Dicarbonyl­dichloridobis(trimethyl­phosphane)iron(II)–carbonyl­dichlorido­tris(trimethyl­phosphane)iron(II)–tetra­hydro­furan (1/1/2)

Rath, N.P.; Stouffer, M.; Janssen, M.K.; Bleeke, J.R.

doi:10.1107/S1600536811009305

metal-organic compounds

CRYSTALLOGRAPHIC
COMMUNICATIONS

ISSN: 2056-9890

Volume 67| Part 4| April 2011| Page m462

doi:10.1107/S1600536811009305

Open

access

Dicarbonyldichloridobis(trimethylphosphane)iron(II)–carbonyldichloridotris(trimethylphosphane)iron(II)–tetrahydrofuran (1/1/2)

Nigam P. Rath,^a ^* Meghan Stouffer,^b Matthew K. Janssen ^b and John R. Bleeke ^b

^aDepartment of Chemistry and Biochemistry and Center for Nanoscience, University of Missouri–St Louis, 1 University Boulevard, St Louis, MO 63121-4400, USA, and ^bDepartment of Chemistry, Washington University, One Brookings Drive, St Louis, MO 63130-4899, USA
^*Correspondence e-mail: rathn@umsl.edu

(Received 25 February 2011; accepted 10 March 2011; online 19 March 2011)

The asymmetric unit of the title crystal, [FeCl₂(C₃H₉P)₃(CO)]·[FeCl₂(C₃H₉P)₂(CO)₂]·2C₄H₈O, contains half molecules of the two closely related Fe^II complexes lying on mirror planes and a tetrahydrofuran solvent molecule, one C atom of which is disordered over two sets of sites with site occupancy factors 0.633 (9) and 0.367 (9). In both Fe^II complex molecules, a distorted octahedral coordination geometry has been observed around the Fe atoms. Weak intermolecular C—H⋯O interactions are observed in the crystal structure.

Related literature

For the synthetic background, see: Harris et al. (1978 ). For the crystal structure of a related complex, see: Venturi et al. (2004 ).

Experimental

Crystal data

[FeCl₂(C₃H₉P)₃(CO)]·[FeCl₂(C₃H₉P)₂(CO)₂]·2C₄H₈O
M_r = 862.10
Orthorhombic, P n m a
a = 10.8391 (9) Å
b = 16.9670 (12) Å
c = 22.2871 (18) Å
V = 4098.8 (6) Å³
Z = 4
Mo Kα radiation
μ = 1.20 mm⁻¹
T = 100 K
0.20 × 0.12 × 0.10 mm

Data collection

Bruker APEXII CCD diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2008 ) T_min = 0.800, T_max = 0.895
144514 measured reflections
4904 independent reflections
3939 reflections with I > 2σ(I)
R_int = 0.090

Refinement

R[F² > 2σ(F²)] = 0.034
wR(F²) = 0.081
S = 1.06
4904 reflections
218 parameters
1 restraint
H-atom parameters constrained
Δρ_max = 0.68 e Å⁻³
Δρ_min = −0.70 e Å⁻³

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
C42—H42B⋯O1Sⁱ	0.98	2.53	3.422 (3)	151
C43—H43C⋯O1ⁱ	0.98	2.58	3.510 (3)	158
C43—H43A⋯O1ⁱⁱ	0.98	2.43	3.392 (3)	167
Symmetry codes: (i) $[x-{\script{1\over 2}}, y, -z+{\script{3\over 2}}]$ ; (ii) $[-x+{\script{3\over 2}}, -y+1, z+{\script{1\over 2}}]$ .

Data collection: APEX2 (Bruker, 2010 ); cell refinement: SAINT (Bruker, 2009 ); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008) and Mercury (Macrae et al., 2008 ); software used to prepare material for publication: SHELXTL and PLATON (Spek, 2009 ).

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536811009305/pv2394sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536811009305/pv2394Isup2.hkl

checkCIF report

Comment top

An interesting cocrystallization has occurred from a reaction of CO with Cl₂Fe(PMe₃)₂, resulting in compound (I), C₈H₁₈Cl₂FeO₂P₂, from the addition of two equivalents of CO to Cl₂Fe(PMe₃)₂ and compound (II), C₁₀H₂₇Cl₂FeOP₃, probably from the addition of one equivalent of CO, followed by the rapid addition of one equivalent of free PMe₃, which is present in the reaction solution. In this paper, we report the crystal structure of the two compounds, (I) and (II) which have been cocrystallized along with a molecule of tetrahydrofuran solvate per molecule of complex (Fig. 1).

