trans-Bis­[ethane-1,2-diyl­bis­(di­phenyl­phosphane)-κ2P,P′]­bis­(thio­cyanato-κN)molybdenum(II) toluene solvate

Philippopoulos, A.I.; Ziemer, B.; Filippou, A.C.

doi:10.1107/S1600536802020123

trans-Bis[ethane-1,2-diylbis(diphenylphosphane)-κ2P,P′]bis(thiocyanato-κN)molybdenum(II) toluene solvate

A. I. Philippopoulos, B. Ziemer and A. C. Filippou

The complex trans-[Mo(NCS)₂(dppe)₂] [dppe is ethane-1,2-diylbis(diphenylphosphane), C₂₆H₂₄P₂] was obtained upon air oxidation of [N(n-Bu)₄][Mo(NCS)(dppe)₂(N₂)] and the crystal structure of its toluene solvate, [Mo(NCS)₂(C₂₆H₂₄P₂)₂]·C₇H₈, has been determined. The complex molecule reveals a distorted octahedral coordination geometry, with two trans-oriented N-bonded thiocyanate ligands. The Mo atom resides on a crystallographic center of symmetry.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802020123/bt6200sup1.cif Contains datablocks global, I
	Structure factor file (CIF format) https://doi.org/10.1107/S1600536802020123/bt6200Isup2.hkl Contains datablock I

CCDC reference: 202280

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Key indicators

Single-crystal X-ray study
T = 180 K
Mean (C-C) = 0.006 Å
Disorder in solvent or counterion
R factor = 0.040
wR factor = 0.101
Data-to-parameter ratio = 15.8

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No syntax errors found

ADDSYM reports no extra symmetry


 Alert Level C:



PLAT_202  Alert C Isotropic non-H Atoms in Anion/Solvent       =          2

PLAT_302  Alert C Anion/Solvent Disorder .......................      30.00 Perc.


 0 Alert Level A = Potentially serious problem

 0 Alert Level B = Potential problem

 2 Alert Level C = Please check

Comment top

Recently, we have shown that the reactions of the dinitrogen complexes trans-[M(dppe)₂(N₂)₂] [M = Mo, W; dppe is ethane-1,2-diylbis(diphenylphosphane), Ph₂PCH₂CH₂PPh₂] with the germanium(II) halides Cp*GeX (Cp* = C₅Me₅; X = Cl, Br, I) afford the germylyne complexes trans-[X(dppe)₂M≡Ge—(η1-Cp*)] (Filippou, Philippopoulos et al., 2000; Filippou, Portius et al., 2002). Furthermore, the tungsten derivative trans-[I(dppe)₂W≡Ge—(η1-Cp*)] was shown to undergo iodide/pseudohalide ligand exchange with an excess of M'Y (M' = Na, K; Y = CN, NCO, N₃, NCS) to yield the germylyne complexes trans-[Y(dppe)₂W≡Ge—(η1-Cp*)] (Filippou, Philippopoulos et al., 2002). Looking for an alternative approach to the analogous molybdenum compounds, we prepared the anionic dinitrogen complex [N(n—Bu)₄][Mo(NCS)(dppe)₂(N₂)], following the method of Chatt et al. (1980). Exposure of this complex to air was reported to give trans-[Mo(NCS)₂(dppe)₂], (1), which was characterized by IR spectroscopy and elemental analysis (Chatt et al., 1980). However, the molecular structure of (1) remained unknown until today. Dark-green single crystals of the toluene solvate of (1), viz. (1α), were obtained from a THF/toluene solution upon cooling from 293 to 238 K. The title compound, (1α), crystallizes in the same space group (P2₁/c) as the chloro complex trans-[MoCl₂(dppe)₂]·2C₄H₈O (Filippou, Portius et al., 2000). The 16 valence-electron complex (1) reveals a distorted octahedral geometry at the Mo atom, which bears two trans-arranged N-bonded thiocyanate ligands and lies on a crystallographic center of symmetry. Distortion is evidenced in the tilt of the axial isothiocyanate ligands with respect to the equatorial plane spanned by the four P atoms, the angle between the N—Mo—N' axis and the P₄ plane being 82.9°. A similar tilt of the axial chloro ligands (80.5°) was observed in trans-[MoCl₂(dppe)₂]·2C₄H₈O (Filippou, Portius et al., 2000). The isothiocyanate ligands feature an almost linear Mo—N—C1—S array in (1α), with Mo—N—C1 and N—C1—S angles of 176.2 (3) and 178.0 (4)°, respectively. The Mo—N bonds of (1α) [2.086 (3) Å] are slightly shorter than those of the few other structurally characterized molybdenum(II) isothiocyanate complexes (Bino & Cotton, 1979; Müller & Mohan, 1981) and the mean Mo—P bond length of (1α) (2.503 Å) compares well with that of trans-[MoCl₂(dppe)₂]·2C₄H₈O (average Mo—P = 2.499 Å; Filippou, Portius et al., 2000) or trans-[MoCl₂(dppe)₂]·CH₂Cl₂ (average Mo—P = 2.497 Å; Nardelli et al., 1980).

