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Acta Cryst. (2008). E64, m517    [ doi:10.1107/S1600536808005503 ]

The galla[1]ferrocenophane {[dimethyl(2-pyridyl)silyl]bis(trimethylsilyl)methyl-[kappa]2C,N}(ferrocene-1,1'-diyl)gallium(III)

J. A. Schachner, J. W. Quail and J. Müller

Abstract top

The title compound, [GaFe(C5H4)2(C14H28NSi3)] or [{(2-H4C5N)Me2Si}(Me3Si)2C]Ga(C5H4)2Fe, a galla[1]ferrocenophane, crystallizes with two independent molecules in the asymmetric unit. In these strained sandwich compounds, the angles between the planes of the two [pi]-ligands are 15.4 (2) and 16.4 (2)°, with gallium in a distorted tetrahedral coordination environment.

Comment top

After the first report of the synthesis of a [1]ferrocenophane by Osborne and Whiteley in 1975 (Osborne et al., 1975), Manners and coworkers discovered that thermal ring-opening polymerization (ROP) of dimethylsila[1]ferrocenophane yield high-molecular weight polymers (Foucher et al., 1992). This discovery was a breakthrough in the area of organometallic polymers. Recently, the field of strained sandwich compounds was reviewed by Manners (Herbert et al., 2007) and Rehahn (Bellas et al., 2007).

Over the last four years, we characterized aluminium- and gallium-bridged [1]ferrocenophanes (Schachner et al., 2005a, b), (Lund et al., 2006), [1]chromarenophanes (Lund et al., 2006), [1]vanadarenophanes (Lund et al., 2006), [1]ruthenocenophanes (Schachner et al., 2007), and [1]molybdarenophanes (Lund et al., 2007).

We published the synthesis and characterization of the first strained sandwich compound with gallium in the bridging position in 2005 (Schachner et al., 2005b) (Scheme 1). However, details of the molecular structure of the title compound could not be extracted from the single-crystal X-ray analysis; only the molecular framework was revealed with certainty from the analysis (Schachner et al., 2005b). After several attempts, we succeeded in growing single crystals of high quality that allowed a complete structural solution of the compound. The galla[1]ferrocenophane crystallizes in the monoclinic space group P21/c with two independent molecules in the asymmetric unit. Figure 1 depicts the two independent species. In both molecules the bond lengths around the bridging Ga atoms are very similar (Ga1a—C16a = 2.018 (3); Ga1b—C16b = 2.026 (3); Ga1a—C21a = 2.023 (3); Ga1b—C21b = 2.023 (3); Ga1a—N1a = 2.084 (3); Ga1b—N1b = 2.050 (3); Ga1a—C7a = 2.043 (3); Ga1b—C7b = 2.038 (3) Å). [1]Metallacyclophanes can only be ring-open polymerized because they are intrinsically strained. The so-called α angle in strained sandwich compounds is defined as the angle between the two planes of two π-ligands. The angle between the two least squares planes of C16 - C20 and C21 - C25 are 15.4 (2)° for molecule (Ia) and 16.4 (2)° for molecule (Ib). Both values compare well with the value of the 15.83 (19)° found for the only other known galla[1]ferrocenophane (Lund et al., 2006).

Related literature top

The synthesis of the title compound was described by Schachner et al. (2005b). A related galla[1]ferrocenophane was published by Lund et al. (2006). For related literature, see: Bellas & Rehahn (2007); Foucher et al. (1992); Herbert et al. (2007); Lund et al. (2007); Osborne & Whiteley (1975); Schachner et al. (2005a, 2007).

Experimental top

The title compound was synthesized as described in the literature (Schachner et al. 2005b). Single crystals were obtained by crystallization from a hexane solution at ca -25°C.

Refinement top

H atoms were placed in calculated positions with C—H = 0.95Å and Uiso constrained to be 1.2 times Ueq of the carrier atom for aromatic protons and C—H = 0.98Å with Uiso constrained to 1.5 times Ueq of the carrier atom for methyl hydrogen atoms.

Computing details top

Data collection: COLLECT (Nonius, 1998); cell refinement: SCALEPACK (Otwinowski & Minor, 1997); data reduction: SCALEPACK and DENZO (Otwinowski & Minor, 1997); program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008) and PLATON (Spek, 2003).

