Trichloridobis(ethyl­diphenyl­phosphine)(tetra­hydro­furan)­molybdenum(III)

Kruczyński, T.; Pikies, J.; Ponikiewski, Ł.

doi:10.1107/S1600536810021690

metal-organic compounds

CRYSTALLOGRAPHIC
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ISSN: 2056-9890

Volume 66| Part 7| July 2010| Page m786

doi:10.1107/S1600536810021690

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Trichloridobis(ethyldiphenylphosphine)(tetrahydrofuran)molybdenum(III)

Tomasz Kruczyński,^a Jerzy Pikies ^a and Łukasz Ponikiewski ^a ^*

^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 Mo^III 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 & Vidyasagar (1995 ); Hofacker et al. (1989 ); Borgmann et al. (1997 ). For the synthesis, see: Anker et al. (1975 ).

Experimental

Crystal data

[MoCl₃(C₄H₈O)(C₁₄H₁₅P)₂]
M_r = 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 )] T_min = 0.937, T_max = 0.970
25240 measured reflections
7022 independent reflections
2985 reflections with I > 2σ(I)
R_int = 0.089

Refinement

R[F² > 2σ(F²)] = 0.044
wR(F²) = 0.115
S = 0.81
7022 reflections
385 parameters
H-atom parameters constrained
Δρ_max = 0.70 e Å⁻³
Δρ_min = −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 ); 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 ).

Supporting information

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536810021690/ez2211sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536810021690/ez2211Isup2.hkl

checkCIF report

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 Mo^III 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)

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

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
M_r = 702.85	D_x = 1.438 Mg m⁻³
Monoclinic, P2₁/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 5220 reflections
a = 15.437 Å	θ = 2.0–28.9°
b = 13.356 Å	µ = 0.77 mm⁻¹
c = 20.229 Å	T = 120 K
β = 128.87°	Block, orange
V = 3247.1 Å³	0.13 × 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 monochromator	2985 reflections with I > 2σ(I)
Detector resolution: 8.1883 pixels mm^-1	R_int = 0.089
ω scans	θ_max = 27°, θ_min = 2°
Absorption correction: analytical [CrysAlis RED (Oxford Diffraction, 2006). based on expressions derived by Clark & Reid (1995)]	h = −15→19
T_min = 0.937, T_max = 0.97	k = −16→17
25240 measured reflections	l = −25→22

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)] = 0.044	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.115	H-atom parameters constrained
S = 0.81	w = 1/[σ²(F_o²) + (0.0551P)²] where P = (F_o² + 2F_c²)/3
7022 reflections	(Δ/σ)_max = 0.001
385 parameters	Δρ_max = 0.70 e Å⁻³
0 restraints	Δρ_min = −0.54 e Å⁻³

Crystal data top

[MoCl₃(C₄H₈O)(C₁₄H₁₅P)₂]	V = 3247.1 Å³
M_r = 702.85	Z = 4
Monoclinic, P2₁/c	Mo Kα radiation
a = 15.437 Å	µ = 0.77 mm⁻¹
b = 13.356 Å	T = 120 K
c = 20.229 Å	0.13 × 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)
T_min = 0.937, T_max = 0.97	R_int = 0.089
25240 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.044	0 restraints
wR(F²) = 0.115	H-atom parameters constrained
S = 0.81	Δρ_max = 0.70 e Å⁻³
7022 reflections	Δρ_min = −0.54 e Å⁻³
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

