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

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890

Tri­chloridobis(ethyl­di­phenyl­phosphine)(tetra­hydro­furan)­molybdenum(III)

aChemical Faculty, Gdańsk University of Technology, Narutowicza 11/12, Gdańsk PL 80233, Poland
*Correspondence e-mail: lukas_ponikiewski@vp.pl

(Received 10 May 2010; accepted 7 June 2010; online 16 June 2010)

In the mononuclear title compound, [MoCl3(C4H8O)(C14H15P)2], obtained by the reaction of trichloro­tris­(tetra­hydro­furan)­molybdenum(III) and ethyl­diphenyl­phosphine in tetra­hydro­furan (THF) solution, the MoIII atom is six-coordinated by one O atom of a THF mol­ecule, two P atoms from two ethyl­diphenyl­phosphine ligands and three Cl atoms in a distorted octa­hedral geometry. The C atoms of the THF molecule are disordered over two positions in a 0.55 (2):0.45 (2) ratio.

Related literature

For the structures of similar molybdenum complexes and for bond-length data, see: Cotton & Jianrui (1996[Cotton, F. A. & Jianrui, S. (1996). Inorg. Chim. Acta, 251, 101-104.]); Cotton & Vidyasagar (1995[Cotton, F. A. & Vidyasagar, K. (1995). Polyhedron, 14, 3077-3085.]); Hofacker et al. (1989[Hofacker, P., Friebel, C., Debhnicke, K., Bauml, P., Hiller, W. & Strähle, J. (1989). Z. Naturforsch. Teil B, 44, 1161-1166.]); Borgmann et al. (1997[Borgmann, C., Limberg, C. & Driess, A. (1997). J. Organomet. Chem. 541, 367-375.]). For the synthesis, see: Anker et al. (1975[Anker, M. W., Chatt, J., Leigh, G. J. & Wedd, A. G. (1975). J. Chem. Soc. Dalton Trans. pp. 2639-2645.]).

[Scheme 1]

Experimental

Crystal data
  • [MoCl3(C4H8O)(C14H15P)2]

  • Mr = 702.85

  • Monoclinic, P 21 /c

  • a = 15.437 Å

  • b = 13.356 Å

  • c = 20.229 Å

  • β = 128.87°

  • V = 3247.1 Å3

  • Z = 4

  • Mo Kα radiation

  • μ = 0.77 mm−1

  • T = 120 K

  • 0.13 × 0.10 × 0.04 mm

Data collection
  • Oxford Diffraction KM-4/Xcalibur diffractometer with a Sapphire2 detector

  • Absorption correction: analytical [CrysAlis RED (Oxford Diffraction, 2006[Oxford Diffraction (2006). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Abingdon, England.]). based on expressions derived by Clark & Reid (1995[Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897.])] Tmin = 0.937, Tmax = 0.970

  • 25240 measured reflections

  • 7022 independent reflections

  • 2985 reflections with I > 2σ(I)

  • Rint = 0.089

Refinement
  • R[F2 > 2σ(F2)] = 0.044

  • wR(F2) = 0.115

  • S = 0.81

  • 7022 reflections

  • 385 parameters

  • H-atom parameters constrained

  • Δρmax = 0.70 e Å−3

  • Δρmin = −0.54 e Å−3

Table 1
Selected bond lengths (Å)

Mo1—O1 2.206 (3)
Mo1—Cl1 2.3871 (13)
Mo1—Cl2 2.3822 (13)
Mo1—Cl3 2.4126 (13)
Mo1—P1 2.5964 (14)
Mo1—P2 2.5974 (13)

Data collection: CrysAlis CCD (Oxford Diffraction, 2006[Oxford Diffraction (2006). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Abingdon, England.]); cell refinement: CrysAlis RED (Oxford Diffraction, 2006[Oxford Diffraction (2006). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Abingdon, England.]); data reduction: CrysAlis RED; 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 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


Comment top

The title molecule [MoCl3(PEtPh2)(THF)] was prepared as a potential adduct for synthesis with lithium phosphanides of the formula R2P—P(SiMe3)Li (R = tBu, iPr, Et2N, iPr2N).

The MoIII atom resides in a distorted MoCl3OP2 octahedral environment. The equatorial positions are occupied by three Cl atoms and one O atom from the THF, while the axial positions are occupied by P atoms from two ethyldiphenylphosphine residues. The Mo—Cl bond length [2.3871 (13) Å, 2.3822 (13) Å, 2.4126 (13) Å], the Mo—P bond length [2.5964 (14) Å, 2.5974 (13) Å] and the Mo—O bond length [2.206 (3) Å] are very similar to the previously reported molybdenum complexes (Cotton & Vidyasagar, 1995; Cotton & Jianrui, 1996; Hofacker et al., 1989; Borgmann et al., 1997).

