Penta­carbonyl­(tetra­phenyl­diphosphine mono­sulfide-P)­chromium(0)

Jones, P.G.; Fischer, A.K.; Farkens, M.; Schmutzler, R.

doi:10.1107/S1600536802014125

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Pentacarbonyl(tetraphenyldiphosphine monosulfide-P)chromium(0)

P. G. Jones, A. K. Fischer, M. Farkens and R. Schmutzler

In the title compound, [Cr(C₂₄H₂₀P₂S)(CO)₅], the key bond lengths are P1-P2 2.2659 (15), P2-S 1.9531 (15), P1-C 1.830, 1.833 (3), P2-C 1.821, 1.822 (3) and P1-Cr 2.3921 (13) Å. The conformation about the P-P bond is defined by the torsion angle S-P2-P1-Cr of -58.60 (7)°.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802014125/cv6136sup1.cif Contains datablocks I, global
	Structure factor file (CIF format) https://doi.org/10.1107/S1600536802014125/cv6136Isup2.hkl Contains datablock I

CCDC reference: 197447

checkCIF report

Key indicators

Single-crystal X-ray study
T = 178 K
Mean (C-C) = 0.005 Å
R factor = 0.040
wR factor = 0.108
Data-to-parameter ratio = 13.3

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry

General Notes



ABSTM_02  When printed, the submitted absorption T values will be replaced
          by the scaled T values. Since the ratio of scaled T's is
          identical to the ratio of reported T values, the scaling does
          not imply a change to the absorption corrections used in the
          study.
          Ratio of Tmax expected/reported      0.884
          Tmax scaled      0.877 Tmin scaled      0.708

Comment top

The title compound, (I), arose during studies (see Experimental) of thioureas substituted with phosphorus-containing groups (Farkens, 1991). It was characterized by this structure determination.

The molecule of (I) is shown in Fig. 1. A search of the Cambridge Structural Database (CSD, Version of April 2002; Allen & Kennard, 1993) revealed no other complexes of any tetra(organyl)diphosphine monosulfide (in the strict sense of a compound containing a P—P bond). The key bond lengths are P1—P2 2.2659 (15), P2—S 1.9531 (15), P1—C 1.830, 1.833 (3) and P2—C 1.821 1.822 (3) Å. These may be compared, although the two systems clearly differ chemically in many respects, with values for uncomplexed tetramethyldiphosphane monosulfide (Gruber et al., 1990): P—P 2.201 (1), P—S 1.970 (1), P^III—C 1.830 and 1.834 (1), and P(S)—C 1.803 and 1.803 (1) Å. The P—P bond in (I) may be regarded as long, and it is reasonable to propose steric effects as the cause. A CSD search revealed 57 structures with (C)₂P—P(C)₂ single bonds, involving 69 bonds in the range 2.104–2.310 Å (average 2.216 Å).

The P—Cr distance is 2.3921 (13) Å, and the Cr—C bond trans to Cr—P is by far the shortest at 1.865 (4) Å, cf. average 1.903 Å for the other four Cr—C bonds. The conformation about the P—P bond is defined by the torsion angle S—P2—P1—Cr of −58.60 (7)° (in the above-mentioned diphosphine monosulfide, the S atom is trans to the lone pair at the other phosphorus). As expected, the largest angles at phosphorus are those involving the Cr atom at P1 and the S atom at P2.

Two short H···O contacts could reasonably be interpreted as weak hydrogen bonds (Table 2).

Experimental top

The reaction between (norbornadiene)Cr(CO)₄ and N,N'-bis(diphenylphosphino)-N,N'-dimethylthiourea in dichloromethane led to a complex mixture of products. The mixture was dissolved in diethyl ether, from which the title compound crystallized in 13% yield (Farkens, 1991). The decomposition of the thiourea to tetraphenyldiphosphine monosulfide has been observed before in our laboratory (Gruber, 1989).

