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Acta Crystallogr Sect E Struct Rep Online. 2008 June 1; 64(Pt 6): m835.
Published online 2008 May 21. doi:  10.1107/S1600536808014931
PMCID: PMC2961392

μ-Bis(diphenyl­phosphan­yl)borato-κ2 P:P′-bis­[dicarbon­yl(η5-cyclo­penta­dien­yl)iron(II)] tetrachloridoferrate(III) chloro­form solvate

Abstract

The title compound, [Fe2(C5H5)2(C24H22BP2)(CO)4][FeCl4]·CHCl3, is an oxidation product of CpFe(CO)2PPh2BH3. One pair of phenyl rings attached to the two different P atoms are almost parallel, as are the other pair [dihedral angles = 8.7 (5) and 8.9 (5)°]. The planes of the two cyclo­penta­dienyl rings are inclined by 26.8 (7)° with respect to each other. The carbonyl groups at each Fe atom are almost perpendicular [C—Fe—C = 92.6 (6) and 94.3 (5)°].

Related literature

For related literature, see: Kückmann et al. (2007 [triangle]).

An external file that holds a picture, illustration, etc.
Object name is e-64-0m835-scheme1.jpg

Experimental

Crystal data

  • [Fe2(C5H5)2(C24H22BP2)(CO)4][FeCl4]·CHCl3
  • M r = 1054.10
  • Monoclinic, An external file that holds a picture, illustration, etc.
Object name is e-64-0m835-efi1.jpg
  • a = 16.0627 (17) Å
  • b = 17.8223 (17) Å
  • c = 17.205 (2) Å
  • β = 113.296 (8)°
  • V = 4523.8 (9) Å3
  • Z = 4
  • Mo Kα radiation
  • μ = 1.47 mm−1
  • T = 173 (2) K
  • 0.11 × 0.07 × 0.02 mm

Data collection

  • Stoe IPDSII two-circle diffractometer
  • Absorption correction: multi-scan (MULABS; Spek, 2003 [triangle]; Blessing, 1995 [triangle]) T min = 0.855, T max = 0.971
  • 44600 measured reflections
  • 8506 independent reflections
  • 3324 reflections with I > 2σ(I)
  • R int = 0.088

Refinement

  • R[F 2 > 2σ(F 2)] = 0.111
  • wR(F 2) = 0.176
  • S = 0.99
  • 8506 reflections
  • 505 parameters
  • H-atom parameters constrained
  • Δρmax = 0.80 e Å−3
  • Δρmin = −0.60 e Å−3

Data collection: X-AREA (Stoe & Cie, 2001 [triangle]); cell refinement: X-AREA; data reduction: X-AREA; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 [triangle]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 [triangle]); molecular graphics: XP in SHELXTL-Plus (Sheldrick, 2008 [triangle]); software used to prepare material for publication: SHELXL97 and PLATON (Spek, 2003 [triangle]).

Supplementary Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536808014931/bq2081sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808014931/bq2081Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

supplementary crystallographic information

Comment

Very recently we have described the synthesis of CpFe(CO)2PPh2BH3 (Kückmann et al., 2007). We report here air oxidation of CpFe(CO)2PPh2BH3 in chloroform and the result of the X-ray crystal structure analysis of the obtained oxidation product, [(CpFe(CO)2PPh2)2BH2][FeCl4].

The title compound is an oxidation product of CpFe(CO)2PPh2BH3. It is composed of cations, anions and neutral chloroform molecules. Pairs of phenyl rings attached to each of the two P atoms are almost coparallel [dihedral angles 8.7 (5)° and 8.9 (5)°]. The planes of the two cp rings are inclined by 26.8 (7)° with respect to each other. The carbonyl groups at each Fe atom are almost mutually perpendicular [C—Fe—C angle 92.6 (6)° and 94.3 (5)°].

Experimental

In an NMR tube a solution of CpFe(CO)2PPh2BH3 (Kückmann et al., 2007) (0.2 mmol) in 0.6 ml CDCl3 was exposed to air for several days at room temperature. Single crystals of the title compound were grown from this solution at room temperature.

Refinement

H atoms were refined with fixed individual displacement parameters [U(H) = 1.2 Ueq(C,B)] using a riding model with B—H = 0.99 Å, Caromatic—H = 0.95Å and Cl3C—H = 1.0 Å.

Figures

Fig. 1.
Perspective view of the title compound with the atom numbering scheme; displacement ellipsoids are at the 50% probability level; H atoms are omitted for clarity. The FeCl4 anion and the CHCl3 solvent are omitted for clarity.

Crystal data

[Fe2(C5H5)2(C24H22BP2)(CO)4][FeCl4]·CHCl3F000 = 2124
Mr = 1054.10Dx = 1.548 Mg m3
Monoclinic, P21/nMo Kα radiation λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 6332 reflections
a = 16.0627 (17) Åθ = 3.6–24.5º
b = 17.8223 (17) ŵ = 1.47 mm1
c = 17.205 (2) ÅT = 173 (2) K
β = 113.296 (8)ºPlate, brown
V = 4523.8 (9) Å30.11 × 0.07 × 0.02 mm
Z = 4

Data collection

Stoe IPDSII two-circle diffractometer8506 independent reflections
Radiation source: fine-focus sealed tube3324 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.089
T = 173(2) Kθmax = 25.8º
ω scansθmin = 3.6º
Absorption correction: multi-scan(MULABS; Spek, 2003; Blessing, 1995)h = −19→19
Tmin = 0.855, Tmax = 0.971k = −21→21
44600 measured reflectionsl = −20→18