Experimental top

A Schlenk tube was charged with a mixture of trans-[Mo(dppe)₂(N₂)₂] (663 mg, 0.699 mmol) and [N(n—Bu)₄](NCS) (211 mg, 0.702 mmol). THF (40 ml) was added to the mixture and the resulting clear orange solution was stirred at ambient temperature overnight under an N₂ atmosphere. Within ca 20 min, the color of the solution changed to deep red. At the end of the reaction, the solution was concentrated to half of its volume and stored for 2 h at 237 K to afford a mixture of yellow and red–black crystalline material. The supernatant dark-red solution was decanted, treated with toluene (35 ml) and then stirred for 1–2 minutes in air. Dark-green single crystals of (1α) were obtained upon cooling the resulting yellow solution for 3 d at 237 K.

Structure description top

Computing details top

Data collection: STADI4 (Stoe & Cie, 1997); cell refinement: STADI4; data reduction: X-RED (Stoe & Cie, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 1999); software used to prepare material for publication: SHELXL97.

Figures top

Fig. 1. The molecular structure of (1α), showing 50% probability displacement ellipsoids (DIAMOND; Brandenburg, 1999). Labels of atoms related by symmetry, all H atoms and the disordered solvent molecule have been omitted for clarity.

trans-Bis[ethane-1,2-diylbis(diphenylphosphane)-κ2P,P']bis(thiocyanato- κN)molybdenum(II) toluene solvate top

Crystal data top

[Mo(NCS)₂(C₂₆H₂₄P₂)₂]·C₇H₈	F(000) = 1140
M_r = 1101.02	D_x = 1.374 Mg m⁻³
Monoclinic, P2₁/c	Mo Kα radiation, λ = 0.71073 Å
a = 9.6277 (13) Å	Cell parameters from 72 reflections
b = 17.017 (2) Å	θ = 14.0–14.8°
c = 16.755 (2) Å	µ = 0.49 mm⁻¹
β = 104.172 (11)°	T = 180 K
V = 2661.5 (6) Å³	Block, black
Z = 2	0.68 × 0.62 × 0.48 mm

Data collection top

Stoe STADI-4 diffractometer	3796 reflections with I > 2σ(I)
Radiation source: fine-focus sealed X-ray tube	R_int = 0.098
Planar graphite monochromator	θ_max = 25.3°, θ_min = 1.7°
2θ/ω scans	h = −11→11
Absorption correction: ψ scan (North et al., 1968)	k = 0→20
T_min = 0.733, T_max = 0.800	l = −2→20
4828 measured reflections	3 standard reflections every 120 min
4820 independent reflections	intensity decay: 3.8%

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)] = 0.040	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.101	H-atom parameters constrained
S = 1.09	w = 1/[σ²(F_o²) + (0.0348P)² + 3.8899P] where P = (F_o² + 2F_c²)/3
4820 reflections	(Δ/σ)_max = 0.001
306 parameters	Δρ_max = 0.74 e Å⁻³
5 restraints	Δρ_min = −0.43 e Å⁻³

Crystal data top

[Mo(NCS)₂(C₂₆H₂₄P₂)₂]·C₇H₈	V = 2661.5 (6) Å³
M_r = 1101.02	Z = 2
Monoclinic, P2₁/c	Mo Kα radiation
a = 9.6277 (13) Å	µ = 0.49 mm⁻¹
b = 17.017 (2) Å	T = 180 K
c = 16.755 (2) Å	0.68 × 0.62 × 0.48 mm
β = 104.172 (11)°

