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1,3-Bis­(di­phenyl­phosphino)propane-2κ2P,P′-di­carbonyl-1κ2C-chloro-2κCl-{μ-2,2′,2′′-nitrilo­tri­ethane­thiol­ato(3–)-1κ4N,S,S′,S′′:2κ2S,S′}iron(II)nickel(II) aceto­nitrile solvate

CROSSMARK_Color_square_no_text.svg

aDepartment of Biological Chemistry, John Innes Centre, Norwich Research Park, Colney, Norwich NR4 7UH, England, and bDepartment of Chemistry, University of Sussex, Falmer, Brighton BN1 9QJ, England
*Correspondence e-mail: dave.evans@bbsrc.ac.uk

(Received 20 May 2005; accepted 7 June 2005; online 17 June 2005)

The structure of the neutral title complex, [{Fe[(SCH2CH2)3N](CO)2-S,S′}NiCl{[P(C6H5)2]2(CH2)3}]·CH3CN or [FeNi(C6H12NS3)Cl(C27H26P2)(CO)2]·C2H3N, is described. There are two independent complex mol­ecules and two solvent mol­ecules in the asymmetric unit. The Fe atoms are octa­hedrally coordinated; the three S atoms and a C atom of one of the two CO ligands form the equatorial plane, with the N atom of the (SCH2CH2)3N ligand and the second carbonyl C atom lying in the axial positions. The Ni atoms are square pyramidally coordinated, with the two bridging S atoms and the P atoms of the 1,3-bis­(diphenyl­phosphino)propane ligand forming the basal plane and the Cl atom lying in the apical position.

Comment

The title compound, (I)[link], was prepared as a further example of a synthetic structural analogue of the dimetallic active site of the enzyme nickel–iron hydrogenase (Evans & Pickett, 2003[Evans, D. J. & Pickett, C. J. (2003). Chem. Soc. Rev. 32, 268-275.]; Davies et al., 1999[Davies, S. C., Evans, D. J., Hughes, D. L., Longhurst, S. & Sanders, J. R. (1999). Chem. Commun. pp. 1935-1936.]; Smith et al., 2002[Smith, M. C., Barclay, J. E., Cramer, S. P., Davies, S. C., Gu, W.-W., Hughes, D. L., Longhurst, S. & Evans, D. J. (2002). J. Chem. Soc. Dalton Trans. pp. 2641-2647.], 2003[Smith, M. C., Barclay, J. E., Davies, S. C., Hughes, D. L. & Evans, D. J. (2003). Dalton Trans. pp. 4147-4151.]). Compound (I)[link] is closely related to [{Fe[(SCH2CH2)3N](CO)2-S,S′}NiCl{[P(C6H5)2]2(CH2)2}], (II) (Davies et al., 1999[Davies, S. C., Evans, D. J., Hughes, D. L., Longhurst, S. & Sanders, J. R. (1999). Chem. Commun. pp. 1935-1936.]; Smith et al., 2002[Smith, M. C., Barclay, J. E., Cramer, S. P., Davies, S. C., Gu, W.-W., Hughes, D. L., Longhurst, S. & Evans, D. J. (2002). J. Chem. Soc. Dalton Trans. pp. 2641-2647.]), in which the chelating diphosphane is 1,2-bis­(di­phenyl­phosphino)ethane (dppe), whereas in (I)[link] it is 1,3-bis­(di­phenyl­phosphino)propane (dppp).

[Scheme 1]

The asymmetric unit consists of two complex molecules and two solvent molecules. The S3C equatorial planes of the octa­hedrally coordinated Fe atoms are slightly distorted, with deviations from the mean planes lying in the range −0.069 (3) to 0.074 (3) Å in mol­ecule 1 (the negative sign indicates the opposite side of the mean plane) and −0.060 (3) to 0.063 (3) Å in mol­ecule 2. The Fe atoms are displaced from these mean equatorial planes by 0.067 (2) and 0.1400 (12) Å, respectively, towards the axial CO ligand. The S2P2 basal planes of the square pyramidally coordinated Ni atoms are also slightly distorted, with deviations from the mean planes lying in the range −0.054 (3) to 0.053 (3) Å in mol­ecule 1 and −0.035 (3) to 0.035 (3) Å in mol­ecule 2. The Ni atoms are displaced 0.3227 (13) and 0.3175 (14) Å, respectively, from these mean planes, towards the Cl atoms. The S3C and S2P2 mean planes are not coplanar, with an angle between their normals of 16.31 (6)°; in (II), this angle is 19.38 (7)°.

Bond dimensions about the Fe and Ni atoms are not unusual and are comparable to those in (II) [see Table 1[link] for dimensions in (I)]. The Fe—C bond to the equatorial CO ligand is slightly longer than those to the axial CO ligand in both mol­ecules of (I)[link] and in complex (II); in the second mol­ecule of (I)[link] it is longer than in the first and in (II) as a result of unresolved disorder in the O atom [Fe—Ceq = 1.783 (12) Å and Fe—Caxial = 1.741 (10) in (II)].

The unusual torsion angles in the (SCH2CH2)3N ligand in (I)[link] are also found in (II); the usual pseudo-threefold rotation about the Fe—N bond is removed by the non-bridging SCH2CH2 `arm' in both structures (see Fig. 2[link]). Other bond dimensions in the ligands are as expected.

The mol­ecules are arranged within the crystal structure with the complex mol­ecules forming chains parallel to the crystallographic a axis; the solvent mol­ecules occupy the centres of the channels enclosed by four such chains (see Fig. 3[link]).

[Figure 1]
Figure 1
The asymmetric unit of (I)[link], showing displacement ellipsoids at the 50% probability level. H atoms have been omitted.
[Figure 2]
Figure 2
View along the N—Fe—C—O axis of (a) mol­ecule 1 and (b) mol­ecule 2, showing the deviation from the pseudo-threefold rotation of the (SCH2CH2)3N ligand. H atoms have been omitted.
[Figure 3]
Figure 3
The packing, viewed along the crystallographic a axis. Atoms are represented by arbitrary spheres. H atoms have been omitted.

Experimental

Under an atmosphere of carbon monoxide, a mixture of [NiCl2(dppp)] (0.21 g, 0.39 mmol) and (NEt4)[Fe{(SCH2CH2)3N}-(CO)] (0.16 g, 0.39 mmol) in MeCN (100 ml) was refluxed with stirring for 2.5 h. After cooling overnight, crystals were collected by filtration and dried (0.31 g, 97%). Analysis expected for C37H41ClFeN2NiO2P2S3: C 52.1, H 4.8, N 3.3%; found C 51.7, H 4.9, N 3.2%. ν(CO), KBr: 1944 and 2006 cm−1; Mössbauer (solid, 80 K, relative to iron foil at 298 K) isomer shift 0.07 mm s−1, quadrupole splitting 0.56 mm s−1.