Atoms C29, C30, C31, C32 from the THF molecule were disordered over two positions. During the refinement process the disorder models were refined with occupancies of 0.55 (2) and 0.45 (2).

Related literature top

For the structures of similar molybdenum complexes and for bond-length data, see: Cotton & Jianrui (1996); Cotton & Vidyasagar (1995); Hofacker et al. (1989); Borgmann et al. (1997). For the synthesis, see: Anker et al. (1975).

Experimental top

The title compound was prepared according to the previously published method (Anker et al., 1975)

Refinement top

Atoms C29, C30, C31, C32 were disordered over two positions. During the refinement process the disorder models were refined with occupancies of 0.55 (2) and 0.45 (2). H atoms bonded to C were included in calculated positions and refined as riding on their parent C atom with C—H = 0.95 Å, Uiso(H) = 1.2 Ueq(C) for aromatic; C—H = 0.99 Å, Uiso(H) = 1.2 Ueq(C) for methylene; and C—H = 0.98 Å, Uiso(H) = 1.5 Ueq(C) for methyl atoms.

Computing details top

Data collection: CrysAlis CCD (Oxford Diffraction, 2006); cell refinement: CrysAlis RED (Oxford Diffraction, 2006); data reduction: CrysAlis RED (Oxford Diffraction, 2006); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).

Figures top
[Figure 1] Fig. 1. The molecular structure of the title compound showing the atomic numbering scheme. Displacement ellipsoids are drawn at the 50% probability level. For clarity, all H atoms and the minor component of the disorder have been omitted.
Trichloridobis(ethyldiphenylphosphine)(tetrahydrofuran)molybdenum(III) top
Crystal data top
[MoCl3(C4H8O)(C14H15P)2]F(000) = 1444
Mr = 702.85Dx = 1.438 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 5220 reflections
a = 15.437 Åθ = 2.0–28.9°
b = 13.356 ŵ = 0.77 mm1
c = 20.229 ÅT = 120 K
β = 128.87°Block, orange
V = 3247.1 Å30.13 × 0.1 × 0.04 mm
Z = 4
Data collection top
Oxford Diffraction KM-4/Xcalibur
diffractometer with a Sapphire2 (large Be window) detector
7022 independent reflections
Graphite monochromator2985 reflections with I > 2σ(I)
Detector resolution: 8.1883 pixels mm-1Rint = 0.089
ω scansθmax = 27°, θmin = 2°
Absorption correction: analytical
[CrysAlis RED (Oxford Diffraction, 2006). based on expressions derived by Clark & Reid (1995)]
h = 1519
Tmin = 0.937, Tmax = 0.97k = 1617
25240 measured reflectionsl = 2522
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)] = 0.044Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.115H-atom parameters constrained
S = 0.81 w = 1/[σ2(Fo2) + (0.0551P)2]
where P = (Fo2 + 2Fc2)/3
7022 reflections(Δ/σ)max = 0.001
385 parametersΔρmax = 0.70 e Å3
0 restraintsΔρmin = 0.54 e Å3
Crystal data top
[MoCl3(C4H8O)(C14H15P)2]V = 3247.1 Å3
Mr = 702.85Z = 4
Monoclinic, P21/cMo Kα radiation
a = 15.437 ŵ = 0.77 mm1
b = 13.356 ÅT = 120 K
c = 20.229 Å0.13 × 0.1 × 0.04 mm
β = 128.87°
Data collection top
Oxford Diffraction KM-4/Xcalibur
diffractometer with a Sapphire2 (large Be window) detector
7022 independent reflections
Absorption correction: analytical
[CrysAlis RED (Oxford Diffraction, 2006). based on expressions derived by Clark & Reid (1995)]
2985 reflections with I > 2σ(I)
Tmin = 0.937, Tmax = 0.97Rint = 0.089
25240 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0440 restraints
wR(F2) = 0.115H-atom parameters constrained
S = 0.81Δρmax = 0.70 e Å3
7022 reflectionsΔρmin = 0.54 e Å3
385 parameters
Special details top

Experimental. CrysAlis RED (Oxford Diffraction, 2006) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by Clark & Reid (1995)