Refinement

Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.111H-atom parameters constrained
wR(F2) = 0.176  w = 1/[σ2(Fo2) + (0.0133P)2] where P = (Fo2 + 2Fc2)/3
S = 0.99(Δ/σ)max < 0.001
8506 reflectionsΔρmax = 0.80 e Å3
505 parametersΔρmin = −0.60 e Å3
Primary atom site location: structure-invariant direct methodsExtinction correction: none

Special details

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)

xyzUiso*/Ueq
B10.7751 (9)0.2979 (10)0.8313 (8)0.031 (3)
H1A0.80930.34310.86000.037*
H1B0.81190.25410.86090.037*
Fe10.70461 (11)0.29478 (10)0.99844 (10)0.0235 (4)
Fe20.92129 (11)0.30470 (10)0.72844 (10)0.0228 (4)
P10.66442 (19)0.29568 (18)0.85413 (17)0.0197 (6)
P20.7737 (2)0.29796 (18)0.71644 (18)0.0231 (7)
C10.7935 (9)0.2299 (7)1.0123 (7)0.028 (3)
O10.8519 (7)0.1879 (6)1.0251 (7)0.059 (3)
C20.7777 (9)0.3741 (7)1.0121 (7)0.034 (3)
O20.8262 (7)0.4231 (5)1.0217 (6)0.043 (3)
C30.9563 (9)0.2289 (7)0.8019 (9)0.033 (3)
O30.9828 (7)0.1817 (5)0.8526 (7)0.050 (3)
C40.9460 (8)0.3751 (6)0.8084 (7)0.021 (3)
O40.9641 (6)0.4213 (5)0.8581 (6)0.036 (2)
C110.6176 (9)0.3548 (8)1.0417 (8)0.039 (4)
H110.61170.40791.04060.046*
C120.5664 (8)0.3034 (8)0.9779 (8)0.037 (3)
H120.51770.31620.92630.045*
C130.5997 (9)0.2295 (7)1.0036 (8)0.037 (4)
H130.57910.18510.97100.044*
C140.6680 (10)0.2335 (8)1.0851 (9)0.043 (4)
H140.69970.19191.11810.051*
C150.6819 (9)0.3087 (9)1.1101 (8)0.042 (4)
H150.72530.32691.16220.051*
C210.5872 (8)0.3745 (6)0.8036 (8)0.025 (3)
C220.5883 (9)0.4404 (6)0.8455 (8)0.030 (3)
H220.62690.44490.90370.036*
C230.5331 (9)0.5011 (7)0.8036 (9)0.040 (4)
H230.53660.54620.83410.048*
C240.4739 (9)0.4976 (7)0.7195 (8)0.039 (4)
H240.43590.53870.69240.047*
C250.4724 (9)0.4322 (7)0.6769 (8)0.037 (3)
H250.43240.42830.61900.044*
C260.5276 (8)0.3711 (7)0.7154 (7)0.026 (3)
H260.52590.32720.68350.031*
C310.6003 (8)0.2122 (6)0.8099 (7)0.021 (3)
C320.5039 (8)0.2071 (7)0.7774 (7)0.032 (3)
H320.46980.25020.77870.038*
C330.4592 (9)0.1417 (6)0.7443 (9)0.036 (3)
H330.39480.14110.72090.043*
C340.5051 (9)0.0776 (7)0.7441 (11)0.042 (4)
H340.47250.03280.72140.051*
C350.6013 (8)0.0771 (7)0.7775 (9)0.032 (3)
H350.63360.03250.77740.039*
C360.6472 (9)0.1438 (6)0.8106 (8)0.027 (3)
H360.71160.14380.83430.032*
C410.7122 (8)0.3789 (6)0.6556 (8)0.026 (3)
C420.7131 (9)0.4462 (7)0.6993 (9)0.032 (3)
H420.74550.44820.75900.038*
C430.6678 (8)0.5093 (7)0.6568 (8)0.032 (3)
H430.67020.55410.68750.039*
C440.6192 (10)0.5081 (8)0.5706 (8)0.038 (4)
H440.58680.55140.54230.045*
C450.6178 (9)0.4432 (8)0.5254 (9)0.038 (3)
H450.58570.44180.46570.045*
C460.6634 (8)0.3818 (8)0.5683 (8)0.035 (3)
H460.66180.33780.53650.042*
C510.7135 (7)0.2153 (6)0.6561 (7)0.023 (3)
C520.6165 (8)0.2150 (7)0.6108 (8)0.032 (3)
H520.58230.25870.60990.038*
C530.5731 (9)0.1508 (7)0.5685 (9)0.037 (4)
H530.50920.15150.53830.044*
C540.6208 (10)0.0849 (7)0.5692 (8)0.039 (4)
H540.59010.04130.54020.046*
C550.7130 (10)0.0853 (7)0.6129 (8)0.037 (3)
H550.74630.04090.61460.044*
C560.7596 (9)0.1499 (6)0.6555 (7)0.027 (3)
H560.82370.14850.68410.032*
C610.8766 (10)0.3001 (10)0.5953 (8)0.051 (4)
H610.81640.28950.55710.061*
C620.9107 (10)0.3710 (7)0.6238 (8)0.033 (3)
H620.87800.41690.60980.040*
C631.0042 (10)0.3620 (9)0.6785 (9)0.046 (4)
H631.04520.40140.70590.055*
C641.0246 (10)0.2864 (9)0.6845 (8)0.043 (4)
H641.08180.26500.71800.051*
C650.9461 (11)0.2457 (9)0.6322 (8)0.044 (4)
H650.94100.19290.62370.053*
Fe30.72051 (13)0.61469 (11)0.12242 (12)0.0352 (5)
Cl310.6037 (3)0.5782 (2)0.0096 (2)0.0469 (10)
Cl320.6747 (3)0.6715 (3)0.2116 (3)0.0857 (19)
Cl330.7923 (3)0.5112 (2)0.1841 (3)0.0557 (11)
Cl340.8099 (3)0.6898 (3)0.0894 (3)0.0657 (13)
C50.8024 (11)0.4708 (9)0.3879 (11)0.059 (5)
H50.77510.49690.33200.071*
Cl510.7504 (4)0.3814 (3)0.3768 (3)0.0885 (17)
Cl520.7830 (4)0.5251 (3)0.4605 (3)0.0782 (15)
Cl530.9181 (4)0.4590 (4)0.4120 (5)0.119 (2)

