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metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890
Volume 68| Part 8| August 2012| Page m1077
https://doi.org/10.1107/S1600536812031649

Dicarbon­yl(η5-cyclo­penta­dien­yl)(hexa­methyl­ene­tetra­mine-κN1)iron(II) tetra­fluoridoborate

Cyprian M. M'thiruaine,a Holger B. Friedricha and Bernard Omondia*

aSchool of Chemistry, University of KwaZulu-Natal, Private Bag X54001, Durban 4000, South Africa
*Correspondence e-mail: owaga@ukzn.ac.za

(Received 19 June 2012; accepted 11 July 2012; online 18 July 2012)

In the structure of the title compound, [Fe(C5H5)(C6H12N4)(CO)2]BF4, the arrangement around the FeII atom corresponds to that of a three-legged piano stool. The cyclo­penta­dienyl ligand occupies three coordination sites of the apical position in a η5 fashion, while two CO ligands and one N atom of the hexa­methyl­ene­tetra­mine ligand occupy the remaining coordination sites to complete a distorted octa­hedral geometry. The asymmetric unit consists of two sets of crystallographically independent cations and anions with the r.m.s. deviations of the overlay of non-H atoms of each pair being 0.081 and 0.120 Å, respectively. The Fe—N bond lengths are 2.0459 (15) and 2.0490 (14) Å, while the Fe—Cp(centroid) distances are 1.7257 (3) and 1.7246 (3) Å. One of the anions displays disorder, with the F atoms having occupancies of 0.58 (4) and 0.42 (4).

Related literature

For the synthesis of the title compound and structure of the dinuclear compound [Fe2(η5-C5H5)2(C6H12N4)(CO)4](BF4)2, see: M'thiruaine, Friedrich, Changamu & Bala (2012[M'thiruaine, C. M., Friedrich, H. B., Changamu, E. O. & Bala, M. D. (2012). Inorg. Chim. Acta, 390, 83-94.]). For other related compounds, see: Matos & Verkade (2003[Matos, R. M. & Verkade, J. G. (2003). J. Braz. Chem. Soc. 14, 71-75.]); M'thiruaine, Friedrich, Changamu & Fernandes (2012[M'thiruaine, C. M., Friedrich, H. B., Changamu, E. O. & Fernandes, M. A. (2012). Acta Cryst. E68, m931.]); M'thiruaine et al. (2011[M'thiruaine, C. M., Friedrich, H. B., Changamu, E. O. & Bala, M. D. (2011). Inorg. Chim. Acta, 366, 105-115.]).

[Scheme 1]

Experimental

Crystal data

  • [Fe(C5H5)(C6H12N4)(CO)2]BF4

  • Mr = 403.97

  • Monoclinic, P 21 /c

  • a = 15.1054 (6) Å

  • b = 14.6407 (6) Å

  • c = 14.2267 (6) Å

  • β = 96.997 (2)°

  • V = 3122.9 (2) Å3

  • Z = 8

  • Mo Kα radiation

  • μ = 1.03 mm−1

  • T = 173 K

  • 0.42 × 0.19 × 0.16 mm
Data collection

  • Bruker SMART APEXII CCD diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2008[Bruker (2008). APEX2, SAINT-Plus, XPREP and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.673, Tmax = 0.853

  • 62504 measured reflections

  • 7768 independent reflections

  • 6765 reflections with I > 2σ(I)

  • Rint = 0.033
Refinement

  • R[F2 > 2σ(F2)] = 0.034

  • wR(F2) = 0.092

  • S = 1.08

  • 7768 reflections

  • 488 parameters

  • 12 restraints

  • H-atom parameters constrained

  • Δρmax = 0.63 e Å−3

  • Δρmin = −0.43 e Å−3

Data collection: APEX2 (Bruker, 2008[Bruker (2008). APEX2, SAINT-Plus, XPREP and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT-Plus (Bruker, 2008[Bruker (2008). APEX2, SAINT-Plus, XPREP and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT-Plus and XPREP (Bruker, 2008[Bruker (2008). APEX2, SAINT-Plus, XPREP and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: ORTEP-3 (Farrugia, 1997[Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565.]); software used to prepare material for publication: WinGX (Farrugia, 1999[Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838.]).

Supporting information

Crystal structure: contains datablocks global, I. DOI: https://doi.org/10.1107/S1600536812031649/kj2206sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536812031649/kj2206Isup2.hkl

checkCIF report


Comment top

The title compound was obtained as part of our ongoing investigation of the reactions of substitutionally unsaturated metal complexes with nitrogen donor ligands. The synthesis and characterization data was previously reported by us. (M'thiruaine et al., 2011; M'thiruaine, Friedrich, Changamu & Fernandes, 2012). The asymmetric unit consists of two independent molecules of [Fe(η5-C5H5){N4(CH2)6}(CO)2]+ and two molecules of BF4-. The structure exhibits a typical three legged piano stool structure with FeII coordinated by one nitrogen atom of the hexamethylenetetramine ligand and two of the CO ligands. The coordination geometry around Fe is that of the distorted octahedral in which three sites are occupied by the η5-cyclopentadienyl ligand, two by the CO ligands and one by an N atom of the hexamethylenetetramine. Its structure is closely similar to that of recently reported pentamethylcyclopentadienyl analogue compound [Fe{η5-C5(CH3)5}{N4(CH2)6}(CO)2]BF4 (M'thiruaine, Friedrich, Changamu & Fernandes, 2012). One of the anions displays disorder with the fluorine atoms having occupancies of 0.58 (4) for F1A, F2A, F3A and F4A, and 0.42 (4) for F1B, F2B, F3B and F4B.

The asymmetric unit consist of two sets of crystallographically independent molecules of the cations [r.m.s = 0.081 Å] and anions [r.m.s. = 0.120 Å]. The cations are related by a non-crystallographic translation across the ac diagonal. The Fe—N bonds distances are 2.0458 (15) and 2.0489 (14) Å, which are slightly shorter than the correspomding distances of the Cp* analogue (M'thiruaine, Friedrich, Changamu & Fernandes, 2012) (2.069 (2) Å) and of the dinuclear complex [{Cp(CO)2Fe}2{N4(CH2)6}]2+ (M'thiruaine, Friedrich, Changamu & Bala, 2012) (2.0817 (17) and 2.0858 (18) Å) as well as that of [(CO)4Fe{N2(CH2)6}] (Matos and Verkade, 2003) (2.092 (4) Å).

Related literature top

For the synthesis of the title compound and structure of the dinuclear compound [Fe2(η5-C5H5)2{N4(CH2)6}(CO)4](BF4)2, see: M'thiruaine, Friedrich, Changamu & Bala (2012). For other related compounds, see: Matos & Verkade (2003); M'thiruaine, Friedrich, Changamu & Fernandes (2012); M'thiruaine et al. (2011).