Computing details top

Data collection: P3 (Nicolet, 1987); cell refinement: P3; data reduction: XDISK (Nicolet, 1987); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP (Siemens, 1994); software used to prepare material for publication: SHELXL97.

Figures top

Fig. 1. The molecule of compound (I) in the crystal. Displacement ellipsoids represent 30% probability levels. H-atom radii are arbitrary.

(Tetraphenyldiphosphinmonosulfide-P)pentacarbonylchromium(0) top

Crystal data top

[Cr(C₂₄H₂₀P₂S)(CO)₅]	Z = 2
M_r = 594.45	F(000) = 608
Triclinic, P1	D_x = 1.466 Mg m⁻³
a = 9.840 (3) Å	Mo Kα radiation, λ = 0.71073 Å
b = 10.089 (5) Å	Cell parameters from 50 reflections
c = 14.967 (6) Å	θ = 10–11.5°
α = 77.90 (3)°	µ = 0.66 mm⁻¹
β = 84.43 (3)°	T = 178 K
γ = 68.02 (3)°	Tablet, yellow
V = 1347.0 (10) Å³	0.5 × 0.5 × 0.2 mm

Data collection top

Nicolet R3 diffractometer	3476 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	R_int = 0.038
Graphite monochromator	θ_max = 25.1°, θ_min = 3.1°
ω scans	h = −11→11
Absorption correction: ψ scan (XEMP; Nicolet, 1987)	k = −11→11
T_min = 0.801, T_max = 0.991	l = −12→17
5120 measured reflections	3 standard reflections every 147 reflections
4578 independent reflections	intensity decay: none

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) = 0.108	H-atom parameters constrained
S = 1.03	w = 1/[σ²(F_o²) + (0.0464P)² + 1.6663P] where P = (F_o² + 2F_c²)/3
4578 reflections	(Δ/σ)_max < 0.001
343 parameters	Δρ_max = 0.48 e Å⁻³
0 restraints	Δρ_min = −0.47 e Å⁻³

Crystal data top

[Cr(C₂₄H₂₀P₂S)(CO)₅]	γ = 68.02 (3)°
M_r = 594.45	V = 1347.0 (10) Å³
Triclinic, P1	Z = 2
a = 9.840 (3) Å	Mo Kα radiation
b = 10.089 (5) Å	µ = 0.66 mm⁻¹
c = 14.967 (6) Å	T = 178 K
α = 77.90 (3)°	0.5 × 0.5 × 0.2 mm
β = 84.43 (3)°

Data collection top

Nicolet R3 diffractometer	3476 reflections with I > 2σ(I)
Absorption correction: ψ scan (XEMP; Nicolet, 1987)	R_int = 0.038
T_min = 0.801, T_max = 0.991	3 standard reflections every 147 reflections
5120 measured reflections	intensity decay: none
4578 independent reflections

Refinement top

R[F² > 2σ(F²)] = 0.040	0 restraints
wR(F²) = 0.108	H-atom parameters constrained
S = 1.03	Δρ_max = 0.48 e Å⁻³
4578 reflections	Δρ_min = −0.47 e Å⁻³
343 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.