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
B10.020 (7)0.038 (8)0.024 (7)−0.002 (7)−0.003 (6)−0.005 (7)
Fe10.0215 (9)0.0301 (9)0.0164 (9)0.0028 (8)0.0048 (7)0.0030 (8)
Fe20.0220 (9)0.0238 (9)0.0221 (9)−0.0005 (8)0.0082 (7)0.0007 (8)
P10.0193 (15)0.0222 (15)0.0151 (14)0.0010 (14)0.0040 (12)0.0018 (13)
P20.0236 (16)0.0216 (14)0.0186 (15)−0.0004 (15)0.0024 (12)0.0003 (14)
C10.038 (8)0.036 (7)0.013 (6)−0.002 (6)0.015 (6)0.004 (5)
O10.055 (7)0.068 (8)0.054 (7)0.048 (6)0.023 (6)0.034 (6)
C20.043 (9)0.030 (7)0.013 (6)−0.004 (6)−0.005 (6)0.004 (5)
O20.051 (7)0.046 (6)0.026 (5)−0.010 (5)0.010 (5)−0.002 (4)
C30.023 (7)0.029 (7)0.042 (8)−0.013 (6)0.008 (6)−0.004 (6)
O30.045 (6)0.033 (6)0.063 (7)0.017 (5)0.011 (5)0.022 (5)
C40.020 (6)0.026 (6)0.019 (6)−0.001 (5)0.009 (5)0.005 (5)
O40.041 (6)0.042 (5)0.024 (5)−0.010 (4)0.011 (4)−0.009 (4)
C110.026 (7)0.051 (9)0.032 (8)−0.011 (6)0.004 (6)−0.016 (6)
C120.026 (7)0.053 (8)0.032 (7)0.013 (7)0.011 (6)0.008 (7)
C130.047 (9)0.049 (8)0.012 (6)−0.010 (7)0.009 (6)0.008 (5)
C140.038 (9)0.058 (10)0.031 (8)0.000 (7)0.014 (7)0.027 (7)
C150.036 (8)0.070 (11)0.024 (7)−0.009 (8)0.015 (6)0.013 (7)
C210.019 (6)0.023 (6)0.032 (7)−0.008 (5)0.010 (5)0.006 (5)
C220.033 (8)0.027 (6)0.021 (7)0.009 (6)−0.001 (6)0.000 (5)
C230.048 (9)0.018 (6)0.042 (9)0.010 (6)0.006 (7)−0.001 (6)
C240.035 (8)0.034 (7)0.030 (8)0.016 (6)−0.007 (6)0.008 (6)
C250.043 (9)0.045 (8)0.011 (6)0.001 (6)−0.001 (6)0.004 (6)
C260.017 (6)0.032 (7)0.024 (7)−0.016 (5)0.004 (5)−0.008 (5)
C310.030 (7)0.021 (6)0.012 (5)0.007 (5)0.006 (5)−0.001 (5)
C320.035 (7)0.031 (7)0.035 (7)−0.007 (6)0.019 (6)−0.007 (6)
C330.025 (7)0.027 (7)0.060 (10)−0.004 (5)0.023 (7)−0.005 (6)
C340.032 (8)0.018 (7)0.078 (12)−0.003 (6)0.024 (8)−0.004 (7)
C350.015 (7)0.036 (7)0.044 (8)0.005 (5)0.010 (6)0.000 (6)
C360.031 (7)0.023 (6)0.028 (7)0.011 (5)0.013 (6)0.006 (5)
C410.028 (7)0.020 (6)0.030 (7)0.008 (5)0.011 (6)0.004 (5)
C420.022 (7)0.035 (7)0.035 (8)0.005 (6)0.008 (6)0.013 (6)
C430.032 (8)0.029 (7)0.041 (8)−0.014 (6)0.019 (6)0.007 (6)
C440.044 (9)0.040 (8)0.022 (7)0.007 (7)0.006 (6)0.017 (6)
C450.034 (8)0.045 (8)0.030 (8)0.017 (7)0.008 (6)0.005 (6)
C460.024 (7)0.042 (8)0.032 (7)−0.002 (6)0.004 (6)−0.008 (6)
C510.019 (6)0.021 (6)0.022 (6)−0.002 (5)0.000 (5)−0.003 (5)
C520.017 (6)0.035 (7)0.041 (8)0.005 (5)0.009 (6)0.001 (6)
C530.023 (7)0.032 (7)0.048 (9)−0.017 (6)0.006 (6)−0.028 (6)
C540.052 (10)0.035 (8)0.023 (7)−0.025 (7)0.008 (7)−0.018 (6)
C550.046 (9)0.023 (6)0.031 (8)−0.004 (6)0.003 (6)−0.010 (5)
C560.033 (7)0.034 (7)0.015 (6)−0.002 (6)0.011 (5)−0.008 (5)
C610.051 (10)0.079 (11)0.022 (7)0.006 (10)0.014 (7)−0.006 (9)
C620.053 (9)0.020 (7)0.033 (8)−0.008 (6)0.024 (7)−0.002 (6)
C630.045 (9)0.071 (11)0.030 (8)−0.023 (8)0.023 (7)−0.011 (7)
C640.040 (8)0.066 (11)0.026 (7)0.020 (8)0.018 (6)0.001 (7)
C650.069 (11)0.052 (9)0.022 (8)−0.015 (8)0.029 (8)−0.015 (7)
Fe30.0253 (10)0.0465 (12)0.0245 (10)0.0111 (9)−0.0003 (8)−0.0047 (9)
Cl310.040 (2)0.052 (2)0.033 (2)0.0042 (17)−0.0024 (16)−0.0157 (17)
Cl320.045 (3)0.147 (5)0.054 (3)0.027 (3)0.008 (2)−0.050 (3)
Cl330.050 (2)0.058 (2)0.049 (2)0.025 (2)0.0098 (19)0.0118 (19)
Cl340.051 (2)0.075 (3)0.055 (3)−0.010 (2)0.004 (2)0.008 (2)
C50.055 (11)0.063 (11)0.045 (10)0.007 (9)0.003 (8)0.012 (8)
Cl510.115 (4)0.072 (3)0.063 (3)0.008 (3)0.018 (3)0.003 (3)
Cl520.105 (4)0.061 (3)0.076 (3)0.016 (3)0.044 (3)0.014 (2)
Cl530.080 (4)0.184 (7)0.103 (5)0.014 (4)0.047 (4)0.014 (5)