Experimental top

The title compound was prepared according to a reported procedure (M'thiruaine, Friedrich, Changamu & Bala, 2012) and crystals were grown by layering a concentrated solution of the compound in acetone with Et2O and the mixture kept undisturbed in the dark for four weeks.

Refinement top

Carbon-bound H-atoms were placed in calculated positions [C—H = 0.97 Å for for methylene H atoms and 0.98 for methine H atoms; Uiso(H) = 1.2Ueq(C)] and were included in the refinement in the riding model approximation. One of the tetrafluoroborate anions was refined with a disorder model. The total occupancy of each atom was constrained to 1; the occupancy for sites F1A, F2A, F3A and F4A was 0.58 (4) and 0.42 (4) for F1B, F2B, F3B and F4B. F4A and F4B were refined with restraints to prevent extreme anisotropy. One reflection (1 0 0) was omited from the hkl file.

Structure description top

The title compound was obtained as part of our ongoing investigation of the reactions of substitutionally unsaturated metal complexes with nitrogen donor ligands. The synthesis and characterization data was previously reported by us. (M'thiruaine et al., 2011; M'thiruaine, Friedrich, Changamu & Fernandes, 2012). The asymmetric unit consists of two independent molecules of [Fe(η5-C5H5){N4(CH2)6}(CO)2]+ and two molecules of BF4-. The structure exhibits a typical three legged piano stool structure with FeII coordinated by one nitrogen atom of the hexamethylenetetramine ligand and two of the CO ligands. The coordination geometry around Fe is that of the distorted octahedral in which three sites are occupied by the η5-cyclopentadienyl ligand, two by the CO ligands and one by an N atom of the hexamethylenetetramine. Its structure is closely similar to that of recently reported pentamethylcyclopentadienyl analogue compound [Fe{η5-C5(CH3)5}{N4(CH2)6}(CO)2]BF4 (M'thiruaine, Friedrich, Changamu & Fernandes, 2012). One of the anions displays disorder with the fluorine atoms having occupancies of 0.58 (4) for F1A, F2A, F3A and F4A, and 0.42 (4) for F1B, F2B, F3B and F4B.

The asymmetric unit consist of two sets of crystallographically independent molecules of the cations [r.m.s = 0.081 Å] and anions [r.m.s. = 0.120 Å]. The cations are related by a non-crystallographic translation across the ac diagonal. The Fe—N bonds distances are 2.0458 (15) and 2.0489 (14) Å, which are slightly shorter than the correspomding distances of the Cp* analogue (M'thiruaine, Friedrich, Changamu & Fernandes, 2012) (2.069 (2) Å) and of the dinuclear complex [{Cp(CO)2Fe}2{N4(CH2)6}]2+ (M'thiruaine, Friedrich, Changamu & Bala, 2012) (2.0817 (17) and 2.0858 (18) Å) as well as that of [(CO)4Fe{N2(CH2)6}] (Matos and Verkade, 2003) (2.092 (4) Å).

For the synthesis of the title compound and structure of the dinuclear compound [Fe2(η5-C5H5)2{N4(CH2)6}(CO)4](BF4)2, see: M'thiruaine, Friedrich, Changamu & Bala (2012). For other related compounds, see: Matos & Verkade (2003); M'thiruaine, Friedrich, Changamu & Fernandes (2012); M'thiruaine et al. (2011).

Computing details top

Data collection: APEX2 (Bruker, 2008); cell refinement: SAINT-Plus (Bruker, 2008); data reduction: SAINT-Plus and XPREP (Bruker, 2008); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).