The asymmetric unit of the title crystal contains half molecules of the two compounds, (I) and (II), lying on mirror planes and a molecule of tetrahydrofuran solvate, C₄H₈O; a carbon atom of the solvent molecule is disordered over two sites C4S and C4S' with site occupancy factors 0.633 (9) and 0.367 (9). In compound (I), the PMe₃ ligands occupying axial positions, are trans with respect to each other with an angle of 175.20 (4)° and the CO and Cl are trans with respect to each other at equatorial positions. In compound (II), the trans PMe₃ ligands are located at 166.41 (4)° to each other; the 3^rd PMe₃ is trans to a Cl. The octahedral coordination is completed with the 2nd Cl being trans to a CO ligand. In both compounds, the ligands around Fe lie in slightly distorted octahedral coordination geometry. An overlay plot of the two molecules drawn by Mercury (Macrae et al., 2008) shows the close similarity of the two molecules (Fig. 2).

There are weak intermolecular interactions of the type C–H···O which are observed between both the carbonyl O atoms of (I) and a methyl hydrogen atom of (II). The O of the solvent THF also has weak interactions with a methyl hydrogen atoms of (II) (Table 1).

Related literature top

For the synthetic background, see: Harris et al. (1978). For the crystal structure of a related complex, see: Venturi et al. (2004).

Experimental top

FeCl₂ (0.21 g, 1.62 x 10 ^-3 mol) and PMe₃ (0.40 ml, 3.86 x 10^-3) were stirred in 20 ml of THF for 10 min, producing a clear gray solution of Cl₂Fe(PMe₃)₂ (Harris et al., 1978) in the presence of excess PMe₃. Carbon monoxide was then bubbled through the solution until the color changed to an intense orange. The THF solvent was removed under vacuum and the resulting powder was extracted with pentane. After filtration through Celite, the pentane was removed under vacuum. The product was dissolved in a 1:2 mixture of THF and pentane and cooled to 243 K, causing orange crystals to form overnight.

Computing details top

Data collection: APEX2 (Bruker, 2010); cell refinement: SAINT (Bruker, 2009); data reduction: SAINT (Bruker, 2009); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008) and Mercury (Macrae, et al., 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008) and PLATON (Spek, 2009).

Figures top

	Fig. 1. The molecular structure of (I) and (II) with atom labels and 50% probability displacement ellipsoids for non-H atoms. Disordered atoms in the solvent are omitted for clarity. Symmetry codes represented by A in atomic labels: for (I) = x, 0.5 - y, z and for (II) = x, 1.5 - y, z.
	Fig. 2. Overlay plot of the two molecules.
	Fig. 3. A unit cell packing plot of the title crystal; H atoms have been omitted for clarity.

Dicarbonyldichloridobis(trimethylphosphane)iron(II)– carbonyldichloridotris(trimethylphosphane)iron(II)–tetrahydrofuran (1/1/2) top

Crystal data top

[FeCl₂(C₃H₉P)₃(CO)]·[FeCl₂(C₃H₉P)₂(CO)₂]·2C₄H₈O	D_x = 1.397 Mg m⁻³
M_r = 862.10	Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, Pnma	Cell parameters from 9975 reflections
a = 10.8391 (9) Å	θ = 2.6–27.4°
b = 16.9670 (12) Å	µ = 1.20 mm⁻¹
c = 22.2871 (18) Å	T = 100 K
V = 4098.8 (6) Å³	Plate, light yellow
Z = 4	0.20 × 0.12 × 0.10 mm
F(000) = 1808

Data collection top

Bruker APEXII CCD diffractometer	4904 independent reflections
Radiation source: fine-focus sealed tube	3939 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.090
Detector resolution: 8.3333 pixels mm^-1	θ_max = 27.6°, θ_min = 1.5°
ϕ and ω scans	h = −14→14
Absorption correction: multi-scan (SADABS; Bruker, 2008)	k = −21→22
T_min = 0.800, T_max = 0.895	l = −29→29
144514 measured reflections

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.034	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.081	H-atom parameters constrained
S = 1.06	w = 1/[σ²(F_o²) + (0.0323P)² + 5.017P] where P = (F_o² + 2F_c²)/3
4904 reflections	(Δ/σ)_max = 0.002
218 parameters	Δρ_max = 0.68 e Å⁻³
1 restraint	Δρ_min = −0.70 e Å⁻³

