
O1—H10.72 (5)C41—C461.415 (5)
B2—N121.584 (5)C42—C431.396 (5)
B2—N221.610 (5)C42—H420.9500
B2—C411.625 (5)C43—C441.408 (5)
B2—C21.644 (6)C44—C451.387 (5)
C2—C281.537 (6)C44—H440.9500
C2—C261.540 (6)C45—C461.386 (5)
C2—C271.547 (6)C45—H450.9500
C26—H26A0.9800C46—H460.9500
C26—H26B0.9800O51—C551.447 (13)
C26—H26C0.9800O51—C521.429 (17)
C27—H27A0.9800C52—C531.485 (9)
C27—H27B0.9800C52—H52A0.9900
C27—H27C0.9800C52—H52B0.9900
C28—H28A0.9800C53—C541.491 (10)
C28—H28B0.9800C53—H53A0.9900
C28—H28C0.9800C53—H53B0.9900
N11—C151.337 (5)C54—C551.472 (9)
N11—N121.357 (5)C54—H54A0.9900
N12—C131.351 (5)C54—H54B0.9900
C13—C141.357 (7)C55—H55A0.9900
C13—H130.9500C55—H55B0.9900
O1i—Fe1—N11130.37 (12)C13—C14—H14127.8
O1i—Fe1—N21135.07 (12)C15—C14—H14127.8
N11—Fe1—N2191.19 (13)N11—C15—C14109.6 (4)
O1i—Fe1—N3179.47 (12)N11—C15—H15125.2
N11—Fe1—N31103.53 (13)C14—C15—H15125.2
N21—Fe1—N31110.22 (13)C25—N21—N22107.1 (3)
O1—B1—N32i99.5 (3)C25—N21—Fe1136.8 (3)
O1—B1—C43107.7 (3)N22—N21—Fe1115.6 (2)
N32i—B1—C43106.7 (3)C23—N22—N21108.3 (3)
O1—B1—C1110.0 (3)C23—N22—B2135.1 (4)
N32i—B1—C1110.4 (3)N21—N22—B2116.6 (3)
C43—B1—C1120.5 (3)N22—C23—C24109.1 (4)
C18—C1—C17108.9 (4)N22—C23—H23125.5
C18—C1—C16106.6 (4)C24—C23—H23125.5
C17—C1—C16107.4 (4)C23—C24—C25105.3 (4)
C18—C1—B1111.4 (4)C23—C24—H24127.3
C17—C1—B1112.4 (4)C25—C24—H24127.3
C16—C1—B1109.9 (3)N21—C25—C24110.2 (4)
C1—C16—H16A109.5N21—C25—H25124.9
C1—C16—H16B109.5C24—C25—H25124.9
H16A—C16—H16B109.5C35—N31—N32105.9 (3)
C1—C16—H16C109.5C35—N31—Fe1137.6 (3)
H16A—C16—H16C109.5N32—N31—Fe1114.5 (2)
H16B—C16—H16C109.5C33—N32—N31109.1 (3)
C1—C17—H17A109.5C33—N32—B1i130.3 (3)
C1—C17—H17B109.5N31—N32—B1i120.6 (3)
H17A—C17—H17B109.5N32—C33—C34109.6 (4)
C1—C17—H17C109.5N32—C33—H33125.2
H17A—C17—H17C109.5C34—C33—H33125.2
H17B—C17—H17C109.5C33—C34—C35103.8 (4)
C1—C18—H18A109.5C33—C34—H34128.1
C1—C18—H18B109.5C35—C34—H34128.1
H18A—C18—H18B109.5N31—C35—C34111.6 (4)
C1—C18—H18C109.5N31—C35—H35124.2
H18A—C18—H18C109.5C34—C35—H35124.2
H18B—C18—H18C109.5C42—C41—C46116.2 (3)
B1—O1—Fe1i123.8 (2)C42—C41—B2122.1 (3)
B1—O1—H1125 (4)C46—C41—B2121.5 (3)
Fe1i—O1—H1111 (4)C43—C42—C41124.7 (3)
N12—B2—N22104.7 (3)C43—C42—H42117.6
N12—B2—C41106.8 (3)C41—C42—H42117.6
N22—B2—C41105.7 (3)C42—C43—C44116.0 (3)