Figures top
[Figure 1] Fig. 1. Fig. 1: Molecular structure of the title complex with the atom labeling scheme. Ellipsoids are drawn at 50% probability level.
Dicarbonyl(η5-cyclopentadienyl)(hexamethylenetetramine- κN1)iron(II) tetrafluoridoborate top
Crystal data top
[Fe(C5H5)(C6H12N4)(CO)2]BF4F(000) = 1648
Mr = 403.97Dx = 1.718 Mg m−3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 63978 reflections
a = 15.1054 (6) Åθ = 1.9–28.3°
b = 14.6407 (6) ŵ = 1.03 mm−1
c = 14.2267 (6) ÅT = 173 K
β = 96.997 (2)°Block, yellow
V = 3122.9 (2) Å30.42 × 0.19 × 0.16 mm
Z = 8
Data collection top
Bruker SMART APEXII CCD
diffractometer		6765 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.033
φ and ω scansθmax = 28.3°, θmin = 1.9°
Absorption correction: multi-scan
(SADABS; Bruker, 2008)		h = −20→20
Tmin = 0.673, Tmax = 0.853k = −19→19
62504 measured reflectionsl = −18→18
7768 independent reflections
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)] = 0.034Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.092H-atom parameters constrained
S = 1.08 w = 1/[σ2(Fo2) + (0.0391P)2 + 2.9672P]
where P = (Fo2 + 2Fc2)/3
7768 reflections(Δ/σ)max = 0.026
488 parametersΔρmax = 0.63 e Å−3
12 restraintsΔρmin = −0.43 e Å−3
Crystal data top
[Fe(C5H5)(C6H12N4)(CO)2]BF4V = 3122.9 (2) Å3
Mr = 403.97Z = 8
Monoclinic, P21/cMo Kα radiation
a = 15.1054 (6) ŵ = 1.03 mm−1
b = 14.6407 (6) ÅT = 173 K
c = 14.2267 (6) Å0.42 × 0.19 × 0.16 mm
β = 96.997 (2)°
Data collection top
Bruker SMART APEXII CCD
diffractometer		7768 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2008)		6765 reflections with I > 2σ(I)
Tmin = 0.673, Tmax = 0.853Rint = 0.033
62504 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.03412 restraints
wR(F2) = 0.092H-atom parameters constrained
S = 1.08Δρmax = 0.63 e Å−3
7768 reflectionsΔρmin = −0.43 e Å−3
488 parameters
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*/UeqOcc. (<1)
C10.86930 (13)−0.03952 (15)0.80821 (16)0.0275 (4)
H10.8674−0.10070.83930.033*
C20.87149 (14)0.04629 (15)0.85391 (15)0.0292 (4)
H20.87230.05630.92350.035*
C30.87061 (14)0.11633 (15)0.78406 (17)0.0323 (5)
H30.87090.18370.79570.039*
C40.86568 (13)0.07273 (17)0.69515 (16)0.0339 (5)
H40.86390.10440.63270.041*
C50.86628 (13)−0.02251 (17)0.70865 (16)0.0320 (5)
H50.863−0.06990.65770.038*
C61.04710 (15)0.07326 (13)0.88830 (14)0.0270 (4)
C71.04138 (12)−0.07593 (12)0.78590 (13)0.0204 (4)
C81.16153 (11)0.07250 (12)0.72516 (14)0.0199 (4)
H8A1.17680.09810.78950.024*
H8B1.17230.00580.72890.024*
C91.19672 (12)0.07558 (13)0.56646 (14)0.0235 (4)
H9A1.20720.00880.56780.028*
H9B1.23620.10320.52350.028*
C101.08860 (12)0.19357 (13)0.52845 (13)0.0214 (4)
H10A1.12650.22220.48460.026*
H10B1.02560.20680.50470.026*
C111.05207 (13)0.19222 (12)0.68625 (13)0.0200 (4)
H11A0.98920.20660.66270.024*
H11B1.06540.2190.75030.024*
C121.04575 (12)0.05226 (12)0.59314 (12)0.0189 (3)
H12A1.0556−0.01460.59470.023*
H12B0.98260.06340.56830.023*
C131.20368 (13)0.21211 (12)0.65816 (15)0.0241 (4)
H13A1.24310.24050.61560.029*
H13B1.2190.23840.72220.029*
C140.35418 (12)0.09213 (13)0.27619 (14)0.0213 (4)
H140.34910.15980.28350.026*
C150.35489 (12)0.02563 (13)0.34992 (14)0.0219 (4)
H150.34970.03870.4180.026*
C160.36150 (12)−0.06169 (13)0.30960 (14)0.0226 (4)
H160.3617−0.12130.3440.027*
C170.36425 (12)−0.05030 (14)0.21025 (14)0.0237 (4)
H170.3679−0.10030.1630.028*
C180.35832 (12)0.04445 (14)0.19039 (14)0.0224 (4)
H180.35880.0730.12660.027*
C190.52488 (12)0.07220 (13)0.39393 (13)0.0210 (4)
C200.53847 (12)−0.08684 (12)0.31050 (13)0.0192 (3)
C210.54333 (12)0.17549 (11)0.19492 (13)0.0170 (3)
H21A0.48110.18760.16720.02*
H21B0.55220.20340.25880.02*
C220.69695 (12)0.19948 (12)0.17685 (14)0.0212 (4)
H22A0.73830.22890.13710.025*
H22B0.70760.22660.2410.025*
C230.69925 (12)0.06230 (13)0.08670 (14)0.0216 (4)
H23A0.7117−0.00410.08940.026*
H23B0.74050.09090.04630.026*
C240.54675 (12)0.03453 (12)0.10393 (12)0.0177 (3)
H24A0.5587−0.0320.1070.021*
H24B0.48430.04340.07510.021*
C250.65477 (11)0.05894 (12)0.24201 (13)0.0182 (3)
H25A0.66590.0850.30660.022*
H25B0.6671−0.00740.24670.022*
C260.58916 (13)0.17684 (12)0.04086 (13)0.0210 (4)
H26A0.62890.2065−0.00040.025*
H26B0.52680.18790.01310.025*
B10.32781 (15)0.21448 (14)0.93390 (14)0.0203 (4)
B21.18854 (14)−0.20775 (13)0.54535 (13)0.0169 (4)