Geometric parameters (Å, °)

B1—P21.967 (14)C31—C361.430 (15)
B1—P11.967 (15)C32—C331.370 (16)
B1—H1A0.9900C32—H320.9500
B1—H1B0.9900C33—C341.360 (17)
Fe1—C11.778 (14)C33—H330.9500
Fe1—C21.793 (14)C34—C351.420 (18)
Fe1—C132.079 (14)C34—H340.9500
Fe1—C152.107 (13)C35—C361.397 (17)
Fe1—C142.111 (13)C35—H350.9500
Fe1—C122.111 (13)C36—H360.9500
Fe1—C112.115 (15)C41—C461.394 (17)
Fe1—P12.305 (3)C41—C421.414 (17)
Fe2—C31.783 (14)C42—C431.381 (16)
Fe2—C41.786 (12)C42—H420.9500
Fe2—C622.102 (13)C43—C441.375 (18)
Fe2—C642.104 (14)C43—H430.9500
Fe2—C632.112 (15)C44—C451.390 (19)
Fe2—C612.114 (13)C44—H440.9500
Fe2—C652.128 (14)C45—C461.361 (17)
Fe2—P22.301 (4)C45—H450.9500
P1—C311.799 (12)C46—H460.9500
P1—C211.848 (12)C51—C561.383 (16)
P2—C411.825 (12)C51—C521.441 (16)
P2—C511.841 (11)C52—C531.387 (16)
C1—O11.153 (14)C52—H520.9500
C2—O21.138 (14)C53—C541.398 (18)
C3—O31.164 (14)C53—H530.9500
C4—O41.140 (13)C54—C551.370 (19)
C11—C121.416 (18)C54—H540.9500
C11—C151.471 (18)C55—C561.410 (15)
C11—H110.9500C55—H550.9500
C12—C131.425 (18)C56—H560.9500
C12—H120.9500C61—C621.39 (2)
C13—C141.401 (18)C61—C651.42 (2)
C13—H130.9500C61—H610.9500
C14—C151.40 (2)C62—C631.43 (2)
C14—H140.9500C62—H620.9500
C15—H150.9500C63—C641.38 (2)
C21—C221.374 (17)C63—H630.9500
C21—C261.439 (16)C64—C651.425 (19)
C22—C231.403 (16)C64—H640.9500
C22—H220.9500C65—H650.9500
C23—C241.383 (18)Fe3—Cl322.193 (5)
C23—H230.9500Fe3—Cl342.196 (5)
C24—C251.373 (18)Fe3—Cl312.198 (4)
C24—H240.9500Fe3—Cl332.211 (4)
C25—C261.394 (17)C5—Cl521.703 (19)
C25—H250.9500C5—Cl531.749 (18)
C26—H260.9500C5—Cl511.775 (17)
C31—C321.426 (16)C5—H51.0000
P2—B1—P1123.2 (6)C21—C22—C23120.9 (11)
P2—B1—H1A106.5C21—C22—H22119.5
P1—B1—H1A106.5C23—C22—H22119.5
P2—B1—H1B106.5C24—C23—C22122.5 (12)
P1—B1—H1B106.5C24—C23—H23118.8
H1A—B1—H1B106.5C22—C23—H23118.8
C1—Fe1—C292.6 (6)C25—C24—C23117.1 (11)
C1—Fe1—C13104.6 (5)C25—C24—H24121.4
C2—Fe1—C13159.4 (6)C23—C24—H24121.4
C1—Fe1—C15112.0 (5)C24—C25—C26122.4 (11)
C2—Fe1—C1597.4 (6)C24—C25—H25118.8
C13—Fe1—C1565.9 (5)C26—C25—H25118.8
C1—Fe1—C1490.1 (6)C25—C26—C21120.1 (11)
C2—Fe1—C14131.8 (6)C25—C26—H26120.0
C13—Fe1—C1439.1 (5)C21—C26—H26120.0
C15—Fe1—C1438.7 (6)C32—C31—C36115.8 (11)
C1—Fe1—C12143.6 (6)C32—C31—P1124.8 (9)
C2—Fe1—C12123.7 (6)C36—C31—P1119.3 (9)
C13—Fe1—C1239.8 (5)C33—C32—C31121.8 (12)
C15—Fe1—C1266.1 (5)C33—C32—H32119.1
C14—Fe1—C1265.7 (5)C31—C32—H32119.1
C1—Fe1—C11152.7 (5)C34—C33—C32121.3 (13)
C2—Fe1—C1192.6 (6)C34—C33—H33119.3