Figures top
[Figure 1] Fig. 1. Plot of the two independent molecules of with thermal ellipsoids at the 50% probability level. H atoms are omitted for claritity.
[Figure 2] Fig. 2. The formation of the title compound.
{[dimethyl(2-pyridyl)silyl]bis(trimethylsilyl)methyl-κ2C,N}(ferrocene-1,1'- diyl)gallium(III) top
Crystal data top
[GaFe(C5H4)2(C14H28NSi3)]F000 = 2288
Mr = 548.38Dx = 1.386 Mg m−3
Monoclinic, P21/cMo Kα radiation
λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 91449 reflections
a = 9.64630 (10) Åθ = 1.0–26.0º
b = 35.2258 (4) ŵ = 1.73 mm−1
c = 15.4862 (2) ÅT = 173 (2) K
β = 92.5212 (7)ºChip, orange
V = 5257.10 (11) Å30.20 × 0.12 × 0.12 mm
Z = 8
Data collection top
Nonius KappaCCD diffractometer10370 independent reflections
Radiation source: fine-focus sealed tube7767 reflections with I > 2σ(I)
Monochromator: horizonally mounted graphite crystalRint = 0.079
Detector resolution: 9 pixels mm-1θmax = 26.1º
T = 173(2) Kθmin = 1.4º
φ scans, and ω scans with κ offsetsh = −11→11
Absorption correction: ψ scan
(SHELXTL; Sheldrick, 2008)		k = −43→43
Tmin = 0.692, Tmax = 0.811l = −19→19
58270 measured 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)] = 0.043H-atom parameters constrained
wR(F2) = 0.088  w = 1/[σ2(Fo2) + (0.0238P)2 + 7.0617P]
where P = (Fo2 + 2Fc2)/3
S = 1.04(Δ/σ)max = 0.001
10370 reflectionsΔρmax = 0.36 e Å−3
557 parametersΔρmin = −0.45 e Å−3
Primary atom site location: structure-invariant direct methodsExtinction correction: none
Crystal data top
[GaFe(C5H4)2(C14H28NSi3)]V = 5257.10 (11) Å3
Mr = 548.38Z = 8
Monoclinic, P21/cMo Kα
a = 9.64630 (10) ŵ = 1.73 mm−1
b = 35.2258 (4) ÅT = 173 (2) K
c = 15.4862 (2) Å0.20 × 0.12 × 0.12 mm
β = 92.5212 (7)º
Data collection top
Nonius KappaCCD diffractometer10370 independent reflections
Absorption correction: ψ scan
(SHELXTL; Sheldrick, 2008)		7767 reflections with I > 2σ(I)
Tmin = 0.692, Tmax = 0.811Rint = 0.079
58270 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.043557 parameters
wR(F2) = 0.088H-atom parameters constrained
S = 1.04Δρmax = 0.36 e Å−3
10370 reflectionsΔρmin = −0.45 e Å−3
Special details top