Data collection top

Stoe STADI-4 diffractometer	3796 reflections with I > 2σ(I)
Absorption correction: ψ scan (North et al., 1968)	R_int = 0.098
T_min = 0.733, T_max = 0.800	3 standard reflections every 120 min
4828 measured reflections	intensity decay: 3.8%
4820 independent reflections

Refinement top

R[F² > 2σ(F²)] = 0.040	5 restraints
wR(F²) = 0.101	H-atom parameters constrained
S = 1.09	Δρ_max = 0.74 e Å⁻³
4820 reflections	Δρ_min = −0.43 e Å⁻³
306 parameters

Special details top

Experimental. During data collection the crystal was in cold N₂ gas of a cryostream cooler (Oxford Cryosystems).

Measurement: 2Θ/ω-scan,ratio=1.0,width(ω)=1.75–1.9°

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)
C1	0.2192 (4)	0.5707 (2)	0.3717 (2)	0.0354 (8)
C2	0.1881 (4)	0.4709 (2)	0.5650 (2)	0.0334 (8)
H2A	0.1309	0.4732	0.6067	0.040*
H2B	0.1313	0.4956	0.5139	0.040*
C3	0.2181 (4)	0.3853 (2)	0.5480 (2)	0.0353 (8)
H3A	0.1283	0.3604	0.5166	0.042*
H3B	0.2499	0.3570	0.6010	0.042*
C4	0.4313 (4)	0.2789 (2)	0.5255 (2)	0.0321 (8)
C5	0.5761 (4)	0.2663 (2)	0.5518 (3)	0.0487 (10)
H5	0.6407	0.3082	0.5503	0.058*
C6	0.6294 (5)	0.1928 (3)	0.5805 (3)	0.0601 (12)
H6	0.7299	0.1848	0.5983	0.072*
C7	0.5374 (5)	0.1321 (2)	0.5830 (2)	0.0513 (10)
H7	0.5736	0.0821	0.6034	0.062*
C8	0.3931 (5)	0.1438 (2)	0.5559 (3)	0.0554 (11)
H8	0.3288	0.1017	0.5570	0.067*
C9	0.3409 (5)	0.2157 (2)	0.5272 (3)	0.0513 (11)
H9	0.2404	0.2227	0.5080	0.062*
C10	0.2561 (4)	0.3498 (2)	0.3844 (2)	0.0346 (8)
C11	0.3200 (5)	0.3023 (2)	0.3360 (2)	0.0495 (10)
H11	0.4130	0.2815	0.3583	0.059*
C12	0.2495 (6)	0.2850 (3)	0.2557 (3)	0.0707 (15)
H12	0.2943	0.2531	0.2227	0.085*
C13	0.1132 (7)	0.3145 (3)	0.2235 (3)	0.0796 (17)
H13	0.0634	0.3015	0.1688	0.096*
C14	0.0493 (5)	0.3627 (3)	0.2705 (3)	0.0675 (14)
H14	−0.0434	0.3838	0.2479	0.081*
C15	0.1210 (4)	0.3801 (2)	0.3502 (2)	0.0463 (10)
H15	0.0770	0.4134	0.3823	0.056*
C16	0.2873 (4)	0.6237 (2)	0.6201 (2)	0.0353 (8)
C17	0.1865 (4)	0.6597 (2)	0.5570 (2)	0.0414 (9)
H17	0.1520	0.6328	0.5063	0.050*
C18	0.1358 (4)	0.7343 (2)	0.5672 (3)	0.0500 (10)
H18	0.0667	0.7581	0.5236	0.060*
C19	0.1849 (5)	0.7742 (2)	0.6402 (3)	0.0557 (11)
H19	0.1499	0.8253	0.6470	0.067*
C20	0.2845 (5)	0.7397 (3)	0.7027 (3)	0.0628 (13)
H20	0.3185	0.7670	0.7531	0.075*
C21	0.3366 (5)	0.6646 (2)	0.6931 (2)	0.0499 (10)
H21	0.4062	0.6414	0.7369	0.060*
C22	0.4318 (4)	0.4881 (2)	0.7067 (2)	0.0336 (8)
C23	0.5762 (4)	0.5028 (2)	0.7431 (2)	0.0380 (8)
H23	0.6314	0.5334	0.7147	0.046*
C24	0.6390 (5)	0.4731 (2)	0.8202 (2)	0.0514 (11)
H24	0.7371	0.4837	0.8448	0.062*
C25	0.5596 (6)	0.4281 (3)	0.8616 (3)	0.0619 (13)
H25	0.6033	0.4069	0.9143	0.074*
C26	0.4171 (6)	0.4140 (3)	0.8264 (3)	0.0594 (12)
H26	0.3627	0.3835	0.8552	0.071*
C27	0.3517 (5)	0.4438 (2)	0.7494 (2)	0.0469 (10)
H27	0.2530	0.4341	0.7259	0.056*
C28	−0.0776 (19)	0.4379 (9)	0.0514 (11)	0.140 (6)*	0.50
H28	−0.1097	0.3872	0.0653	0.168*	0.50
C29	−0.1165 (9)	0.5006 (6)	0.0944 (6)	0.144 (3)*