Crystal data top

[FeCl₂(C₃H₉P)₃(CO)]·[FeCl₂(C₃H₉P)₂(CO)₂]·2C₄H₈O	V = 4098.8 (6) Å³
M_r = 862.10	Z = 4
Orthorhombic, Pnma	Mo Kα radiation
a = 10.8391 (9) Å	µ = 1.20 mm⁻¹
b = 16.9670 (12) Å	T = 100 K
c = 22.2871 (18) Å	0.20 × 0.12 × 0.10 mm

Data collection top

Bruker APEXII CCD diffractometer	4904 independent reflections
Absorption correction: multi-scan (SADABS; Bruker, 2008)	3939 reflections with I > 2σ(I)
T_min = 0.800, T_max = 0.895	R_int = 0.090
144514 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.034	1 restraint
wR(F²) = 0.081	H-atom parameters constrained
S = 1.06	Δρ_max = 0.68 e Å⁻³
4904 reflections	Δρ_min = −0.70 e Å⁻³
218 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. SHELX restraints used:

delu o2 c2

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
Fe1	0.74441 (4)	0.2500	0.609986 (19)	0.01347 (10)
Cl1	0.64447 (5)	0.14941 (3)	0.66198 (2)	0.02064 (12)
P1	0.89145 (8)	0.2500	0.68214 (4)	0.01903 (18)
P2	0.58528 (8)	0.2500	0.54398 (4)	0.01575 (17)
O1	0.86416 (17)	0.37737 (10)	0.54685 (8)	0.0268 (4)
C1	0.8188 (2)	0.32598 (13)	0.57122 (10)	0.0180 (5)
C11	0.9949 (3)	0.33405 (17)	0.68026 (13)	0.0353 (7)
H11A	0.9465	0.3828	0.6812	0.053*
H11B	1.0441	0.3324	0.6434	0.053*
H11C	1.0498	0.3323	0.7152	0.053*
C12	0.8343 (4)	0.2500	0.75831 (15)	0.0277 (8)
H12A	0.7861	0.2036	0.7650	0.042*
H12B	0.9084	0.2500	0.7829	0.042*
C21	0.5823 (2)	0.33398 (15)	0.49372 (12)	0.0258 (5)
H21A	0.5116	0.3294	0.4665	0.039*
H21B	0.6587	0.3354	0.4703	0.039*
H21C	0.5749	0.3826	0.5172	0.039*
C22	0.4336 (3)	0.2500	0.57645 (16)	0.0263 (8)
H22A	0.3697	0.2500	0.5460	0.039*
H22B	0.4224	0.2044	0.6013	0.039*
Fe2	0.39182 (4)	0.7500	0.91114 (2)	0.01534 (11)
Cl2	0.17671 (7)	0.7500	0.90064 (4)	0.02288 (17)
Cl3	0.38648 (9)	0.7500	1.01832 (4)	0.0306 (2)
P3	0.43591 (8)	0.7500	0.81372 (4)	0.01842 (18)
P4	0.36847 (6)	0.61635 (3)	0.91539 (3)	0.01807 (13)
O2	0.6473 (3)	0.7500	0.92770 (12)	0.0318 (6)
C2	0.5567 (5)	0.7500	0.92171 (15)	0.0287 (9)
C31	0.3099 (3)	0.7500	0.76165 (16)	0.0280 (8)
H31A	0.3440	0.7500	0.7207	0.042*
H31B	0.2601	0.7974	0.7654	0.042*
C32	0.5302 (2)	0.66852 (14)	0.78642 (11)	0.0229 (5)
H32A	0.4848	0.6189	0.7912	0.034*
H32B	0.6071	0.6661	0.8095	0.034*
H32C	0.5493	0.6767	0.7439	0.034*
C41	0.2881 (3)	0.58171 (15)	0.98174 (11)	0.0291 (6)
H41A	0.2086	0.6088	0.9851	0.044*
H41B	0.3381	0.5929	1.0174	0.044*
H41C	0.2743	0.5248	0.9786	0.044*
C42	0.2761 (2)	0.56933 (14)	0.85754 (11)	0.0247 (5)
H42A	0.2698	0.5128	0.8659	0.037*
H42B	0.3152	0.5772	0.8184	0.037*
H42C	0.1933	0.5926	0.8572	0.037*
C43	0.5079 (2)	0.55672 (14)	0.91735 (11)	0.0240 (5)
H43A	0.5573	0.5712	0.9525	0.036*
H43B	0.5560	0.5659	0.8808	0.036*
H43C	0.4855	0.5009	0.9198	0.036*
C1S	0.7599 (3)	0.48598 (17)	0.79495 (13)	0.0420 (7)
H1S1	0.7804	0.4575	0.7575	0.050*
H1S2	0.6691	0.4908	0.7978	0.050*