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

	x	y	z	U_iso*/U_eq
Cr	0.12119 (5)	0.22328 (5)	0.40722 (3)	0.02628 (15)
S	0.06062 (9)	0.57737 (10)	0.15723 (6)	0.0382 (2)
P1	0.23659 (8)	0.21117 (8)	0.25938 (5)	0.02230 (19)
P2	0.25228 (8)	0.42161 (8)	0.17823 (5)	0.02327 (19)
O1	0.3039 (3)	−0.0945 (3)	0.47601 (17)	0.0481 (7)
O2	0.3385 (3)	0.3212 (3)	0.48080 (17)	0.0508 (7)
O3	−0.0302 (3)	0.2233 (3)	0.59188 (18)	0.0514 (7)
O4	−0.1003 (3)	0.1140 (3)	0.35052 (18)	0.0489 (7)
O5	−0.0987 (3)	0.5345 (3)	0.3672 (2)	0.0626 (8)
C1	0.4255 (3)	0.0849 (3)	0.2502 (2)	0.0240 (6)
C2	0.4827 (3)	0.0388 (3)	0.1683 (2)	0.0299 (7)
H2	0.4217	0.0691	0.1168	0.036*
C3	0.6278 (4)	−0.0508 (4)	0.1620 (3)	0.0378 (8)
H3	0.6666	−0.0801	0.1056	0.045*
C4	0.7171 (4)	−0.0983 (4)	0.2370 (3)	0.0425 (9)
H4	0.8160	−0.1620	0.2327	0.051*
C5	0.6619 (4)	−0.0527 (4)	0.3175 (2)	0.0400 (9)
H5	0.7235	−0.0837	0.3688	0.048*
C6	0.5170 (3)	0.0381 (4)	0.3248 (2)	0.0321 (7)
H6	0.4799	0.0687	0.3810	0.038*
C7	0.1355 (3)	0.1573 (3)	0.1860 (2)	0.0237 (6)
C8	0.0092 (4)	0.2571 (4)	0.1432 (2)	0.0365 (8)
H8	−0.0171	0.3576	0.1435	0.044*
C9	−0.0793 (4)	0.2120 (4)	0.0998 (3)	0.0450 (9)
H9	−0.1650	0.2815	0.0699	0.054*
C10	−0.0430 (4)	0.0660 (4)	0.1002 (2)	0.0407 (9)
H10	−0.1036	0.0350	0.0704	0.049*
C11	0.0804 (4)	−0.0344 (4)	0.1435 (2)	0.0405 (9)
H11	0.1046	−0.1350	0.1442	0.049*
C12	0.1698 (3)	0.0107 (4)	0.1862 (2)	0.0322 (7)
H12	0.2554	−0.0594	0.2159	0.039*
C13	0.3465 (3)	0.3827 (3)	0.0705 (2)	0.0245 (6)
C14	0.2578 (4)	0.3983 (4)	−0.0014 (2)	0.0325 (7)
H14	0.1543	0.4310	0.0070	0.039*
C15	0.3201 (4)	0.3664 (4)	−0.0847 (2)	0.0397 (8)
H15	0.2593	0.3772	−0.1334	0.048*
C16	0.4705 (4)	0.3189 (4)	−0.0978 (2)	0.0358 (8)
H16	0.5133	0.2968	−0.1551	0.043*
C17	0.5573 (4)	0.3040 (4)	−0.0273 (2)	0.0378 (8)
H17	0.6607	0.2715	−0.0362	0.045*
C18	0.4972 (3)	0.3354 (4)	0.0562 (2)	0.0324 (7)
H18	0.5592	0.3245	0.1042	0.039*
C19	0.3649 (3)	0.4636 (3)	0.2496 (2)	0.0265 (7)
C20	0.5115 (3)	0.3782 (4)	0.2695 (2)	0.0311 (7)
H20	0.5586	0.2917	0.2455	0.037*
C21	0.5876 (4)	0.4198 (4)	0.3243 (3)	0.0435 (9)
H21	0.6875	0.3623	0.3370	0.052*
C22	0.5201 (4)	0.5442 (4)	0.3606 (3)	0.0466 (10)
H22	0.5737	0.5726	0.3976	0.056*
C23	0.3750 (4)	0.6270 (4)	0.3433 (2)	0.0412 (9)
H23	0.3280	0.7119	0.3689	0.049*
C24	0.2971 (4)	0.5864 (4)	0.2883 (2)	0.0336 (8)
H24	0.1966	0.6432	0.2771	0.040*
C25	0.2382 (4)	0.0257 (4)	0.4483 (2)	0.0333 (8)
C26	0.2590 (4)	0.2869 (4)	0.4496 (2)	0.0346 (8)
C27	0.0275 (4)	0.2238 (4)	0.5217 (2)	0.0365 (8)
C28	−0.0164 (4)	0.1567 (4)	0.3695 (2)	0.0334 (8)
C29	−0.0118 (4)	0.4205 (4)	0.3756 (2)	0.0376 (8)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Cr	0.0250 (3)	0.0285 (3)	0.0259 (3)	−0.0090 (2)	0.0015 (2)	−0.0087 (2)
S	0.0323 (5)	0.0326 (5)	0.0487 (5)	−0.0077 (4)	−0.0059 (4)	−0.0106 (4)