H29A	−0.1717	0.4988	0.1354	0.173*	0.50
H29B	−0.1435	0.4498	0.1085	0.173*	0.50
H29C	−0.1265	0.5229	0.1461	0.173*	0.50
H29D	−0.2216	0.4958	0.0766	0.173*	0.50
C30	−0.0644 (19)	0.5707 (9)	0.0696 (11)	0.151 (7)*	0.50
H30	−0.0760	0.6196	0.0965	0.181*	0.50
C31	−0.0004 (12)	0.5598 (7)	0.0069 (7)	0.173 (4)*
H31	0.0270	0.6080	−0.0147	0.208*
C32	−0.0400 (14)	0.5014 (10)	0.0341 (8)	0.097 (4)*	0.50
N	0.3213 (3)	0.54434 (17)	0.41527 (17)	0.0307 (6)
P1	0.35788 (9)	0.37521 (5)	0.48864 (5)	0.0279 (2)
P2	0.35653 (9)	0.52638 (5)	0.60272 (5)	0.0290 (2)
S	0.07691 (11)	0.61012 (7)	0.31294 (7)	0.0554 (3)
Mo	0.5000	0.5000	0.5000	0.02374 (11)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
C1	0.040 (2)	0.038 (2)	0.0334 (19)	−0.0087 (16)	0.0173 (17)	0.0026 (16)
C2	0.0275 (17)	0.0388 (19)	0.0376 (19)	−0.0052 (14)	0.0152 (15)	−0.0025 (15)
C3	0.0365 (19)	0.039 (2)	0.0348 (19)	−0.0106 (16)	0.0161 (15)	−0.0037 (16)
C4	0.0371 (19)	0.0317 (19)	0.0278 (17)	−0.0042 (15)	0.0086 (15)	−0.0012 (14)
C5	0.045 (2)	0.034 (2)	0.067 (3)	−0.0062 (18)	0.015 (2)	0.0027 (19)
C6	0.051 (3)	0.043 (3)	0.082 (3)	0.010 (2)	0.007 (2)	0.009 (2)
C7	0.074 (3)	0.034 (2)	0.045 (2)	0.001 (2)	0.013 (2)	0.0083 (18)
C8	0.067 (3)	0.035 (2)	0.063 (3)	−0.011 (2)	0.013 (2)	0.011 (2)
C9	0.048 (2)	0.037 (2)	0.066 (3)	−0.0104 (18)	0.008 (2)	0.011 (2)
C10	0.044 (2)	0.0287 (18)	0.0305 (18)	−0.0114 (16)	0.0081 (16)	0.0007 (14)
C11	0.071 (3)	0.040 (2)	0.036 (2)	0.002 (2)	0.010 (2)	−0.0059 (17)
C12	0.115 (4)	0.054 (3)	0.039 (2)	0.003 (3)	0.011 (3)	−0.013 (2)
C13	0.108 (4)	0.076 (4)	0.038 (3)	−0.018 (3)	−0.015 (3)	−0.008 (2)
C14	0.058 (3)	0.082 (4)	0.051 (3)	−0.011 (3)	−0.010 (2)	0.007 (3)
C15	0.042 (2)	0.052 (3)	0.042 (2)	−0.0077 (19)	0.0060 (18)	0.0005 (19)
C16	0.0372 (19)	0.0331 (19)	0.042 (2)	−0.0023 (15)	0.0226 (16)	−0.0024 (16)
C17	0.043 (2)	0.038 (2)	0.046 (2)	0.0003 (17)	0.0181 (18)	−0.0040 (17)
C18	0.049 (2)	0.043 (2)	0.061 (3)	0.0055 (19)	0.020 (2)	0.000 (2)
C19	0.068 (3)	0.035 (2)	0.072 (3)	0.001 (2)	0.032 (3)	−0.009 (2)
C20	0.084 (3)	0.048 (3)	0.059 (3)	0.001 (2)	0.022 (3)	−0.019 (2)
C21	0.064 (3)	0.045 (2)	0.041 (2)	0.000 (2)	0.015 (2)	−0.0086 (18)
C22	0.047 (2)	0.0286 (19)	0.0268 (17)	−0.0003 (15)	0.0128 (15)	−0.0038 (14)
C23	0.049 (2)	0.040 (2)	0.0264 (17)	0.0051 (18)	0.0120 (15)	−0.0041 (16)
C24	0.066 (3)	0.052 (3)	0.034 (2)	0.020 (2)	0.008 (2)	−0.0030 (18)
C25	0.104 (4)	0.049 (3)	0.033 (2)	0.029 (3)	0.020 (2)	0.0110 (19)
C26	0.102 (4)	0.043 (2)	0.043 (2)	−0.006 (2)	0.036 (3)	0.0051 (19)
C27	0.068 (3)	0.043 (2)	0.037 (2)	−0.007 (2)	0.026 (2)	−0.0024 (17)
N	0.0336 (16)	0.0329 (16)	0.0277 (15)	−0.0038 (13)	0.0117 (13)	−0.0018 (12)
P1	0.0312 (4)	0.0272 (5)	0.0270 (4)	−0.0060 (4)	0.0104 (4)	−0.0012 (3)
P2	0.0311 (4)	0.0319 (5)	0.0266 (4)	−0.0042 (4)	0.0119 (4)	−0.0035 (3)
S	0.0364 (5)	0.0718 (8)	0.0558 (7)	0.0041 (5)	0.0072 (5)	0.0259 (6)
Mo	0.0257 (2)	0.0247 (2)	0.02231 (19)	−0.00377 (17)	0.00874 (14)	−0.00124 (17)