C2S	0.8096 (3)	0.44219 (17)	0.84835 (14)	0.0413 (7)
H2S1	0.7417	0.4181	0.8717	0.050*
H2S2	0.8672	0.4001	0.8355	0.050*
C3S	0.8759 (3)	0.50294 (18)	0.88488 (13)	0.0400 (7)
H3S1	0.8205	0.5280	0.9146	0.048*	0.633 (9)
H3S2	0.9481	0.4801	0.9059	0.048*	0.633 (9)
C4S	0.9139 (6)	0.5590 (4)	0.8379 (3)	0.0371 (13)	0.633 (9)
H4S1	0.9280	0.6118	0.8555	0.044*	0.633 (9)
H4S2	0.9912	0.5411	0.8186	0.044*	0.633 (9)
O1S	0.8150 (2)	0.56183 (12)	0.79471 (9)	0.0454 (6)
H3S3	0.9638	0.4884	0.8897	0.048*	0.367 (9)
H3S4	0.8382	0.5075	0.9252	0.048*	0.367 (9)
C4S'	0.8641 (11)	0.5827 (7)	0.8499 (5)	0.0371 (13)	0.367 (9)
H4S3	0.8085	0.6195	0.8713	0.044*	0.367 (9)
H4S4	0.9457	0.6080	0.8450	0.044*	0.367 (9)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Fe1	0.0166 (2)	0.0124 (2)	0.0114 (2)	0.000	−0.00049 (17)	0.000
Cl1	0.0240 (3)	0.0195 (3)	0.0184 (3)	−0.0034 (2)	0.0011 (2)	0.0051 (2)
P1	0.0192 (4)	0.0221 (4)	0.0157 (4)	0.000	−0.0032 (3)	0.000
P2	0.0188 (4)	0.0154 (4)	0.0130 (4)	0.000	−0.0015 (3)	0.000
O1	0.0345 (10)	0.0197 (9)	0.0262 (9)	−0.0062 (7)	0.0047 (8)	0.0025 (7)
C1	0.0199 (11)	0.0182 (11)	0.0159 (11)	0.0019 (9)	−0.0024 (9)	−0.0033 (9)
C11	0.0331 (15)	0.0431 (16)	0.0295 (14)	−0.0166 (12)	−0.0103 (12)	0.0045 (12)
C12	0.032 (2)	0.036 (2)	0.0151 (17)	0.000	−0.0034 (15)	0.000
C21	0.0278 (13)	0.0243 (13)	0.0253 (13)	0.0000 (10)	−0.0057 (10)	0.0076 (10)
C22	0.0202 (17)	0.035 (2)	0.0233 (18)	0.000	−0.0009 (14)	0.000
Fe2	0.0170 (2)	0.0139 (2)	0.0151 (2)	0.000	0.00190 (18)	0.000
Cl2	0.0173 (4)	0.0231 (4)	0.0282 (4)	0.000	0.0019 (3)	0.000
Cl3	0.0299 (5)	0.0303 (5)	0.0314 (5)	0.000	0.0029 (4)	0.000
P3	0.0199 (4)	0.0185 (4)	0.0168 (4)	0.000	−0.0012 (3)	0.000
P4	0.0214 (3)	0.0147 (3)	0.0181 (3)	−0.0008 (2)	0.0026 (2)	0.0005 (2)
O2	0.0430 (17)	0.0244 (14)	0.0281 (15)	0.000	0.0089 (13)	0.000
C2	0.066 (3)	0.0088 (15)	0.0116 (16)	0.000	0.0014 (18)	0.000
C31	0.0295 (19)	0.0314 (19)	0.0231 (18)	0.000	−0.0049 (15)	0.000
C32	0.0262 (12)	0.0209 (12)	0.0216 (12)	0.0000 (9)	0.0044 (10)	−0.0014 (9)
C41	0.0387 (15)	0.0201 (12)	0.0284 (13)	−0.0003 (11)	0.0112 (12)	0.0053 (10)
C42	0.0257 (13)	0.0197 (12)	0.0287 (13)	−0.0063 (10)	−0.0027 (10)	−0.0017 (10)
C43	0.0267 (13)	0.0182 (12)	0.0272 (13)	0.0027 (10)	−0.0013 (10)	−0.0005 (10)
C1S	0.066 (2)	0.0282 (15)	0.0321 (15)	−0.0039 (14)	−0.0086 (15)	−0.0017 (12)
C2S	0.055 (2)	0.0303 (15)	0.0383 (17)	−0.0008 (14)	−0.0094 (15)	0.0058 (13)
C3S	0.0549 (19)	0.0383 (17)	0.0269 (14)	−0.0017 (14)	−0.0064 (14)	0.0052 (12)
C4S	0.040 (4)	0.042 (3)	0.029 (3)	−0.013 (2)	−0.008 (2)	0.005 (2)
O1S	0.0659 (15)	0.0324 (11)	0.0378 (12)	−0.0139 (10)	−0.0191 (11)	0.0110 (9)
C3S'	0.0549 (19)	0.0383 (17)	0.0269 (14)	−0.0017 (14)	−0.0064 (14)	0.0052 (12)
C4S'	0.040 (4)	0.042 (3)	0.029 (3)	−0.013 (2)	−0.008 (2)	0.005 (2)
O1S'	0.0659 (15)	0.0324 (11)	0.0378 (12)	−0.0139 (10)	−0.0191 (11)	0.0110 (9)