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
Fe1A0.30497 (5)0.055334 (13)1.00300 (3)0.02692 (12)
Ga1A0.14191 (4)0.116989 (10)0.94201 (2)0.02454 (10)
N1A0.0812 (3)0.11264 (7)0.81155 (17)0.0257 (6)
Si1A0.05479 (11)0.18896 (3)0.85081 (6)0.0299 (2)
Si2A−0.13709 (10)0.15670 (3)0.98932 (7)0.0317 (2)
Si3A0.14012 (11)0.19919 (3)1.04473 (7)0.0317 (2)
C2A0.0799 (4)0.08122 (10)0.7626 (2)0.0334 (9)
H2A0.10570.05780.78890.040*
C3A0.0429 (4)0.08158 (11)0.6762 (2)0.0379 (9)
H3A0.04200.05870.64370.045*
C4A0.0070 (4)0.11542 (11)0.6368 (2)0.0374 (9)
H4A−0.01840.11640.57690.045*
C5A0.0090 (4)0.14802 (10)0.6872 (2)0.0343 (9)
H5A−0.01480.17170.66130.041*
C6A0.0454 (3)0.14648 (9)0.7748 (2)0.0275 (8)
C7A0.0484 (3)0.16817 (9)0.9611 (2)0.0255 (8)
C8A−0.0866 (5)0.22219 (11)0.8131 (3)0.0520 (12)
H8A−0.17670.20960.81710.078*
H8B−0.07300.22940.75300.078*
H8C−0.08420.24490.84960.078*
C9A0.2214 (5)0.21208 (12)0.8242 (3)0.0541 (12)
H9A0.23130.23610.85580.081*
H9B0.22150.21700.76190.081*
H9C0.29900.19530.84100.081*
C10A−0.2308 (4)0.13154 (13)0.8976 (3)0.0521 (12)
H10A−0.32640.12630.91300.078*
H10B−0.18350.10760.88610.078*
H10C−0.23150.14760.84590.078*
C11A−0.2409 (4)0.19977 (11)1.0156 (3)0.0498 (11)
H11A−0.33870.19271.01910.075*
H11B−0.23140.21890.97030.075*
H11C−0.20670.21021.07120.075*
C12A−0.1518 (4)0.12448 (11)1.0844 (3)0.0467 (11)
H12A−0.10440.13601.13520.070*
H12B−0.10880.10001.07200.070*
H12C−0.24990.12061.09570.070*
C13A0.1152 (5)0.18302 (12)1.1584 (2)0.0528 (12)
H13A0.13770.15601.16340.079*
H13B0.01840.18711.17280.079*
H13C0.17640.19761.19820.079*
C14A0.0752 (4)0.24962 (10)1.0403 (3)0.0466 (11)
H14A0.13080.26521.08120.070*
H14B−0.02220.25031.05560.070*
H14C0.08350.25960.98170.070*
C15A0.3327 (4)0.20227 (11)1.0337 (3)0.0474 (11)
H15A0.37650.21201.08750.071*
H15B0.35280.21940.98600.071*
H15C0.36960.17701.02170.071*
C16A0.0984 (3)0.06751 (9)1.0006 (2)0.0298 (8)
C17A0.1548 (4)0.06341 (11)1.0879 (2)0.0368 (9)
H17A0.15350.08261.13110.044*
C18A0.2125 (4)0.02665 (11)1.1002 (3)0.0431 (10)
H18A0.25730.01731.15180.052*
C19A0.1917 (4)0.00647 (11)1.0221 (3)0.0418 (10)
H19A0.2191−0.01901.01170.050*
C20A0.1222 (4)0.03111 (10)0.9615 (3)0.0344 (9)
H20A0.09530.02450.90370.041*
C21A0.3479 (3)0.10609 (9)0.9457 (2)0.0273 (8)
C22A0.4259 (4)0.10155 (10)1.0276 (2)0.0317 (8)
H22A0.42060.11821.07560.038*
C23A0.5110 (4)0.06870 (10)1.0254 (2)0.0341 (9)
H23A0.57100.05971.07120.041*
C24A0.4909 (4)0.05174 (10)0.9432 (2)0.0323 (8)
H24A0.53450.02930.92370.039*
C25A0.3930 (4)0.07447 (9)0.8946 (2)0.0280 (8)
H25A0.36170.06950.83670.034*
Fe1B0.77578 (5)0.031639 (13)0.33294 (3)0.02690 (12)
Ga1B0.63939 (4)0.087176 (10)0.43069 (2)0.02319 (9)
N1b0.6415 (3)0.07546 (8)0.56039 (18)0.0275 (7)
Si1B0.55460 (11)0.15070 (3)0.55006 (7)0.0372 (3)
Si2B0.59969 (11)0.17257 (3)0.35803 (7)0.0360 (3)
Si3B0.34124 (10)0.12263 (3)0.41012 (7)0.0292 (2)
C2B0.6827 (4)0.04260 (10)0.5972 (2)0.0333 (9)
H2B0.71000.02240.56100.040*
C3B0.6869 (4)0.03707 (11)0.6852 (2)0.0401 (10)
H3B0.71740.01360.70940.048*
C4B0.6463 (4)0.06618 (13)0.7373 (3)0.0443 (10)
H4B0.64870.06310.79830.053*