Geometric parameters (Å, º) top

C1—N	1.161 (4)	C19—C20	1.367 (6)
C1—S	1.624 (4)	C19—H19	0.9500
C2—C3	1.526 (5)	C20—C21	1.396 (6)
C2—P2	1.848 (3)	C20—H20	0.9500
C2—H2A	0.9900	C21—H21	0.9500
C2—H2B	0.9900	C22—C27	1.394 (5)
C3—P1	1.867 (3)	C22—C23	1.398 (5)
C3—H3A	0.9900	C22—P2	1.834 (3)
C3—H3B	0.9900	C23—C24	1.381 (5)
C4—C5	1.372 (5)	C23—H23	0.9500
C4—C9	1.388 (5)	C24—C25	1.384 (6)
C4—P1	1.831 (4)	C24—H24	0.9500
C5—C6	1.393 (6)	C25—C26	1.375 (7)
C5—H5	0.9500	C25—H25	0.9500
C6—C7	1.368 (6)	C26—C27	1.385 (6)
C6—H6	0.9500	C26—H26	0.9500
C7—C8	1.366 (6)	C27—H27	0.9500
C7—H7	0.9500	C28—C31ⁱ	1.371 (18)
C8—C9	1.365 (6)	C28—C29	1.389 (13)
C8—H8	0.9500	C28—H28	0.9638
C9—H9	0.9500	C29—C32	1.389 (12)
C10—C15	1.386 (5)	C29—C30	1.396 (13)
C10—C11	1.392 (5)	C29—H29A	0.9665
C10—P1	1.832 (3)	C29—H29B	0.9497
C11—C12	1.382 (6)	C29—H29C	0.9719
C11—H11	0.9500	C29—H29D	0.9853
C12—C13	1.385 (7)	C30—C31	1.354 (14)
C12—H12	0.9500	C30—C32	1.37 (2)
C13—C14	1.381 (7)	C30—H30	0.9652
C13—H13	0.9500	C31—C32ⁱ	1.356 (16)
C14—C15	1.378 (6)	C31—C28ⁱ	1.371 (18)
C14—H14	0.9500	C31—H31	0.9587
C15—H15	0.9500	C32—C31ⁱ	1.356 (16)
C16—C21	1.387 (5)	N—Mo	2.086 (3)
C16—C17	1.390 (5)	P1—Mo	2.5081 (9)
C16—P2	1.835 (4)	P2—Mo	2.4971 (9)
C17—C18	1.387 (5)	Mo—Nⁱⁱ	2.086 (3)
C17—H17	0.9500	Mo—P2ⁱⁱ	2.4971 (9)
C18—C19	1.377 (6)	Mo—P1ⁱⁱ	2.5081 (9)
C18—H18	0.9500