Crystal data
  • [FeNi(C6H12NS3)Cl(C27H26P2)(CO)2]·C2H3N

  • Mr = 853.85

  • Orthorhombic, P c a 21

  • a = 20.6025 (4) Å

  • b = 12.4769 (2) Å

  • c = 29.7090 (6) Å

  • V = 7636.9 (2) Å3

  • Z = 8

  • Dx = 1.485 Mg m−3

  • Mo Kα radiation

  • Cell parameters from 24708 reflections

  • θ = 3.7–23.8°

  • μ = 1.23 mm−1

  • T = 173 (2) K

  • Plate, brown

  • 0.2 × 0.2 × 0.02 mm

Data collection
  • Nonius KappaCCD diffractometer

  • φ and ω scans

  • Absorption correction: multi-scan(Blessing, 1995[Blessing, R. H. (1995). Acta Cryst. A51, 33-38.])Tmin = 0.823, Tmax = 0.979

  • 24708 measured reflections

  • 10246 independent reflections

  • 8837 reflections with I > 2σ(I)

  • Rint = 0.052

  • θmax = 23.7°

  • h = −22 → 22

  • k = −14 → 13

  • l = −27 → 33

Refinement
  • Refinement on F2

  • R[F2 > 2σ(F2)] = 0.052

  • wR(F2) = 0.107

  • S = 1.07

  • 10246 reflections

  • 884 parameters

  • H-atom parameters constrained

  • w = 1/[σ2(Fo2) + 30.7123P] where P = (Fo2 + 2Fc2)/3

  • (Δ/σ)max = 0.006

  • Δρmax = 0.88 e Å−3

  • Δρmin = −0.63 e Å−3

  • Absolute structure: Flack (1983[Flack, H. D. (1983). Acta Cryst. A39, 876-881.]), 4317 Friedel pairs

  • Flack parameter: 0.604 (14)

Table 1
Selected geometric parameters (Å, °)[link]

Ni—P1 2.2012 (14)
Ni—P2 2.2060 (15)
Ni—S3 2.2517 (13)
Ni—S1 2.2574 (15)
Ni—Cl 2.5787 (14)
Fe—C35 1.759 (6)
Fe—C34 1.829 (6)
Fe—N 2.048 (4)
Fe—S1 2.2865 (15)
Fe—S2 2.2978 (16)
Fe—S3 2.3159 (15)
O1—C34 1.065 (7)
O2—C35 1.151 (7)
Ni1b—P1b 2.2018 (15)
Ni1b—P2b 2.2046 (15)
Ni1b—S1b 2.2495 (16)
Ni1b—S3b 2.2536 (14)
Ni1b—Cl1b 2.5971 (16)
Fe2b—C35b 1.760 (6)
Fe2b—C34b 1.912 (7)
Fe2b—N1b 2.065 (5)
Fe2b—S2b 2.2839 (19)
Fe2b—S1b 2.2909 (16)
Fe2b—S3b 2.3029 (15)
O1b—C34b 0.861 (8)
O2b—C35b 1.137 (7)
P1—Ni—P2 92.88 (5)
P1—Ni—S3 165.43 (6)
P2—Ni—S3 88.90 (5)
P1—Ni—S1 87.87 (5)
P2—Ni—S1 160.38 (6)
S3—Ni—S1 85.67 (5)
P1—Ni—Cl 88.51 (5)
P2—Ni—Cl 92.94 (5)
S3—Ni—Cl 105.85 (5)
S1—Ni—Cl 106.68 (5)
C35—Fe—C34 91.6 (2)
C35—Fe—N 175.2 (2)
C34—Fe—N 92.5 (2)
C35—Fe—S1 95.72 (19)
C34—Fe—S1 96.10 (18)
N—Fe—S1 86.26 (12)
C35—Fe—S2 90.91 (19)
C34—Fe—S2 87.63 (18)
N—Fe—S2 86.83 (12)
S1—Fe—S2 172.29 (7)
C35—Fe—S3 88.34 (18)
C34—Fe—S3 179.60 (19)
N—Fe—S3 87.58 (12)
S1—Fe—S3 83.53 (5)
S2—Fe—S3 92.76 (6)
Ni—S1—Fe 95.51 (6)
O1—C34—Fe 175.3 (5)
O2—C35—Fe 176.9 (5)
P1b—Ni1b—P2b 92.84 (6)
P1b—Ni1b—S1b 87.92 (6)
P2b—Ni1b—S1b 161.55 (6)
P1b—Ni1b—S3b 164.85 (6)
P2b—Ni1b—S3b 88.78 (5)
S1b—Ni1b—S3b 85.85 (5)
P1b—Ni1b—Cl1b 88.79 (5)
P2b—Ni1b—Cl1b 92.29 (5)
S1b—Ni1b—Cl1b 106.16 (6)
S3b—Ni1b—Cl1b 106.21 (5)
C35b—Fe2b—C34b 90.1 (3)
C35b—Fe2b—N1b 177.9 (2)
C34b—Fe2b—N1b 91.8 (2)
C35b—Fe2b—S2b 94.41 (19)
C34b—Fe2b—S2b 87.86 (18)
N1b—Fe2b—S2b 86.57 (13)
C35b—Fe2b—S1b 92.44 (18)
C34b—Fe2b—S1b 95.97 (18)
N1b—Fe2b—S1b 86.47 (13)
S2b—Fe2b—S1b 172.15 (7)
C35b—Fe2b—S3b 90.78 (19)
C34b—Fe2b—S3b 179.1 (2)
N1b—Fe2b—S3b 87.29 (13)
S2b—Fe2b—S3b 92.30 (6)
S1b—Fe2b—S3b 83.76 (5)
Ni1B—S1B—Fe2B 95.18 (6)
Fe—S1—C29—C28 −9.4 (6)
S1—C29—C28—N 38.6 (8)
C29—C28—N—Fe −51.9 (7)
Fe—S2—C31—C30 23.7 (6)
S2—C31—C30—N −51.7 (8)
C31—C30—N—Fe 55.3 (7)
Fe—S3—C33—C32 −38.3 (6)
S3—C33—C32—N 45.8 (8)
C33—C32—N—Fe −27.3 (8)
Fe2b—S1b—C29b—C28b −3.0 (8)
S1b—C29b—C28b—N1b 29.6 (12)
C29b—C28b—N1b—Fe2b −43.0 (10)
Fe2b—S2b—C31b—C30b 25.8 (8)
S2b—C31b—C30b—N1b −54.9 (10)
C31b—C30b—N1b—Fe2b 58.7 (9)
Fe2b—S3b—C33b—C32b −35.8 (7)
S3b—C33b—C32b—N1b 42.1 (10)
C33b—C32b—N1b—Fe2b −24.5 (10)
P1—C1—C2—C3 −68.5 (8)
C1—C2—C3—P2 69.7 (8)
P1b—C1b—C2b—C3b −69.3 (8)
C1b—C2b—C3b—P2b 67.1 (8)

H atoms were not located for the CH3CN solvent mol­ecules. The value of the Flack (1983[Flack, H. D. (1983). Acta Cryst. A39, 876-881.]) parameter indicates an inversion twin. All other H atoms were positioned geometrically (C—H = 0.95–0.99 Å) and refined as riding [Uiso(H) = 1.2Ueq(C)].

Data collection: COLLECT (Nonius, 2000[Nonius (2000). COLLECT. Nonius BV, Delft, The Netherlands.]); cell refinement: HKL SCALEPACK (Otwinowski & Minor, 1997[Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, Macromolecular Crystallography, Part A, edited by C. W. Carter Jr & R. M. Sweet, pp. 307-326. New York: Academic Press.]); data reduction: HKL DENZO (Otwinowski & Minor, 1997[Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, Macromolecular Crystallography, Part A, edited by C. W. Carter Jr & R. M. Sweet, pp. 307-326. New York: Academic Press.]) and SCALEPACK; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997[Sheldrick, G. M. (1997). SHELXS97 and SHELXL97. University of Göttingen, Germany.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997[Sheldrick, G. M. (1997). SHELXS97 and SHELXL97. University of Göttingen, Germany.]); molecular graphics: ORTEP-3 for Windows (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


Computing details top

Data collection: Collect (Nonius, 2000); cell refinement: HKL SCALEPACK (Otwinowski & Minor, 1997); data reduction: HKL DENZO (Otwinowski & Minor, 1997) and SCALEPACK; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).