P1	0.0210 (4)	0.0235 (4)	0.0235 (4)	−0.0079 (3)	−0.0023 (3)	−0.0061 (3)
P2	0.0222 (4)	0.0219 (4)	0.0263 (4)	−0.0072 (3)	−0.0029 (3)	−0.0064 (3)
O1	0.0527 (16)	0.0344 (15)	0.0443 (15)	−0.0035 (13)	0.0030 (12)	−0.0054 (12)
O2	0.0583 (17)	0.076 (2)	0.0383 (14)	−0.0420 (16)	0.0004 (12)	−0.0207 (14)
O3	0.0471 (16)	0.0629 (18)	0.0383 (15)	−0.0131 (14)	0.0133 (13)	−0.0162 (13)
O4	0.0420 (15)	0.0630 (18)	0.0549 (17)	−0.0323 (14)	0.0076 (12)	−0.0182 (14)
O5	0.0576 (18)	0.0338 (16)	0.078 (2)	−0.0006 (14)	0.0144 (15)	−0.0092 (14)
C1	0.0206 (15)	0.0214 (16)	0.0314 (17)	−0.0087 (13)	−0.0002 (12)	−0.0059 (13)
C2	0.0304 (17)	0.0277 (17)	0.0353 (18)	−0.0139 (14)	0.0006 (14)	−0.0077 (14)
C3	0.038 (2)	0.0325 (19)	0.045 (2)	−0.0148 (16)	0.0101 (16)	−0.0133 (16)
C4	0.0242 (17)	0.0287 (19)	0.065 (3)	−0.0028 (15)	0.0035 (17)	−0.0037 (18)
C5	0.0281 (18)	0.040 (2)	0.042 (2)	−0.0064 (16)	−0.0068 (15)	0.0037 (17)
C6	0.0257 (16)	0.0367 (19)	0.0304 (18)	−0.0091 (15)	−0.0002 (13)	−0.0033 (15)
C7	0.0258 (15)	0.0263 (16)	0.0232 (15)	−0.0137 (13)	−0.0018 (12)	−0.0049 (13)
C8	0.0358 (19)	0.0293 (18)	0.047 (2)	−0.0136 (15)	−0.0133 (16)	−0.0035 (16)
C9	0.044 (2)	0.049 (2)	0.048 (2)	−0.0264 (19)	−0.0226 (17)	0.0054 (18)
C10	0.049 (2)	0.057 (2)	0.0329 (19)	−0.036 (2)	−0.0030 (16)	−0.0122 (17)
C11	0.047 (2)	0.037 (2)	0.050 (2)	−0.0229 (18)	0.0062 (17)	−0.0222 (17)
C12	0.0280 (17)	0.0294 (18)	0.0408 (19)	−0.0107 (14)	0.0000 (14)	−0.0102 (15)
C13	0.0306 (16)	0.0176 (15)	0.0275 (16)	−0.0090 (13)	−0.0035 (13)	−0.0071 (12)
C14	0.0287 (17)	0.0345 (19)	0.0322 (18)	−0.0090 (15)	−0.0038 (14)	−0.0053 (15)
C15	0.048 (2)	0.044 (2)	0.0318 (19)	−0.0170 (18)	−0.0074 (16)	−0.0127 (16)
C16	0.046 (2)	0.0350 (19)	0.0299 (18)	−0.0184 (17)	0.0071 (15)	−0.0095 (15)
C17	0.0317 (18)	0.044 (2)	0.043 (2)	−0.0179 (16)	0.0079 (15)	−0.0153 (17)
C18	0.0284 (17)	0.041 (2)	0.0309 (18)	−0.0162 (15)	−0.0004 (14)	−0.0076 (15)
C19	0.0298 (16)	0.0250 (16)	0.0279 (17)	−0.0120 (14)	−0.0020 (13)	−0.0078 (13)
C20	0.0294 (17)	0.0322 (18)	0.0329 (18)	−0.0104 (14)	−0.0046 (14)	−0.0088 (14)
C21	0.0330 (19)	0.051 (2)	0.048 (2)	−0.0134 (17)	−0.0117 (16)	−0.0115 (18)
C22	0.051 (2)	0.061 (3)	0.043 (2)	−0.029 (2)	−0.0081 (18)	−0.0207 (19)
C23	0.049 (2)	0.048 (2)	0.038 (2)	−0.0228 (19)	0.0023 (17)	−0.0228 (17)
C24	0.0311 (17)	0.0357 (19)	0.0377 (19)	−0.0140 (15)	0.0016 (14)	−0.0123 (15)
C25	0.0331 (18)	0.041 (2)	0.0270 (17)	−0.0135 (17)	0.0063 (14)	−0.0108 (16)
C26	0.0401 (19)	0.042 (2)	0.0236 (17)	−0.0165 (17)	0.0037 (14)	−0.0099 (15)
C27	0.0307 (18)	0.036 (2)	0.040 (2)	−0.0062 (15)	0.0007 (16)	−0.0128 (16)
C28	0.0320 (18)	0.037 (2)	0.0316 (18)	−0.0138 (16)	0.0048 (14)	−0.0075 (15)
C29	0.0373 (19)	0.032 (2)	0.042 (2)	−0.0111 (17)	0.0073 (16)	−0.0123 (16)