N11.06343 (9)0.08967 (10)0.69277 (10)0.0151 (3)
N21.11003 (11)0.23350 (10)0.62362 (11)0.0209 (3)
N31.21930 (10)0.11287 (11)0.66204 (12)0.0222 (3)
N41.10294 (10)0.09386 (11)0.52956 (11)0.0201 (3)
N50.55772 (9)0.07343 (9)0.20366 (10)0.0145 (3)
N60.60404 (10)0.21776 (10)0.13595 (11)0.0189 (3)
N70.71550 (10)0.10091 (10)0.18284 (11)0.0197 (3)
N80.60659 (10)0.07755 (10)0.04412 (11)0.0193 (3)
O11.08297 (13)0.09476 (12)0.95985 (11)0.0436 (4)
O21.07359 (9)−0.14597 (9)0.79173 (12)0.0314 (3)
O30.55295 (10)0.10444 (11)0.46397 (10)0.0318 (3)
O40.57492 (9)−0.15342 (9)0.32834 (11)0.0265 (3)
F1A0.2452 (6)0.2217 (16)0.8959 (7)0.071 (3)0.58 (4)
F2A0.3595 (6)0.3019 (6)0.9694 (4)0.0415 (16)0.58 (4)
F3A0.313 (2)0.1541 (5)0.9998 (6)0.073 (4)0.58 (4)
F4A0.3667 (12)0.1825 (12)0.8619 (12)0.056 (3)0.58 (4)
F1B0.2404 (8)0.2517 (10)0.8923 (7)0.045 (2)0.42 (4)
F2B0.3690 (8)0.2897 (11)0.9743 (7)0.065 (3)0.42 (4)
F3B0.3532 (9)0.1541 (7)1.0064 (8)0.0482 (19)0.42 (4)
F4B0.3880 (12)0.1945 (13)0.8637 (15)0.040 (2)0.42 (4)
F51.23942 (12)−0.14457 (10)0.50207 (12)0.0563 (4)
F61.13743 (11)−0.16773 (11)0.60532 (11)0.0495 (4)
F71.24900 (10)−0.26959 (10)0.59476 (9)0.0434 (4)
F81.13740 (10)−0.25675 (15)0.47543 (13)0.0673 (6)
Fe10.983683 (17)0.031636 (17)0.782706 (18)0.01738 (7)
Fe20.473433 (16)0.015894 (16)0.289440 (17)0.01452 (7)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.0159 (9)0.0308 (10)0.0367 (11)0.0006 (7)0.0069 (8)0.0042 (8)
C20.0257 (10)0.0341 (11)0.0306 (11)0.0085 (8)0.0141 (8)0.0059 (8)
C30.0240 (10)0.0317 (11)0.0442 (12)0.0125 (8)0.0162 (9)0.0123 (9)
C40.0137 (9)0.0554 (14)0.0330 (11)0.0105 (9)0.0052 (8)0.0164 (10)
C50.0116 (8)0.0503 (13)0.0339 (11)−0.0003 (8)0.0016 (8)−0.0037 (10)
C60.0370 (11)0.0218 (9)0.0228 (10)−0.0029 (8)0.0054 (8)0.0008 (7)
C70.0140 (8)0.0209 (9)0.0266 (9)−0.0040 (7)0.0033 (7)0.0007 (7)
C80.0122 (8)0.0188 (8)0.0273 (9)−0.0004 (6)−0.0028 (7)0.0041 (7)
C90.0171 (9)0.0209 (9)0.0341 (10)0.0003 (7)0.0094 (8)−0.0011 (7)
C100.0193 (9)0.0230 (9)0.0215 (9)0.0006 (7)0.0009 (7)0.0033 (7)
C110.0255 (9)0.0126 (8)0.0221 (9)0.0045 (7)0.0036 (7)0.0003 (6)
C120.0169 (8)0.0205 (8)0.0194 (8)−0.0031 (7)0.0028 (7)−0.0050 (7)
C130.0223 (9)0.0172 (8)0.0312 (10)−0.0060 (7)−0.0027 (8)0.0019 (7)
C140.0136 (8)0.0208 (9)0.0298 (10)0.0041 (7)0.0032 (7)0.0024 (7)
C150.0153 (8)0.0264 (9)0.0251 (9)0.0025 (7)0.0062 (7)0.0012 (7)
C160.0131 (8)0.0205 (9)0.0344 (10)−0.0022 (7)0.0035 (7)0.0038 (7)
C170.0136 (8)0.0263 (9)0.0305 (10)−0.0030 (7)0.0001 (7)−0.0068 (8)
C180.0122 (8)0.0312 (10)0.0233 (9)−0.0005 (7)0.0002 (7)0.0038 (7)
C190.0187 (9)0.0212 (9)0.0235 (9)−0.0013 (7)0.0037 (7)0.0003 (7)
C200.0156 (8)0.0183 (8)0.0241 (9)−0.0049 (7)0.0043 (7)0.0010 (7)
C210.0184 (8)0.0106 (7)0.0221 (9)0.0006 (6)0.0022 (7)0.0001 (6)
C220.0180 (9)0.0172 (8)0.0278 (9)−0.0060 (7)0.0002 (7)0.0013 (7)
C230.0161 (8)0.0208 (9)0.0290 (10)−0.0001 (7)0.0064 (7)0.0004 (7)
C240.0170 (8)0.0172 (8)0.0193 (8)−0.0036 (6)0.0035 (7)−0.0049 (6)
C250.0123 (8)0.0177 (8)0.0239 (9)−0.0005 (6)−0.0004 (7)0.0043 (7)
C260.0208 (9)0.0207 (9)0.0215 (9)−0.0014 (7)0.0023 (7)0.0043 (7)
B10.0285 (11)0.0201 (10)0.0119 (9)0.0064 (8)0.0009 (8)−0.0050 (7)
B20.0206 (10)0.0182 (9)0.0112 (8)0.0048 (7)−0.0012 (7)−0.0018 (7)
N10.0135 (7)0.0133 (6)0.0181 (7)0.0017 (5)0.0003 (5)−0.0015 (5)
N20.0240 (8)0.0148 (7)0.0235 (8)0.0009 (6)0.0010 (6)0.0012 (6)
N30.0146 (7)0.0182 (7)0.0331 (9)−0.0017 (6)0.0004 (6)0.0046 (6)
N40.0180 (7)0.0211 (7)0.0220 (8)−0.0030 (6)0.0054 (6)−0.0028 (6)
N50.0130 (7)0.0109 (6)0.0191 (7)−0.0001 (5)0.0000 (5)−0.0006 (5)
N60.0186 (7)0.0141 (7)0.0238 (8)−0.0017 (5)0.0018 (6)0.0025 (6)
N70.0138 (7)0.0178 (7)0.0274 (8)−0.0021 (6)0.0015 (6)0.0040 (6)
N80.0167 (7)0.0201 (7)0.0216 (8)−0.0026 (6)0.0040 (6)−0.0012 (6)
O10.0653 (12)0.0411 (9)0.0227 (8)−0.0158 (8)−0.0016 (8)−0.0032 (7)
O20.0222 (7)0.0177 (7)0.0560 (10)0.0011 (5)0.0115 (7)0.0059 (6)
O30.0325 (8)0.0376 (8)0.0243 (7)−0.0066 (7)−0.0001 (6)−0.0066 (6)
O40.0189 (7)0.0173 (6)0.0435 (8)0.0020 (5)0.0049 (6)0.0076 (6)
F1A0.035 (2)0.126 (9)0.051 (3)−0.004 (4)−0.005 (2)−0.042 (4)
F2A0.074 (4)0.0210 (19)0.035 (2)−0.0067 (18)0.028 (3)−0.0028 (14)
F3A0.154 (12)0.0319 (18)0.038 (2)0.012 (4)0.026 (5)0.0130 (15)
F4A0.069 (6)0.059 (5)0.040 (3)0.034 (4)0.010 (4)−0.005 (3)