	x	y	z	U_iso*/U_eq	Occ. (<1)
Mo1	0.57979 (3)	0.74957 (4)	0.63166 (2)	0.03356 (12)
Cl1	0.53421 (13)	0.92350 (10)	0.61183 (10)	0.0612 (4)
Cl2	0.62891 (9)	0.74919 (11)	0.76928 (7)	0.0511 (3)
Cl3	0.62090 (10)	0.57325 (9)	0.64269 (9)	0.0488 (3)
P1	0.78469 (10)	0.78721 (10)	0.69759 (9)	0.0415 (3)
P2	0.37606 (10)	0.70228 (10)	0.56343 (8)	0.0370 (3)
O1	0.5361 (2)	0.7484 (3)	0.50482 (18)	0.0411 (7)
C1	0.8589 (4)	0.8883 (4)	0.7753 (3)	0.0495 (14)
C2	0.8104 (5)	0.9421 (5)	0.8018 (4)	0.075 (2)
H2A	0.7358	0.9277	0.7785	0.09*
C3	0.8682 (6)	1.0174 (6)	0.8621 (5)	0.099 (3)
H3A	0.8334	1.0547	0.8797	0.118*
C4	0.9750 (6)	1.0370 (5)	0.8957 (4)	0.084 (2)
H4A	1.0161	1.0871	0.938	0.101*
C5	1.0232 (5)	0.9849 (5)	0.8687 (4)	0.0711 (19)
H5A	1.0976	1	0.8918	0.085*
C6	0.9674 (4)	0.9118 (4)	0.8095 (4)	0.0645 (17)
H6A	1.0026	0.8765	0.7913	0.077*
C7	0.8016 (4)	0.8198 (4)	0.6187 (3)	0.0462 (13)
C8	0.8262 (6)	0.7500 (6)	0.5828 (4)	0.0873 (15)
H8A	0.8389	0.6826	0.6018	0.105*
C9	0.8329 (5)	0.7744 (6)	0.5206 (4)	0.084 (2)
H9A	0.8507	0.7242	0.4977	0.101*
C10	0.8145 (5)	0.8694 (6)	0.4914 (4)	0.080 (2)
H10A	0.8208	0.8866	0.449	0.096*
C11	0.7871 (6)	0.9387 (5)	0.5234 (4)	0.0873 (15)
H11A	0.7712	1.0052	0.5021	0.105*
C12	0.7820 (7)	0.9141 (5)	0.5872 (5)	0.098 (2)
H12A	0.7641	0.9649	0.6097	0.117*
C13	0.8800 (4)	0.6808 (4)	0.7548 (4)	0.0563 (16)
H13A	0.85	0.6221	0.7166	0.068*
H13B	0.9529	0.6977	0.7698	0.068*
C14	0.8976 (5)	0.6530 (5)	0.8342 (4)	0.084 (2)
H14A	0.9562	0.6022	0.8654	0.126*
H14B	0.8283	0.6261	0.8194	0.126*
H14C	0.9198	0.7126	0.87	0.126*
C15	0.2980 (4)	0.7756 (3)	0.5873 (3)	0.0414 (13)
C16	0.1881 (4)	0.7565 (4)	0.5442 (3)	0.0572 (14)
H16A	0.1526	0.705	0.5026	0.069*
C17	0.1273 (5)	0.8118 (5)	0.5608 (4)	0.0656 (17)
H17A	0.051	0.7972	0.5318	0.079*
C18	0.1780 (5)	0.8869 (5)	0.6187 (4)	0.0639 (17)
H18A	0.1364	0.9264	0.6291	0.077*
C19	0.2870 (5)	0.9059 (5)	0.6615 (4)	0.0675 (18)
H19A	0.3217	0.9584	0.7021	0.081*
C20	0.3483 (4)	0.8502 (4)	0.6471 (3)	0.0524 (14)
H20A	0.4255	0.8633	0.6785	0.063*
C21	0.2853 (4)	0.7107 (4)	0.4475 (3)	0.0416 (13)
C22	0.2670 (4)	0.6302 (4)	0.3982 (3)	0.0497 (14)
H22A	0.2983	0.567	0.4241	0.06*
C23	0.2041 (4)	0.6398 (5)	0.3121 (3)	0.0594 (16)
H23A	0.1927	0.5835	0.2787	0.071*
C24	0.1579 (4)	0.7294 (5)	0.2740 (3)	0.0630 (18)