N—C1—S	178.0 (4)	C27—C22—C23	119.3 (3)
C3—C2—P2	111.2 (2)	C27—C22—P2	122.7 (3)
C3—C2—H2A	109.4	C23—C22—P2	118.0 (3)
P2—C2—H2A	109.4	C24—C23—C22	120.3 (4)
C3—C2—H2B	109.4	C24—C23—H23	119.9
P2—C2—H2B	109.4	C22—C23—H23	119.9
H2A—C2—H2B	108.0	C23—C24—C25	120.2 (4)
C2—C3—P1	112.4 (2)	C23—C24—H24	119.9
C2—C3—H3A	109.1	C25—C24—H24	119.9
P1—C3—H3A	109.1	C26—C25—C24	119.8 (4)
C2—C3—H3B	109.1	C26—C25—H25	120.1
P1—C3—H3B	109.1	C24—C25—H25	120.1
H3A—C3—H3B	107.8	C25—C26—C27	121.0 (4)
C5—C4—C9	117.8 (3)	C25—C26—H26	119.5
C5—C4—P1	121.7 (3)	C27—C26—H26	119.5
C9—C4—P1	120.5 (3)	C26—C27—C22	119.5 (4)
C4—C5—C6	120.7 (4)	C26—C27—H27	120.2
C4—C5—H5	119.7	C22—C27—H27	120.2
C6—C5—H5	119.7	C31ⁱ—C28—C29	127.8 (15)
C7—C6—C5	120.2 (4)	C31ⁱ—C28—H28	117.4
C7—C6—H6	119.9	C29—C28—H28	114.8
C5—C6—H6	119.9	C32—C28—H29B	105.8
C8—C7—C6	119.5 (4)	C28—C29—C30	109.8 (10)
C8—C7—H7	120.2	C28—C29—H29A	127.5
C6—C7—H7	120.2	C30—C29—H29A	122.7
C9—C8—C7	120.3 (4)	C32—C29—H29B	114.6
C9—C8—H8	119.9	C30—C29—H29C	93.1
C7—C8—H8	119.9	H29B—C29—H29C	92.3
C8—C9—C4	121.6 (4)	C28—C29—H29D	99.6
C8—C9—H9	119.2	C32—C29—H29D	118.0
C4—C9—H9	119.2	C30—C29—H29D	113.5
C15—C10—C11	118.6 (4)	H29C—C29—H29D	89.1
C15—C10—P1	122.4 (3)	C31—C30—C29	112.3 (13)
C11—C10—P1	118.9 (3)	C31—C30—H30	127.3
C12—C11—C10	120.6 (4)	C29—C30—H30	120.4
C12—C11—H11	119.7	C32—C31—C28ⁱ	125.2 (14)
C10—C11—H11	119.7	C30—C31—H31	113.3
C11—C12—C13	119.7 (5)	C32ⁱ—C31—H31	109.1
C11—C12—H12	120.2	C31ⁱ—C32—C29	129.1 (16)
C13—C12—H12	120.2	C1—N—Mo	176.2 (3)
C14—C13—C12	120.3 (4)	C4—P1—C10	100.52 (16)
C14—C13—H13	119.8	C4—P1—C3	99.91 (16)
C12—C13—H13	119.8	C10—P1—C3	104.00 (16)
C15—C14—C13	119.5 (5)	C4—P1—Mo	125.01 (11)
C15—C14—H14	120.2	C10—P1—Mo	115.26 (11)
C13—C14—H14	120.2	C3—P1—Mo	109.43 (11)
C14—C15—C10	121.2 (4)	C22—P2—C16	104.17 (16)
C14—C15—H15	119.4	C22—P2—C2	104.63 (16)
C10—C15—H15	119.4	C16—P2—C2	101.09 (16)
C21—C16—C17	118.3 (4)	C22—P2—Mo	115.71 (11)
C21—C16—P2	122.3 (3)	C16—P2—Mo	123.73 (11)
C17—C16—P2	119.4 (3)	C2—P2—Mo	105.06 (11)
C18—C17—C16	120.8 (4)	Nⁱⁱ—Mo—N	180.000 (1)
C18—C17—H17	119.6	Nⁱⁱ—Mo—P2	95.70 (8)
C16—C17—H17	119.6	N—Mo—P2	84.30 (8)
C19—C18—C17	120.4 (4)	Nⁱⁱ—Mo—P2ⁱⁱ	84.30 (8)
C19—C18—H18	119.8	N—Mo—P2ⁱⁱ	95.70 (8)
C17—C18—H18	119.8	P2—Mo—P2ⁱⁱ	180.0
C20—C19—C18	119.5 (4)	Nⁱⁱ—Mo—P1ⁱⁱ	84.88 (8)
C20—C19—H19	120.2	N—Mo—P1ⁱⁱ	95.12 (8)
C18—C19—H19	120.2	P2—Mo—P1ⁱⁱ	100.31 (3)
C19—C20—C21	120.6 (4)	P2ⁱⁱ—Mo—P1ⁱⁱ	79.69 (3)
C19—C20—H20	119.7	Nⁱⁱ—Mo—P1	95.12 (8)
C21—C20—H20	119.7	N—Mo—P1	84.88 (8)
C16—C21—C20	120.4 (4)	P2—Mo—P1	79.69 (3)
C16—C21—H21	119.8	P2ⁱⁱ—Mo—P1	100.31 (3)
C20—C21—H21	119.8	P1ⁱⁱ—Mo—P1	180.0