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)
Mo10.57979 (3)0.74957 (4)0.63166 (2)0.03356 (12)
Cl10.53421 (13)0.92350 (10)0.61183 (10)0.0612 (4)
Cl20.62891 (9)0.74919 (11)0.76928 (7)0.0511 (3)
Cl30.62090 (10)0.57325 (9)0.64269 (9)0.0488 (3)
P10.78469 (10)0.78721 (10)0.69759 (9)0.0415 (3)
P20.37606 (10)0.70228 (10)0.56343 (8)0.0370 (3)
O10.5361 (2)0.7484 (3)0.50482 (18)0.0411 (7)
C10.8589 (4)0.8883 (4)0.7753 (3)0.0495 (14)
C20.8104 (5)0.9421 (5)0.8018 (4)0.075 (2)
H2A0.73580.92770.77850.09*
C30.8682 (6)1.0174 (6)0.8621 (5)0.099 (3)
H3A0.83341.05470.87970.118*
C40.9750 (6)1.0370 (5)0.8957 (4)0.084 (2)
H4A1.01611.08710.9380.101*
C51.0232 (5)0.9849 (5)0.8687 (4)0.0711 (19)
H5A1.097610.89180.085*
C60.9674 (4)0.9118 (4)0.8095 (4)0.0645 (17)
H6A1.00260.87650.79130.077*
C70.8016 (4)0.8198 (4)0.6187 (3)0.0462 (13)
C80.8262 (6)0.7500 (6)0.5828 (4)0.0873 (15)
H8A0.83890.68260.60180.105*
C90.8329 (5)0.7744 (6)0.5206 (4)0.084 (2)
H9A0.85070.72420.49770.101*
C100.8145 (5)0.8694 (6)0.4914 (4)0.080 (2)
H10A0.82080.88660.4490.096*
C110.7871 (6)0.9387 (5)0.5234 (4)0.0873 (15)
H11A0.77121.00520.50210.105*
C120.7820 (7)0.9141 (5)0.5872 (5)0.098 (2)
H12A0.76410.96490.60970.117*
C130.8800 (4)0.6808 (4)0.7548 (4)0.0563 (16)
H13A0.850.62210.71660.068*
H13B0.95290.69770.76980.068*
C140.8976 (5)0.6530 (5)0.8342 (4)0.084 (2)
H14A0.95620.60220.86540.126*
H14B0.82830.62610.81940.126*
H14C0.91980.71260.870.126*
C150.2980 (4)0.7756 (3)0.5873 (3)0.0414 (13)
C160.1881 (4)0.7565 (4)0.5442 (3)0.0572 (14)
H16A0.15260.7050.50260.069*
C170.1273 (5)0.8118 (5)0.5608 (4)0.0656 (17)
H17A0.0510.79720.53180.079*
C180.1780 (5)0.8869 (5)0.6187 (4)0.0639 (17)
H18A0.13640.92640.62910.077*
C190.2870 (5)0.9059 (5)0.6615 (4)0.0675 (18)
H19A0.32170.95840.70210.081*
C200.3483 (4)0.8502 (4)0.6471 (3)0.0524 (14)
H20A0.42550.86330.67850.063*
C210.2853 (4)0.7107 (4)0.4475 (3)0.0416 (13)
C220.2670 (4)0.6302 (4)0.3982 (3)0.0497 (14)
H22A0.29830.5670.42410.06*
C230.2041 (4)0.6398 (5)0.3121 (3)0.0594 (16)
H23A0.19270.58350.27870.071*
C240.1579 (4)0.7294 (5)0.2740 (3)0.0630 (18)
H24A0.11370.73570.21410.076*
C250.1750 (4)0.8081 (5)0.3209 (4)0.0621 (16)
H25A0.14270.87070.29420.075*
C260.2390 (4)0.8001 (4)0.4079 (4)0.0599 (16)
H26A0.25090.85740.44050.072*
C270.3571 (4)0.5747 (4)0.5836 (3)0.0466 (13)
H27A0.27650.55980.54680.056*
H27B0.39130.52810.56780.056*
C280.4074 (4)0.5557 (4)0.6752 (3)0.0624 (16)
H28A0.39790.4850.68240.094*
H28B0.36990.59770.69010.094*
H28C0.48680.57210.71230.094*
C290.542 (4)0.6602 (15)0.4672 (19)0.064 (3)0.55 (2)
H29A0.48190.61280.45020.077*0.55 (2)
H29B0.61460.62630.50770.077*0.55 (2)
C300.5284 (16)0.6963 (11)0.3911 (10)0.066 (3)0.55 (2)
H30A0.49190.64490.34580.079*0.55 (2)