H24A	0.1137	0.7357	0.2141	0.076*
C25	0.1750 (4)	0.8081 (5)	0.3209 (4)	0.0621 (16)
H25A	0.1427	0.8707	0.2942	0.075*
C26	0.2390 (4)	0.8001 (4)	0.4079 (4)	0.0599 (16)
H26A	0.2509	0.8574	0.4405	0.072*
C27	0.3571 (4)	0.5747 (4)	0.5836 (3)	0.0466 (13)
H27A	0.2765	0.5598	0.5468	0.056*
H27B	0.3913	0.5281	0.5678	0.056*
C28	0.4074 (4)	0.5557 (4)	0.6752 (3)	0.0624 (16)
H28A	0.3979	0.485	0.6824	0.094*
H28B	0.3699	0.5977	0.6901	0.094*
H28C	0.4868	0.5721	0.7123	0.094*
C29	0.542 (4)	0.6602 (15)	0.4672 (19)	0.064 (3)	0.55 (2)
H29A	0.4819	0.6128	0.4502	0.077*	0.55 (2)
H29B	0.6146	0.6263	0.5077	0.077*	0.55 (2)
C30	0.5284 (16)	0.6963 (11)	0.3911 (10)	0.066 (3)	0.55 (2)
H30A	0.4919	0.6449	0.3458	0.079*	0.55 (2)
H30B	0.6012	0.7139	0.4062	0.079*	0.55 (2)
C31	0.4556 (16)	0.7877 (16)	0.3635 (13)	0.073 (5)	0.55 (2)
H31A	0.4697	0.8363	0.3343	0.088*	0.55 (2)
H31B	0.3758	0.7691	0.325	0.088*	0.55 (2)
C32	0.488 (5)	0.8294 (17)	0.4431 (19)	0.068 (7)	0.55 (2)
H32A	0.5427	0.8838	0.4634	0.081*	0.55 (2)
H32B	0.4218	0.857	0.4344	0.081*	0.55 (2)
C29A	0.541 (5)	0.6650 (18)	0.461 (2)	0.056 (3)	0.45 (2)
H29C	0.5087	0.604	0.4656	0.067*	0.45 (2)
H29D	0.6191	0.6509	0.4857	0.067*	0.45 (2)
C30A	0.474 (2)	0.6981 (14)	0.3695 (13)	0.075 (4)	0.45 (2)
H30C	0.4962	0.6617	0.3397	0.091*	0.45 (2)
H30D	0.393	0.6895	0.3382	0.091*	0.45 (2)
C31A	0.506 (2)	0.8069 (16)	0.3820 (17)	0.063 (4)	0.45 (2)
H31C	0.4502	0.8462	0.3304	0.076*	0.45 (2)
H31D	0.5797	0.8153	0.3959	0.076*	0.45 (2)
C32A	0.510 (6)	0.839 (2)	0.455 (3)	0.064 (7)	0.45 (2)
H32C	0.5683	0.8906	0.4901	0.077*	0.45 (2)
H32D	0.4375	0.867	0.4346	0.077*	0.45 (2)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Mo1	0.0421 (2)	0.0281 (2)	0.0318 (2)	0.00186 (18)	0.02382 (17)	0.0012 (2)
Cl1	0.0978 (11)	0.0283 (8)	0.0685 (10)	0.0094 (7)	0.0575 (9)	0.0041 (7)
Cl2	0.0565 (7)	0.0651 (8)	0.0343 (6)	−0.0004 (7)	0.0297 (6)	0.0013 (8)
Cl3	0.0583 (8)	0.0320 (7)	0.0577 (9)	0.0070 (6)	0.0372 (7)	0.0059 (6)
P1	0.0426 (8)	0.0390 (8)	0.0446 (8)	−0.0019 (5)	0.0281 (7)	−0.0007 (6)
P2	0.0405 (7)	0.0363 (8)	0.0323 (8)	0.0025 (5)	0.0220 (6)	−0.0010 (6)
O1	0.0568 (19)	0.0352 (18)	0.0328 (16)	0.0028 (17)	0.0288 (15)	0.0022 (19)
C1	0.057 (4)	0.048 (4)	0.045 (3)	−0.008 (2)	0.032 (3)	−0.005 (3)
C2	0.076 (4)	0.081 (5)	0.086 (5)	−0.033 (3)	0.060 (4)	−0.042 (4)