Geometric parameters (Å, º) top

Cr—C27	1.865 (4)	C8—H8	0.9500
Cr—C25	1.893 (4)	C9—C10	1.378 (5)
Cr—C28	1.895 (4)	C9—H9	0.9500
Cr—C26	1.909 (4)	C10—C11	1.369 (5)
Cr—C29	1.916 (4)	C10—H10	0.9500
Cr—P1	2.3921 (13)	C11—C12	1.386 (5)
S—P2	1.9531 (15)	C11—H11	0.9500
P1—C1	1.830 (3)	C12—H12	0.9500
P1—C7	1.833 (3)	C13—C18	1.387 (4)
P1—P2	2.2659 (15)	C13—C14	1.399 (4)
P2—C13	1.821 (3)	C14—C15	1.381 (5)
P2—C19	1.822 (3)	C14—H14	0.9500
O1—C25	1.146 (4)	C15—C16	1.382 (5)
O2—C26	1.135 (4)	C15—H15	0.9500
O3—C27	1.144 (4)	C16—C17	1.371 (5)
O4—C28	1.144 (4)	C16—H16	0.9500
O5—C29	1.138 (4)	C17—C18	1.376 (5)
C1—C6	1.391 (4)	C17—H17	0.9500
C1—C2	1.394 (4)	C18—H18	0.9500
C2—C3	1.382 (5)	C19—C24	1.387 (4)
C2—H2	0.9500	C19—C20	1.399 (4)
C3—C4	1.383 (5)	C20—C21	1.381 (5)
C3—H3	0.9500	C20—H20	0.9500
C4—C5	1.371 (5)	C21—C22	1.380 (5)
C4—H4	0.9500	C21—H21	0.9500
C5—C6	1.384 (5)	C22—C23	1.376 (5)
C5—H5	0.9500	C22—H22	0.9500
C6—H6	0.9500	C23—C24	1.389 (5)
C7—C8	1.384 (4)	C23—H23	0.9500
C7—C12	1.388 (4)	C24—H24	0.9500
C8—C9	1.384 (5)