H30B0.60120.71390.40620.079*0.55 (2)
C310.4556 (16)0.7877 (16)0.3635 (13)0.073 (5)0.55 (2)
H31A0.46970.83630.33430.088*0.55 (2)
H31B0.37580.76910.3250.088*0.55 (2)
C320.488 (5)0.8294 (17)0.4431 (19)0.068 (7)0.55 (2)
H32A0.54270.88380.46340.081*0.55 (2)
H32B0.42180.8570.43440.081*0.55 (2)
C29A0.541 (5)0.6650 (18)0.461 (2)0.056 (3)0.45 (2)
H29C0.50870.6040.46560.067*0.45 (2)
H29D0.61910.65090.48570.067*0.45 (2)
C30A0.474 (2)0.6981 (14)0.3695 (13)0.075 (4)0.45 (2)
H30C0.49620.66170.33970.091*0.45 (2)
H30D0.3930.68950.33820.091*0.45 (2)
C31A0.506 (2)0.8069 (16)0.3820 (17)0.063 (4)0.45 (2)
H31C0.45020.84620.33040.076*0.45 (2)
H31D0.57970.81530.39590.076*0.45 (2)
C32A0.510 (6)0.839 (2)0.455 (3)0.064 (7)0.45 (2)
H32C0.56830.89060.49010.077*0.45 (2)
H32D0.43750.8670.43460.077*0.45 (2)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mo10.0421 (2)0.0281 (2)0.0318 (2)0.00186 (18)0.02382 (17)0.0012 (2)
Cl10.0978 (11)0.0283 (8)0.0685 (10)0.0094 (7)0.0575 (9)0.0041 (7)
Cl20.0565 (7)0.0651 (8)0.0343 (6)0.0004 (7)0.0297 (6)0.0013 (8)
Cl30.0583 (8)0.0320 (7)0.0577 (9)0.0070 (6)0.0372 (7)0.0059 (6)
P10.0426 (8)0.0390 (8)0.0446 (8)0.0019 (5)0.0281 (7)0.0007 (6)
P20.0405 (7)0.0363 (8)0.0323 (8)0.0025 (5)0.0220 (6)0.0010 (6)
O10.0568 (19)0.0352 (18)0.0328 (16)0.0028 (17)0.0288 (15)0.0022 (19)
C10.057 (4)0.048 (4)0.045 (3)0.008 (2)0.032 (3)0.005 (3)
C20.076 (4)0.081 (5)0.086 (5)0.033 (3)0.060 (4)0.042 (4)
C30.109 (6)0.114 (6)0.105 (6)0.055 (5)0.083 (5)0.069 (5)
C40.088 (5)0.074 (5)0.069 (5)0.040 (4)0.039 (4)0.031 (4)
C50.055 (4)0.062 (5)0.075 (5)0.018 (3)0.031 (4)0.012 (4)
C60.060 (4)0.057 (4)0.080 (5)0.013 (3)0.046 (4)0.011 (3)
C70.049 (3)0.046 (4)0.053 (3)0.004 (2)0.036 (3)0.004 (3)
C80.154 (5)0.060 (3)0.093 (4)0.013 (3)0.099 (4)0.013 (3)
C90.100 (5)0.096 (6)0.086 (5)0.038 (4)0.073 (4)0.009 (4)
C100.114 (5)0.085 (6)0.089 (5)0.006 (4)0.087 (5)0.007 (4)
C110.154 (5)0.060 (3)0.093 (4)0.013 (3)0.099 (4)0.013 (3)
C120.204 (8)0.041 (4)0.116 (6)0.005 (4)0.133 (6)0.006 (4)
C130.048 (3)0.049 (4)0.066 (4)0.003 (2)0.033 (3)0.014 (3)
C140.074 (4)0.084 (5)0.067 (5)0.013 (3)0.031 (4)0.029 (4)
C150.046 (3)0.042 (4)0.033 (3)0.007 (2)0.024 (3)0.002 (2)
C160.051 (3)0.067 (4)0.057 (3)0.003 (3)0.036 (3)0.008 (3)
C170.058 (4)0.086 (5)0.064 (4)0.018 (3)0.044 (4)0.009 (4)
C180.072 (4)0.069 (5)0.061 (4)0.028 (3)0.047 (4)0.010 (3)
C190.079 (5)0.070 (5)0.056 (4)0.011 (3)0.044 (4)0.011 (3)
C200.051 (3)0.061 (4)0.042 (3)0.004 (3)0.028 (3)0.005 (3)
C210.040 (3)0.044 (3)0.036 (3)0.002 (2)0.022 (3)0.006 (2)
C220.054 (3)0.050 (4)0.048 (3)0.005 (2)0.033 (3)0.001 (3)
C230.060 (4)0.072 (5)0.035 (3)0.003 (3)0.024 (3)0.012 (3)
C240.056 (4)0.089 (5)0.030 (3)0.013 (3)0.020 (3)0.005 (3)