C13—Fe1—C1167.0 (5)C32—C33—H33119.3
C15—Fe1—C1140.8 (5)C33—C34—C35120.6 (12)
C14—Fe1—C1166.8 (6)C33—C34—H34119.7
C12—Fe1—C1139.2 (5)C35—C34—H34119.7
C1—Fe1—P191.0 (4)C36—C35—C34118.3 (12)
C2—Fe1—P191.5 (4)C36—C35—H35120.9
C13—Fe1—P199.4 (4)C34—C35—H35120.9
C15—Fe1—P1154.9 (4)C35—C36—C31122.1 (11)
C14—Fe1—P1136.6 (4)C35—C36—H36119.0
C12—Fe1—P189.5 (4)C31—C36—H36119.0
C11—Fe1—P1115.7 (4)C46—C41—C42115.1 (11)
C3—Fe2—C494.3 (5)C46—C41—P2126.4 (10)
C3—Fe2—C62158.3 (6)C42—C41—P2118.5 (9)
C4—Fe2—C62100.5 (5)C43—C42—C41121.1 (13)
C3—Fe2—C6493.7 (6)C43—C42—H42119.4
C4—Fe2—C64114.8 (6)C41—C42—H42119.4
C62—Fe2—C6465.7 (5)C44—C43—C42121.0 (13)
C3—Fe2—C63125.6 (6)C44—C43—H43119.5
C4—Fe2—C6389.4 (5)C42—C43—H43119.5
C62—Fe2—C6339.7 (5)C43—C44—C45119.5 (12)
C64—Fe2—C6338.3 (6)C43—C44—H44120.2
C3—Fe2—C61128.0 (7)C45—C44—H44120.2
C4—Fe2—C61137.6 (6)C46—C45—C44118.6 (13)
C62—Fe2—C6138.4 (6)C46—C45—H45120.7
C64—Fe2—C6165.3 (6)C44—C45—H45120.7
C63—Fe2—C6164.9 (6)C45—C46—C41124.6 (13)
C3—Fe2—C6594.2 (6)C45—C46—H46117.7
C4—Fe2—C65153.3 (6)C41—C46—H46117.7
C62—Fe2—C6565.7 (5)C56—C51—C52117.4 (10)
C64—Fe2—C6539.3 (5)C56—C51—P2121.1 (9)
C63—Fe2—C6565.2 (6)C52—C51—P2121.5 (9)
C61—Fe2—C6539.2 (6)C53—C52—C51119.9 (11)
C3—Fe2—P292.8 (4)C53—C52—H52120.1
C4—Fe2—P290.7 (4)C51—C52—H52120.1
C62—Fe2—P2102.7 (4)C52—C53—C54121.9 (11)
C64—Fe2—P2153.0 (4)C52—C53—H53119.1
C63—Fe2—P2141.5 (5)C54—C53—H53119.1
C61—Fe2—P290.3 (4)C55—C54—C53118.0 (11)
C65—Fe2—P2114.1 (4)C55—C54—H54121.0
C31—P1—C21105.3 (5)C53—C54—H54121.0
C31—P1—B1110.1 (6)C54—C55—C56121.7 (12)
C21—P1—B1112.4 (6)C54—C55—H55119.2
C31—P1—Fe1108.6 (4)C56—C55—H55119.2
C21—P1—Fe1111.2 (4)C51—C56—C55121.1 (12)
B1—P1—Fe1109.0 (4)C51—C56—H56119.4
C41—P2—C51105.4 (5)C55—C56—H56119.4
C41—P2—B1111.4 (6)C62—C61—C65109.5 (13)
C51—P2—B1111.2 (6)C62—C61—Fe270.4 (8)
C41—P2—Fe2108.3 (4)C65—C61—Fe270.9 (8)
C51—P2—Fe2112.6 (4)C62—C61—H61125.3
B1—P2—Fe2107.9 (4)C65—C61—H61125.3
O1—C1—Fe1176.9 (11)Fe2—C61—H61125.1
O2—C2—Fe1178.0 (12)C61—C62—C63107.2 (13)
O3—C3—Fe2176.5 (11)C61—C62—Fe271.2 (8)
O4—C4—Fe2177.2 (11)C63—C62—Fe270.5 (8)
C12—C11—C15105.5 (12)C61—C62—H62126.4
C12—C11—Fe170.3 (8)C63—C62—H62126.4
C15—C11—Fe169.3 (8)Fe2—C62—H62123.5
C12—C11—H11127.2C64—C63—C62108.3 (13)
C15—C11—H11127.2C64—C63—Fe270.5 (9)
Fe1—C11—H11124.8C62—C63—Fe269.8 (8)
C11—C12—C13109.0 (12)C64—C63—H63125.8
C11—C12—Fe170.6 (8)C62—C63—H63125.8
C13—C12—Fe168.9 (8)Fe2—C63—H63125.4
C11—C12—H12125.5C63—C64—C65109.0 (13)
C13—C12—H12125.5C63—C64—Fe271.2 (8)