C27—Cr—C25	88.48 (15)	C10—C9—H9	120.1
C27—Cr—C28	88.55 (15)	C8—C9—H9	120.1
C25—Cr—C28	87.44 (15)	C11—C10—C9	120.1 (3)
C27—Cr—C26	89.65 (15)	C11—C10—H10	119.9
C25—Cr—C26	91.50 (15)	C9—C10—H10	119.9
C28—Cr—C26	177.94 (14)	C10—C11—C12	120.0 (3)
C27—Cr—C29	85.89 (15)	C10—C11—H11	120.0
C25—Cr—C29	173.94 (14)	C12—C11—H11	120.0
C28—Cr—C29	90.19 (15)	C11—C12—C7	120.6 (3)
C26—Cr—C29	90.69 (16)	C11—C12—H12	119.7
C27—Cr—P1	176.55 (11)	C7—C12—H12	119.7
C25—Cr—P1	89.77 (10)	C18—C13—C14	118.7 (3)
C28—Cr—P1	88.40 (10)	C18—C13—P2	125.1 (2)
C26—Cr—P1	93.36 (10)	C14—C13—P2	116.2 (2)
C29—Cr—P1	95.75 (11)	C15—C14—C13	120.2 (3)
C1—P1—C7	103.54 (14)	C15—C14—H14	119.9
C1—P1—P2	101.21 (10)	C13—C14—H14	119.9
C7—P1—P2	104.56 (10)	C14—C15—C16	120.4 (3)
C1—P1—Cr	119.02 (11)	C14—C15—H15	119.8
C7—P1—Cr	110.78 (10)	C16—C15—H15	119.8
P2—P1—Cr	116.02 (5)	C17—C16—C15	119.3 (3)
C13—P2—C19	110.90 (14)	C17—C16—H16	120.3
C13—P2—S	111.01 (11)	C15—C16—H16	120.3
C19—P2—S	111.67 (11)	C16—C17—C18	121.1 (3)
C13—P2—P1	107.35 (10)	C16—C17—H17	119.4
C19—P2—P1	103.03 (11)	C18—C17—H17	119.4
S—P2—P1	112.55 (6)	C17—C18—C13	120.2 (3)
C6—C1—C2	118.7 (3)	C17—C18—H18	119.9
C6—C1—P1	119.9 (2)	C13—C18—H18	119.9
C2—C1—P1	121.3 (2)	C24—C19—C20	118.9 (3)
C3—C2—C1	120.1 (3)	C24—C19—P2	116.7 (2)
C3—C2—H2	119.9	C20—C19—P2	124.4 (2)
C1—C2—H2	119.9	C21—C20—C19	119.9 (3)
C2—C3—C4	120.6 (3)	C21—C20—H20	120.0
C2—C3—H3	119.7	C19—C20—H20	120.0
C4—C3—H3	119.7	C22—C21—C20	120.7 (3)
C5—C4—C3	119.6 (3)	C22—C21—H21	119.7
C5—C4—H4	120.2	C20—C21—H21	119.7
C3—C4—H4	120.2	C23—C22—C21	119.9 (3)
C4—C5—C6	120.5 (3)	C23—C22—H22	120.1
C4—C5—H5	119.7	C21—C22—H22	120.1
C6—C5—H5	119.7	C22—C23—C24	120.0 (3)
C5—C6—C1	120.5 (3)	C22—C23—H23	120.0
C5—C6—H6	119.8	C24—C23—H23	120.0
C1—C6—H6	119.8	C19—C24—C23	120.5 (3)
C8—C7—C12	118.5 (3)	C19—C24—H24	119.7
C8—C7—P1	121.0 (2)	C23—C24—H24	119.7
C12—C7—P1	119.4 (2)	O1—C25—Cr	176.9 (3)
C9—C8—C7	120.8 (3)	O2—C26—Cr	175.3 (3)
C9—C8—H8	119.6	O3—C27—Cr	179.6 (3)
C7—C8—H8	119.6	O4—C28—Cr	177.1 (3)
C10—C9—C8	119.9 (3)	O5—C29—Cr	171.5 (3)