F1B0.039 (3)0.074 (5)0.024 (3)0.009 (3)0.015 (2)0.008 (4)
F2B0.055 (4)0.049 (5)0.081 (6)−0.009 (3)−0.031 (5)−0.014 (3)
F3B0.066 (5)0.038 (2)0.042 (3)0.016 (3)0.012 (3)0.022 (2)
F4B0.050 (5)0.040 (3)0.034 (4)0.021 (3)0.023 (4)0.001 (3)
F50.0730 (12)0.0375 (8)0.0622 (10)0.0071 (8)0.0233 (9)0.0146 (7)
F60.0527 (9)0.0541 (9)0.0432 (8)0.0255 (7)0.0116 (7)−0.0125 (7)
F70.0462 (8)0.0527 (9)0.0333 (7)0.0256 (7)0.0121 (6)0.0164 (6)
F80.0338 (8)0.1018 (15)0.0636 (11)0.0017 (9)−0.0049 (7)−0.0475 (10)
Fe10.01647 (13)0.01728 (13)0.01851 (13)0.00332 (9)0.00265 (10)0.00090 (9)
Fe20.01275 (12)0.01259 (12)0.01814 (13)0.00006 (8)0.00148 (9)−0.00002 (9)
Geometric parameters (Å, º) top
C1—C21.413 (3)C16—C171.429 (3)
C1—C51.433 (3)C16—Fe22.0855 (18)
C1—Fe12.087 (2)C16—H161
C1—H11C17—C181.416 (3)
C2—C31.427 (3)C17—Fe22.1157 (18)
C2—Fe12.0887 (19)C17—H171
C2—H21C18—Fe22.1418 (18)
C3—C41.411 (3)C18—H181
C3—Fe12.113 (2)C19—O31.137 (2)
C3—H31C19—Fe21.7921 (19)
C4—C51.408 (3)C20—O41.133 (2)
C4—Fe12.133 (2)C20—Fe21.8016 (18)
C4—H41C21—N61.454 (2)
C5—Fe12.104 (2)C21—N51.513 (2)
C5—H51C21—H21A0.99
C6—O11.138 (3)C21—H21B0.99
C6—Fe11.788 (2)C22—N71.471 (2)
C7—O21.134 (2)C22—N61.477 (2)
C7—Fe11.7978 (19)C22—H22A0.99
C8—N31.452 (2)C22—H22B0.99
C8—N11.518 (2)C23—N71.473 (2)
C8—H8A0.99C23—N81.473 (2)
C8—H8B0.99C23—H23A0.99
C9—N31.466 (3)C23—H23B0.99
C9—N41.474 (2)C24—N81.458 (2)
C9—H9A0.99C24—N51.519 (2)
C9—H9B0.99C24—H24A0.99
C10—N21.474 (2)C24—H24B0.99
C10—N41.476 (2)C25—N71.455 (2)
C10—H10A0.99C25—N51.516 (2)
C10—H10B0.99C25—H25A0.99
C11—N21.454 (2)C25—H25B0.99
C11—N11.513 (2)C26—N61.471 (2)
C11—H11A0.99C26—N81.477 (2)
C11—H11B0.99C26—H26A0.99
C12—N41.458 (2)C26—H26B0.99
C12—N11.513 (2)B1—F1A1.303 (11)
C12—H12A0.99B1—F3A1.328 (8)
C12—H12B0.99B1—F4A1.326 (16)
C13—N31.472 (2)B1—F2B1.357 (11)
C13—N21.474 (2)B1—F3B1.377 (10)
C13—H13A0.99B1—F2A1.436 (7)
C13—H13B0.99B1—F4B1.460 (17)
C14—C181.414 (3)B1—F1B1.483 (12)
C14—C151.430 (3)B2—F61.352 (2)
C14—Fe22.1079 (18)B2—F81.383 (2)
C14—H141B2—F51.393 (3)
C15—C161.410 (3)B2—F71.411 (2)
C15—Fe22.0838 (18)N1—Fe12.0459 (15)
C15—H151N5—Fe22.0490 (14)
C2—C1—C5107.24 (19)N5—C25—H25A109.1
C2—C1—Fe170.29 (12)N7—C25—H25B109.1
C5—C1—Fe170.66 (12)N5—C25—H25B109.1
C2—C1—H1126.4H25A—C25—H25B107.8
C5—C1—H1126.4N6—C26—N8111.42 (14)
Fe1—C1—H1126.4N6—C26—H26A109.3
C1—C2—C3108.7 (2)N8—C26—H26A109.3
C1—C2—Fe170.15 (11)N6—C26—H26B109.3
C3—C2—Fe171.05 (11)N8—C26—H26B109.3
C1—C2—H2125.6H26A—C26—H26B108
C3—C2—H2125.6F1A—B1—F3A96 (2)
Fe1—C2—H2125.6F1A—B1—F4A101.6 (9)
C4—C3—C2107.1 (2)F3A—B1—F4A116.1 (7)
C4—C3—Fe171.38 (12)F1A—B1—F2B118.5 (8)
C2—C3—Fe169.24 (11)F3A—B1—F2B110.5 (10)
C4—C3—H3126.4F4A—B1—F2B112.9 (11)
C2—C3—H3126.4F1A—B1—F3B121.9 (14)
Fe1—C3—H3126.4F4A—B1—F3B104.0 (8)
C5—C4—C3109.10 (19)F2B—B1—F3B97.6 (10)
C5—C4—Fe169.50 (12)F1A—B1—F2A109.6 (8)
C3—C4—Fe169.81 (12)F3A—B1—F2A115.0 (6)
C5—C4—H4125.4F4A—B1—F2A115.2 (10)
C3—C4—H4125.4F3B—B1—F2A105.0 (7)
Fe1—C4—H4125.4F1A—B1—F4B112.2 (9)
C4—C5—C1107.8 (2)F3A—B1—F4B121.6 (11)
C4—C5—Fe171.71 (13)F2B—B1—F4B99.2 (10)
C1—C5—Fe169.35 (12)F3B—B1—F4B104.1 (10)
C4—C5—H5126.1F2A—B1—F4B102.2 (8)
C1—C5—H5126.1F3A—B1—F1B107.8 (14)
Fe1—C5—H5126.1F4A—B1—F1B106.2 (9)
O1—C6—Fe1173.88 (19)F2B—B1—F1B102.2 (7)
O2—C7—Fe1175.25 (17)F3B—B1—F1B133.4 (8)
N3—C8—N1112.50 (14)F2A—B1—F1B93.2 (6)
N3—C8—H8A109.1F4B—B1—F1B113.5 (10)
N1—C8—H8A109.1F6—B2—F8111.51 (17)
N3—C8—H8B109.1F6—B2—F5112.30 (17)
N1—C8—H8B109.1F8—B2—F5108.44 (17)
H8A—C8—H8B107.8F6—B2—F7110.39 (15)
N3—C9—N4111.56 (14)F8—B2—F7107.23 (17)
N3—C9—H9A109.3F5—B2—F7106.73 (16)
N4—C9—H9A109.3C12—N1—C11107.23 (13)
N3—C9—H9B109.3C12—N1—C8106.19 (13)
N4—C9—H9B109.3C11—N1—C8106.39 (13)
H9A—C9—H9B108C12—N1—Fe1112.67 (10)
N2—C10—N4111.52 (15)C11—N1—Fe1112.30 (10)
N2—C10—H10A109.3C8—N1—Fe1111.63 (10)
N4—C10—H10A109.3C11—N2—C13109.43 (15)
N2—C10—H10B109.3C11—N2—C10108.47 (14)
N4—C10—H10B109.3C13—N2—C10108.45 (15)
H10A—C10—H10B108C8—N3—C9109.42 (14)
N2—C11—N1112.18 (14)C8—N3—C13108.63 (15)
N2—C11—H11A109.2C9—N3—C13108.34 (15)
N1—C11—H11A109.2C12—N4—C9108.63 (15)
N2—C11—H11B109.2C12—N4—C10108.82 (14)
N1—C11—H11B109.2C9—N4—C10108.48 (14)
H11A—C11—H11B107.9C21—N5—C25106.91 (13)
N4—C12—N1112.32 (14)C21—N5—C24107.17 (13)
N4—C12—H12A109.1C25—N5—C24105.93 (13)
N1—C12—H12A109.1C21—N5—Fe2111.19 (10)
N4—C12—H12B109.1C25—N5—Fe2111.84 (10)