C3	0.109 (6)	0.114 (6)	0.105 (6)	−0.055 (5)	0.083 (5)	−0.069 (5)
C4	0.088 (5)	0.074 (5)	0.069 (5)	−0.040 (4)	0.039 (4)	−0.031 (4)
C5	0.055 (4)	0.062 (5)	0.075 (5)	−0.018 (3)	0.031 (4)	−0.012 (4)
C6	0.060 (4)	0.057 (4)	0.080 (5)	−0.013 (3)	0.046 (4)	−0.011 (3)
C7	0.049 (3)	0.046 (4)	0.053 (3)	−0.004 (2)	0.036 (3)	−0.004 (3)
C8	0.154 (5)	0.060 (3)	0.093 (4)	0.013 (3)	0.099 (4)	0.013 (3)
C9	0.100 (5)	0.096 (6)	0.086 (5)	0.038 (4)	0.073 (4)	0.009 (4)
C10	0.114 (5)	0.085 (6)	0.089 (5)	0.006 (4)	0.087 (5)	0.007 (4)
C11	0.154 (5)	0.060 (3)	0.093 (4)	0.013 (3)	0.099 (4)	0.013 (3)
C12	0.204 (8)	0.041 (4)	0.116 (6)	0.005 (4)	0.133 (6)	0.006 (4)
C13	0.048 (3)	0.049 (4)	0.066 (4)	0.003 (2)	0.033 (3)	0.014 (3)
C14	0.074 (4)	0.084 (5)	0.067 (5)	0.013 (3)	0.031 (4)	0.029 (4)
C15	0.046 (3)	0.042 (4)	0.033 (3)	0.007 (2)	0.024 (3)	0.002 (2)
C16	0.051 (3)	0.067 (4)	0.057 (3)	0.003 (3)	0.036 (3)	−0.008 (3)
C17	0.058 (4)	0.086 (5)	0.064 (4)	0.018 (3)	0.044 (4)	0.009 (4)
C18	0.072 (4)	0.069 (5)	0.061 (4)	0.028 (3)	0.047 (4)	0.010 (3)
C19	0.079 (5)	0.070 (5)	0.056 (4)	0.011 (3)	0.044 (4)	−0.011 (3)
C20	0.051 (3)	0.061 (4)	0.042 (3)	0.004 (3)	0.028 (3)	−0.005 (3)
C21	0.040 (3)	0.044 (3)	0.036 (3)	0.002 (2)	0.022 (3)	−0.006 (2)
C22	0.054 (3)	0.050 (4)	0.048 (3)	0.005 (2)	0.033 (3)	0.001 (3)
C23	0.060 (4)	0.072 (5)	0.035 (3)	0.003 (3)	0.024 (3)	−0.012 (3)
C24	0.056 (4)	0.089 (5)	0.030 (3)	0.013 (3)	0.020 (3)	−0.005 (3)
C25	0.067 (4)	0.061 (4)	0.047 (4)	0.022 (3)	0.030 (3)	0.013 (3)
C26	0.076 (4)	0.047 (4)	0.047 (4)	0.014 (3)	0.034 (3)	0.002 (3)
C27	0.051 (3)	0.040 (3)	0.052 (3)	−0.004 (2)	0.034 (3)	0.001 (3)
C28	0.077 (4)	0.059 (4)	0.058 (4)	−0.004 (3)	0.045 (3)	0.014 (3)
C29	0.089 (5)	0.066 (4)	0.053 (5)	−0.004 (4)	0.052 (5)	−0.013 (4)
C30	0.084 (6)	0.076 (5)	0.053 (6)	−0.004 (5)	0.051 (6)	−0.011 (4)
C31	0.086 (14)	0.083 (10)	0.040 (9)	−0.014 (9)	0.035 (11)	0.004 (7)
C32	0.094 (19)	0.057 (6)	0.049 (8)	0.010 (8)	0.043 (12)	0.020 (6)
C29A	0.086 (5)	0.055 (5)	0.052 (5)	−0.005 (4)	0.056 (5)	−0.012 (4)
C30A	0.094 (7)	0.077 (6)	0.058 (6)	−0.003 (6)	0.049 (6)	−0.014 (5)
C31A	0.076 (14)	0.085 (10)	0.036 (10)	−0.011 (9)	0.039 (12)	0.003 (7)
C32A	0.092 (19)	0.055 (6)	0.047 (8)	0.008 (8)	0.044 (12)	0.020 (6)