C25—Cr—P1—C1	−29.32 (15)	P2—P1—C7—C12	145.4 (2)
C28—Cr—P1—C1	−116.76 (15)	Cr—P1—C7—C12	−88.9 (2)
C26—Cr—P1—C1	62.17 (16)	C12—C7—C8—C9	−1.4 (5)
C29—Cr—P1—C1	153.20 (15)	P1—C7—C8—C9	−169.7 (3)
C25—Cr—P1—C7	90.49 (15)	C7—C8—C9—C10	1.0 (6)
C28—Cr—P1—C7	3.04 (15)	C8—C9—C10—C11	0.1 (6)
C26—Cr—P1—C7	−178.02 (15)	C9—C10—C11—C12	−0.7 (5)
C29—Cr—P1—C7	−86.99 (15)	C10—C11—C12—C7	0.2 (5)
C25—Cr—P1—P2	−150.53 (11)	C8—C7—C12—C11	0.8 (5)
C28—Cr—P1—P2	122.02 (11)	P1—C7—C12—C11	169.3 (3)
C26—Cr—P1—P2	−59.04 (12)	C19—P2—C13—C18	23.4 (3)
C29—Cr—P1—P2	31.99 (12)	S—P2—C13—C18	148.1 (3)
C1—P1—P2—C13	48.63 (15)	P1—P2—C13—C18	−88.5 (3)
C7—P1—P2—C13	−58.72 (15)	C19—P2—C13—C14	−158.7 (2)
Cr—P1—P2—C13	178.96 (10)	S—P2—C13—C14	−33.9 (3)
C1—P1—P2—C19	−68.50 (15)	P1—P2—C13—C14	89.5 (2)
C7—P1—P2—C19	−175.85 (14)	C18—C13—C14—C15	0.2 (5)
Cr—P1—P2—C19	61.83 (11)	P2—C13—C14—C15	−177.8 (3)
C1—P1—P2—S	171.07 (11)	C13—C14—C15—C16	0.0 (5)
C7—P1—P2—S	63.72 (11)	C14—C15—C16—C17	−0.1 (5)
Cr—P1—P2—S	−58.60 (7)	C15—C16—C17—C18	0.1 (5)
C7—P1—C1—C6	−146.8 (3)	C16—C17—C18—C13	0.1 (5)
P2—P1—C1—C6	105.1 (2)	C14—C13—C18—C17	−0.3 (5)
Cr—P1—C1—C6	−23.3 (3)	P2—C13—C18—C17	177.6 (3)
C7—P1—C1—C2	36.1 (3)	C13—P2—C19—C24	132.2 (3)
P2—P1—C1—C2	−72.0 (2)	S—P2—C19—C24	7.9 (3)
Cr—P1—C1—C2	159.5 (2)	P1—P2—C19—C24	−113.2 (2)
C6—C1—C2—C3	−0.4 (4)	C13—P2—C19—C20	−49.9 (3)
P1—C1—C2—C3	176.8 (2)	S—P2—C19—C20	−174.3 (2)
C1—C2—C3—C4	1.3 (5)	P1—P2—C19—C20	64.7 (3)
C2—C3—C4—C5	−1.7 (5)	C24—C19—C20—C21	−2.4 (5)
C3—C4—C5—C6	1.2 (5)	P2—C19—C20—C21	179.8 (3)
C4—C5—C6—C1	−0.2 (5)	C19—C20—C21—C22	0.8 (5)
C2—C1—C6—C5	−0.2 (5)	C20—C21—C22—C23	0.8 (6)
P1—C1—C6—C5	−177.3 (3)	C21—C22—C23—C24	−0.8 (6)
C1—P1—C7—C8	−152.0 (3)	C20—C19—C24—C23	2.4 (5)
P2—P1—C7—C8	−46.4 (3)	P2—C19—C24—C23	−179.7 (3)
Cr—P1—C7—C8	79.3 (3)	C22—C23—C24—C19	−0.8 (5)
C1—P1—C7—C12	39.8 (3)