P2—C2—C3—P1	−46.3 (3)	C11—C10—P1—Mo	91.4 (3)
C9—C4—C5—C6	−1.2 (6)	C2—C3—P1—C4	151.6 (3)
P1—C4—C5—C6	179.2 (3)	C2—C3—P1—C10	−104.9 (3)
C4—C5—C6—C7	−0.2 (7)	C2—C3—P1—Mo	18.8 (3)
C5—C6—C7—C8	1.1 (7)	C27—C22—P2—C16	90.4 (3)
C6—C7—C8—C9	−0.6 (7)	C23—C22—P2—C16	−91.0 (3)
C7—C8—C9—C4	−0.7 (7)	C27—C22—P2—C2	−15.3 (3)
C5—C4—C9—C8	1.6 (6)	C23—C22—P2—C2	163.3 (3)
P1—C4—C9—C8	−178.8 (3)	C27—C22—P2—Mo	−130.4 (3)
C15—C10—C11—C12	−0.7 (6)	C23—C22—P2—Mo	48.2 (3)
P1—C10—C11—C12	−176.8 (3)	C21—C16—P2—C22	22.0 (3)
C10—C11—C12—C13	−0.8 (7)	C17—C16—P2—C22	−160.9 (3)
C11—C12—C13—C14	1.8 (8)	C21—C16—P2—C2	130.3 (3)
C12—C13—C14—C15	−1.3 (8)	C17—C16—P2—C2	−52.6 (3)
C13—C14—C15—C10	−0.2 (7)	C21—C16—P2—Mo	−113.0 (3)
C11—C10—C15—C14	1.2 (6)	C17—C16—P2—Mo	64.1 (3)
P1—C10—C15—C14	177.2 (3)	C3—C2—P2—C22	−70.5 (3)
C21—C16—C17—C18	−0.6 (5)	C3—C2—P2—C16	−178.5 (2)
P2—C16—C17—C18	−177.8 (3)	C3—C2—P2—Mo	51.8 (3)
C16—C17—C18—C19	0.2 (6)	C22—P2—Mo—Nⁱⁱ	−8.71 (15)
C17—C18—C19—C20	0.1 (7)	C16—P2—Mo—Nⁱⁱ	121.69 (16)
C18—C19—C20—C21	0.1 (7)	C2—P2—Mo—Nⁱⁱ	−123.53 (15)
C17—C16—C21—C20	0.7 (6)	C22—P2—Mo—N	171.29 (15)
P2—C16—C21—C20	177.8 (3)	C16—P2—Mo—N	−58.31 (16)
C19—C20—C21—C16	−0.4 (7)	C2—P2—Mo—N	56.47 (15)
C27—C22—C23—C24	0.7 (5)	C22—P2—Mo—P1ⁱⁱ	−94.52 (13)
P2—C22—C23—C24	−178.0 (3)	C16—P2—Mo—P1ⁱⁱ	35.88 (15)
C22—C23—C24—C25	0.5 (6)	C2—P2—Mo—P1ⁱⁱ	150.66 (12)
C23—C24—C25—C26	−1.1 (6)	C22—P2—Mo—P1	85.48 (13)
C24—C25—C26—C27	0.5 (7)	C16—P2—Mo—P1	−144.12 (15)
C25—C26—C27—C22	0.6 (6)	C2—P2—Mo—P1	−29.34 (12)
C23—C22—C27—C26	−1.2 (5)	C4—P1—Mo—Nⁱⁱ	−14.26 (15)
P2—C22—C27—C26	177.4 (3)	C10—P1—Mo—Nⁱⁱ	−139.49 (15)
C5—C4—P1—C10	121.5 (3)	C3—P1—Mo—Nⁱⁱ	103.77 (15)
C9—C4—P1—C10	−58.1 (3)	C4—P1—Mo—N	165.74 (15)
C5—C4—P1—C3	−132.1 (3)	C10—P1—Mo—N	40.51 (15)
C9—C4—P1—C3	48.3 (3)	C3—P1—Mo—N	−76.23 (15)
C5—C4—P1—Mo	−9.8 (4)	C4—P1—Mo—P2	−109.14 (14)
C9—C4—P1—Mo	170.6 (3)	C10—P1—Mo—P2	125.63 (14)
C15—C10—P1—C4	138.3 (3)	C3—P1—Mo—P2	8.89 (13)
C11—C10—P1—C4	−45.7 (3)	C4—P1—Mo—P2ⁱⁱ	70.86 (14)
C15—C10—P1—C3	35.2 (3)	C10—P1—Mo—P2ⁱⁱ	−54.37 (14)
C11—C10—P1—C3	−148.8 (3)	C3—P1—Mo—P2ⁱⁱ	−171.11 (13)
C15—C10—P1—Mo	−84.5 (3)