N12—B2—C2113.3 (3)C42—C43—B1125.2 (3)
N22—B2—C2112.6 (3)C44—C43—B1118.5 (3)
C41—B2—C2113.0 (3)C45—C44—C43121.8 (3)
C28—C2—C26107.9 (4)C45—C44—H44119.1
C28—C2—C27105.5 (4)C43—C44—H44119.1
C26—C2—C27107.9 (4)C46—C45—C44120.3 (3)
C28—C2—B2109.2 (3)C46—C45—H45119.8
C26—C2—B2116.3 (4)C44—C45—H45119.8
C27—C2—B2109.5 (4)C45—C46—C41121.0 (3)
C2—C26—H26A109.5C45—C46—H46119.5
C2—C26—H26B109.5C41—C46—H46119.5
H26A—C26—H26B109.5C55—O51—C52116.5 (13)
C2—C26—H26C109.5O51—C52—C53101.5 (13)
H26A—C26—H26C109.5O51—C52—H52A111.5
H26B—C26—H26C109.5C53—C52—H52A111.5
C2—C27—H27A109.5O51—C52—H52B111.5
C2—C27—H27B109.5C53—C52—H52B111.5
H27A—C27—H27B109.5H52A—C52—H52B109.3
C2—C27—H27C109.5C52—C53—C54105.8 (13)
H27A—C27—H27C109.5C52—C53—H53A110.6
H27B—C27—H27C109.5C54—C53—H53A110.6
C2—C28—H28A109.5C52—C53—H53B110.6
C2—C28—H28B109.5C54—C53—H53B110.6
H28A—C28—H28B109.5H53A—C53—H53B108.7
C2—C28—H28C109.5C55—C54—C53106.8 (10)
H28A—C28—H28C109.5C55—C54—H54A110.4
H28B—C28—H28C109.5C53—C54—H54A110.4
C15—N11—N12107.8 (3)C55—C54—H54B110.4
C15—N11—Fe1136.3 (3)C53—C54—H54B110.4
N12—N11—Fe1115.5 (2)H54A—C54—H54B108.6
C13—N12—N11107.7 (3)C54—C55—O51100.1 (10)
C13—N12—B2134.6 (3)C54—C55—H55A111.8
N11—N12—B2117.7 (3)O51—C55—H55A111.8
N12—C13—C14110.4 (4)C54—C55—H55B111.8
N12—C13—H13124.8O51—C55—H55B111.8
C14—C13—H13124.8H55A—C55—H55B109.5
C13—C14—C15104.4 (4)
O1—B1—C1—C1855.2 (4)C41—B2—N22—C23134.9 (4)
N32i—B1—C1—C18164.1 (3)C2—B2—N22—C2311.0 (6)
C43—B1—C1—C18−70.9 (5)N12—B2—N22—N2167.6 (4)
O1—B1—C1—C17177.7 (3)C41—B2—N22—N21−45.0 (4)
N32i—B1—C1—C17−73.4 (4)C2—B2—N22—N21−168.9 (3)
C43—B1—C1—C1751.6 (5)N21—N22—C23—C240.3 (5)
O1—B1—C1—C16−62.7 (5)B2—N22—C23—C24−179.6 (4)
N32i—B1—C1—C1646.1 (5)N22—C23—C24—C25−0.3 (5)
C43—B1—C1—C16171.1 (4)N22—N21—C25—C240.0 (5)
N32i—B1—O1—Fe1i−12.4 (4)Fe1—N21—C25—C24−171.5 (3)
C43—B1—O1—Fe1i−123.4 (3)C23—C24—C25—N210.1 (5)
C1—B1—O1—Fe1i103.5 (3)O1i—Fe1—N31—C35−165.3 (4)
N12—B2—C2—C28−63.1 (4)N11—Fe1—N31—C35−36.0 (4)
N22—B2—C2—C28178.4 (3)N21—Fe1—N31—C3560.4 (4)
C41—B2—C2—C2858.6 (4)O1i—Fe1—N31—N32−4.4 (2)
N12—B2—C2—C2659.2 (5)N11—Fe1—N31—N32124.9 (2)
N22—B2—C2—C26−59.3 (5)N21—Fe1—N31—N32−138.7 (2)
C41—B2—C2—C26−179.1 (4)C35—N31—N32—C33−0.2 (4)
N12—B2—C2—C27−178.2 (3)Fe1—N31—N32—C33−166.9 (3)