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
C22—H22···O2ⁱ	0.95	2.65	3.581 (4)	166
C21—H21···O4ⁱⁱ	0.95	2.57	3.426 (5)	149

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

Experimental details

Crystal data
Chemical formula	[Cr(C₂₄H₂₀P₂S)(CO)₅]
M_r	594.45
Crystal system, space group	Triclinic, P1
Temperature (K)	178
a, b, c (Å)	9.840 (3), 10.089 (5), 14.967 (6)
α, β, γ (°)	77.90 (3), 84.43 (3), 68.02 (3)
V (Å³)	1347.0 (10)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	0.66
Crystal size (mm)	0.5 × 0.5 × 0.2

Data collection
Diffractometer	Nicolet R3 diffractometer
Absorption correction	ψ scan (XEMP; Nicolet, 1987)
T_min, T_max	0.801, 0.991
No. of measured, independent and observed [I > 2σ(I)] reflections	5120, 4578, 3476
R_int	0.038
(sin θ/λ)_max (Å⁻¹)	0.596

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.040, 0.108, 1.03
No. of reflections	4578
No. of parameters	343
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.48, −0.47

Computer programs: P3 (Nicolet, 1987), P3, XDISK (Nicolet, 1987), SHELXS97 (Sheldrick, 1990), SHELXL97 (Sheldrick, 1997), XP (Siemens, 1994), SHELXL97.

Selected geometric parameters (Å, º) top

Cr—C27	1.865 (4)	S—P2	1.9531 (15)
Cr—C25	1.893 (4)	P1—C1	1.830 (3)
Cr—C28	1.895 (4)	P1—C7	1.833 (3)
Cr—C26	1.909 (4)	P1—P2	2.2659 (15)
Cr—C29	1.916 (4)	P2—C13	1.821 (3)
Cr—P1	2.3921 (13)	P2—C19	1.822 (3)

C27—Cr—C25	88.48 (15)	C29—Cr—P1	95.75 (11)
C27—Cr—C28	88.55 (15)	C1—P1—C7	103.54 (14)
C25—Cr—C28	87.44 (15)	C1—P1—P2	101.21 (10)
C27—Cr—C26	89.65 (15)	C7—P1—P2	104.56 (10)
C25—Cr—C26	91.50 (15)	C1—P1—Cr	119.02 (11)
C28—Cr—C26	177.94 (14)	C7—P1—Cr	110.78 (10)
C27—Cr—C29	85.89 (15)	P2—P1—Cr	116.02 (5)
C25—Cr—C29	173.94 (14)	C13—P2—C19	110.90 (14)
C28—Cr—C29	90.19 (15)	C13—P2—S	111.01 (11)
C26—Cr—C29	90.69 (16)	C19—P2—S	111.67 (11)
C27—Cr—P1	176.55 (11)	C13—P2—P1	107.35 (10)
C25—Cr—P1	89.77 (10)	C19—P2—P1	103.03 (11)
C28—Cr—P1	88.40 (10)	S—P2—P1	112.55 (6)
C26—Cr—P1	93.36 (10)

C1—P1—P2—C13	48.63 (15)	Cr—P1—P2—C19	61.83 (11)
C7—P1—P2—C13	−58.72 (15)	C1—P1—P2—S	171.07 (11)
Cr—P1—P2—C13	178.96 (10)	C7—P1—P2—S	63.72 (11)
C1—P1—P2—C19	−68.50 (15)	Cr—P1—P2—S	−58.60 (7)
C7—P1—P2—C19	−175.85 (14)

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
C22—H22···O2ⁱ	0.95	2.65	3.581 (4)	166.4
C21—H21···O4ⁱⁱ	0.95	2.57	3.426 (5)	149.3

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

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