Fe1—C12—H12126.6C65—C64—Fe271.2 (8)
C14—C13—C12108.2 (12)C63—C64—H64125.5
C14—C13—Fe171.7 (8)C65—C64—H64125.5
C12—C13—Fe171.4 (8)Fe2—C64—H64123.7
C14—C13—H13125.9C61—C65—C64106.0 (13)
C12—C13—H13125.9C61—C65—Fe269.9 (8)
Fe1—C13—H13122.7C64—C65—Fe269.4 (7)
C15—C14—C13108.8 (12)C61—C65—H65127.0
C15—C14—Fe170.5 (7)C64—C65—H65127.0
C13—C14—Fe169.2 (8)Fe2—C65—H65125.3
C15—C14—H14125.6Cl32—Fe3—Cl34109.5 (2)
C13—C14—H14125.6Cl32—Fe3—Cl31110.40 (17)
Fe1—C14—H14126.3Cl34—Fe3—Cl31111.66 (18)
C14—C15—C11108.3 (12)Cl32—Fe3—Cl33107.7 (2)
C14—C15—Fe170.8 (8)Cl34—Fe3—Cl33111.25 (19)
C11—C15—Fe169.9 (7)Cl31—Fe3—Cl33106.17 (17)
C14—C15—H15125.9Cl52—C5—Cl53112.4 (10)
C11—C15—H15125.9Cl52—C5—Cl51112.0 (10)
Fe1—C15—H15125.0Cl53—C5—Cl51109.1 (9)
C22—C21—C26117.0 (11)Cl52—C5—H5107.7
C22—C21—P1122.4 (9)Cl53—C5—H5107.7
C26—C21—P1120.5 (9)Cl51—C5—H5107.7
P2—B1—P1—C3160.2 (11)B1—P1—C21—C2680.9 (11)
P2—B1—P1—C21−57.0 (11)Fe1—P1—C21—C26−156.6 (8)
P2—B1—P1—Fe1179.2 (8)C26—C21—C22—C230.2 (19)
C1—Fe1—P1—C3178.3 (6)P1—C21—C22—C23175.6 (11)
C2—Fe1—P1—C31171.0 (6)C21—C22—C23—C242(2)
C13—Fe1—P1—C31−26.6 (6)C22—C23—C24—C25−2(2)
C15—Fe1—P1—C31−78.1 (11)C23—C24—C25—C260(2)
C14—Fe1—P1—C31−12.9 (8)C24—C25—C26—C212(2)
C12—Fe1—P1—C31−65.3 (6)C22—C21—C26—C25−1.8 (18)
C11—Fe1—P1—C31−95.5 (6)P1—C21—C26—C25−177.2 (10)
C1—Fe1—P1—C21−166.2 (6)C21—P1—C31—C32−26.4 (11)
C2—Fe1—P1—C21−73.5 (6)B1—P1—C31—C32−147.9 (10)
C13—Fe1—P1—C2188.9 (6)Fe1—P1—C31—C3292.8 (10)
C15—Fe1—P1—C2137.4 (11)C21—P1—C31—C36157.2 (10)
C14—Fe1—P1—C21102.6 (7)B1—P1—C31—C3635.8 (11)
C12—Fe1—P1—C2150.2 (6)Fe1—P1—C31—C36−83.5 (9)
C11—Fe1—P1—C2120.0 (6)C36—C31—C32—C33−3.8 (17)
C1—Fe1—P1—B1−41.6 (7)P1—C31—C32—C33179.8 (10)
C2—Fe1—P1—B151.0 (7)C31—C32—C33—C343(2)
C13—Fe1—P1—B1−146.6 (7)C32—C33—C34—C35−1(2)
C15—Fe1—P1—B1161.9 (11)C33—C34—C35—C360(2)
C14—Fe1—P1—B1−132.9 (8)C34—C35—C36—C31−1(2)
C12—Fe1—P1—B1174.7 (7)C32—C31—C36—C353.1 (17)
C11—Fe1—P1—B1144.5 (7)P1—C31—C36—C35179.8 (10)
P1—B1—P2—C4159.4 (11)C51—P2—C41—C46−28.6 (13)
P1—B1—P2—C51−57.8 (11)B1—P2—C41—C46−149.3 (12)
P1—B1—P2—Fe2178.2 (8)Fe2—P2—C41—C4692.1 (12)
C3—Fe2—P2—C41171.4 (6)C51—P2—C41—C42151.7 (11)
C4—Fe2—P2—C4177.1 (6)B1—P2—C41—C4231.0 (12)
C62—Fe2—P2—C41−23.9 (6)Fe2—P2—C41—C42−87.6 (10)
C64—Fe2—P2—C41−84.8 (10)C46—C41—C42—C430.4 (19)
C63—Fe2—P2—C41−12.9 (8)P2—C41—C42—C43−179.9 (10)
C61—Fe2—P2—C41−60.5 (7)C41—C42—C43—C441(2)
C65—Fe2—P2—C41−92.7 (6)C42—C43—C44—C45−2(2)
C3—Fe2—P2—C51−72.5 (6)C43—C44—C45—C461(2)