C250.067 (4)0.061 (4)0.047 (4)0.022 (3)0.030 (3)0.013 (3)
C260.076 (4)0.047 (4)0.047 (4)0.014 (3)0.034 (3)0.002 (3)
C270.051 (3)0.040 (3)0.052 (3)0.004 (2)0.034 (3)0.001 (3)
C280.077 (4)0.059 (4)0.058 (4)0.004 (3)0.045 (3)0.014 (3)
C290.089 (5)0.066 (4)0.053 (5)0.004 (4)0.052 (5)0.013 (4)
C300.084 (6)0.076 (5)0.053 (6)0.004 (5)0.051 (6)0.011 (4)
C310.086 (14)0.083 (10)0.040 (9)0.014 (9)0.035 (11)0.004 (7)
C320.094 (19)0.057 (6)0.049 (8)0.010 (8)0.043 (12)0.020 (6)
C29A0.086 (5)0.055 (5)0.052 (5)0.005 (4)0.056 (5)0.012 (4)
C30A0.094 (7)0.077 (6)0.058 (6)0.003 (6)0.049 (6)0.014 (5)
C31A0.076 (14)0.085 (10)0.036 (10)0.011 (9)0.039 (12)0.003 (7)
C32A0.092 (19)0.055 (6)0.047 (8)0.008 (8)0.044 (12)0.020 (6)
Geometric parameters (Å, º) top
Mo1—O12.206 (3)C16—H16A0.95
Mo1—Cl12.3871 (13)C17—C181.356 (8)
Mo1—Cl22.3822 (13)C17—H17A0.95
Mo1—Cl32.4126 (13)C18—C191.348 (7)
Mo1—P12.5964 (14)C18—H18A0.95
Mo1—P22.5974 (13)C19—C201.371 (7)
P1—C71.824 (6)C19—H19A0.95
P1—C11.830 (5)C20—H20A0.95
P1—C131.840 (5)C21—C261.364 (7)
P2—C271.818 (5)C21—C221.370 (7)
P2—C211.830 (5)C22—C231.368 (7)
P2—C151.838 (5)C22—H22A0.95
O1—C291.434 (15)C23—C241.358 (8)
O1—C29A1.453 (16)C23—H23A0.95
O1—C321.455 (15)C24—C251.326 (7)
O1—C32A1.459 (17)C24—H24A0.95
C1—C21.366 (7)C25—C261.380 (7)
C1—C61.389 (7)C25—H25A0.95
C2—C31.390 (8)C26—H26A0.95
C2—H2A0.95C27—C281.514 (7)
C3—C41.358 (9)C27—H27A0.99
C3—H3A0.95C27—H27B0.99
C4—C51.359 (9)C28—H28A0.98
C4—H4A0.95C28—H28B0.98
C5—C61.355 (8)C28—H28C0.98
C5—H5A0.95C29—C301.499 (17)
C6—H6A0.95C29—H29A0.99
C7—C121.358 (8)C29—H29B0.99
C7—C81.373 (8)C30—C311.510 (16)
C8—C91.364 (9)C30—H30A0.99
C8—H8A0.95C30—H30B0.99
C9—C101.352 (9)C31—C321.464 (16)
C9—H9A0.95C31—H31A0.99
C10—C111.341 (8)C31—H31B0.99
C10—H10A0.95C32—H32A0.99
C11—C121.381 (9)C32—H32B0.99
C11—H11A0.95C29A—C30A1.514 (18)
C12—H12A0.95C29A—H29C0.99
C13—C141.498 (8)C29A—H29D0.99
C13—H13A0.99C30A—C31A1.506 (17)
C13—H13B0.99C30A—H30C0.99
C14—H14A0.98C30A—H30D0.99
C14—H14B0.98C31A—C32A1.509 (18)
C14—H14C0.98C31A—H31C0.99
C15—C161.359 (7)C31A—H31D0.99
C15—C201.371 (7)C32A—H32C0.99
C16—C171.391 (7)C32A—H32D0.99
O1—Mo1—Cl2179.21 (10)C18—C17—H17A120.3
O1—Mo1—Cl188.22 (10)C16—C17—H17A120.3
Cl2—Mo1—Cl192.44 (5)C19—C18—C17120.3 (5)
O1—Mo1—Cl388.34 (10)C19—C18—H18A119.8
Cl2—Mo1—Cl391.01 (5)C17—C18—H18A119.8
Cl1—Mo1—Cl3176.50 (6)C18—C19—C20120.8 (6)
O1—Mo1—P189.05 (9)C18—C19—H19A119.6
Cl2—Mo1—P190.49 (5)C20—C19—H19A119.6
Cl1—Mo1—P191.92 (5)C19—C20—C15119.8 (5)
Cl3—Mo1—P188.66 (4)C19—C20—H20A120.1
O1—Mo1—P289.76 (8)C15—C20—H20A120.1
Cl2—Mo1—P290.67 (4)C26—C21—C22117.8 (5)
Cl1—Mo1—P290.94 (5)C26—C21—P2120.3 (4)
Cl3—Mo1—P288.41 (4)C22—C21—P2121.8 (4)
P1—Mo1—P2176.87 (5)C23—C22—C21120.8 (5)