(I) top
Crystal data top
[Fe(C6H12NS3)(CO)2NiCl(C27H26P2)]·C2H3NF(000) = 3536
Mr = 853.85Dx = 1.485 Mg m3
Orthorhombic, Pca21Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2c -2acCell parameters from 117428 reflections
a = 20.6025 (4) Åθ = 3.7–23.8°
b = 12.4769 (2) ŵ = 1.23 mm1
c = 29.7090 (6) ÅT = 173 K
V = 7636.9 (2) Å3Plate, brown
Z = 80.2 × 0.2 × 0.02 mm
Data collection top
Nonius KappaCCD
diffractometer
10246 independent reflections
Radiation source: Enraf–Nonius FR5908837 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.052
Detector resolution: 9 pixels mm-1θmax = 23.7°, θmin = 3.8°
φ or ω? scansh = 2222
Absorption correction: multi-scan
(Blessing, 1995)
k = 1413
Tmin = 0.823, Tmax = 0.979l = 2733
24708 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)] = 0.052H-atom parameters constrained
wR(F2) = 0.107 w = 1/[σ2(Fo2) + 30.7123P]
where P = (Fo2 + 2Fc2)/3
S = 1.07(Δ/σ)max = 0.006
10246 reflectionsΔρmax = 0.88 e Å3
884 parametersΔρmin = 0.63 e Å3
1 restraintAbsolute structure: Flack (1983), 4317 Friedel pairs?
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.604 (14)
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. H atoms were omitted for the CH3CN solvate molecules.