C4—Fe2—P2—C51−166.8 (5)C44—C45—C46—C410(2)
C62—Fe2—P2—C5192.2 (5)C42—C41—C46—C45−1(2)
C64—Fe2—P2—C5131.4 (10)P2—C41—C46—C45179.5 (11)
C63—Fe2—P2—C51103.2 (8)C41—P2—C51—C56147.2 (11)
C61—Fe2—P2—C5155.6 (7)B1—P2—C51—C56−92.0 (11)
C65—Fe2—P2—C5123.4 (6)Fe2—P2—C51—C5629.3 (11)
C3—Fe2—P2—B150.6 (7)C41—P2—C51—C52−35.5 (11)
C4—Fe2—P2—B1−43.7 (6)B1—P2—C51—C5285.3 (11)
C62—Fe2—P2—B1−144.6 (6)Fe2—P2—C51—C52−153.4 (9)
C64—Fe2—P2—B1154.5 (10)C56—C51—C52—C53−0.2 (19)
C63—Fe2—P2—B1−133.7 (8)P2—C51—C52—C53−177.7 (11)
C61—Fe2—P2—B1178.7 (7)C51—C52—C53—C541(2)
C65—Fe2—P2—B1146.5 (7)C52—C53—C54—C550(2)
C1—Fe1—C11—C12−113.7 (12)C53—C54—C55—C56−1(2)
C2—Fe1—C11—C12145.6 (8)C52—C51—C56—C55−0.8 (18)
C13—Fe1—C11—C12−36.8 (8)P2—C51—C56—C55176.6 (10)
C15—Fe1—C11—C12−116.1 (12)C54—C55—C56—C511(2)
C14—Fe1—C11—C12−79.4 (9)C3—Fe2—C61—C62−155.8 (9)
P1—Fe1—C11—C1252.7 (9)C4—Fe2—C61—C6219.0 (13)
C1—Fe1—C11—C152.4 (15)C64—Fe2—C61—C62−81.4 (9)
C2—Fe1—C11—C15−98.3 (8)C63—Fe2—C61—C62−39.0 (9)
C13—Fe1—C11—C1579.2 (8)C65—Fe2—C61—C62−119.9 (13)
C14—Fe1—C11—C1536.6 (8)P2—Fe2—C61—C62110.4 (8)
C12—Fe1—C11—C15116.1 (12)C3—Fe2—C61—C65−35.9 (12)
P1—Fe1—C11—C15168.8 (7)C4—Fe2—C61—C65138.9 (10)
C15—C11—C12—C13−2.4 (15)C62—Fe2—C61—C65119.9 (13)
Fe1—C11—C12—C1358.3 (9)C64—Fe2—C61—C6538.5 (9)
C15—C11—C12—Fe1−60.7 (9)C63—Fe2—C61—C6580.9 (10)
C1—Fe1—C12—C11134.9 (10)P2—Fe2—C61—C65−129.7 (9)
C2—Fe1—C12—C11−42.7 (10)C65—C61—C62—C631.4 (16)
C13—Fe1—C12—C11120.4 (11)Fe2—C61—C62—C6361.7 (9)
C15—Fe1—C12—C1139.9 (8)C65—C61—C62—Fe2−60.4 (10)
C14—Fe1—C12—C1182.5 (9)C3—Fe2—C62—C6160.8 (17)
P1—Fe1—C12—C11−134.2 (8)C4—Fe2—C62—C61−167.1 (9)
C1—Fe1—C12—C1314.5 (12)C64—Fe2—C62—C6180.3 (9)
C2—Fe1—C12—C13−163.2 (8)C63—Fe2—C62—C61116.8 (12)
C15—Fe1—C12—C13−80.5 (8)C65—Fe2—C62—C6137.0 (9)
C14—Fe1—C12—C13−37.9 (8)P2—Fe2—C62—C61−73.9 (9)
C11—Fe1—C12—C13−120.4 (11)C3—Fe2—C62—C63−56.0 (17)
P1—Fe1—C12—C13105.4 (7)C4—Fe2—C62—C6376.1 (9)
C11—C12—C13—C143.4 (16)C64—Fe2—C62—C63−36.5 (8)
Fe1—C12—C13—C1462.7 (10)C61—Fe2—C62—C63−116.8 (12)
C11—C12—C13—Fe1−59.3 (10)C65—Fe2—C62—C63−79.8 (9)
C1—Fe1—C13—C1471.5 (10)P2—Fe2—C62—C63169.3 (8)
C2—Fe1—C13—C14−74.1 (17)C61—C62—C63—C64−1.9 (16)
C15—Fe1—C13—C14−36.4 (9)Fe2—C62—C63—C6460.3 (10)
C12—Fe1—C13—C14−117.3 (12)C61—C62—C63—Fe2−62.2 (9)
C11—Fe1—C13—C14−81.0 (9)C3—Fe2—C63—C6438.8 (11)
P1—Fe1—C13—C14165.0 (8)C4—Fe2—C63—C64133.6 (9)
C1—Fe1—C13—C12−171.2 (8)C62—Fe2—C63—C64−119.0 (12)
C2—Fe1—C13—C1243.2 (17)C61—Fe2—C63—C64−81.3 (9)
C15—Fe1—C13—C1281.0 (8)C65—Fe2—C63—C64−37.8 (8)