C7—P1—C1102.7 (2)C23—C22—H22A119.6
C7—P1—C13103.8 (3)C21—C22—H22A119.6
C1—P1—C13101.9 (3)C24—C23—C22120.4 (6)
C7—P1—Mo1113.20 (16)C24—C23—H23A119.8
C1—P1—Mo1119.23 (19)C22—C23—H23A119.8
C13—P1—Mo1114.15 (18)C25—C24—C23119.6 (6)
C27—P2—C21104.1 (2)C25—C24—H24A120.2
C27—P2—C15102.5 (2)C23—C24—H24A120.2
C21—P2—C15101.7 (2)C24—C25—C26120.9 (6)
C27—P2—Mo1114.84 (16)C24—C25—H25A119.6
C21—P2—Mo1111.36 (16)C26—C25—H25A119.6
C15—P2—Mo1120.40 (17)C21—C26—C25120.6 (6)
C29—O1—C32108.9 (15)C21—C26—H26A119.7
C29A—O1—C32104.0 (14)C25—C26—H26A119.7
C29—O1—C32A113.6 (15)C28—C27—P2113.6 (4)
C29A—O1—C32A108.5 (16)C28—C27—H27A108.8
C29—O1—Mo1123.2 (9)P2—C27—H27A108.8
C29A—O1—Mo1128.2 (10)C28—C27—H27B108.8
C32—O1—Mo1127.6 (11)P2—C27—H27B108.8
C32A—O1—Mo1122.9 (12)H27A—C27—H27B107.7
C2—C1—C6118.3 (5)C27—C28—H28A109.5
C2—C1—P1121.5 (4)C27—C28—H28B109.5
C6—C1—P1120.2 (4)H28A—C28—H28B109.5
C1—C2—C3121.1 (6)C27—C28—H28C109.5
C1—C2—H2A119.5H28A—C28—H28C109.5
C3—C2—H2A119.5H28B—C28—H28C109.5
C4—C3—C2119.2 (7)O1—C29—C30105.5 (14)
C4—C3—H3A120.4O1—C29—H29A110.6
C2—C3—H3A120.4C30—C29—H29A110.6
C5—C4—C3120.0 (6)O1—C29—H29B110.6
C5—C4—H4A120C30—C29—H29B110.6
C3—C4—H4A120H29A—C29—H29B108.8
C6—C5—C4121.3 (6)C29—C30—C31103.3 (18)
C6—C5—H5A119.3C29—C30—H30A111.1
C4—C5—H5A119.3C31—C30—H30A111.1
C5—C6—C1120.1 (6)C29—C30—H30B111.1
C5—C6—H6A120C31—C30—H30B111.1
C1—C6—H6A120H30A—C30—H30B109.1
C12—C7—C8115.8 (6)C32—C31—C30104.0 (19)
C12—C7—P1121.3 (5)C32—C31—H31A111
C8—C7—P1122.7 (4)C30—C31—H31A111
C9—C8—C7122.1 (7)C32—C31—H31B111
C9—C8—H8A118.9C30—C31—H31B111
C7—C8—H8A118.9H31A—C31—H31B109
C10—C9—C8120.7 (7)O1—C32—C31107.4 (17)
C10—C9—H9A119.7O1—C32—H32A110.2
C8—C9—H9A119.7C31—C32—H32A110.2
C11—C10—C9118.7 (7)O1—C32—H32B110.2
C11—C10—H10A120.7C31—C32—H32B110.2
C9—C10—H10A120.7H32A—C32—H32B108.5
C10—C11—C12120.4 (6)O1—C29A—C30A105.3 (18)
C10—C11—H11A119.8O1—C29A—H29C110.7
C12—C11—H11A119.8C30A—C29A—H29C110.7
C7—C12—C11122.2 (7)O1—C29A—H29D110.7
C7—C12—H12A118.9C30A—C29A—H29D110.7
C11—C12—H12A118.9H29C—C29A—H29D108.8
C14—C13—P1113.7 (4)C31A—C30A—C29A100 (2)
C14—C13—H13A108.8C31A—C30A—H30C111.8
P1—C13—H13A108.8C29A—C30A—H30C111.8
C14—C13—H13B108.8C31A—C30A—H30D111.8
P1—C13—H13B108.8C29A—C30A—H30D111.8
H13A—C13—H13B107.7H30C—C30A—H30D109.5
C13—C14—H14A109.5C30A—C31A—C32A104 (2)
C13—C14—H14B109.5C30A—C31A—H31C110.9
H14A—C14—H14B109.5C32A—C31A—H31C110.9
C13—C14—H14C109.5C30A—C31A—H31D110.9
H14A—C14—H14C109.5C32A—C31A—H31D110.9
H14B—C14—H14C109.5H31C—C31A—H31D108.9
C16—C15—C20119.4 (5)O1—C32A—C31A105 (2)
C16—C15—P2119.5 (4)O1—C32A—H32C110.7
C20—C15—P2121.1 (4)C31A—C32A—H32C110.7
C15—C16—C17120.3 (6)O1—C32A—H32D110.7
C15—C16—H16A119.8C31A—C32A—H32D110.7
C17—C16—H16A119.8H32C—C32A—H32D108.8
C18—C17—C16119.4 (6)