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
Ni0.31580 (3)0.45332 (5)0.09044 (2)0.01991 (16)
Fe0.31008 (4)0.67952 (5)0.15192 (2)0.02202 (19)
Cl0.38331 (6)0.46280 (10)0.01746 (4)0.0283 (3)
S10.37554 (7)0.53252 (10)0.14477 (5)0.0261 (4)
S20.24863 (7)0.83311 (11)0.14947 (6)0.0371 (4)
S30.25547 (6)0.60378 (9)0.09167 (5)0.0222 (3)
P10.36558 (6)0.30219 (10)0.10683 (5)0.0213 (3)
P20.23460 (7)0.37016 (10)0.05694 (5)0.0206 (3)
O10.3765 (2)0.7682 (4)0.22910 (16)0.0607 (15)
O20.2146 (2)0.5822 (4)0.21136 (14)0.0522 (13)
N0.3700 (2)0.7517 (3)0.10603 (14)0.0237 (12)
C10.3604 (3)0.1952 (4)0.06428 (18)0.0283 (15)
H1A0.3830.1310.07590.034*
H1B0.38370.2190.03690.034*
C20.2923 (2)0.1643 (4)0.05141 (18)0.0221 (13)
H2A0.29390.09850.03280.027*
H2B0.26760.14750.07910.027*
C30.2562 (3)0.2519 (4)0.02522 (18)0.0247 (14)
H3A0.28370.27410.00050.03*
H3B0.2160.22040.01270.03*
C40.3346 (2)0.2377 (4)0.15762 (18)0.0233 (14)
C50.3599 (3)0.1412 (4)0.17244 (19)0.0338 (16)
H50.39760.11260.15850.041*
C60.3306 (3)0.0856 (5)0.2077 (2)0.0453 (19)
H60.34570.01660.21630.054*
C70.2780 (3)0.1339 (6)0.2302 (2)0.0494 (19)
H70.25830.09820.25490.059*
C80.2550 (3)0.2326 (6)0.2168 (2)0.047 (2)
H80.21930.26440.2320.057*
C90.2838 (3)0.2843 (5)0.18156 (18)0.0355 (17)
H90.26880.35350.17320.043*
C100.4536 (2)0.3113 (4)0.11620 (17)0.0209 (13)
C110.4951 (3)0.3159 (4)0.0793 (2)0.0334 (16)
H110.4780.31750.04960.04*
C120.5619 (3)0.3182 (4)0.0861 (2)0.0355 (16)
H120.59020.31820.06090.043*
C130.5875 (3)0.3203 (4)0.1287 (2)0.0394 (17)
H130.63320.32130.13290.047*
C140.5468 (3)0.3209 (5)0.1650 (2)0.0428 (18)
H140.56430.32510.19460.051*
C150.4797 (3)0.3155 (4)0.15904 (19)0.0319 (16)
H150.45180.31480.18450.038*
C160.1716 (2)0.3275 (4)0.09666 (17)0.0214 (13)
C170.1544 (3)0.3955 (4)0.13105 (18)0.0272 (15)
H170.17190.46590.13180.033*
C180.1117 (3)0.3632 (5)0.16473 (19)0.0321 (16)
H180.10030.41090.18840.039*
C190.0864 (3)0.2615 (5)0.1633 (2)0.0371 (17)
H190.05820.23820.18660.045*
C200.1014 (3)0.1927 (5)0.12845 (19)0.0340 (16)
H200.08290.12310.12730.041*
C210.1441 (3)0.2265 (4)0.0948 (2)0.0303 (15)
H210.15440.17990.07050.036*
C220.1909 (3)0.4486 (4)0.01484 (18)0.0252 (14)
C230.1256 (3)0.4710 (4)0.01890 (19)0.0320 (15)
H230.10220.44540.04430.038*
C240.0935 (3)0.5310 (4)0.0139 (2)0.0384 (17)
H240.04830.54490.01120.046*
C250.1277 (3)0.5698 (4)0.0500 (2)0.0411 (17)
H250.1060.61140.07220.049*
C260.1925 (3)0.5492 (4)0.0544 (2)0.0360 (16)
H260.21580.57710.07940.043*
C270.2246 (3)0.4872 (4)0.02205 (19)0.0317 (16)
H270.26940.47160.02540.038*
C280.4397 (3)0.7145 (4)0.1139 (2)0.0360 (17)
H28A0.45570.74480.14260.043*
H28B0.46770.74220.08940.043*
C290.4449 (3)0.5936 (4)0.1155 (2)0.0355 (17)
H29A0.44710.56530.08440.043*
H29B0.48550.57330.13110.043*
C300.3694 (3)0.8705 (4)0.1134 (2)0.0317 (16)
H30A0.38860.88750.1430.038*
H30B0.39570.90620.08990.038*
C310.2998 (3)0.9119 (4)0.1115 (2)0.0341 (16)
H31A0.29870.98830.12050.041*
H31B0.28310.90630.08030.041*
C320.3548 (3)0.7250 (4)0.0577 (2)0.0348 (16)
H32A0.36640.78730.03860.042*
H32B0.38230.6640.04820.042*
C330.2844 (3)0.6965 (4)0.04927 (19)0.0273 (15)
H33A0.25770.76250.04990.033*
H33B0.280.66360.01910.033*
C340.3534 (3)0.7384 (4)0.19960 (18)0.0273 (15)
C350.2534 (3)0.6183 (5)0.18797 (18)0.0310 (16)
Ni1B0.44894 (3)0.04767 (5)0.08998 (2)0.02046 (17)
Fe2B0.45935 (4)0.17831 (6)0.15060 (3)0.0243 (2)
Cl1B0.37760 (7)0.03749 (11)0.01804 (5)0.0343 (4)
S1B0.39179 (7)0.03313 (11)0.14485 (5)0.0295 (4)
S2B0.52230 (9)0.32868 (14)0.14654 (7)0.0539 (5)
S3B0.51087 (6)0.10121 (10)0.08990 (5)0.0217 (3)
P1B0.39939 (7)0.19807 (11)0.10794 (5)0.0240 (4)
P2B0.52737 (7)0.13218 (10)0.05408 (5)0.0214 (4)
O1B0.3979 (3)0.2697 (4)0.2241 (2)0.0724 (18)
O2B0.5449 (2)0.0636 (3)0.21111 (14)0.0466 (13)
N1B0.3986 (2)0.2527 (3)0.10496 (15)0.0293 (13)
C1B0.3990 (3)0.3008 (4)0.06485 (18)0.0254 (14)
H1B10.37570.36430.07660.03*
H1B20.37450.27380.03850.03*
C2B0.4664 (3)0.3360 (4)0.04915 (19)0.0280 (15)
H2B10.46180.4010.03030.034*
H2B20.49250.35570.07590.034*
C3B0.5039 (3)0.2500 (4)0.02196 (18)0.0226 (14)
H3B10.47660.22680.00360.027*
H3B20.54360.28330.00930.027*
C4B0.4336 (2)0.2665 (4)0.15613 (18)0.0256 (14)
C5B0.4853 (3)0.2249 (5)0.1791 (2)0.0340 (16)
H5B0.50070.15560.17120.041*
C6B0.5159 (3)0.2807 (5)0.2136 (2)0.0464 (19)
H6B0.55180.24960.22880.056*
C7B0.4944 (4)0.3808 (5)0.2258 (2)0.048 (2)
H7B0.51610.42090.24840.058*
C8B0.4400 (4)0.4215 (5)0.2042 (2)0.049 (2)
H8B0.42240.48830.21370.059*
C9B0.4115 (3)0.3675 (5)0.1698 (2)0.0413 (18)
H9B0.37560.39890.15470.05*
C10B0.3133 (3)0.1854 (4)0.1226 (2)0.0365 (18)
C11B0.2664 (3)0.1792 (5)0.0880 (3)0.0470 (19)
H11B0.27960.18170.05740.056*
C12B0.2013 (3)0.1696 (5)0.0986 (3)0.060 (2)
H12B0.16950.16670.07540.072*
C13B0.1832 (4)0.1644 (5)0.1428 (3)0.070 (3)
H13B0.13840.15750.14980.084*
C14B0.2272 (3)0.1688 (5)0.1773 (3)0.064 (2)
H14B0.21280.16580.20770.076*
C15B0.2949 (3)0.1780 (5)0.1674 (2)0.049 (2)
H15B0.32640.17910.19080.059*
C16B0.5912 (2)0.1767 (4)0.09261 (17)0.0213 (13)
C17B0.6102 (3)0.1082 (4)0.12771 (18)0.0266 (15)
H17B0.59260.03790.12940.032*
C18B0.6529 (3)0.1410 (4)0.1590 (2)0.0328 (16)
H18B0.66540.09280.18220.039*
C19B0.6788 (3)0.2411 (5)0.1584 (2)0.0325 (16)
H19B0.70710.2640.18170.039*
C20B0.6634 (3)0.3097 (4)0.1230 (2)0.0334 (16)
H20B0.68310.37840.12130.04*
C21B0.6193 (3)0.2783 (4)0.0903 (2)0.0262 (14)
H21B0.60840.32560.06640.031*
C22B0.5708 (3)0.0520 (4)0.01205 (18)0.0240 (14)
C23B0.6360 (3)0.0269 (4)0.0164 (2)0.0328 (16)
H23B0.65970.05140.04180.039*
C24B0.6667 (3)0.0341 (5)0.0165 (2)0.0386 (17)
H24B0.71120.0520.01280.046*
C25B0.6347 (3)0.0686 (5)0.0536 (2)0.0416 (18)
H25B0.65650.11020.07580.05*
C26B0.5692 (3)0.0419 (5)0.0588 (2)0.0451 (19)
H26B0.54640.06440.0850.054*
C27B0.5377 (3)0.0163 (4)0.0265 (2)0.0305 (16)