Geometric parameters (Å, º) top

Fe1—C1ⁱ	1.749 (2)	P4—C42	1.817 (2)
Fe1—C1	1.749 (2)	P4—C43	1.819 (2)
Fe1—P1	2.2641 (10)	O2—C2	0.991 (5)
Fe1—P2	2.2670 (9)	C31—H31A	0.9837
Fe1—Cl1ⁱ	2.3300 (6)	C31—H31B	0.9732
Fe1—Cl1	2.3300 (6)	C32—H32A	0.9800
P1—C12	1.807 (4)	C32—H32B	0.9800
P1—C11	1.814 (3)	C32—H32C	0.9800
P1—C11ⁱ	1.814 (3)	C41—H41A	0.9800
P2—C22	1.796 (4)	C41—H41B	0.9800
P2—C21	1.813 (2)	C41—H41C	0.9800
P2—C21ⁱ	1.813 (2)	C42—H42A	0.9800
O1—C1	1.139 (3)	C42—H42B	0.9800
C11—H11A	0.9800	C42—H42C	0.9800
C11—H11B	0.9800	C43—H43A	0.9800
C11—H11C	0.9800	C43—H43B	0.9800
C12—H12A	0.9565	C43—H43C	0.9800
C12—H12B	0.9731	C1S—O1S	1.419 (3)
C21—H21A	0.9800	C1S—C2S	1.503 (4)
C21—H21B	0.9800	C1S—H1S1	0.9899
C21—H21C	0.9800	C1S—H1S2	0.9896
C22—H22A	0.9693	C2S—C3S	1.497 (4)
C22—H22B	0.9597	C2S—H2S1	0.9895
Fe2—C2	1.803 (5)	C2S—H2S2	0.9908
Fe2—P3	2.2232 (10)	C3S—C4S	1.472 (6)
Fe2—P4ⁱⁱ	2.2837 (6)	C3S—H3S1	0.9900
Fe2—P4	2.2838 (6)	C3S—H3S2	0.9900
Fe2—Cl2	2.3433 (9)	C4S—O1S	1.442 (6)
Fe2—Cl3	2.3895 (11)	C4S—H4S1	0.9900
P3—C31	1.792 (4)	C4S—H4S2	0.9900
P3—C32	1.823 (2)	C4S'—H4S3	0.9900
P3—C32ⁱⁱ	1.823 (2)	C4S'—H4S4	0.9900
P4—C41	1.814 (2)