O1—Mo1—P1—C711.0 (2)P1—C7—C8—C9176.5 (5)
Cl2—Mo1—P1—C7169.7 (2)C7—C8—C9—C100.5 (12)
Cl1—Mo1—P1—C777.2 (2)C8—C9—C10—C111.4 (11)
Cl3—Mo1—P1—C799.3 (2)C9—C10—C11—C122.3 (11)
O1—Mo1—P1—C1131.9 (2)C8—C7—C12—C110.5 (11)
Cl2—Mo1—P1—C148.8 (2)P1—C7—C12—C11175.6 (6)
Cl1—Mo1—P1—C143.7 (2)C10—C11—C12—C71.4 (12)
Cl3—Mo1—P1—C1139.8 (2)C7—P1—C13—C14168.8 (4)
O1—Mo1—P1—C13107.4 (2)C1—P1—C13—C1462.4 (5)
Cl2—Mo1—P1—C1371.9 (2)Mo1—P1—C13—C1467.6 (5)
Cl1—Mo1—P1—C13164.4 (2)C27—P2—C15—C1658.1 (5)
Cl3—Mo1—P1—C1319.1 (2)C21—P2—C15—C1649.4 (5)
O1—Mo1—P2—C27108.1 (2)Mo1—P2—C15—C16173.0 (4)
Cl2—Mo1—P2—C2771.3 (2)C27—P2—C15—C20122.9 (4)
Cl1—Mo1—P2—C27163.7 (2)C21—P2—C15—C20129.7 (4)
Cl3—Mo1—P2—C2719.7 (2)Mo1—P2—C15—C206.1 (5)
O1—Mo1—P2—C219.9 (2)C20—C15—C16—C170.2 (8)
Cl2—Mo1—P2—C21170.76 (18)P2—C15—C16—C17179.3 (4)
Cl1—Mo1—P2—C2178.31 (18)C15—C16—C17—C181.8 (9)
Cl3—Mo1—P2—C2198.26 (18)C16—C17—C18—C191.9 (9)
O1—Mo1—P2—C15128.8 (2)C17—C18—C19—C200.3 (9)
Cl2—Mo1—P2—C1551.90 (18)C18—C19—C20—C151.3 (9)
Cl1—Mo1—P2—C1540.55 (18)C16—C15—C20—C191.3 (8)
Cl3—Mo1—P2—C15142.89 (18)P2—C15—C20—C19177.8 (4)
Cl1—Mo1—O1—C29180 (2)C27—P2—C21—C26150.8 (5)
Cl3—Mo1—O1—C290 (2)C15—P2—C21—C2644.6 (5)
P1—Mo1—O1—C2989 (2)Mo1—P2—C21—C2684.9 (5)
P2—Mo1—O1—C2989 (2)C27—P2—C21—C2233.3 (5)
Cl1—Mo1—O1—C29A179 (3)C15—P2—C21—C22139.5 (4)
Cl3—Mo1—O1—C29A2 (3)Mo1—P2—C21—C2291.0 (4)
P1—Mo1—O1—C29A87 (3)C26—C21—C22—C230.1 (8)
P2—Mo1—O1—C29A90 (3)P2—C21—C22—C23176.1 (4)
Cl1—Mo1—O1—C326 (3)C21—C22—C23—C240.6 (9)
Cl3—Mo1—O1—C32173 (3)C22—C23—C24—C250.7 (9)
P1—Mo1—O1—C3298 (3)C23—C24—C25—C260.1 (9)
P2—Mo1—O1—C3285 (3)C22—C21—C26—C250.7 (8)
Cl1—Mo1—O1—C32A7 (4)P2—C21—C26—C25176.7 (4)
Cl3—Mo1—O1—C32A173 (4)C24—C25—C26—C210.6 (9)
P1—Mo1—O1—C32A85 (4)C21—P2—C27—C28169.0 (4)
P2—Mo1—O1—C32A98 (4)C15—P2—C27—C2863.3 (4)
C7—P1—C1—C2128.5 (5)Mo1—P2—C27—C2869.0 (4)
C13—P1—C1—C2124.3 (5)C32—O1—C29—C3017 (4)
Mo1—P1—C1—C22.4 (6)C32A—O1—C29—C305 (5)
C7—P1—C1—C652.0 (5)Mo1—O1—C29—C30168.8 (15)
C13—P1—C1—C655.3 (5)O1—C29—C30—C3130 (4)
Mo1—P1—C1—C6178.0 (4)C29—C30—C31—C3233 (4)
C6—C1—C2—C30.9 (10)C29—O1—C32—C314 (5)
P1—C1—C2—C3178.7 (6)C29A—O1—C32—C316 (5)
C1—C2—C3—C40.6 (12)C32A—O1—C32—C31120 (18)
C2—C3—C4—C51.6 (12)Mo1—O1—C32—C31170.0 (17)
C3—C4—C5—C61.2 (11)C30—C31—C32—O123 (4)
C4—C5—C6—C10.3 (10)C32—O1—C29A—C30A11 (4)
C2—C1—C6—C51.3 (9)C32A—O1—C29A—C30A22 (5)
P1—C1—C6—C5178.2 (5)Mo1—O1—C29A—C30A165.2 (15)
C1—P1—C7—C1247.7 (6)O1—C29A—C30A—C31A38 (4)
C13—P1—C7—C12153.6 (5)C29A—C30A—C31A—C32A39 (4)
Mo1—P1—C7—C1282.1 (5)C29—O1—C32A—C31A4 (6)
C1—P1—C7—C8137.5 (5)C29A—O1—C32A—C31A3 (6)
C13—P1—C7—C831.6 (6)C32—O1—C32A—C31A73 (13)
Mo1—P1—C7—C892.7 (5)Mo1—O1—C32A—C31A170 (2)
C12—C7—C8—C91.4 (10)C30A—C31A—C32A—O127 (5)