Geometric parameters (Å, º) top

Mo1—O1	2.206 (3)	C16—H16A	0.95
Mo1—Cl1	2.3871 (13)	C17—C18	1.356 (8)
Mo1—Cl2	2.3822 (13)	C17—H17A	0.95
Mo1—Cl3	2.4126 (13)	C18—C19	1.348 (7)
Mo1—P1	2.5964 (14)	C18—H18A	0.95
Mo1—P2	2.5974 (13)	C19—C20	1.371 (7)
P1—C7	1.824 (6)	C19—H19A	0.95
P1—C1	1.830 (5)	C20—H20A	0.95
P1—C13	1.840 (5)	C21—C26	1.364 (7)
P2—C27	1.818 (5)	C21—C22	1.370 (7)
P2—C21	1.830 (5)	C22—C23	1.368 (7)
P2—C15	1.838 (5)	C22—H22A	0.95
O1—C29	1.434 (15)	C23—C24	1.358 (8)
O1—C29A	1.453 (16)	C23—H23A	0.95
O1—C32	1.455 (15)	C24—C25	1.326 (7)
O1—C32A	1.459 (17)	C24—H24A	0.95
C1—C2	1.366 (7)	C25—C26	1.380 (7)
C1—C6	1.389 (7)	C25—H25A	0.95
C2—C3	1.390 (8)	C26—H26A	0.95
C2—H2A	0.95	C27—C28	1.514 (7)
C3—C4	1.358 (9)	C27—H27A	0.99
C3—H3A	0.95	C27—H27B	0.99
C4—C5	1.359 (9)	C28—H28A	0.98
C4—H4A	0.95	C28—H28B	0.98
C5—C6	1.355 (8)	C28—H28C	0.98
C5—H5A	0.95	C29—C30	1.499 (17)
C6—H6A	0.95	C29—H29A	0.99
C7—C12	1.358 (8)	C29—H29B	0.99
C7—C8	1.373 (8)	C30—C31	1.510 (16)
C8—C9	1.364 (9)	C30—H30A	0.99
C8—H8A	0.95	C30—H30B	0.99
C9—C10	1.352 (9)	C31—C32	1.464 (16)
C9—H9A	0.95	C31—H31A	0.99
C10—C11	1.341 (8)	C31—H31B	0.99
C10—H10A	0.95	C32—H32A	0.99
C11—C12	1.381 (9)	C32—H32B	0.99
C11—H11A	0.95	C29A—C30A	1.514 (18)
C12—H12A	0.95	C29A—H29C	0.99
C13—C14	1.498 (8)	C29A—H29D	0.99
C13—H13A	0.99	C30A—C31A	1.506 (17)
C13—H13B	0.99	C30A—H30C	0.99
C14—H14A	0.98	C30A—H30D	0.99
C14—H14B	0.98	C31A—C32A	1.509 (18)
C14—H14C	0.98	C31A—H31C	0.99
C15—C16	1.359 (7)	C31A—H31D	0.99
C15—C20	1.371 (7)	C32A—H32C	0.99
C16—C17	1.391 (7)	C32A—H32D	0.99