N1—C12—H12B109.1C24—N5—Fe2113.40 (10)
H12A—C12—H12B107.9C21—N6—C26108.70 (14)
N3—C13—N2111.41 (15)C21—N6—C22109.35 (14)
N3—C13—H13A109.3C26—N6—C22108.65 (14)
N2—C13—H13A109.3C25—N7—C22108.59 (14)
N3—C13—H13B109.3C25—N7—C23109.26 (14)
N2—C13—H13B109.3C22—N7—C23108.29 (14)
H13A—C13—H13B108C24—N8—C23108.68 (14)
C18—C14—C15107.45 (17)C24—N8—C26108.82 (14)
C18—C14—Fe271.86 (10)C23—N8—C26108.60 (14)
C15—C14—Fe269.15 (10)C6—Fe1—C793.95 (9)
C18—C14—H14126.3C6—Fe1—N195.05 (8)
C15—C14—H14126.3C7—Fe1—N193.38 (7)
Fe2—C14—H14126.3C6—Fe1—C1113.22 (9)
C16—C15—C14108.27 (17)C7—Fe1—C188.13 (8)
C16—C15—Fe270.30 (10)N1—Fe1—C1151.53 (7)
C14—C15—Fe270.96 (10)C6—Fe1—C286.60 (9)
C16—C15—H15125.9C7—Fe1—C2119.82 (8)
C14—C15—H15125.9N1—Fe1—C2146.62 (7)
Fe2—C15—H15125.9C1—Fe1—C239.56 (8)
C15—C16—C17107.98 (17)C6—Fe1—C5151.87 (9)
C15—C16—Fe270.17 (10)C7—Fe1—C593.38 (9)
C17—C16—Fe271.26 (10)N1—Fe1—C5111.58 (7)
C15—C16—H16126C1—Fe1—C539.99 (8)
C17—C16—H16126C2—Fe1—C566.26 (9)
Fe2—C16—H16126C6—Fe1—C398.24 (10)
C18—C17—C16107.63 (17)C7—Fe1—C3154.68 (8)
C18—C17—Fe271.57 (11)N1—Fe1—C3107.47 (7)
C16—C17—Fe268.98 (10)C1—Fe1—C366.67 (8)
C18—C17—H17126.2C2—Fe1—C339.71 (8)
C16—C17—H17126.2C5—Fe1—C365.97 (9)
Fe2—C17—H17126.2C6—Fe1—C4135.95 (10)
C14—C18—C17108.64 (17)C7—Fe1—C4129.04 (9)
C14—C18—Fe269.27 (10)N1—Fe1—C491.81 (7)
C17—C18—Fe269.57 (11)C1—Fe1—C465.90 (8)
C14—C18—H18125.7C2—Fe1—C465.45 (8)
C17—C18—H18125.7C5—Fe1—C438.79 (9)
Fe2—C18—H18125.7C3—Fe1—C438.81 (9)
O3—C19—Fe2174.69 (17)C19—Fe2—C2094.22 (8)
O4—C20—Fe2174.77 (16)C19—Fe2—N593.83 (7)
N6—C21—N5111.92 (14)C20—Fe2—N594.39 (7)
N6—C21—H21A109.2C19—Fe2—C1586.20 (8)
N5—C21—H21A109.2C20—Fe2—C15117.84 (8)
N6—C21—H21B109.2N5—Fe2—C15147.71 (7)
N5—C21—H21B109.2C19—Fe2—C16114.42 (8)
H21A—C21—H21B107.9C20—Fe2—C1687.55 (8)
N7—C22—N6111.47 (14)N5—Fe2—C16151.50 (7)
N7—C22—H22A109.3C15—Fe2—C1639.53 (7)
N6—C22—H22A109.3C19—Fe2—C1496.32 (8)
N7—C22—H22B109.3C20—Fe2—C14154.12 (8)
N6—C22—H22B109.3N5—Fe2—C14108.38 (6)
H22A—C22—H22B108C15—Fe2—C1439.89 (7)
N7—C23—N8111.49 (14)C16—Fe2—C1466.57 (7)
N7—C23—H23A109.3C19—Fe2—C17152.07 (8)
N8—C23—H23A109.3C20—Fe2—C1794.59 (8)
N7—C23—H23B109.3N5—Fe2—C17111.83 (7)
N8—C23—H23B109.3C15—Fe2—C1766.29 (8)
H23A—C23—H23B108C16—Fe2—C1739.76 (8)
N8—C24—N5112.23 (13)C14—Fe2—C1765.96 (7)
N8—C24—H24A109.2C19—Fe2—C18133.73 (8)
N5—C24—H24A109.2C20—Fe2—C18130.92 (8)
N8—C24—H24B109.2N5—Fe2—C1892.38 (6)
N5—C24—H24B109.2C15—Fe2—C1865.71 (7)
H24A—C24—H24B107.9C16—Fe2—C1865.79 (7)
N7—C25—N5112.53 (14)C14—Fe2—C1838.86 (7)
N7—C25—H25A109.1C17—Fe2—C1838.86 (7)
C5—C1—C2—C3−0.5 (2)C3—C2—Fe1—C1−119.0 (2)
Fe1—C1—C2—C360.88 (14)C1—C2—Fe1—C538.58 (13)
C5—C1—C2—Fe1−61.34 (13)C3—C2—Fe1—C5−80.39 (15)
C1—C2—C3—C41.4 (2)C1—C2—Fe1—C3119.0 (2)
Fe1—C2—C3—C461.71 (14)C1—C2—Fe1—C481.25 (14)
C1—C2—C3—Fe1−60.31 (14)C3—C2—Fe1—C4−37.72 (14)
C2—C3—C4—C5−1.8 (2)C4—C5—Fe1—C696.1 (2)
Fe1—C3—C4—C558.52 (14)C1—C5—Fe1—C6−21.8 (3)
C2—C3—C4—Fe1−60.33 (14)C4—C5—Fe1—C7−159.01 (13)
C3—C4—C5—C11.5 (2)C1—C5—Fe1—C783.04 (13)
Fe1—C4—C5—C160.24 (14)C4—C5—Fe1—N1−64.02 (13)
C3—C4—C5—Fe1−58.71 (15)C1—C5—Fe1—N1178.02 (11)
C2—C1—C5—C4−0.6 (2)C4—C5—Fe1—C1117.95 (18)
Fe1—C1—C5—C4−61.75 (14)C4—C5—Fe1—C279.79 (13)
C2—C1—C5—Fe161.10 (14)C1—C5—Fe1—C2−38.17 (12)
C18—C14—C15—C161.3 (2)C4—C5—Fe1—C336.18 (12)
Fe2—C14—C15—C16−60.70 (13)C1—C5—Fe1—C3−81.77 (13)
C18—C14—C15—Fe262.03 (12)C1—C5—Fe1—C4−117.95 (18)
C14—C15—C16—C17−0.5 (2)C4—C3—Fe1—C6168.18 (14)
Fe2—C15—C16—C17−61.57 (13)C2—C3—Fe1—C6−74.45 (15)
C14—C15—C16—Fe261.11 (13)C4—C3—Fe1—C7−73.9 (2)
C15—C16—C17—C18−0.6 (2)C2—C3—Fe1—C743.5 (3)
Fe2—C16—C17—C18−61.48 (13)C4—C3—Fe1—N170.21 (14)
C15—C16—C17—Fe260.88 (13)C2—C3—Fe1—N1−172.42 (13)
C15—C14—C18—C17−1.7 (2)C4—C3—Fe1—C1−80.01 (14)
Fe2—C14—C18—C1758.57 (13)C2—C3—Fe1—C137.36 (14)
C15—C14—C18—Fe2−60.29 (12)C4—C3—Fe1—C2−117.4 (2)
C16—C17—C18—C141.4 (2)C4—C3—Fe1—C5−36.17 (13)
Fe2—C17—C18—C14−58.39 (13)C2—C3—Fe1—C581.21 (15)
C16—C17—C18—Fe259.83 (13)C2—C3—Fe1—C4117.4 (2)
N4—C12—N1—C1156.03 (18)C5—C4—Fe1—C6−137.60 (15)
N4—C12—N1—C8−57.41 (18)C3—C4—Fe1—C6−16.95 (19)
N4—C12—N1—Fe1−179.91 (11)C5—C4—Fe1—C727.41 (17)
N2—C11—N1—C12−56.77 (18)C3—C4—Fe1—C7148.06 (13)
N2—C11—N1—C856.53 (18)C5—C4—Fe1—N1123.24 (13)
N2—C11—N1—Fe1178.94 (11)C3—C4—Fe1—N1−116.11 (13)
N3—C8—N1—C1256.63 (18)C5—C4—Fe1—C1−38.46 (13)