C1ⁱ—Fe1—C1	94.97 (15)	C31—P3—Fe2	117.95 (13)
C1ⁱ—Fe1—P1	91.50 (8)	C32—P3—Fe2	116.50 (8)
C1—Fe1—P1	91.50 (8)	C32ⁱⁱ—P3—Fe2	116.50 (8)
C1ⁱ—Fe1—P2	91.74 (8)	C41—P4—C42	99.88 (13)
C1—Fe1—P2	91.74 (8)	C41—P4—C43	101.48 (12)
P1—Fe1—P2	175.20 (4)	C42—P4—C43	103.34 (12)
C1ⁱ—Fe1—Cl1ⁱ	179.61 (8)	C41—P4—Fe2	114.12 (9)
C1—Fe1—Cl1ⁱ	85.42 (7)	C42—P4—Fe2	117.88 (8)
P1—Fe1—Cl1ⁱ	88.51 (2)	C43—P4—Fe2	117.46 (8)
P2—Fe1—Cl1ⁱ	88.22 (2)	O2—C2—Fe2	179.8 (4)
C1ⁱ—Fe1—Cl1	85.42 (7)	P3—C31—H31A	108.3
C1—Fe1—Cl1	179.61 (8)	P3—C31—H31B	111.6
P1—Fe1—Cl1	88.51 (2)	H31A—C31—H31B	106.7
P2—Fe1—Cl1	88.22 (2)	P3—C32—H32A	109.5
Cl1ⁱ—Fe1—Cl1	94.19 (3)	P3—C32—H32B	109.5
C12—P1—C11	103.51 (12)	H32A—C32—H32B	109.5
C12—P1—C11ⁱ	103.51 (12)	P3—C32—H32C	109.5
C11—P1—C11ⁱ	103.6 (2)	H32A—C32—H32C	109.5
C12—P1—Fe1	115.20 (13)	H32B—C32—H32C	109.5
C11—P1—Fe1	114.74 (9)	P4—C41—H41A	109.5
C11ⁱ—P1—Fe1	114.74 (9)	P4—C41—H41B	109.5
C22—P2—C21	103.45 (11)	H41A—C41—H41B	109.5
C22—P2—C21ⁱ	103.45 (11)	P4—C41—H41C	109.5
C21—P2—C21ⁱ	103.62 (18)	H41A—C41—H41C	109.5
C22—P2—Fe1	115.78 (12)	H41B—C41—H41C	109.5
C21—P2—Fe1	114.50 (9)	P4—C42—H42A	109.5
C21ⁱ—P2—Fe1	114.50 (9)	P4—C42—H42B	109.5
O1—C1—Fe1	177.4 (2)	H42A—C42—H42B	109.5
P1—C11—H11A	109.5	P4—C42—H42C	109.5
P1—C11—H11B	109.5	H42A—C42—H42C	109.5
H11A—C11—H11B	109.5	H42B—C42—H42C	109.5
P1—C11—H11C	109.5	P4—C43—H43A	109.5
H11A—C11—H11C	109.5	P4—C43—H43B	109.5
H11B—C11—H11C	109.5	H43A—C43—H43B	109.5
P1—C12—H12A	109.5	P4—C43—H43C	109.5
P1—C12—H12B	104.3	H43A—C43—H43C	109.5
H12A—C12—H12B	111.3	H43B—C43—H43C	109.5
P2—C21—H21A	109.5	O1S—C1S—C2S	107.5 (2)
P2—C21—H21B	109.5	O1S—C1S—H1S1	110.2
H21A—C21—H21B	109.5	C2S—C1S—H1S1	110.2
P2—C21—H21C	109.5	O1S—C1S—H1S2	110.1
H21A—C21—H21C	109.5	C2S—C1S—H1S2	110.3
H21B—C21—H21C	109.5	H1S1—C1S—H1S2	108.5
P2—C22—H22A	111.9	C3S—C2S—C1S	105.2 (2)
P2—C22—H22B	110.4	C3S—C2S—H2S1	110.8
H22A—C22—H22B	108.2	C1S—C2S—H2S1	110.7
C2—Fe2—P3	85.09 (11)	C3S—C2S—H2S2	110.5
C2—Fe2—P4ⁱⁱ	96.00 (2)	C1S—C2S—H2S2	110.7
P3—Fe2—P4ⁱⁱ	93.689 (19)	H2S1—C2S—H2S2	108.9
C2—Fe2—P4	96.00 (2)	C4S—C3S—C2S	101.1 (3)
P3—Fe2—P4	93.687 (19)	C4S—C3S—H3S1	111.6
P4ⁱⁱ—Fe2—P4	166.40 (4)	C2S—C3S—H3S1	111.6
C2—Fe2—Cl2	178.23 (11)	C4S—C3S—H3S2	111.6
P3—Fe2—Cl2	96.68 (4)	C2S—C3S—H3S2	111.6
P4ⁱⁱ—Fe2—Cl2	83.905 (19)	H3S1—C3S—H3S2	109.4
P4—Fe2—Cl2	83.906 (19)	O1S—C4S—C3S	106.8 (4)
C2—Fe2—Cl3	83.88 (11)	O1S—C4S—H4S1	110.4
P3—Fe2—Cl3	168.98 (4)	C3S—C4S—H4S1	110.4
P4ⁱⁱ—Fe2—Cl3	87.469 (19)	O1S—C4S—H4S2	110.4
P4—Fe2—Cl3	87.471 (19)	C3S—C4S—H4S2	110.4
Cl2—Fe2—Cl3	94.34 (3)	H4S1—C4S—H4S2	108.6
C31—P3—C32	102.17 (11)	C1S—O1S—C4S	106.3 (3)
C31—P3—C32ⁱⁱ	102.17 (11)	H4S3—C4S'—H4S4	108.9
C32—P3—C32ⁱⁱ	98.60 (16)