C5B0.6016 (4)0.10014 (12)0.6998 (2)0.0423 (10)
H5B0.57220.12040.73530.051*
C6B0.5999 (4)0.10457 (10)0.6105 (2)0.0325 (8)
C7B0.5295 (4)0.13650 (9)0.4346 (2)0.0281 (8)
C8B0.7064 (5)0.18256 (12)0.5764 (3)0.0607 (13)
H8D0.78960.17210.55140.091*
H8E0.72110.18440.63930.091*
H8F0.68770.20790.55240.091*
C9B0.4067 (5)0.17341 (14)0.6057 (3)0.0661 (15)
H9D0.38480.19790.57860.099*
H9E0.43300.17730.66690.099*
H9F0.32510.15680.60060.099*
C10B0.7926 (4)0.17796 (11)0.3689 (3)0.0554 (13)
H10D0.81650.19630.41470.083*
H10E0.82750.18710.31410.083*
H10F0.83490.15340.38340.083*
C11B0.5249 (5)0.22135 (10)0.3737 (3)0.0552 (12)
H11D0.53950.22900.43430.083*
H11E0.42530.22100.35840.083*
H11F0.57110.23950.33650.083*
C12B0.5588 (5)0.16013 (12)0.2420 (3)0.0544 (12)
H12D0.60850.17740.20460.082*
H12E0.45870.16250.22950.082*
H12F0.58790.13400.23120.082*
C13B0.3019 (4)0.09920 (11)0.3038 (2)0.0414 (10)
H13D0.34880.07450.30260.062*
H13E0.33480.11530.25730.062*
H13F0.20150.09550.29580.062*
C14B0.2193 (4)0.16437 (12)0.4105 (3)0.0508 (11)
H14D0.12340.15520.41040.076*
H14E0.23190.17990.35880.076*
H14F0.23930.17970.46230.076*
C15B0.2855 (4)0.08709 (12)0.4914 (3)0.0465 (10)
H15D0.18680.08130.48090.070*
H15E0.30050.09750.54970.070*
H15F0.34010.06380.48610.070*
C16B0.8391 (3)0.07929 (9)0.3993 (2)0.0290 (8)
C17B0.8717 (4)0.08150 (10)0.3093 (2)0.0364 (9)
H17B0.83920.10070.27020.044*
C18B0.9598 (4)0.05080 (11)0.2876 (3)0.0432 (10)
H18B0.99460.04590.23230.052*
C19B0.9862 (4)0.02905 (10)0.3628 (3)0.0375 (9)
H19B1.04260.00700.36730.045*
C20B0.9137 (3)0.04586 (10)0.4309 (2)0.0311 (8)
H20B0.91400.03660.48860.037*
C21B0.5751 (3)0.04071 (9)0.3634 (2)0.0278 (8)
C22B0.5895 (4)0.04133 (10)0.2716 (2)0.0325 (8)
H22B0.56750.06240.23530.039*
C23B0.6413 (4)0.00605 (10)0.2423 (2)0.0367 (9)
H23B0.6596−0.00050.18440.044*
C24B0.6603 (4)−0.01748 (10)0.3161 (2)0.0332 (9)
H24B0.6943−0.04280.31650.040*
C25B0.6200 (3)0.00323 (9)0.3893 (2)0.0277 (8)
H25B0.6222−0.00620.44680.033*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe1A0.0237 (3)0.0279 (3)0.0293 (3)0.0008 (2)0.0036 (2)0.0040 (2)
Ga1A0.0245 (2)0.02234 (19)0.0269 (2)0.00140 (16)0.00234 (16)0.00005 (16)
N1A0.0240 (16)0.0248 (15)0.0285 (16)0.0033 (12)0.0020 (13)−0.0026 (12)
Si1A0.0384 (6)0.0232 (5)0.0281 (6)0.0002 (4)0.0015 (5)0.0006 (4)
Si2A0.0253 (6)0.0349 (6)0.0352 (6)0.0012 (4)0.0047 (4)−0.0018 (5)
Si3A0.0360 (6)0.0266 (5)0.0321 (6)0.0001 (4)−0.0032 (5)−0.0039 (4)
C2A0.038 (2)0.0275 (19)0.035 (2)0.0055 (16)−0.0009 (17)−0.0054 (16)
C3A0.040 (2)0.037 (2)0.037 (2)0.0049 (18)−0.0002 (18)−0.0118 (18)
C4A0.035 (2)0.051 (2)0.026 (2)0.0050 (18)−0.0028 (17)−0.0065 (18)
C5A0.034 (2)0.036 (2)0.033 (2)0.0057 (17)0.0007 (17)0.0033 (17)
C6A0.0212 (18)0.0318 (19)0.030 (2)0.0002 (15)0.0021 (15)0.0006 (15)
C7A0.0252 (19)0.0224 (17)0.0289 (19)−0.0001 (14)0.0019 (15)−0.0025 (14)
C8A0.079 (3)0.037 (2)0.040 (3)0.020 (2)−0.005 (2)0.0018 (19)
C9A0.071 (3)0.053 (3)0.039 (3)−0.027 (2)0.012 (2)−0.002 (2)
C10A0.032 (2)0.067 (3)0.058 (3)−0.011 (2)0.003 (2)−0.013 (2)
C11A0.035 (2)0.054 (3)0.061 (3)0.012 (2)0.009 (2)−0.002 (2)