O1—Mo1—Cl2	179.21 (10)	C18—C17—H17A	120.3
O1—Mo1—Cl1	88.22 (10)	C16—C17—H17A	120.3
Cl2—Mo1—Cl1	92.44 (5)	C19—C18—C17	120.3 (5)
O1—Mo1—Cl3	88.34 (10)	C19—C18—H18A	119.8
Cl2—Mo1—Cl3	91.01 (5)	C17—C18—H18A	119.8
Cl1—Mo1—Cl3	176.50 (6)	C18—C19—C20	120.8 (6)
O1—Mo1—P1	89.05 (9)	C18—C19—H19A	119.6
Cl2—Mo1—P1	90.49 (5)	C20—C19—H19A	119.6
Cl1—Mo1—P1	91.92 (5)	C19—C20—C15	119.8 (5)
Cl3—Mo1—P1	88.66 (4)	C19—C20—H20A	120.1
O1—Mo1—P2	89.76 (8)	C15—C20—H20A	120.1
Cl2—Mo1—P2	90.67 (4)	C26—C21—C22	117.8 (5)
Cl1—Mo1—P2	90.94 (5)	C26—C21—P2	120.3 (4)
Cl3—Mo1—P2	88.41 (4)	C22—C21—P2	121.8 (4)
P1—Mo1—P2	176.87 (5)	C23—C22—C21	120.8 (5)
C7—P1—C1	102.7 (2)	C23—C22—H22A	119.6
C7—P1—C13	103.8 (3)	C21—C22—H22A	119.6
C1—P1—C13	101.9 (3)	C24—C23—C22	120.4 (6)
C7—P1—Mo1	113.20 (16)	C24—C23—H23A	119.8
C1—P1—Mo1	119.23 (19)	C22—C23—H23A	119.8
C13—P1—Mo1	114.15 (18)	C25—C24—C23	119.6 (6)
C27—P2—C21	104.1 (2)	C25—C24—H24A	120.2
C27—P2—C15	102.5 (2)	C23—C24—H24A	120.2
C21—P2—C15	101.7 (2)	C24—C25—C26	120.9 (6)
C27—P2—Mo1	114.84 (16)	C24—C25—H25A	119.6
C21—P2—Mo1	111.36 (16)	C26—C25—H25A	119.6
C15—P2—Mo1	120.40 (17)	C21—C26—C25	120.6 (6)
C29—O1—C32	108.9 (15)	C21—C26—H26A	119.7
C29A—O1—C32	104.0 (14)	C25—C26—H26A	119.7
C29—O1—C32A	113.6 (15)	C28—C27—P2	113.6 (4)
C29A—O1—C32A	108.5 (16)	C28—C27—H27A	108.8
C29—O1—Mo1	123.2 (9)	P2—C27—H27A	108.8
C29A—O1—Mo1	128.2 (10)	C28—C27—H27B	108.8
C32—O1—Mo1	127.6 (11)	P2—C27—H27B	108.8
C32A—O1—Mo1	122.9 (12)	H27A—C27—H27B	107.7
C2—C1—C6	118.3 (5)	C27—C28—H28A	109.5
C2—C1—P1	121.5 (4)	C27—C28—H28B	109.5
C6—C1—P1	120.2 (4)	H28A—C28—H28B	109.5
C1—C2—C3	121.1 (6)	C27—C28—H28C	109.5
C1—C2—H2A	119.5	H28A—C28—H28C	109.5
C3—C2—H2A	119.5	H28B—C28—H28C	109.5
C4—C3—C2	119.2 (7)	O1—C29—C30	105.5 (14)
C4—C3—H3A	120.4	O1—C29—H29A	110.6
C2—C3—H3A	120.4	C30—C29—H29A	110.6
C5—C4—C3	120.0 (6)	O1—C29—H29B	110.6
C5—C4—H4A	120	C30—C29—H29B	110.6
C3—C4—H4A	120	H29A—C29—H29B	108.8
C6—C5—C4	121.3 (6)	C29—C30—C31	103.3 (18)
C6—C5—H5A	119.3	C29—C30—H30A	111.1
C4—C5—H5A	119.3	C31—C30—H30A	111.1
C5—C6—C1	120.1 (6)	C29—C30—H30B	111.1
C5—C6—H6A	120	C31—C30—H30B	111.1
C1—C6—H6A	120	H30A—C30—H30B	109.1
C12—C7—C8	115.8 (6)	C32—C31—C30	104.0 (19)
C12—C7—P1	121.3 (5)	C32—C31—H31A	111
C8—C7—P1	122.7 (4)	C30—C31—H31A	111
C9—C8—C7	122.1 (7)	C32—C31—H31B	111
C9—C8—H8A	118.9	C30—C31—H31B	111
C7—C8—H8A	118.9	H31A—C31—H31B	109
C10—C9—C8	120.7 (7)	O1—C32—C31	107.4 (17)
C10—C9—H9A	119.7	O1—C32—H32A	110.2
C8—C9—H9A	119.7	C31—C32—H32A	110.2
C11—C10—C9	118.7 (7)	O1—C32—H32B	110.2
C11—C10—H10A	120.7	C31—C32—H32B	110.2
C9—C10—H10A	120.7	H32A—C32—H32B	108.5
C10—C11—C12	120.4 (6)	O1—C29A—C30A	105.3 (18)
C10—C11—H11A	119.8	O1—C29A—H29C	110.7
C12—C11—H11A	119.8	C30A—C29A—H29C	110.7
C7—C12—C11	122.2 (7)	O1—C29A—H29D	110.7
C7—C12—H12A	118.9	C30A—C29A—H29D	110.7
C11—C12—H12A	118.9	H29C—C29A—H29D	108.8
C14—C13—P1	113.7 (4)	C31A—C30A—C29A	100 (2)
C14—C13—H13A	108.8	C31A—C30A—H30C	111.8
P1—C13—H13A	108.8	C29A—C30A—H30C	111.8
C14—C13—H13B	108.8	C31A—C30A—H30D	111.8
P1—C13—H13B	108.8	C29A—C30A—H30D	111.8
H13A—C13—H13B	107.7	H30C—C30A—H30D	109.5
C13—C14—H14A	109.5	C30A—C31A—C32A	104 (2)
C13—C14—H14B	109.5	C30A—C31A—H31C	110.9
H14A—C14—H14B	109.5	C32A—C31A—H31C	110.9
C13—C14—H14C	109.5	C30A—C31A—H31D	110.9
H14A—C14—H14C	109.5	C32A—C31A—H31D	110.9
H14B—C14—H14C	109.5	H31C—C31A—H31D	108.9
C16—C15—C20	119.4 (5)	O1—C32A—C31A	105 (2)
C16—C15—P2	119.5 (4)	O1—C32A—H32C	110.7
C20—C15—P2	121.1 (4)	C31A—C32A—H32C	110.7
C15—C16—C17	120.3 (6)	O1—C32A—H32D	110.7
C15—C16—H16A	119.8	C31A—C32A—H32D	110.7
C17—C16—H16A	119.8	H32C—C32A—H32D	108.8
C18—C17—C16	119.4 (6)