Experimental details

Crystal data
Chemical formula[MoCl3(C4H8O)(C14H15P)2]
Mr702.85
Crystal system, space groupMonoclinic, P21/c
Temperature (K)120
a, b, c (Å)15.437, 13.356, 20.229
β (°) 128.87
V3)3247.1
Z4
Radiation typeMo Kα
µ (mm1)0.77
Crystal size (mm)0.13 × 0.1 × 0.04
Data collection
DiffractometerOxford Diffraction KM-4/Xcalibur
diffractometer with a Sapphire2 (large Be window) detector
Absorption correctionAnalytical
[CrysAlis RED (Oxford Diffraction, 2006). based on expressions derived by Clark & Reid (1995)]
Tmin, Tmax0.937, 0.97
No. of measured, independent and
observed [I > 2σ(I)] reflections
25240, 7022, 2985
Rint0.089
(sin θ/λ)max1)0.639
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.044, 0.115, 0.81
No. of reflections7022
No. of parameters385
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.70, 0.54

Computer programs: CrysAlis CCD (Oxford Diffraction, 2006), CrysAlis RED (Oxford Diffraction, 2006), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), ORTEP-3 for Windows (Farrugia, 1997), WinGX (Farrugia, 1999).

Selected bond lengths (Å) top
Mo1—O12.206 (3)Mo1—Cl32.4126 (13)
Mo1—Cl12.3871 (13)Mo1—P12.5964 (14)
Mo1—Cl22.3822 (13)Mo1—P22.5974 (13)
 

Acknowledgements

The work was undertaken with financial support from the Polish State Committee, grant No. NN204271535.

References

First citationAnker, M. W., Chatt, J., Leigh, G. J. & Wedd, A. G. (1975). J. Chem. Soc. Dalton Trans. pp. 2639–2645.  CrossRef Web of Science
First citationBorgmann, C., Limberg, C. & Driess, A. (1997). J. Organomet. Chem. 541, 367–375.  CSD CrossRef CAS Web of Science
First citationClark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887–897.  CrossRef CAS Web of Science IUCr Journals
First citationCotton, F. A. & Jianrui, S. (1996). Inorg. Chim. Acta, 251, 101–104.  CSD CrossRef CAS Web of Science
First citationCotton, F. A. & Vidyasagar, K. (1995). Polyhedron, 14, 3077–3085.  CSD CrossRef CAS Web of Science
First citationFarrugia, L. J. (1997). J. Appl. Cryst. 30, 565.  CrossRef IUCr Journals
First citationFarrugia, L. J. (1999). J. Appl. Cryst. 32, 837–838.  CrossRef CAS IUCr Journals
First citationHofacker, P., Friebel, C., Debhnicke, K., Bauml, P., Hiller, W. & Strähle, J. (1989). Z. Naturforsch. Teil B, 44, 1161–1166.  CAS
First citationOxford Diffraction (2006). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Abingdon, England.
First citationSheldrick, G. M. (2008). Acta Cryst. A64, 112–122.  Web of Science CrossRef CAS IUCr Journals

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.

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890
Follow Acta Cryst. E
Sign up for e-alerts
Follow Acta Cryst. on Twitter
Follow us on facebook
Sign up for RSS feeds