C12A0.040 (2)0.050 (3)0.051 (3)0.000 (2)0.014 (2)0.005 (2)
C13A0.074 (3)0.053 (3)0.031 (2)−0.007 (2)−0.011 (2)−0.004 (2)
C14A0.054 (3)0.028 (2)0.057 (3)−0.0011 (19)0.000 (2)−0.0091 (19)
C15A0.039 (2)0.042 (2)0.060 (3)−0.0063 (19)−0.006 (2)−0.013 (2)
C16A0.0224 (19)0.0279 (19)0.040 (2)0.0024 (15)0.0076 (16)0.0037 (16)
C17A0.037 (2)0.041 (2)0.034 (2)0.0036 (18)0.0145 (18)0.0059 (17)
C18A0.040 (2)0.048 (2)0.043 (3)0.0067 (19)0.0114 (19)0.020 (2)
C19A0.030 (2)0.028 (2)0.068 (3)−0.0009 (16)0.012 (2)0.013 (2)
C20A0.027 (2)0.0286 (19)0.048 (2)−0.0048 (16)0.0033 (17)0.0056 (17)
C21A0.0251 (19)0.0252 (18)0.032 (2)−0.0035 (15)0.0026 (16)0.0008 (15)
C22A0.031 (2)0.033 (2)0.030 (2)−0.0040 (16)−0.0020 (17)−0.0031 (16)
C23A0.024 (2)0.042 (2)0.035 (2)−0.0011 (16)−0.0045 (17)0.0058 (18)
C24A0.0225 (19)0.033 (2)0.042 (2)0.0056 (16)0.0070 (17)0.0025 (17)
C25A0.028 (2)0.0301 (19)0.0258 (19)−0.0025 (15)0.0031 (15)0.0013 (15)
Fe1B0.0265 (3)0.0251 (3)0.0295 (3)−0.0001 (2)0.0060 (2)−0.0015 (2)
Ga1B0.0232 (2)0.02223 (19)0.0241 (2)0.00140 (15)0.00027 (16)−0.00166 (15)
N1b0.0228 (16)0.0332 (16)0.0263 (16)0.0022 (13)0.0009 (13)−0.0032 (13)
Si1B0.0365 (6)0.0375 (6)0.0365 (6)0.0108 (5)−0.0092 (5)−0.0141 (5)
Si2B0.0334 (6)0.0233 (5)0.0514 (7)0.0015 (4)0.0032 (5)0.0030 (5)
Si3B0.0233 (5)0.0331 (5)0.0311 (6)0.0032 (4)−0.0014 (4)−0.0023 (4)
C2B0.032 (2)0.038 (2)0.030 (2)−0.0004 (17)0.0007 (17)0.0031 (17)
C3B0.037 (2)0.048 (2)0.035 (2)−0.0068 (19)−0.0025 (18)0.0110 (19)
C4B0.039 (2)0.068 (3)0.026 (2)−0.008 (2)0.0026 (18)0.002 (2)
C5B0.032 (2)0.064 (3)0.031 (2)−0.001 (2)0.0026 (18)−0.014 (2)
C6B0.026 (2)0.043 (2)0.028 (2)0.0008 (16)0.0014 (16)−0.0089 (17)
C7B0.028 (2)0.0235 (18)0.033 (2)0.0039 (14)−0.0009 (16)−0.0018 (15)
C8B0.069 (3)0.039 (2)0.071 (3)−0.002 (2)−0.032 (3)−0.013 (2)
C9B0.066 (3)0.088 (4)0.043 (3)0.035 (3)−0.007 (2)−0.033 (3)
C10B0.037 (2)0.026 (2)0.104 (4)−0.0068 (18)0.008 (2)0.009 (2)
C11B0.053 (3)0.026 (2)0.086 (4)0.0087 (19)0.002 (3)0.002 (2)
C12B0.064 (3)0.055 (3)0.045 (3)−0.008 (2)0.013 (2)0.015 (2)
C13B0.029 (2)0.051 (2)0.044 (2)−0.0010 (18)−0.0049 (18)−0.0041 (19)
C14B0.039 (3)0.060 (3)0.053 (3)0.016 (2)−0.009 (2)−0.007 (2)
C15B0.031 (2)0.061 (3)0.048 (3)−0.006 (2)0.0045 (19)0.007 (2)
C16B0.0242 (19)0.0241 (18)0.039 (2)−0.0042 (14)0.0029 (16)−0.0010 (15)
C17B0.037 (2)0.031 (2)0.042 (2)−0.0061 (17)0.0096 (18)0.0056 (17)
C18B0.038 (2)0.042 (2)0.051 (3)−0.0070 (18)0.023 (2)−0.004 (2)
C19B0.024 (2)0.033 (2)0.057 (3)0.0022 (16)0.0098 (18)−0.0003 (19)
C20B0.0223 (19)0.034 (2)0.037 (2)−0.0020 (15)−0.0026 (16)0.0001 (16)
C21B0.0238 (19)0.0278 (18)0.032 (2)−0.0029 (14)0.0023 (16)−0.0037 (15)
C22B0.036 (2)0.0289 (19)0.032 (2)0.0010 (16)−0.0068 (17)−0.0033 (16)
C23B0.045 (2)0.036 (2)0.029 (2)0.0000 (18)0.0047 (18)−0.0105 (17)
C24B0.033 (2)0.0245 (18)0.042 (2)−0.0017 (15)0.0032 (18)−0.0077 (16)
C25B0.0266 (19)0.0262 (18)0.030 (2)−0.0051 (15)0.0012 (16)−0.0036 (15)
Geometric parameters (Å, °) top
Fe1A—C17A2.019 (3)Fe1B—C22B2.024 (4)
Fe1A—C22A2.029 (3)Fe1B—C17B2.026 (3)
Fe1A—C25A2.029 (3)Fe1B—C25B2.034 (3)