H27B0.49290.03270.03010.037*
C28B0.3314 (3)0.2115 (6)0.1110 (3)0.064 (2)
H28C0.31210.24850.13730.077*
H28D0.30580.23280.08420.077*
C29B0.3230 (3)0.0976 (4)0.1174 (3)0.045 (2)
H29C0.3160.06340.08780.054*
H29D0.28360.08540.13580.054*
C30B0.3981 (4)0.3690 (5)0.1132 (3)0.069 (3)
H30C0.38170.38460.14380.082*
H30D0.36990.40570.09110.082*
C31B0.4712 (4)0.4084 (5)0.1082 (3)0.064 (2)
H31C0.47440.48540.11590.076*
H31D0.48590.39880.07670.076*
C32B0.4138 (4)0.2251 (6)0.0561 (2)0.064 (2)
H32C0.38420.16710.04640.077*
H32D0.40440.28870.03730.077*
C33B0.4806 (3)0.1911 (4)0.04729 (18)0.0264 (15)
H33C0.50890.25510.04590.032*
H33D0.48250.1550.01760.032*
C34B0.4154 (3)0.2430 (5)0.2004 (2)0.0323 (17)
C35B0.5116 (3)0.1112 (4)0.18801 (19)0.0305 (16)
N20.2291 (4)0.4853 (8)0.3224 (3)0.160 (3)
N2B0.4973 (3)0.0005 (6)0.3194 (3)0.093 (3)
C360.3436 (4)0.5235 (8)0.2875 (3)0.095 (3)
C370.2791 (5)0.5062 (6)0.3067 (3)0.081 (3)
C36B0.3942 (4)0.0543 (9)0.2759 (3)0.099 (4)
C37B0.4515 (4)0.0249 (7)0.3007 (3)0.068 (3)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni0.0181 (3)0.0166 (3)0.0250 (4)0.0006 (3)0.0001 (3)0.0011 (3)
Fe0.0248 (4)0.0188 (4)0.0225 (4)0.0003 (3)0.0007 (3)0.0024 (3)
Cl0.0309 (7)0.0225 (6)0.0316 (8)0.0039 (6)0.0071 (6)0.0006 (6)
S10.0283 (7)0.0219 (7)0.0282 (8)0.0009 (6)0.0052 (6)0.0025 (6)
S20.0346 (8)0.0296 (7)0.0470 (9)0.0042 (7)0.0003 (7)0.0026 (7)
S30.0213 (6)0.0170 (6)0.0283 (8)0.0006 (6)0.0024 (6)0.0012 (6)
P10.0171 (7)0.0217 (7)0.0250 (8)0.0010 (6)0.0021 (6)0.0013 (6)
P20.0231 (7)0.0165 (6)0.0222 (8)0.0011 (6)0.0006 (6)0.0002 (6)
O10.072 (3)0.057 (3)0.054 (3)0.011 (3)0.001 (3)0.008 (2)
O20.049 (3)0.068 (3)0.039 (3)0.015 (2)0.008 (2)0.002 (2)
N0.031 (3)0.015 (2)0.025 (3)0.003 (2)0.0064 (19)0.0075 (18)
C10.040 (3)0.014 (3)0.030 (3)0.000 (3)0.002 (3)0.001 (2)
C20.020 (3)0.015 (2)0.032 (3)0.001 (2)0.000 (2)0.004 (2)
C30.022 (3)0.025 (3)0.027 (3)0.002 (2)0.001 (2)0.001 (2)
C40.021 (3)0.016 (3)0.033 (3)0.007 (2)0.005 (2)0.002 (2)
C50.043 (4)0.021 (3)0.037 (4)0.007 (3)0.002 (3)0.001 (3)
C60.069 (4)0.037 (3)0.030 (4)0.014 (3)0.007 (3)0.007 (3)
C70.045 (4)0.078 (5)0.024 (4)0.024 (4)0.001 (3)0.016 (3)
C80.027 (3)0.085 (5)0.030 (4)0.007 (4)0.004 (3)0.009 (3)
C90.025 (3)0.056 (4)0.026 (3)0.001 (3)0.001 (3)0.007 (3)
C100.027 (3)0.011 (2)0.025 (3)0.001 (2)0.006 (2)0.001 (2)
C110.023 (3)0.038 (3)0.039 (4)0.001 (3)0.004 (3)0.004 (3)
C120.034 (3)0.037 (3)0.036 (3)0.009 (3)0.010 (3)0.004 (3)
C130.018 (3)0.033 (3)0.067 (4)0.004 (3)0.013 (3)0.003 (3)
C140.030 (3)0.055 (4)0.043 (4)0.001 (3)0.006 (3)0.003 (3)
C150.023 (3)0.043 (3)0.030 (3)0.001 (3)0.009 (2)0.002 (3)
C160.013 (2)0.024 (3)0.028 (3)0.014 (2)0.003 (2)0.006 (2)
C170.026 (3)0.025 (3)0.031 (3)0.002 (3)0.004 (2)0.001 (2)
C180.029 (3)0.038 (3)0.029 (3)0.003 (3)0.003 (3)0.004 (3)
C190.024 (3)0.046 (4)0.041 (4)0.000 (3)0.006 (3)0.005 (3)
C200.027 (3)0.039 (3)0.036 (3)0.013 (3)0.000 (3)0.005 (3)
C210.027 (3)0.027 (3)0.037 (3)0.003 (2)0.002 (3)0.004 (3)
C220.029 (3)0.015 (3)0.031 (3)0.005 (2)0.003 (3)0.003 (2)
C230.041 (3)0.028 (3)0.027 (3)0.002 (3)0.003 (3)0.000 (3)
C240.041 (3)0.032 (3)0.042 (4)0.003 (3)0.015 (3)0.005 (3)
C250.049 (4)0.031 (3)0.044 (4)0.004 (3)0.023 (3)0.006 (3)
C260.046 (4)0.030 (3)0.032 (3)0.019 (3)0.008 (3)0.011 (3)
C270.028 (3)0.038 (3)0.029 (3)0.007 (3)0.012 (3)0.000 (3)
C280.019 (3)0.039 (3)0.049 (4)0.006 (3)0.003 (3)0.009 (3)
C290.022 (3)0.033 (3)0.051 (4)0.003 (3)0.007 (3)0.005 (3)
C300.033 (3)0.024 (3)0.039 (4)0.006 (3)0.004 (3)0.003 (3)
C310.043 (4)0.022 (3)0.037 (4)0.007 (3)0.002 (3)0.002 (3)
C320.038 (3)0.028 (3)0.039 (4)0.003 (3)0.006 (3)0.005 (3)
C330.027 (3)0.020 (3)0.035 (3)0.003 (2)0.006 (3)0.009 (2)
C340.025 (3)0.039 (3)0.018 (3)0.000 (3)0.001 (2)0.012 (2)
C350.036 (3)0.039 (3)0.019 (3)0.002 (3)0.001 (3)0.003 (3)
Ni1B0.0192 (3)0.0153 (3)0.0269 (4)0.0002 (3)0.0012 (3)0.0002 (3)
Fe2B0.0289 (4)0.0196 (4)0.0245 (4)0.0009 (4)0.0069 (3)0.0001 (3)
Cl1B0.0354 (8)0.0289 (7)0.0385 (8)0.0039 (7)0.0149 (6)0.0001 (7)
S1B0.0301 (8)0.0210 (7)0.0374 (9)0.0033 (6)0.0135 (6)0.0024 (6)
S2B0.0527 (11)0.0488 (10)0.0602 (12)0.0017 (9)0.0091 (9)0.0036 (9)
S3B0.0219 (7)0.0193 (6)0.0240 (7)0.0009 (6)0.0018 (6)0.0022 (6)
P1B0.0200 (7)0.0178 (7)0.0343 (8)0.0017 (6)0.0002 (6)0.0010 (6)
P2B0.0204 (7)0.0197 (7)0.0239 (8)0.0038 (6)0.0008 (6)0.0013 (6)
O1B0.071 (4)0.060 (3)0.087 (4)0.010 (3)0.015 (3)0.033 (3)
O2B0.054 (3)0.051 (3)0.035 (3)0.000 (2)0.010 (2)0.000 (2)
N1B0.030 (3)0.022 (2)0.036 (3)0.003 (2)0.010 (2)0.004 (2)
C1B0.023 (3)0.026 (3)0.027 (3)0.005 (2)0.010 (2)0.000 (2)
C2B0.037 (3)0.018 (3)0.029 (3)0.008 (3)0.006 (3)0.006 (2)
C3B0.027 (3)0.018 (3)0.023 (3)0.002 (2)0.004 (2)0.001 (2)
C4B0.017 (3)0.033 (3)0.026 (3)0.004 (3)0.001 (2)0.005 (3)
C5B0.034 (3)0.030 (3)0.038 (4)0.003 (3)0.003 (3)0.007 (3)
C6B0.036 (4)0.064 (4)0.039 (4)0.000 (3)0.002 (3)0.015 (3)
C7B0.070 (5)0.052 (4)0.023 (4)0.014 (4)0.002 (3)0.005 (3)
C8B0.083 (5)0.031 (3)0.034 (4)0.004 (4)0.001 (4)0.014 (3)
C9B0.059 (4)0.031 (3)0.034 (4)0.005 (3)0.000 (3)0.001 (3)
C10B0.021 (3)0.021 (3)0.067 (5)0.007 (3)0.005 (3)0.006 (3)
C11B0.028 (3)0.034 (3)0.079 (5)0.002 (3)0.007 (3)0.001 (3)
C12B0.013 (3)0.037 (4)0.130 (7)0.005 (3)0.004 (4)0.017 (4)
C13B0.028 (4)0.048 (4)0.135 (8)0.009 (3)0.017 (4)0.025 (5)
C14B0.041 (4)0.043 (4)0.107 (6)0.009 (3)0.036 (4)0.018 (4)
C15B0.042 (4)0.030 (3)0.076 (5)0.006 (3)0.025 (3)0.007 (3)
C16B0.020 (3)0.025 (3)0.018 (3)0.008 (2)0.001 (2)0.003 (2)
C17B0.021 (3)0.022 (3)0.037 (3)0.005 (3)0.002 (3)0.003 (3)
C18B0.027 (3)0.029 (3)0.043 (4)0.000 (3)0.008 (3)0.004 (3)
C19B0.021 (3)0.042 (3)0.034 (4)0.001 (3)0.004 (3)0.010 (3)
C20B0.030 (3)0.025 (3)0.045 (4)0.008 (3)0.003 (3)0.003 (3)
C21B0.027 (3)0.021 (3)0.030 (3)0.004 (2)0.002 (3)0.002 (3)