N22—B2—C2—C2763.3 (4)C35—N31—N32—B1i−179.6 (3)
C41—B2—C2—C27−56.5 (4)Fe1—N31—N32—B1i13.7 (4)
O1i—Fe1—N11—C1571.6 (4)N31—N32—C33—C340.0 (5)
N21—Fe1—N11—C15−127.1 (4)B1i—N32—C33—C34179.3 (4)
N31—Fe1—N11—C15−16.0 (4)N32—C33—C34—C350.3 (5)
O1i—Fe1—N11—N12−116.0 (2)N32—N31—C35—C340.4 (5)
N21—Fe1—N11—N1245.2 (3)Fe1—N31—C35—C34162.3 (3)
N31—Fe1—N11—N12156.4 (2)C33—C34—C35—N31−0.4 (5)
C15—N11—N12—C13−1.2 (4)N12—B2—C41—C4237.8 (5)
Fe1—N11—N12—C13−175.7 (3)N22—B2—C41—C42148.9 (4)
C15—N11—N12—B2177.9 (3)C2—B2—C41—C42−87.5 (4)
Fe1—N11—N12—B23.4 (4)N12—B2—C41—C46−147.9 (4)
N22—B2—N12—C13113.1 (5)N22—B2—C41—C46−36.8 (5)
C41—B2—N12—C13−135.0 (4)C2—B2—C41—C4686.8 (4)
C2—B2—N12—C13−9.9 (6)C46—C41—C42—C431.2 (6)
N22—B2—N12—N11−65.7 (4)B2—C41—C42—C43175.8 (4)
C41—B2—N12—N1146.2 (4)C41—C42—C43—C44−0.7 (6)
C2—B2—N12—N11171.3 (3)C41—C42—C43—B1172.1 (4)
N11—N12—C13—C141.0 (4)O1—B1—C43—C42−105.1 (4)
B2—N12—C13—C14−177.9 (4)N32i—B1—C43—C42148.9 (4)
N12—C13—C14—C15−0.4 (5)C1—B1—C43—C4222.1 (6)
N12—N11—C15—C141.0 (5)O1—B1—C43—C4467.6 (4)
Fe1—N11—C15—C14173.8 (3)N32i—B1—C43—C44−38.5 (4)
C13—C14—C15—N11−0.4 (5)C1—B1—C43—C44−165.2 (4)
O1i—Fe1—N21—C25−72.2 (4)C42—C43—C44—C45−0.3 (6)
N11—Fe1—N21—C25128.0 (4)B1—C43—C44—C45−173.6 (4)
N31—Fe1—N21—C2523.2 (4)C43—C44—C45—C460.8 (6)
O1i—Fe1—N21—N22116.8 (3)C44—C45—C46—C41−0.3 (6)
N11—Fe1—N21—N22−42.9 (3)C42—C41—C46—C45−0.7 (6)
N31—Fe1—N21—N22−147.8 (2)B2—C41—C46—C45−175.3 (4)
C25—N21—N22—C23−0.2 (4)C55—O51—C52—C53−4(2)
Fe1—N21—N22—C23173.4 (3)O51—C52—C53—C5420.9 (17)
C25—N21—N22—B2179.7 (3)C52—C53—C54—C55−31.5 (17)
Fe1—N21—N22—B2−6.7 (4)C53—C54—C55—O5127.2 (15)
N12—B2—N22—C23−112.5 (5)C52—O51—C55—C54−14.7 (17)
Symmetry codes: (i) −x+1, −y+1, −z+1.
references
References top

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Sheldrick, G. M. (1990). Acta Cryst. A46, 467–473.

Sheldrick, G. M. (1991). SHELXTL-Plus. Release 4.1. Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA.

Sheldrick, G. M. (1997). SHELXL97. University of Göttingen, Germany.

Spek, A. L. (2003). J. Appl. Cryst. 36, 7–13.

Stoe & Cie (2001). X-AREA. Stoe & Cie, Darmstadt, Germany.

Zhang, F., Morawitz, T., Bieller, S., Bolte, M., Lerner, H.-W. & Wagner, M. (2007). J. Chem. Soc. Dalton Trans. DOI 10.1039/b707807b.