Fe1A—C16A2.037 (3)Fe1B—C20B2.036 (4)
Fe1A—C20A2.037 (4)Fe1B—C21B2.038 (3)
Fe1A—C21A2.047 (3)Fe1B—C16B2.047 (3)
Fe1A—C18A2.049 (4)Fe1B—C18B2.051 (4)
Fe1A—C23A2.057 (4)Fe1B—C19B2.064 (4)
Fe1A—C24A2.058 (3)Fe1B—C24B2.068 (3)
Fe1A—C19A2.067 (4)Fe1B—C23B2.075 (4)
Fe1A—Ga1A2.8200 (6)Fe1B—Ga1B2.8328 (6)
Ga1A—C16A2.018 (3)Ga1B—C21B2.023 (3)
Ga1A—C21A2.023 (3)Ga1B—C16B2.026 (3)
Ga1A—C7A2.043 (3)Ga1B—C7B2.038 (3)
Ga1A—N1A2.084 (3)Ga1B—N1b2.050 (3)
N1A—C2A1.342 (4)N1b—C2B1.342 (4)
N1A—C6A1.359 (4)N1b—C6B1.358 (4)
Si1A—C7A1.862 (3)Si1B—C7B1.863 (4)
Si1A—C9A1.864 (4)Si1B—C8B1.875 (4)
Si1A—C8A1.871 (4)Si1B—C9B1.877 (4)
Si1A—C6A1.904 (3)Si1B—C6B1.916 (4)
Si2A—C12A1.869 (4)Si2B—C10B1.871 (4)
Si2A—C11A1.872 (4)Si2B—C12B1.875 (4)
Si2A—C10A1.873 (4)Si2B—C11B1.883 (4)
Si2A—C7A1.904 (3)Si2B—C7B1.884 (4)
Si3A—C13A1.875 (4)Si3B—C13B1.865 (4)
Si3A—C15A1.877 (4)Si3B—C15B1.871 (4)
Si3A—C14A1.884 (4)Si3B—C14B1.883 (4)
Si3A—C7A1.885 (3)Si3B—C7B1.903 (4)
C2A—C3A1.369 (5)C2B—C3B1.375 (5)
C2A—H2A0.9500C2B—H2B0.9500
C3A—C4A1.376 (5)C3B—C4B1.373 (5)
C3A—H3A0.9500C3B—H3B0.9500
C4A—C5A1.388 (5)C4B—C5B1.390 (6)
C4A—H4A0.9500C4B—H4B0.9500
C5A—C6A1.387 (5)C5B—C6B1.391 (5)
C5A—H5A0.9500C5B—H5B0.9500
C8A—H8A0.9800C8B—H8D0.9800
C8A—H8B0.9800C8B—H8E0.9800
C8A—H8C0.9800C8B—H8F0.9800
C9A—H9A0.9800C9B—H9D0.9800
C9A—H9B0.9800C9B—H9E0.9800
C9A—H9C0.9800C9B—H9F0.9800
C10A—H10A0.9800C10B—H10D0.9800
C10A—H10B0.9800C10B—H10E0.9800
C10A—H10C0.9800C10B—H10F0.9800
C11A—H11A0.9800C11B—H11D0.9800
C11A—H11B0.9800C11B—H11E0.9800
C11A—H11C0.9800C11B—H11F0.9800
C12A—H12A0.9800C12B—H12D0.9800
C12A—H12B0.9800C12B—H12E0.9800
C12A—H12C0.9800C12B—H12F0.9800
C13A—H13A0.9800C13B—H13D0.9800
C13A—H13B0.9800C13B—H13E0.9800
C13A—H13C0.9800C13B—H13F0.9800
C14A—H14A0.9800C14B—H14D0.9800
C14A—H14B0.9800C14B—H14E0.9800
C14A—H14C0.9800C14B—H14F0.9800
C15A—H15A0.9800C15B—H15D0.9800
C15A—H15B0.9800C15B—H15E0.9800
C15A—H15C0.9800C15B—H15F0.9800
C16A—C20A1.441 (5)C16B—C17B1.444 (5)
C16A—C17A1.442 (5)C16B—C20B1.454 (5)
C17A—C18A1.419 (5)C17B—C18B1.425 (5)
C17A—H17A0.9500C17B—H17B0.9500
C18A—C19A1.410 (6)C18B—C19B1.408 (5)
C18A—H18A0.9500C18B—H18B0.9500
C19A—C20A1.423 (5)C19B—C20B1.420 (5)
C19A—H19A0.9500C19B—H19B0.9500
C20A—H20A0.9500C20B—H20B0.9500
C21A—C25A1.444 (5)C21B—C22B1.436 (5)
C21A—C22A1.454 (5)C21B—C25B1.441 (5)
C22A—C23A1.420 (5)C22B—C23B1.421 (5)
C22A—H22A0.9500C22B—H22B0.9500
C23A—C24A1.412 (5)C23B—C24B1.418 (5)
C23A—H23A0.9500C23B—H23B0.9500
C24A—C25A1.427 (5)C24B—C25B1.416 (5)
C24A—H24A0.9500C24B—H24B0.9500
C25A—H25A0.9500C25B—H25B0.9500
C17A—Fe1A—C22A100.82 (15)C22B—Fe1B—C17B99.90 (15)
C17A—Fe1A—C25A146.12 (14)C22B—Fe1B—C25B68.11 (14)
C22A—Fe1A—C25A68.32 (14)C17B—Fe1B—C25B148.87 (14)
C17A—Fe1A—C16A41.65 (14)C22B—Fe1B—C20B147.77 (14)
C22A—Fe1A—C16A112.84 (14)C17B—Fe1B—C20B68.45 (15)
C25A—Fe1A—C16A111.08 (14)C25B—Fe1B—C20B105.80 (14)
C17A—Fe1A—C20A68.19 (16)C22B—Fe1B—C21B41.39 (14)
C22A—Fe1A—C20A151.37 (14)C17B—Fe1B—C21B110.61 (14)
C25A—Fe1A—C20A105.44 (15)C25B—Fe1B—C21B41.45 (13)
C16A—Fe1A—C20A41.42 (14)C20B—Fe1B—C21B112.66 (14)