C22B0.034 (3)0.014 (3)0.024 (3)0.007 (2)0.001 (2)0.001 (2)
C23B0.036 (3)0.032 (3)0.030 (3)0.005 (3)0.008 (3)0.003 (3)
C24B0.035 (3)0.032 (3)0.049 (4)0.004 (3)0.016 (3)0.002 (3)
C25B0.061 (4)0.032 (3)0.032 (4)0.006 (3)0.019 (3)0.006 (3)
C26B0.066 (4)0.042 (4)0.027 (4)0.013 (4)0.011 (3)0.002 (3)
C27B0.040 (3)0.018 (3)0.034 (4)0.004 (3)0.000 (3)0.006 (2)
C28B0.037 (4)0.068 (4)0.088 (5)0.020 (4)0.026 (4)0.041 (4)
C29B0.026 (3)0.026 (3)0.083 (5)0.004 (3)0.014 (3)0.003 (3)
C30B0.066 (5)0.032 (4)0.108 (6)0.018 (4)0.037 (4)0.017 (4)
C31B0.091 (6)0.035 (4)0.064 (5)0.003 (4)0.015 (4)0.004 (4)
C32B0.086 (5)0.078 (5)0.030 (4)0.036 (5)0.002 (4)0.023 (4)
C33B0.048 (4)0.014 (3)0.017 (3)0.001 (3)0.005 (3)0.005 (2)
C34B0.027 (3)0.021 (3)0.048 (4)0.010 (3)0.007 (3)0.015 (3)
C35B0.040 (3)0.024 (3)0.028 (3)0.010 (3)0.006 (3)0.001 (3)
N20.091 (5)0.217 (7)0.172 (7)0.084 (6)0.062 (5)0.147 (6)
N2B0.067 (4)0.124 (6)0.086 (6)0.049 (5)0.001 (4)0.017 (5)
C360.071 (6)0.126 (7)0.089 (6)0.026 (6)0.003 (5)0.056 (5)
C370.092 (6)0.068 (4)0.082 (6)0.036 (5)0.018 (5)0.057 (4)
C36B0.068 (6)0.141 (9)0.087 (7)0.009 (6)0.018 (5)0.007 (7)
C37B0.069 (5)0.081 (5)0.053 (5)0.035 (5)0.018 (4)0.010 (4)
Geometric parameters (Å, º) top
Ni—P12.2012 (14)Ni1B—S1B2.2495 (16)
Ni—P22.2060 (15)Ni1B—S3B2.2536 (14)
Ni—S32.2517 (13)Ni1B—Cl1B2.5971 (16)
Ni—S12.2574 (15)Fe2B—C35B1.760 (6)
Ni—Cl2.5787 (14)Fe2B—C34B1.912 (7)
Fe—C351.759 (6)Fe2B—N1B2.065 (5)
Fe—C341.829 (6)Fe2B—S2B2.2839 (19)
Fe—N2.048 (4)Fe2B—S1B2.2909 (16)
Fe—S12.2865 (15)Fe2B—S3B2.3029 (15)
Fe—S22.2978 (16)S1B—C29B1.821 (7)
Fe—S32.3159 (15)S2B—C31B1.844 (8)
S1—C291.838 (6)S3B—C33B1.803 (5)
S2—C311.831 (6)P1B—C4B1.810 (6)
S3—C331.811 (6)P1B—C1B1.812 (5)
P1—C41.825 (5)P1B—C10B1.833 (6)
P1—C101.839 (5)P2B—C3B1.818 (5)
P1—C11.841 (5)P2B—C16B1.830 (5)
P2—C31.807 (5)P2B—C22B1.833 (5)
P2—C221.825 (5)O1B—C34B0.861 (8)
P2—C161.834 (5)O2B—C35B1.137 (7)
O1—C341.065 (7)N1B—C30B1.471 (8)
O2—C351.151 (7)N1B—C28B1.488 (8)
N—C301.499 (6)N1B—C32B1.523 (8)
N—C321.508 (7)C1B—C2B1.529 (8)
N—C281.527 (7)C1B—H1B10.99
C1—C21.505 (7)C1B—H1B20.99
C1—H1A0.99C2B—C3B1.549 (7)
C1—H1B0.99C2B—H2B10.99
C2—C31.533 (7)C2B—H2B20.99
C2—H2A0.99C3B—H3B10.99
C2—H2B0.99C3B—H3B20.99
C3—H3A0.99C4B—C5B1.367 (8)
C3—H3B0.99C4B—C9B1.400 (8)
C4—C51.384 (7)C5B—C6B1.390 (8)
C4—C91.394 (8)C5B—H5B0.95
C5—C61.394 (8)C6B—C7B1.373 (9)
C5—H50.95C6B—H6B0.95
C6—C71.409 (9)C7B—C8B1.387 (10)
C6—H60.95C7B—H7B0.95
C7—C81.379 (9)C8B—C9B1.358 (9)
C7—H70.95C8B—H8B0.95
C8—C91.365 (8)C9B—H9B0.95
C8—H80.95C10B—C15B1.387 (9)
C9—H90.95C10B—C11B1.415 (9)
C10—C151.382 (7)C11B—C12B1.384 (9)
C10—C111.392 (8)C11B—H11B0.95
C11—C121.391 (8)C12B—C13B1.366 (12)
C11—H110.95C12B—H12B0.95
C12—C131.370 (9)C13B—C14B1.371 (11)
C12—H120.95C13B—H13B0.95
C13—C141.368 (8)C14B—C15B1.431 (9)
C13—H130.95C14B—H14B0.95
C14—C151.396 (8)C15B—H15B0.95
C14—H140.95C16B—C21B1.395 (7)
C15—H150.95C16B—C17B1.404 (7)
C16—C171.374 (7)C17B—C18B1.343 (8)
C16—C211.382 (7)C17B—H17B0.95
C17—C181.391 (8)C18B—C19B1.358 (8)
C17—H170.95C18B—H18B0.95
C18—C191.373 (8)C19B—C20B1.391 (8)
C18—H180.95C19B—H19B0.95
C19—C201.380 (8)C20B—C21B1.386 (8)
C19—H190.95C20B—H20B0.95
C20—C211.397 (8)C21B—H21B0.95
C20—H200.95C22B—C23B1.384 (8)
C21—H210.95C22B—C27B1.406 (8)
C22—C231.380 (8)C23B—C24B1.391 (8)
C22—C271.384 (8)C23B—H23B0.95
C23—C241.395 (8)C24B—C25B1.355 (9)
C23—H230.95C24B—H24B0.95
C24—C251.373 (9)C25B—C26B1.399 (9)
C24—H240.95C25B—H25B0.95
C25—C261.366 (9)C26B—C27B1.369 (9)
C25—H250.95C26B—H26B0.95
C26—C271.400 (8)C27B—H27B0.95
C26—H260.95C28B—C29B1.445 (9)
C27—H270.95C28B—H28C0.99
C28—C291.514 (8)C28B—H28D0.99
C28—H28A0.99C29B—H29C0.99
C28—H28B0.99C29B—H29D0.99
C29—H29A0.99C30B—C31B1.591 (11)
C29—H29B0.99C30B—H30C0.99
C30—C311.525 (8)C30B—H30D0.99
C30—H30A0.99C31B—H31C0.99
C30—H30B0.99C31B—H31D0.99
C31—H31A0.99C32B—C33B1.464 (9)
C31—H31B0.99C32B—H32C0.99
C32—C331.514 (8)C32B—H32D0.99
C32—H32A0.99C33B—H33C0.99
C32—H32B0.99C33B—H33D0.99
C33—H33A0.99N2—C371.160 (11)
C33—H33B0.99N2B—C37B1.141 (11)
Ni1B—P1B2.2018 (15)C36—C371.462 (13)
Ni1B—P2B2.2046 (15)C36B—C37B1.439 (12)
P1—Ni—P292.88 (5)P1B—Ni1B—S1B87.92 (6)
P1—Ni—S3165.43 (6)P2B—Ni1B—S1B161.55 (6)
P2—Ni—S388.90 (5)P1B—Ni1B—S3B164.85 (6)
P1—Ni—S187.87 (5)P2B—Ni1B—S3B88.78 (5)
P2—Ni—S1160.38 (6)S1B—Ni1B—S3B85.85 (5)
S3—Ni—S185.67 (5)P1B—Ni1B—Cl1B88.79 (5)
P1—Ni—Cl88.51 (5)P2B—Ni1B—Cl1B92.29 (5)
P2—Ni—Cl92.94 (5)S1B—Ni1B—Cl1B106.16 (6)
S3—Ni—Cl105.85 (5)S3B—Ni1B—Cl1B106.21 (5)
S1—Ni—Cl106.68 (5)C35B—Fe2B—C34B90.1 (3)
C35—Fe—C3491.6 (2)C35B—Fe2B—N1B177.9 (2)
C35—Fe—N175.2 (2)C34B—Fe2B—N1B91.8 (2)
C34—Fe—N92.5 (2)C35B—Fe2B—S2B94.41 (19)
C35—Fe—S195.72 (19)C34B—Fe2B—S2B87.86 (18)
C34—Fe—S196.10 (18)N1B—Fe2B—S2B86.57 (13)
N—Fe—S186.26 (12)C35B—Fe2B—S1B92.44 (18)
C35—Fe—S290.91 (19)C34B—Fe2B—S1B95.97 (18)
C34—Fe—S287.63 (18)N1B—Fe2B—S1B86.47 (13)
N—Fe—S286.83 (12)S2B—Fe2B—S1B172.15 (7)
S1—Fe—S2172.29 (7)C35B—Fe2B—S3B90.78 (19)
C35—Fe—S388.34 (18)C34B—Fe2B—S3B179.1 (2)
C34—Fe—S3179.60 (19)N1B—Fe2B—S3B87.29 (13)
N—Fe—S387.58 (12)S2B—Fe2B—S3B92.30 (6)
S1—Fe—S383.53 (5)S1B—Fe2B—S3B83.76 (5)
S2—Fe—S392.76 (6)C29B—S1B—Ni1B106.3 (2)
C29—S1—Ni105.5 (2)C29B—S1B—Fe2B99.02 (19)
C29—S1—Fe99.79 (18)Ni1B—S1B—Fe2B95.18 (6)
Ni—S1—Fe95.51 (6)C31B—S2B—Fe2B98.7 (2)
C31—S2—Fe98.65 (18)C33B—S3B—Ni1B108.53 (19)
C33—S3—Ni109.84 (18)C33B—S3B—Fe2B97.50 (18)
C33—S3—Fe96.70 (17)Ni1B—S3B—Fe2B94.74 (5)
Ni—S3—Fe94.85 (5)C4B—P1B—C1B103.1 (2)
C4—P1—C10104.3 (2)C4B—P1B—C10B103.2 (3)
C4—P1—C1103.2 (2)C1B—P1B—C10B103.0 (3)
C10—P1—C1101.9 (2)C4B—P1B—Ni1B114.42 (18)
C4—P1—Ni113.45 (17)C1B—P1B—Ni1B115.71 (18)
C10—P1—Ni116.11 (16)C10B—P1B—Ni1B115.63 (19)
C1—P1—Ni116.24 (18)C3B—P2B—C16B105.9 (2)
C3—P2—C22101.7 (2)C3B—P2B—C22B102.3 (2)
C3—P2—C16105.9 (2)C16B—P2B—C22B103.9 (2)