N3—C8—N1—C11−57.39 (18)C3—C4—Fe1—C182.19 (14)
N3—C8—N1—Fe1179.78 (12)C5—C4—Fe1—C2−82.06 (14)
N1—C11—N2—C13−58.67 (19)C3—C4—Fe1—C238.59 (13)
N1—C11—N2—C1059.46 (19)C3—C4—Fe1—C5120.65 (18)
N3—C13—N2—C1159.3 (2)C5—C4—Fe1—C3−120.65 (18)
N3—C13—N2—C10−58.9 (2)C21—N5—Fe2—C19−66.78 (12)
N4—C10—N2—C11−60.45 (19)C25—N5—Fe2—C1952.66 (12)
N4—C10—N2—C1358.31 (19)C24—N5—Fe2—C19172.37 (12)
N1—C8—N3—C9−58.50 (19)C21—N5—Fe2—C20−161.31 (12)
N1—C8—N3—C1359.60 (19)C25—N5—Fe2—C20−41.87 (12)
N4—C9—N3—C858.99 (19)C24—N5—Fe2—C2077.84 (12)
N4—C9—N3—C13−59.29 (19)C21—N5—Fe2—C1522.16 (18)
N2—C13—N3—C8−59.4 (2)C25—N5—Fe2—C15141.60 (14)
N2—C13—N3—C959.4 (2)C24—N5—Fe2—C15−98.69 (15)
N1—C12—N4—C959.75 (18)C21—N5—Fe2—C16105.75 (16)
N1—C12—N4—C10−58.17 (19)C25—N5—Fe2—C16−134.81 (15)
N3—C9—N4—C12−59.39 (19)C24—N5—Fe2—C16−15.1 (2)
N3—C9—N4—C1058.75 (19)C21—N5—Fe2—C1431.19 (13)
N2—C10—N4—C1259.85 (19)C25—N5—Fe2—C14150.62 (11)
N2—C10—N4—C9−58.16 (19)C24—N5—Fe2—C14−89.67 (12)
N6—C21—N5—C2556.37 (18)C21—N5—Fe2—C17101.96 (12)
N6—C21—N5—C24−56.85 (17)C25—N5—Fe2—C17−138.60 (11)
N6—C21—N5—Fe2178.70 (11)C24—N5—Fe2—C17−18.89 (13)
N7—C25—N5—C21−56.97 (18)C21—N5—Fe2—C1867.34 (12)
N7—C25—N5—C2457.09 (17)C25—N5—Fe2—C18−173.22 (12)
N7—C25—N5—Fe2−178.90 (11)C24—N5—Fe2—C18−53.51 (12)
N8—C24—N5—C2156.10 (18)C16—C15—Fe2—C19−137.02 (13)
N8—C24—N5—C25−57.77 (17)C14—C15—Fe2—C19104.57 (12)
N8—C24—N5—Fe2179.20 (11)C16—C15—Fe2—C20−44.25 (14)
N5—C21—N6—C2659.81 (18)C14—C15—Fe2—C20−162.66 (11)
N5—C21—N6—C22−58.66 (18)C16—C15—Fe2—N5131.83 (13)
N8—C26—N6—C21−60.71 (18)C14—C15—Fe2—N513.42 (19)
N8—C26—N6—C2258.20 (18)C14—C15—Fe2—C16−118.41 (17)
N7—C22—N6—C2159.69 (19)C16—C15—Fe2—C14118.41 (17)
N7—C22—N6—C26−58.81 (19)C16—C15—Fe2—C1738.09 (12)
N5—C25—N7—C2259.10 (19)C14—C15—Fe2—C17−80.32 (12)
N5—C25—N7—C23−58.82 (18)C16—C15—Fe2—C1880.80 (12)
N6—C22—N7—C25−59.46 (19)C14—C15—Fe2—C18−37.61 (11)
N6—C22—N7—C2359.07 (18)C15—C16—Fe2—C1948.34 (14)
N8—C23—N7—C2558.91 (19)C17—C16—Fe2—C19166.30 (11)
N8—C23—N7—C22−59.20 (18)C15—C16—Fe2—C20141.86 (12)
N5—C24—N8—C2359.99 (18)C17—C16—Fe2—C20−100.18 (12)
N5—C24—N8—C26−58.10 (18)C15—C16—Fe2—N5−123.47 (15)
N7—C23—N8—C24−59.41 (18)C17—C16—Fe2—N5−5.5 (2)
N7—C23—N8—C2658.82 (18)C17—C16—Fe2—C15117.96 (16)
N6—C26—N8—C2459.87 (18)C15—C16—Fe2—C14−37.94 (11)
N6—C26—N8—C23−58.28 (19)C17—C16—Fe2—C1480.02 (12)
C12—N1—Fe1—C6166.15 (12)C15—C16—Fe2—C17−117.96 (16)
C11—N1—Fe1—C6−72.64 (13)C15—C16—Fe2—C18−80.58 (12)
C8—N1—Fe1—C646.76 (13)C17—C16—Fe2—C1837.38 (11)
C12—N1—Fe1—C771.87 (12)C18—C14—Fe2—C19166.14 (12)
C11—N1—Fe1—C7−166.91 (12)C15—C14—Fe2—C19−76.31 (12)
C8—N1—Fe1—C7−47.52 (12)C18—C14—Fe2—C20−80.4 (2)
C12—N1—Fe1—C1−20.4 (2)C15—C14—Fe2—C2037.1 (2)
C11—N1—Fe1—C1100.77 (17)C18—C14—Fe2—N569.96 (12)
C8—N1—Fe1—C1−139.84 (15)C15—C14—Fe2—N5−172.49 (11)
C12—N1—Fe1—C2−102.37 (16)C18—C14—Fe2—C15−117.55 (16)
C11—N1—Fe1—C218.8 (2)C18—C14—Fe2—C16−79.95 (12)
C8—N1—Fe1—C2138.24 (15)C15—C14—Fe2—C1637.59 (11)
C12—N1—Fe1—C5−23.11 (14)C18—C14—Fe2—C17−36.35 (11)
C11—N1—Fe1—C598.10 (13)C15—C14—Fe2—C1781.20 (12)
C8—N1—Fe1—C5−142.50 (12)C15—C14—Fe2—C18117.55 (16)
C12—N1—Fe1—C3−93.56 (13)C18—C17—Fe2—C1990.6 (2)
C11—N1—Fe1—C327.65 (14)C16—C17—Fe2—C19−27.4 (2)
C8—N1—Fe1—C3147.05 (12)C18—C17—Fe2—C20−161.38 (12)
C12—N1—Fe1—C4−57.41 (13)C16—C17—Fe2—C2080.58 (12)
C11—N1—Fe1—C463.80 (13)C18—C17—Fe2—N5−64.79 (12)
C8—N1—Fe1—C4−176.80 (13)C16—C17—Fe2—N5177.17 (10)
C2—C1—Fe1—C651.64 (15)C18—C17—Fe2—C1580.16 (12)
C5—C1—Fe1—C6168.99 (13)C16—C17—Fe2—C15−37.88 (11)
C2—C1—Fe1—C7145.14 (13)C18—C17—Fe2—C16118.04 (16)
C5—C1—Fe1—C7−97.51 (13)C18—C17—Fe2—C1436.36 (11)
C2—C1—Fe1—N1−121.21 (16)C16—C17—Fe2—C14−81.68 (12)
C5—C1—Fe1—N1−3.9 (2)C16—C17—Fe2—C18−118.04 (16)
C5—C1—Fe1—C2117.35 (18)C14—C18—Fe2—C19−19.24 (16)
C2—C1—Fe1—C5−117.35 (18)C17—C18—Fe2—C19−139.60 (13)
C2—C1—Fe1—C3−37.49 (13)C14—C18—Fe2—C20145.27 (12)
C5—C1—Fe1—C379.86 (14)C17—C18—Fe2—C2024.91 (15)
C2—C1—Fe1—C4−80.03 (14)C14—C18—Fe2—N5−116.84 (11)
C5—C1—Fe1—C437.32 (13)C17—C18—Fe2—N5122.80 (11)
C1—C2—Fe1—C6−133.79 (14)C14—C18—Fe2—C1538.60 (11)
C3—C2—Fe1—C6107.23 (15)C17—C18—Fe2—C15−81.77 (12)
C1—C2—Fe1—C7−41.18 (16)C14—C18—Fe2—C1682.13 (12)
C3—C2—Fe1—C7−160.16 (14)C17—C18—Fe2—C16−38.23 (11)
C1—C2—Fe1—N1132.19 (14)C17—C18—Fe2—C14−120.37 (16)
C3—C2—Fe1—N113.2 (2)C14—C18—Fe2—C17120.37 (16)