C17A—Fe1A—C21A108.92 (14)C22B—Fe1B—C16B109.66 (14)
C22A—Fe1A—C21A41.81 (14)C17B—Fe1B—C16B41.54 (14)
C25A—Fe1A—C21A41.49 (13)C25B—Fe1B—C16B113.43 (13)
C16A—Fe1A—C21A91.43 (13)C20B—Fe1B—C16B41.72 (13)
C20A—Fe1A—C21A114.73 (14)C21B—Fe1B—C16B91.17 (13)
C17A—Fe1A—C18A40.82 (14)C22B—Fe1B—C18B123.19 (16)
C22A—Fe1A—C18A121.54 (17)C17B—Fe1B—C18B40.89 (14)
C25A—Fe1A—C18A169.32 (16)C25B—Fe1B—C18B167.27 (15)
C16A—Fe1A—C18A70.13 (15)C20B—Fe1B—C18B68.09 (16)
C20A—Fe1A—C18A68.05 (16)C21B—Fe1B—C18B150.78 (15)
C21A—Fe1A—C18A148.46 (15)C16B—Fe1B—C18B70.03 (14)
C17A—Fe1A—C23A125.00 (16)C22B—Fe1B—C19B163.05 (15)
C22A—Fe1A—C23A40.68 (14)C17B—Fe1B—C19B68.06 (15)
C25A—Fe1A—C23A68.10 (14)C25B—Fe1B—C19B128.30 (15)
C16A—Fe1A—C23A153.12 (14)C20B—Fe1B—C19B40.51 (14)
C20A—Fe1A—C23A164.90 (15)C21B—Fe1B—C19B152.85 (15)
C21A—Fe1A—C23A70.15 (14)C16B—Fe1B—C19B69.82 (14)
C18A—Fe1A—C23A115.95 (16)C18B—Fe1B—C19B40.01 (15)
C17A—Fe1A—C24A165.05 (16)C22B—Fe1B—C24B67.66 (14)
C22A—Fe1A—C24A68.21 (14)C17B—Fe1B—C24B161.87 (15)
C25A—Fe1A—C24A40.85 (13)C25B—Fe1B—C24B40.39 (13)
C16A—Fe1A—C24A151.13 (14)C20B—Fe1B—C24B129.08 (15)
C20A—Fe1A—C24A126.26 (15)C21B—Fe1B—C24B69.42 (13)
C21A—Fe1A—C24A70.21 (13)C16B—Fe1B—C24B153.66 (14)
C18A—Fe1A—C24A135.74 (15)C18B—Fe1B—C24B134.56 (15)
C23A—Fe1A—C24A40.14 (14)C19B—Fe1B—C24B120.68 (15)
C17A—Fe1A—C19A68.01 (16)C22B—Fe1B—C23B40.54 (13)
C22A—Fe1A—C19A160.83 (16)C17B—Fe1B—C23B122.08 (16)
C25A—Fe1A—C19A129.63 (16)C25B—Fe1B—C23B67.98 (14)
C16A—Fe1A—C19A69.83 (14)C20B—Fe1B—C23B168.41 (14)
C20A—Fe1A—C19A40.58 (15)C21B—Fe1B—C23B69.69 (14)
C21A—Fe1A—C19A155.22 (15)C16B—Fe1B—C23B149.26 (14)
C18A—Fe1A—C19A40.06 (16)C18B—Fe1B—C23B115.85 (16)
C23A—Fe1A—C19A132.79 (15)C19B—Fe1B—C23B135.39 (15)
C24A—Fe1A—C19A119.31 (15)C24B—Fe1B—C23B40.03 (14)
C17A—Fe1A—Ga1A72.79 (10)C22B—Fe1B—Ga1B73.20 (10)
C22A—Fe1A—Ga1A75.67 (10)C17B—Fe1B—Ga1B74.00 (10)
C25A—Fe1A—Ga1A73.41 (10)C25B—Fe1B—Ga1B75.00 (9)
C16A—Fe1A—Ga1A45.66 (9)C20B—Fe1B—Ga1B74.67 (10)
C20A—Fe1A—Ga1A75.81 (10)C21B—Fe1B—Ga1B45.55 (9)
C21A—Fe1A—Ga1A45.78 (10)C16B—Fe1B—Ga1B45.64 (10)
C18A—Fe1A—Ga1A111.81 (11)C18B—Fe1B—Ga1B112.63 (11)
C23A—Fe1A—Ga1A113.63 (10)C19B—Fe1B—Ga1B112.70 (11)
C24A—Fe1A—Ga1A112.37 (10)C24B—Fe1B—Ga1B112.63 (10)
C19A—Fe1A—Ga1A113.50 (11)C23B—Fe1B—Ga1B111.74 (10)
C16A—Ga1A—C21A92.68 (13)C21B—Ga1B—C16B92.22 (13)
C16A—Ga1A—C7A126.52 (13)C21B—Ga1B—C7B123.85 (14)
C21A—Ga1A—C7A127.08 (13)C16B—Ga1B—C7B128.70 (13)
C16A—Ga1A—N1A108.52 (13)C21B—Ga1B—N1b109.34 (12)
C21A—Ga1A—N1A104.33 (12)C16B—Ga1B—N1b103.82 (13)
C7A—Ga1A—N1A95.63 (12)C7B—Ga1B—N1b97.21 (12)
C16A—Ga1A—Fe1A46.20 (10)C21B—Ga1B—Fe1B45.99 (9)
C21A—Ga1A—Fe1A46.49 (9)C16B—Ga1B—Fe1B46.24 (9)
C7A—Ga1A—Fe1A150.96 (10)C7B—Ga1B—Fe1B149.22 (10)
N1A—Ga1A—Fe1A113.39 (7)N1b—Ga1B—Fe1B113.56 (8)
C2A—N1A—C6A119.4 (3)C2B—N1b—C6B119.9 (3)
C2A—N1A—Ga1A127.2 (2)C2B—N1b—Ga1B125.4 (2)
C6A—N1A—Ga1A113.4 (2)C6B—N1b—Ga1B114.7 (2)
C7A—Si1A—C9A115.99 (18)C7B—Si1B—C8B115.92 (19)
C7A—Si1A—C8A118.61 (18)C7B—Si1B—C9B119.06 (18)
C9A—Si1A—C8A106.4 (2)C8B—Si1B—C9B104.3 (2)
C7A—Si1A—C6A104.80 (15)C7B—Si1B—C6B105.00 (15)