C22—P2—C16104.3 (2)C3B—P2B—Ni1B116.50 (18)
C3—P2—Ni115.61 (18)C16B—P2B—Ni1B111.67 (17)
C22—P2—Ni115.54 (17)C22B—P2B—Ni1B115.26 (17)
C16—P2—Ni112.53 (17)C30B—N1B—C28B108.2 (5)
C30—N—C32110.8 (4)C30B—N1B—C32B112.5 (5)
C30—N—C28106.6 (4)C28B—N1B—C32B103.2 (5)
C32—N—C28105.9 (4)C30B—N1B—Fe2B109.8 (4)
C30—N—Fe109.4 (3)C28B—N1B—Fe2B109.3 (4)
C32—N—Fe114.3 (3)C32B—N1B—Fe2B113.5 (4)
C28—N—Fe109.4 (3)C2B—C1B—P1B114.5 (4)
C2—C1—P1114.5 (4)C2B—C1B—H1B1108.6
C2—C1—H1A108.6P1B—C1B—H1B1108.6
P1—C1—H1A108.6C2B—C1B—H1B2108.6
C2—C1—H1B108.6P1B—C1B—H1B2108.6
P1—C1—H1B108.6H1B1—C1B—H1B2107.6
H1A—C1—H1B107.6C1B—C2B—C3B114.4 (4)
C1—C2—C3113.5 (4)C1B—C2B—H2B1108.7
C1—C2—H2A108.9C3B—C2B—H2B1108.7
C3—C2—H2A108.9C1B—C2B—H2B2108.7
C1—C2—H2B108.9C3B—C2B—H2B2108.7
C3—C2—H2B108.9H2B1—C2B—H2B2107.6
H2A—C2—H2B107.7C2B—C3B—P2B114.7 (4)
C2—C3—P2115.9 (4)C2B—C3B—H3B1108.6
C2—C3—H3A108.3P2B—C3B—H3B1108.6
P2—C3—H3A108.3C2B—C3B—H3B2108.6
C2—C3—H3B108.3P2B—C3B—H3B2108.6
P2—C3—H3B108.3H3B1—C3B—H3B2107.6
H3A—C3—H3B107.4C5B—C4B—C9B116.8 (5)
C5—C4—C9118.9 (5)C5B—C4B—P1B121.2 (4)
C5—C4—P1121.0 (4)C9B—C4B—P1B121.9 (4)
C9—C4—P1120.0 (4)C4B—C5B—C6B122.0 (6)
C4—C5—C6120.6 (6)C4B—C5B—H5B119
C4—C5—H5119.7C6B—C5B—H5B119
C6—C5—H5119.7C7B—C6B—C5B120.2 (6)
C5—C6—C7118.5 (6)C7B—C6B—H6B119.9
C5—C6—H6120.7C5B—C6B—H6B119.9
C7—C6—H6120.7C6B—C7B—C8B118.2 (6)
C8—C7—C6120.6 (6)C6B—C7B—H7B120.9
C8—C7—H7119.7C8B—C7B—H7B120.9
C6—C7—H7119.7C9B—C8B—C7B121.0 (6)
C9—C8—C7119.7 (6)C9B—C8B—H8B119.5
C9—C8—H8120.2C7B—C8B—H8B119.5
C7—C8—H8120.2C8B—C9B—C4B121.6 (6)
C8—C9—C4121.4 (6)C8B—C9B—H9B119.2
C8—C9—H9119.3C4B—C9B—H9B119.2
C4—C9—H9119.3C15B—C10B—C11B120.5 (6)
C15—C10—C11119.1 (5)C15B—C10B—P1B119.9 (5)
C15—C10—P1121.6 (4)C11B—C10B—P1B119.5 (5)
C11—C10—P1119.3 (4)C12B—C11B—C10B120.1 (7)
C10—C11—C12119.5 (5)C12B—C11B—H11B120
C10—C11—H11120.2C10B—C11B—H11B120
C12—C11—H11120.2C13B—C12B—C11B119.2 (7)
C13—C12—C11121.0 (5)C13B—C12B—H12B120.4
C13—C12—H12119.5C11B—C12B—H12B120.4
C11—C12—H12119.5C12B—C13B—C14B122.5 (7)
C14—C13—C12119.6 (5)C12B—C13B—H13B118.7
C14—C13—H13120.2C14B—C13B—H13B118.7
C12—C13—H13120.2C13B—C14B—C15B119.6 (8)
C13—C14—C15120.4 (6)C13B—C14B—H14B120.2
C13—C14—H14119.8C15B—C14B—H14B120.2
C15—C14—H14119.8C10B—C15B—C14B118.0 (7)
C10—C15—C14120.3 (5)C10B—C15B—H15B121
C10—C15—H15119.9C14B—C15B—H15B121
C14—C15—H15119.9C21B—C16B—C17B118.3 (5)
C17—C16—C21119.1 (5)C21B—C16B—P2B122.9 (4)
C17—C16—P2118.8 (4)C17B—C16B—P2B118.7 (4)
C21—C16—P2121.9 (4)C18B—C17B—C16B120.7 (5)
C16—C17—C18121.3 (5)C18B—C17B—H17B119.7
C16—C17—H17119.4C16B—C17B—H17B119.7
C18—C17—H17119.4C17B—C18B—C19B121.9 (6)
C19—C18—C17119.0 (5)C17B—C18B—H18B119
C19—C18—H18120.5C19B—C18B—H18B119
C17—C18—H18120.5C18B—C19B—C20B119.1 (5)
C18—C19—C20120.9 (5)C18B—C19B—H19B120.5
C18—C19—H19119.6C20B—C19B—H19B120.5
C20—C19—H19119.6C21B—C20B—C19B120.4 (5)
C19—C20—C21119.4 (5)C21B—C20B—H20B119.8
C19—C20—H20120.3C19B—C20B—H20B119.8
C21—C20—H20120.3C20B—C21B—C16B119.6 (5)
C16—C21—C20120.3 (5)C20B—C21B—H21B120.2
C16—C21—H21119.9C16B—C21B—H21B120.2
C20—C21—H21119.9C23B—C22B—C27B118.4 (5)
C23—C22—C27119.2 (5)C23B—C22B—P2B122.2 (4)
C23—C22—P2122.0 (4)C27B—C22B—P2B119.3 (4)
C27—C22—P2118.8 (4)C22B—C23B—C24B119.9 (6)
C22—C23—C24120.7 (5)C22B—C23B—H23B120.1
C22—C23—H23119.7C24B—C23B—H23B120.1
C24—C23—H23119.7C25B—C24B—C23B121.7 (6)
C25—C24—C23119.5 (6)C25B—C24B—H24B119.1
C25—C24—H24120.2C23B—C24B—H24B119.1
C23—C24—H24120.2C24B—C25B—C26B118.9 (6)
C26—C25—C24120.6 (6)C24B—C25B—H25B120.6
C26—C25—H25119.7C26B—C25B—H25B120.6
C24—C25—H25119.7C27B—C26B—C25B120.4 (6)
C25—C26—C27120.0 (6)C27B—C26B—H26B119.8
C25—C26—H26120C25B—C26B—H26B119.8
C27—C26—H26120C26B—C27B—C22B120.6 (6)
C22—C27—C26120.0 (5)C26B—C27B—H27B119.7
C22—C27—H27120C22B—C27B—H27B119.7
C26—C27—H27120C29B—C28B—N1B117.8 (6)
C29—C28—N111.9 (4)C29B—C28B—H28C107.9
C29—C28—H28A109.2N1B—C28B—H28C107.9
N—C28—H28A109.2C29B—C28B—H28D107.9
C29—C28—H28B109.2N1B—C28B—H28D107.9
N—C28—H28B109.2H28C—C28B—H28D107.2
H28A—C28—H28B107.9C28B—C29B—S1B113.7 (5)
C28—C29—S1111.9 (4)C28B—C29B—H29C108.8
C28—C29—H29A109.2S1B—C29B—H29C108.8
S1—C29—H29A109.2C28B—C29B—H29D108.8
C28—C29—H29B109.2S1B—C29B—H29D108.8
S1—C29—H29B109.2H29C—C29B—H29D107.7
H29A—C29—H29B107.9N1B—C30B—C31B106.4 (5)
N—C30—C31109.8 (4)N1B—C30B—H30C110.5
N—C30—H30A109.7C31B—C30B—H30C110.5
C31—C30—H30A109.7N1B—C30B—H30D110.5
N—C30—H30B109.7C31B—C30B—H30D110.5
C31—C30—H30B109.7H30C—C30B—H30D108.6
H30A—C30—H30B108.2C30B—C31B—S2B108.4 (5)
C30—C31—S2109.7 (4)C30B—C31B—H31C110
C30—C31—H31A109.7S2B—C31B—H31C110
S2—C31—H31A109.7C30B—C31B—H31D110
C30—C31—H31B109.7S2B—C31B—H31D110
S2—C31—H31B109.7H31C—C31B—H31D108.4
H31A—C31—H31B108.2C33B—C32B—N1B115.4 (5)
N—C32—C33114.1 (5)C33B—C32B—H32C108.4
N—C32—H32A108.7N1B—C32B—H32C108.4
C33—C32—H32A108.7C33B—C32B—H32D108.4
N—C32—H32B108.7N1B—C32B—H32D108.4
C33—C32—H32B108.7H32C—C32B—H32D107.5
H32A—C32—H32B107.6C32B—C33B—S3B112.3 (4)
C32—C33—S3110.6 (4)C32B—C33B—H33C109.1
C32—C33—H33A109.5S3B—C33B—H33C109.1
S3—C33—H33A109.5C32B—C33B—H33D109.1
C32—C33—H33B109.5S3B—C33B—H33D109.1
S3—C33—H33B109.5H33C—C33B—H33D107.9
H33A—C33—H33B108.1O1B—C34B—Fe2B175.4 (8)
O1—C34—Fe175.3 (5)O2B—C35B—Fe2B176.9 (5)
O2—C35—Fe176.9 (5)N2—C37—C36175.4 (9)
P1B—Ni1B—P2B92.84 (6)N2B—C37B—C36B178.0 (10)
Fe—S1—C29—C289.4 (6)C29B—C28B—N1B—Fe2B43.0 (10)
S1—C29—C28—N38.6 (8)Fe2B—S2B—C31B—C30B25.8 (8)
C29—C28—N—Fe51.9 (7)S2B—C31B—C30B—N1B54.9 (10)
Fe—S2—C31—C3023.7 (6)C31B—C30B—N1B—Fe2B58.7 (9)
S2—C31—C30—N51.7 (8)Fe2B—S3B—C33B—C32B35.8 (7)
C31—C30—N—Fe55.3 (7)S3B—C33B—C32B—N1B42.1 (10)
Fe—S3—C33—C3238.3 (6)C33B—C32B—N1B—Fe2B24.5 (10)
S3—C33—C32—N45.8 (8)P1—C1—C2—C368.5 (8)
C33—C32—N—Fe27.3 (8)C1—C2—C3—P269.7 (8)
Fe2B—S1B—C29B—C28B3.0 (8)P1B—C1B—C2B—C3B69.3 (8)
S1B—C29B—C28B—N1B29.6 (12)C1B—C2B—C3B—P2B67.1 (8)
 