O1—Mo1—P1—C7	11.0 (2)	P1—C7—C8—C9	176.5 (5)
Cl2—Mo1—P1—C7	−169.7 (2)	C7—C8—C9—C10	−0.5 (12)
Cl1—Mo1—P1—C7	−77.2 (2)	C8—C9—C10—C11	−1.4 (11)
Cl3—Mo1—P1—C7	99.3 (2)	C9—C10—C11—C12	2.3 (11)
O1—Mo1—P1—C1	131.9 (2)	C8—C7—C12—C11	−0.5 (11)
Cl2—Mo1—P1—C1	−48.8 (2)	P1—C7—C12—C11	−175.6 (6)
Cl1—Mo1—P1—C1	43.7 (2)	C10—C11—C12—C7	−1.4 (12)
Cl3—Mo1—P1—C1	−139.8 (2)	C7—P1—C13—C14	168.8 (4)
O1—Mo1—P1—C13	−107.4 (2)	C1—P1—C13—C14	62.4 (5)
Cl2—Mo1—P1—C13	71.9 (2)	Mo1—P1—C13—C14	−67.6 (5)
Cl1—Mo1—P1—C13	164.4 (2)	C27—P2—C15—C16	−58.1 (5)
Cl3—Mo1—P1—C13	−19.1 (2)	C21—P2—C15—C16	49.4 (5)
O1—Mo1—P2—C27	108.1 (2)	Mo1—P2—C15—C16	173.0 (4)
Cl2—Mo1—P2—C27	−71.3 (2)	C27—P2—C15—C20	122.9 (4)
Cl1—Mo1—P2—C27	−163.7 (2)	C21—P2—C15—C20	−129.7 (4)
Cl3—Mo1—P2—C27	19.7 (2)	Mo1—P2—C15—C20	−6.1 (5)
O1—Mo1—P2—C21	−9.9 (2)	C20—C15—C16—C17	−0.2 (8)
Cl2—Mo1—P2—C21	170.76 (18)	P2—C15—C16—C17	−179.3 (4)
Cl1—Mo1—P2—C21	78.31 (18)	C15—C16—C17—C18	1.8 (9)
Cl3—Mo1—P2—C21	−98.26 (18)	C16—C17—C18—C19	−1.9 (9)
O1—Mo1—P2—C15	−128.8 (2)	C17—C18—C19—C20	0.3 (9)
Cl2—Mo1—P2—C15	51.90 (18)	C18—C19—C20—C15	1.3 (9)
Cl1—Mo1—P2—C15	−40.55 (18)	C16—C15—C20—C19	−1.3 (8)
Cl3—Mo1—P2—C15	142.89 (18)	P2—C15—C20—C19	177.8 (4)
Cl1—Mo1—O1—C29	−180 (2)	C27—P2—C21—C26	150.8 (5)
Cl3—Mo1—O1—C29	0 (2)	C15—P2—C21—C26	44.6 (5)
P1—Mo1—O1—C29	89 (2)	Mo1—P2—C21—C26	−84.9 (5)
P2—Mo1—O1—C29	−89 (2)	C27—P2—C21—C22	−33.3 (5)
Cl1—Mo1—O1—C29A	179 (3)	C15—P2—C21—C22	−139.5 (4)
Cl3—Mo1—O1—C29A	−2 (3)	Mo1—P2—C21—C22	91.0 (4)
P1—Mo1—O1—C29A	87 (3)	C26—C21—C22—C23	−0.1 (8)
P2—Mo1—O1—C29A	−90 (3)	P2—C21—C22—C23	−176.1 (4)
Cl1—Mo1—O1—C32	−6 (3)	C21—C22—C23—C24	−0.6 (9)
Cl3—Mo1—O1—C32	173 (3)	C22—C23—C24—C25	0.7 (9)
P1—Mo1—O1—C32	−98 (3)	C23—C24—C25—C26	−0.1 (9)
P2—Mo1—O1—C32	85 (3)	C22—C21—C26—C25	0.7 (8)
Cl1—Mo1—O1—C32A	7 (4)	P2—C21—C26—C25	176.7 (4)
Cl3—Mo1—O1—C32A	−173 (4)	C24—C25—C26—C21	−0.6 (9)
P1—Mo1—O1—C32A	−85 (4)	C21—P2—C27—C28	−169.0 (4)
P2—Mo1—O1—C32A	98 (4)	C15—P2—C27—C28	−63.3 (4)
C7—P1—C1—C2	128.5 (5)	Mo1—P2—C27—C28	69.0 (4)
C13—P1—C1—C2	−124.3 (5)	C32—O1—C29—C30	17 (4)
Mo1—P1—C1—C2	2.4 (6)	C32A—O1—C29—C30	5 (5)
C7—P1—C1—C6	−52.0 (5)	Mo1—O1—C29—C30	−168.8 (15)
C13—P1—C1—C6	55.3 (5)	O1—C29—C30—C31	−30 (4)
Mo1—P1—C1—C6	−178.0 (4)	C29—C30—C31—C32	33 (4)
C6—C1—C2—C3	−0.9 (10)	C29—O1—C32—C31	4 (5)
P1—C1—C2—C3	178.7 (6)	C29A—O1—C32—C31	6 (5)
C1—C2—C3—C4	−0.6 (12)	C32A—O1—C32—C31	120 (18)
C2—C3—C4—C5	1.6 (12)	Mo1—O1—C32—C31	−170.0 (17)
C3—C4—C5—C6	−1.2 (11)	C30—C31—C32—O1	−23 (4)
C4—C5—C6—C1	−0.3 (10)	C32—O1—C29A—C30A	−11 (4)
C2—C1—C6—C5	1.3 (9)	C32A—O1—C29A—C30A	−22 (5)
P1—C1—C6—C5	−178.2 (5)	Mo1—O1—C29A—C30A	165.2 (15)
C1—P1—C7—C12	−47.7 (6)	O1—C29A—C30A—C31A	38 (4)
C13—P1—C7—C12	−153.6 (5)	C29A—C30A—C31A—C32A	−39 (4)
Mo1—P1—C7—C12	82.1 (5)	C29—O1—C32A—C31A	−4 (6)
C1—P1—C7—C8	137.5 (5)	C29A—O1—C32A—C31A	−3 (6)
C13—P1—C7—C8	31.6 (6)	C32—O1—C32A—C31A	−73 (13)
Mo1—P1—C7—C8	−92.7 (5)	Mo1—O1—C32A—C31A	170 (2)
C12—C7—C8—C9	1.4 (10)	C30A—C31A—C32A—O1	27 (5)