C9A—Si1A—C6A102.99 (17)C8B—Si1B—C6B103.99 (18)
C8A—Si1A—C6A106.55 (17)C9B—Si1B—C6B107.4 (2)
C12A—Si2A—C11A105.13 (19)C10B—Si2B—C12B106.0 (2)
C12A—Si2A—C10A105.0 (2)C10B—Si2B—C11B106.32 (19)
C11A—Si2A—C10A107.7 (2)C12B—Si2B—C11B105.7 (2)
C12A—Si2A—C7A114.47 (17)C10B—Si2B—C7B113.31 (18)
C11A—Si2A—C7A113.26 (17)C12B—Si2B—C7B112.28 (17)
C10A—Si2A—C7A110.72 (17)C11B—Si2B—C7B112.59 (18)
C13A—Si3A—C15A105.8 (2)C13B—Si3B—C15B104.13 (19)
C13A—Si3A—C14A105.35 (19)C13B—Si3B—C14B104.19 (18)
C15A—Si3A—C14A105.70 (19)C15B—Si3B—C14B108.8 (2)
C13A—Si3A—C7A113.14 (17)C13B—Si3B—C7B116.39 (16)
C15A—Si3A—C7A114.06 (16)C15B—Si3B—C7B109.75 (17)
C14A—Si3A—C7A112.10 (17)C14B—Si3B—C7B112.94 (17)
N1A—C2A—C3A122.7 (3)N1b—C2B—C3B122.5 (4)
N1A—C2A—H2A118.6N1b—C2B—H2B118.7
C3A—C2A—H2A118.6C3B—C2B—H2B118.7
C2A—C3A—C4A119.4 (3)C4B—C3B—C2B118.7 (4)
C2A—C3A—H3A120.3C4B—C3B—H3B120.6
C4A—C3A—H3A120.3C2B—C3B—H3B120.6
C3A—C4A—C5A118.1 (3)C3B—C4B—C5B119.2 (4)
C3A—C4A—H4A121.0C3B—C4B—H4B120.4
C5A—C4A—H4A121.0C5B—C4B—H4B120.4
C6A—C5A—C4A120.9 (3)C4B—C5B—C6B120.1 (4)
C6A—C5A—H5A119.5C4B—C5B—H5B119.9
C4A—C5A—H5A119.5C6B—C5B—H5B119.9
N1A—C6A—C5A119.5 (3)N1b—C6B—C5B119.5 (3)
N1A—C6A—Si1A115.2 (2)N1b—C6B—Si1B115.3 (3)
C5A—C6A—Si1A125.2 (3)C5B—C6B—Si1B125.0 (3)
Si1A—C7A—Si3A111.64 (17)Si1B—C7B—Si2B112.83 (18)
Si1A—C7A—Si2A111.30 (18)Si1B—C7B—Si3B110.04 (18)
Si3A—C7A—Si2A112.52 (17)Si2B—C7B—Si3B114.48 (18)
Si1A—C7A—Ga1A100.45 (15)Si1B—C7B—Ga1B102.21 (16)
Si3A—C7A—Ga1A114.46 (17)Si2B—C7B—Ga1B110.78 (17)
Si2A—C7A—Ga1A105.75 (15)Si3B—C7B—Ga1B105.57 (15)
Si1A—C8A—H8A109.5Si1B—C8B—H8D109.5
Si1A—C8A—H8B109.5Si1B—C8B—H8E109.5
H8A—C8A—H8B109.5H8D—C8B—H8E109.5
Si1A—C8A—H8C109.5Si1B—C8B—H8F109.5
H8A—C8A—H8C109.5H8D—C8B—H8F109.5
H8B—C8A—H8C109.5H8E—C8B—H8F109.5
Si1A—C9A—H9A109.5Si1B—C9B—H9D109.5
Si1A—C9A—H9B109.5Si1B—C9B—H9E109.5
H9A—C9A—H9B109.5H9D—C9B—H9E109.5
Si1A—C9A—H9C109.5Si1B—C9B—H9F109.5
H9A—C9A—H9C109.5H9D—C9B—H9F109.5
H9B—C9A—H9C109.5H9E—C9B—H9F109.5
Si2A—C10A—H10A109.5Si2B—C10B—H10D109.5
Si2A—C10A—H10B109.5Si2B—C10B—H10E109.5
H10A—C10A—H10B109.5H10D—C10B—H10E109.5
Si2A—C10A—H10C109.5Si2B—C10B—H10F109.5
H10A—C10A—H10C109.5H10D—C10B—H10F109.5
H10B—C10A—H10C109.5H10E—C10B—H10F109.5
Si2A—C11A—H11A109.5Si2B—C11B—H11D109.5
Si2A—C11A—H11B109.5Si2B—C11B—H11E109.5
H11A—C11A—H11B109.5H11D—C11B—H11E109.5
Si2A—C11A—H11C109.5Si2B—C11B—H11F109.5
H11A—C11A—H11C109.5H11D—C11B—H11F109.5
H11B—C11A—H11C109.5H11E—C11B—H11F109.5
Si2A—C12A—H12A109.5Si2B—C12B—H12D109.5
Si2A—C12A—H12B109.5Si2B—C12B—H12E109.5
H12A—C12A—H12B109.5H12D—C12B—H12E109.5
Si2A—C12A—H12C109.5Si2B—C12B—H12F109.5
H12A—C12A—H12C109.5H12D—C12B—H12F109.5
H12B—C12A—H12C109.5H12E—C12B—H12F109.5
Si3A—C13A—H13A109.5Si3B—C13B—H13D109.5
Si3A—C13A—H13B109.5Si3B—C13B—H13E109.5
H13A—C13A—H13B109.5H13D—C13B—H13E109.5
Si3A—C13A—H13C109.5Si3B—C13B—H13F109.5
H13A—C13A—H13C109.5H13D—C13B—H13F109.5
H13B—C13A—H13C109.5H13E—C13B—H13F109.5
Si3A—C14A—H14A109.5Si3B—C14B—H14D109.5
Si3A—C14A—H14B109.5Si3B—C14B—H14E109.5
H14A—C14A—H14B109.5H14D—C14B—H14E109.5
Si3A—C14A—H14C109.5Si3B—C14B—H14F109.5
H14A—C14A—H14C109.5H14D—C14B—H14F