Experimental details

Crystal data
Chemical formula[Fe(C5H5)(C6H12N4)(CO)2]BF4
Mr403.97
Crystal system, space groupMonoclinic, P21/c
Temperature (K)173
a, b, c (Å)15.1054 (6), 14.6407 (6), 14.2267 (6)
β (°) 96.997 (2)
V (Å3)3122.9 (2)
Z8
Radiation typeMo Kα
µ (mm−1)1.03
Crystal size (mm)0.42 × 0.19 × 0.16
Data collection
DiffractometerBruker SMART APEXII CCD
Absorption correctionMulti-scan
(SADABS; Bruker, 2008)
Tmin, Tmax0.673, 0.853
No. of measured, independent and
observed [I > 2σ(I)] reflections		62504, 7768, 6765
Rint0.033
(sin θ/λ)max (Å−1)0.668
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.034, 0.092, 1.08
No. of reflections7768
No. of parameters488
No. of restraints12
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å−3)0.63, −0.43

Computer programs: APEX2 (Bruker, 2008), SAINT-Plus (Bruker, 2008), SAINT-Plus and XPREP (Bruker, 2008), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), ORTEP-3 (Farrugia, 1997), WinGX (Farrugia, 1999).

 

Acknowledgements

Our acknowledgement goes to the University of KwaZulu-Natal for resources and financial support.

References

First citationBruker (2008). APEX2, SAINT-Plus, XPREP and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.  Google Scholar
 First citationFarrugia, L. J. (1997). J. Appl. Cryst. 30, 565.  CrossRef IUCr Journals Google Scholar
 First citationFarrugia, L. J. (1999). J. Appl. Cryst. 32, 837–838.  CrossRef CAS IUCr Journals Google Scholar
 First citationMatos, R. M. & Verkade, J. G. (2003). J. Braz. Chem. Soc. 14, 71–75.  Web of Science CSD CrossRef CAS Google Scholar
 First citationM'thiruaine, C. M., Friedrich, H. B., Changamu, E. O. & Bala, M. D. (2011). Inorg. Chim. Acta, 366, 105–115.  CAS Google Scholar
 First citationM'thiruaine, C. M., Friedrich, H. B., Changamu, E. O. & Bala, M. D. (2012). Inorg. Chim. Acta, 390, 83–94.  CAS Google Scholar
 First citationM'thiruaine, C. M., Friedrich, H. B., Changamu, E. O. & Fernandes, M. A. (2012). Acta Cryst. E68, m931.  CSD CrossRef IUCr Journals Google Scholar
 First citationSheldrick, G. M. (2008). Acta Cryst. A64, 112–122.  Web of Science CrossRef CAS IUCr Journals Google Scholar

This is an open-access article distributed under the terms of the Creative Commons Attribution (CC-BY) Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.

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ISSN: 2056-9890
Volume 68| Part 8| August 2012| Page m1077
https://doi.org/10.1107/S1600536812031649
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