C1ⁱ—Fe1—P1—C12	−132.49 (7)	P4ⁱⁱ—Fe2—P3—C32	153.62 (10)
C1—Fe1—P1—C12	132.49 (7)	P4—Fe2—P3—C32	−37.81 (10)
Cl1ⁱ—Fe1—P1—C12	47.118 (16)	Cl2—Fe2—P3—C32	−122.09 (9)
Cl1—Fe1—P1—C12	−47.117 (16)	Cl3—Fe2—P3—C32	57.91 (9)
C1ⁱ—Fe1—P1—C11	107.43 (14)	C2—Fe2—P3—C32ⁱⁱ	−57.91 (9)
C1—Fe1—P1—C11	12.42 (14)	P4ⁱⁱ—Fe2—P3—C32ⁱⁱ	37.81 (10)
Cl1ⁱ—Fe1—P1—C11	−72.95 (12)	P4—Fe2—P3—C32ⁱⁱ	−153.62 (9)
Cl1—Fe1—P1—C11	−167.19 (12)	Cl2—Fe2—P3—C32ⁱⁱ	122.09 (9)
C1ⁱ—Fe1—P1—C11ⁱ	−12.42 (14)	Cl3—Fe2—P3—C32ⁱⁱ	−57.91 (9)
C1—Fe1—P1—C11ⁱ	−107.43 (14)	C2—Fe2—P4—C41	111.10 (15)
Cl1ⁱ—Fe1—P1—C11ⁱ	167.19 (12)	P3—Fe2—P4—C41	−163.46 (11)
Cl1—Fe1—P1—C11ⁱ	72.96 (12)	P4ⁱⁱ—Fe2—P4—C41	−40.7 (2)
C1ⁱ—Fe1—P2—C22	132.49 (7)	Cl2—Fe2—P4—C41	−67.12 (11)
C1—Fe1—P2—C22	−132.49 (7)	Cl3—Fe2—P4—C41	27.52 (11)
Cl1ⁱ—Fe1—P2—C22	−47.128 (16)	C2—Fe2—P4—C42	−132.18 (15)
Cl1—Fe1—P2—C22	47.126 (16)	P3—Fe2—P4—C42	−46.74 (10)
C1ⁱ—Fe1—P2—C21	−107.25 (12)	P4ⁱⁱ—Fe2—P4—C42	76.00 (19)
C1—Fe1—P2—C21	−12.23 (12)	Cl2—Fe2—P4—C42	49.60 (10)
Cl1ⁱ—Fe1—P2—C21	73.13 (10)	Cl3—Fe2—P4—C42	144.24 (10)
Cl1—Fe1—P2—C21	167.38 (10)	C2—Fe2—P4—C43	−7.49 (15)
C1ⁱ—Fe1—P2—C21ⁱ	12.23 (12)	P3—Fe2—P4—C43	77.96 (10)
C1—Fe1—P2—C21ⁱ	107.25 (12)	P4ⁱⁱ—Fe2—P4—C43	−159.30 (17)
Cl1ⁱ—Fe1—P2—C21ⁱ	−167.39 (10)	Cl2—Fe2—P4—C43	174.30 (10)
Cl1—Fe1—P2—C21ⁱ	−73.14 (10)	Cl3—Fe2—P4—C43	−91.06 (10)
C2—Fe2—P3—C31	180.0	O1S—C1S—C2S—C3S	11.0 (4)
P4ⁱⁱ—Fe2—P3—C31	−84.29 (2)	C1S—C2S—C3S—C4S	−28.5 (4)
P4—Fe2—P3—C31	84.29 (2)	C2S—C3S—C4S—O1S	36.8 (5)
Cl2—Fe2—P3—C31	0.0	C2S—C1S—O1S—C4S	11.8 (4)
Cl3—Fe2—P3—C31	180.000 (1)	C3S—C4S—O1S—C1S	−31.1 (6)
C2—Fe2—P3—C32	57.91 (9)