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

Experimental details

Crystal data
Chemical formula	[Mo(NCS)₂(C₂₆H₂₄P₂)₂]·C₇H₈
M_r	1101.02
Crystal system, space group	Monoclinic, P2₁/c
Temperature (K)	180
a, b, c (Å)	9.6277 (13), 17.017 (2), 16.755 (2)
β (°)	104.172 (11)
V (Å³)	2661.5 (6)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	0.49
Crystal size (mm)	0.68 × 0.62 × 0.48

Data collection
Diffractometer	Stoe STADI-4
Absorption correction	ψ scan (North et al., 1968)
T_min, T_max	0.733, 0.800
No. of measured, independent and observed [I > 2σ(I)] reflections	4828, 4820, 3796
R_int	0.098
(sin θ/λ)_max (Å⁻¹)	0.600

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.040, 0.101, 1.09
No. of reflections	4820
No. of parameters	306
No. of restraints	5
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.74, −0.43

Computer programs: STADI4 (Stoe & Cie, 1997), STADI4, X-RED (Stoe & Cie, 1997), SHELXS97 (Sheldrick, 1990), SHELXL97 (Sheldrick, 1997), DIAMOND (Brandenburg, 1999), SHELXL97.

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trans-Bis­[ethane-1,2-diyl­bis­(di­phenyl­phosphane)-κ2P,P′]­bis­(thio­cyanato-κN)molybdenum(II) toluene solvate

Supporting information

Key indicators

checkCIF results

trans-Bis[ethane-1,2-diylbis(diphenylphosphane)-κ2P,P′]bis(thiocyanato-κN)molybdenum(II) toluene solvate