Acknowledgements

The authors thank the Biotechnology and Biological Sciences Research Council and the John Innes Foundation (SED) for financial support.

References

First citationBlessing, R. H. (1995). Acta Cryst. A51, 33–38.  CrossRef CAS Web of Science IUCr Journals Google Scholar
First citationDavies, S. C., Evans, D. J., Hughes, D. L., Longhurst, S. & Sanders, J. R. (1999). Chem. Commun. pp. 1935–1936.  Web of Science CSD CrossRef Google Scholar
First citationEvans, D. J. & Pickett, C. J. (2003). Chem. Soc. Rev. 32, 268–275.  Web of Science CrossRef PubMed 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 citationFlack, H. D. (1983). Acta Cryst. A39, 876–881.  CrossRef CAS Web of Science IUCr Journals Google Scholar
First citationNonius (2000). COLLECT. Nonius BV, Delft, The Netherlands.  Google Scholar
First citationOtwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, Macromolecular Crystallography, Part A, edited by C. W. Carter Jr & R. M. Sweet, pp. 307–326. New York: Academic Press.  Google Scholar
First citationSheldrick, G. M. (1997). SHELXS97 and SHELXL97. University of Göttingen, Germany.  Google Scholar
First citationSmith, M. C., Barclay, J. E., Cramer, S. P., Davies, S. C., Gu, W.-W., Hughes, D. L., Longhurst, S. & Evans, D. J. (2002). J. Chem. Soc. Dalton Trans. pp. 2641–2647.  Web of Science CSD CrossRef Google Scholar
First citationSmith, M. C., Barclay, J. E., Davies, S. C., Hughes, D. L. & Evans, D. J. (2003). Dalton Trans. pp. 4147–4151.  Web of Science CSD CrossRef Google Scholar

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