Symmetry codes: (i) x, −y+1/2, z; (ii) x, −y+3/2, z.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
C42—H42B···O1Sⁱⁱⁱ	0.98	2.53	3.422 (3)	151
C43—H43C···O1ⁱⁱⁱ	0.98	2.58	3.510 (3)	158
C43—H43A···O1^iv	0.98	2.43	3.392 (3)	167

Symmetry codes: (iii) x−1/2, y, −z+3/2; (iv) −x+3/2, −y+1, z+1/2.

Experimental details

Crystal data
Chemical formula	[FeCl₂(C₃H₉P)₃(CO)]·[FeCl₂(C₃H₉P)₂(CO)₂]·2C₄H₈O
M_r	862.10
Crystal system, space group	Orthorhombic, Pnma
Temperature (K)	100
a, b, c (Å)	10.8391 (9), 16.9670 (12), 22.2871 (18)
V (Å³)	4098.8 (6)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	1.20
Crystal size (mm)	0.20 × 0.12 × 0.10

Data collection
Diffractometer	Bruker APEXII CCD diffractometer
Absorption correction	Multi-scan (SADABS; Bruker, 2008)
T_min, T_max	0.800, 0.895
No. of measured, independent and observed [I > 2σ(I)] reflections	144514, 4904, 3939
R_int	0.090
(sin θ/λ)_max (Å⁻¹)	0.652

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.034, 0.081, 1.06
No. of reflections	4904
No. of parameters	218
No. of restraints	1
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.68, −0.70

Computer programs: APEX2 (Bruker, 2010), SAINT (Bruker, 2009), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008) and Mercury (Macrae, et al., 2008), SHELXTL (Sheldrick, 2008) and PLATON (Spek, 2009).

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
C42—H42B···O1Sⁱ	0.98	2.53	3.422 (3)	151
C43—H43C···O1ⁱ	0.98	2.58	3.510 (3)	158
C43—H43A···O1ⁱⁱ	0.98	2.43	3.392 (3)	167

Symmetry codes: (i) x−1/2, y, −z+3/2; (ii) −x+3/2, −y+1, z+1/2.

Acknowledgements

The authors acknowledge financial support from the National Science Foundation (grant No. CHE 0420497) for the purchase of the X-ray diffractometer.

References

Bruker (2008). SADABS. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Bruker (2009). SAINT. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Bruker (2010). APEX2. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Harris, T. V., Rathke, J. W. & Muetterties, E. L. (1978). J. Am. Chem. Soc. 100, 6966–6977. CrossRef CAS Google Scholar
Macrae, C. F., Bruno, I. J., Chisholm, J. A., Edgington, P. R., McCabe, P., Pidcock, E., Rodriguez-Monge, L., Taylor, R., van de Streek, J. & Wood, P. A. (2008). J. Appl. Cryst. 41, 466–470. Web of Science CrossRef CAS IUCr Journals Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Spek, A. L. (2009). Acta Cryst. D65, 148–155. Web of Science CrossRef CAS IUCr Journals Google Scholar
Venturi, C., Bellachioma, G., Cardaci, G. & Macchioni, A. (2004). Inorg. Chim. Acta, 357, 3712–3720. Web of Science CSD CrossRef CAS 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.

CRYSTALLOGRAPHIC
COMMUNICATIONS

ISSN: 2056-9890

Volume 67| Part 4| April 2011| Page m462

doi:10.1107/S1600536811009305

Open

access

Format		BIBTeX
		EndNote
		RefMan
		Refer
		Medline
		CIF
		SGML
		Plain Text

Format		BIBTeX
		EndNote
		RefMan
		Refer
		Medline
		CIF
		SGML
		Plain Text

Search IUCr Journals		doi		Advanced search
Author		volume	page

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

Di­carbonyl­di­chloridobis(tri­methyl­phosphane)iron(II)–carbonyl­di­chlorido­tris­(tri­methyl­phosphane)iron(II)–tetra­hydro­furan (1/1/2)

Related literature

Experimental

Crystal data

Data collection

Refinement

Supporting information

Acknowledgements

References

metal-organic compounds

Dicarbonyldichloridobis(trimethylphosphane)iron(II)–carbonyldichloridotris(trimethylphosphane)iron(II)–tetrahydrofuran (1/1/2)