C14—Fe1—C13—C12117.3 (12)P2—Fe2—C63—C64−135.9 (8)
C11—Fe1—C13—C1236.3 (8)C3—Fe2—C63—C62157.8 (8)
P1—Fe1—C13—C12−77.7 (7)C4—Fe2—C63—C62−107.3 (8)
C12—C13—C14—C15−2.9 (17)C64—Fe2—C63—C62119.0 (12)
Fe1—C13—C14—C1559.5 (10)C61—Fe2—C63—C6237.8 (8)
C12—C13—C14—Fe1−62.4 (10)C65—Fe2—C63—C6281.2 (8)
C1—Fe1—C14—C15126.5 (9)P2—Fe2—C63—C62−16.9 (12)
C2—Fe1—C14—C1532.9 (12)C62—C63—C64—C651.7 (16)
C13—Fe1—C14—C15−120.1 (13)Fe2—C63—C64—C6561.5 (10)
C12—Fe1—C14—C15−81.5 (9)C62—C63—C64—Fe2−59.8 (10)
C11—Fe1—C14—C15−38.5 (8)C3—Fe2—C64—C63−149.3 (9)
P1—Fe1—C14—C15−141.9 (7)C4—Fe2—C64—C63−52.9 (10)
C1—Fe1—C14—C13−113.4 (9)C62—Fe2—C64—C6337.8 (8)
C2—Fe1—C14—C13153.0 (9)C61—Fe2—C64—C6380.2 (10)
C15—Fe1—C14—C13120.1 (13)C65—Fe2—C64—C63118.6 (13)
C12—Fe1—C14—C1338.6 (9)P2—Fe2—C64—C63107.0 (11)
C11—Fe1—C14—C1381.5 (9)C3—Fe2—C64—C6592.1 (9)
P1—Fe1—C14—C13−21.9 (12)C4—Fe2—C64—C65−171.4 (8)
C13—C14—C15—C111.4 (16)C62—Fe2—C64—C65−80.8 (9)
Fe1—C14—C15—C1160.1 (9)C63—Fe2—C64—C65−118.6 (13)
C13—C14—C15—Fe1−58.7 (10)C61—Fe2—C64—C65−38.4 (9)
C12—C11—C15—C140.7 (15)P2—Fe2—C64—C65−11.5 (15)
Fe1—C11—C15—C14−60.7 (10)C62—C61—C65—C64−0.3 (15)
C12—C11—C15—Fe161.4 (9)Fe2—C61—C65—C64−60.3 (9)
C1—Fe1—C15—C14−60.1 (9)C62—C61—C65—Fe260.0 (10)
C2—Fe1—C15—C14−155.9 (8)C63—C64—C65—C61−0.9 (15)
C13—Fe1—C15—C1436.7 (8)Fe2—C64—C65—C6160.6 (9)
C12—Fe1—C15—C1480.4 (9)C63—C64—C65—Fe2−61.5 (10)
C11—Fe1—C15—C14118.8 (11)C3—Fe2—C65—C61152.4 (10)
P1—Fe1—C15—C1494.4 (12)C4—Fe2—C65—C61−99.4 (15)
C1—Fe1—C15—C11−178.8 (7)C62—Fe2—C65—C61−36.2 (9)
C2—Fe1—C15—C1185.3 (8)C64—Fe2—C65—C61−116.9 (13)
C13—Fe1—C15—C11−82.1 (8)C63—Fe2—C65—C61−80.1 (10)
C14—Fe1—C15—C11−118.8 (11)P2—Fe2—C65—C6157.4 (10)
C12—Fe1—C15—C11−38.4 (7)C3—Fe2—C65—C64−90.7 (9)
P1—Fe1—C15—C11−24.4 (14)C4—Fe2—C65—C6417.5 (17)
C31—P1—C21—C22145.8 (11)C62—Fe2—C65—C6480.7 (9)
B1—P1—C21—C22−94.3 (12)C63—Fe2—C65—C6436.8 (9)
Fe1—P1—C21—C2228.2 (12)C61—Fe2—C65—C64116.9 (13)
C31—P1—C21—C26−39.0 (10)P2—Fe2—C65—C64174.3 (7)

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: BQ2081).

References

  • Blessing, R. H. (1995). Acta Cryst. A51, 33–38. [PubMed]
  • Kückmann, T. I., Dornhaus, F., Bolte, M., Lerner, H.-W., Holthausen, M. C. & Wagner, M. (2007). Eur. J. Inorg. Chem. pp. 1989–2003.
  • Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. [PubMed]
  • Spek, A. L. (2003). J. Appl. Cryst.36, 7–13.
  • Stoe & Cie (2001). X-AREA Stoe & Cie, Darmstadt, Germany.

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