Experimental details

Crystal data
Chemical formula	[MoCl₃(C₄H₈O)(C₁₄H₁₅P)₂]
M_r	702.85
Crystal system, space group	Monoclinic, P2₁/c
Temperature (K)	120
a, b, c (Å)	15.437, 13.356, 20.229
β (°)	128.87
V (Å³)	3247.1
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	0.77
Crystal size (mm)	0.13 × 0.1 × 0.04

Data collection
Diffractometer	Oxford Diffraction KM-4/Xcalibur diffractometer with a Sapphire2 (large Be window) detector
Absorption correction	Analytical [CrysAlis RED (Oxford Diffraction, 2006). based on expressions derived by Clark & Reid (1995)]
T_min, T_max	0.937, 0.97
No. of measured, independent and observed [I > 2σ(I)] reflections	25240, 7022, 2985
R_int	0.089
(sin θ/λ)_max (Å⁻¹)	0.639

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.044, 0.115, 0.81
No. of reflections	7022
No. of parameters	385
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	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—O1	2.206 (3)	Mo1—Cl3	2.4126 (13)
Mo1—Cl1	2.3871 (13)	Mo1—P1	2.5964 (14)
Mo1—Cl2	2.3822 (13)	Mo1—P2	2.5974 (13)

Acknowledgements

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

References

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