Penta­carbonyl­[di­phenyl­(per­fluoro­vinyl)­phosphine]molybdenum(0)

In the title compound, [Mo{(C₂F₃)PPh₂}(CO)₅], the Mo atom occupies the center of a slightly distorted octahedral environment, bound to five carbonyl groups and one phosphine ligand, so that the local symmetry of the Mo(CO)₄P portion of the mol­ecule is approximately C_4v. The P atom sits in a distorted-tetrahedral environment; the C—P—Mo angles are much larger than the C—P—C angles. The C₂F₃ group is rotationally disordered by ∼180°.

Key indicators

• Single-crystal X-ray study
• T = 293 K
• Mean [sigma](C-C) = 0.006 Å
• R factor = 0.034
• wR factor = 0.077
• Data-to-parameter ratio = 11.9

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT242_ALERT_2_C Check Low    U(eq) as Compared to Neighbors ....       C19A
PLAT301_ALERT_3_C Main Residue  Disorder .........................      12.00 Perc.
PLAT764_ALERT_4_C Overcomplete CIF Bond list Detected (Rep/Expd) .       1.21 Ratio

   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
   3 ALERT level C = Check and explain
   0 ALERT level G = General alerts; check

   0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   1 ALERT type 2 Indicator that the structure model may be wrong or deficient
   1 ALERT type 3 Indicator that the structure quality may be low
   1 ALERT type 4 Improvement, methodology, query or suggestion

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Computing details

Data collection: XSCANS (Bruker, 1996); cell refinement: XSCANS (Bruker, 1996); data reduction: XSCANS (Bruker, 1996); program(s) used to solve structure: SHELXS90 (Sheldrick, 1990a); program(s) used to refine structure: SHELXL93 (Sheldrick, 1993); molecular graphics: SHELXTL/PC (Sheldrick, 1990b); software used to prepare material for publication: SHELXTL/PC (Sheldrick, 1990b) and SHELXL93 (Sheldrick, 1993).

Pentacarbonyl[diphenyl(perfluorovinyl)phosphine]molybdenum(0)

Crystal data

[Mo(C14H10F3P)(CO)5]	F(000) = 1984
Mr = 502.18	Dx = 1.647 Mg m^−3
Orthorhombic, Pbca	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2ab	Cell parameters from 100 reflections
a = 10.2463 (4) Å	θ = 7.7–16.7°
b = 16.1386 (9) Å	µ = 0.78 mm^−1
c = 24.5021 (13) Å	T = 293 K
V = 4051.7 (3) Å^3	Parallelepiped, light blue
Z = 8	0.58 × 0.55 × 0.27 mm

Data collection

Siemens Bruker P4 diffractometer	2675 reflections with I > 2σ(I)
Radiation source: normal-focus sealed tube	Rint = 0.030
Graphite monochromator	θmax = 25.0°, θmin = 2.5°
θ/2θ scans	h = −12→1
Absorption correction: integration (XSHELL; Bruker, 1999)	k = −19→1
Tmin = 0.684, Tmax = 0.806	l = −1→29
4476 measured reflections	3 standard reflections every 100 reflections
3555 independent reflections	intensity decay: 1.8%

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.034	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.077	H-atom parameters constrained
S = 1.03	w = 1/[σ^2(Fo^2) + (0.042P)^2 + 0.3244P] where P = (Fo^2 + 2Fc^2)/3
3547 reflections	(Δ/σ)max < 0.001
299 parameters	Δρmax = 0.22 e Å^−3
0 restraints	Δρmin = −0.28 e Å^−3

Special details

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 on F² for ALL reflections except for 8 with very negative F² or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F², conventional R-factors R are based on F, with F set to zero for negative F². The observed criterion of F² > σ(F²) is used only for calculating R factor obs 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 (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
Mo1	0.23006 (3)	0.35087 (2)	0.460350 (11)	0.04649 (12)
P1	0.27613 (8)	0.40695 (5)	0.36646 (3)	0.0467 (2)
O1	0.3249 (4)	0.1728 (2)	0.42318 (14)	0.1017 (11)
O2	0.1561 (3)	0.5296 (2)	0.50596 (12)	0.0909 (9)
O3	0.5224 (3)	0.3853 (2)	0.49815 (13)	0.0982 (10)
O4	−0.0624 (3)	0.3093 (2)	0.42760 (12)	0.0871 (8)
O5	0.1632 (3)	0.2806 (2)	0.57681 (11)	0.0887 (9)
C1	0.2897 (4)	0.2361 (2)	0.4358 (2)	0.0655 (9)
C2	0.1805 (4)	0.4668 (2)	0.48843 (14)	0.0599 (9)
C3	0.4188 (4)	0.3744 (2)	0.48401 (14)	0.0624 (9)
C4	0.0416 (4)	0.3253 (2)	0.43890 (14)	0.0573 (9)
C5	0.1896 (4)	0.3056 (2)	0.5343 (2)	0.0626 (9)
C6	0.2728 (3)	0.3347 (2)	0.30866 (13)	0.0542 (8)
C7	0.1835 (4)	0.2710 (3)	0.3094 (2)	0.0729 (11)
H7A	0.1321	0.2629	0.3418	0.080*
C8	0.1664 (5)	0.2201 (3)	0.2648 (2)	0.0907 (14)
H8A	0.1032	0.1762	0.2657	0.080*
C9	0.2390 (5)	0.2302 (4)	0.2201 (2)	0.100 (2)
H9A	0.2273	0.1939	0.1894	0.080*
C10	0.3300 (5)	0.2934 (4)	0.2180 (2)	0.101 (2)
H10A	0.3803	0.3000	0.1853	0.080*
C11	0.3476 (5)	0.3449 (3)	0.2623 (2)	0.0833 (12)
H11A	0.4114	0.3884	0.2606	0.080*
C12	0.4330 (3)	0.4592 (2)	0.36217 (13)	0.0514 (8)
C13	0.5455 (4)	0.4124 (3)	0.3615 (2)	0.0745 (11)
H13A	0.5398	0.3533	0.3582	0.080*
C14	0.6669 (4)	0.4505 (3)	0.3656 (2)	0.0849 (13)
H14A	0.7450	0.4177	0.3663	0.080*
C15	0.6750 (5)	0.5344 (3)	0.3698 (2)	0.0823 (12)
H15A	0.7585	0.5614	0.3707	0.080*
C16	0.5648 (5)	0.5806 (3)	0.3705 (2)	0.0850 (13)
H16A	0.5706	0.6397	0.3745	0.080*
C17	0.4443 (4)	0.5439 (2)	0.3673 (2)	0.0657 (10)
H17A	0.3676	0.5780	0.3678	0.080*
C18	0.1654 (5)	0.4847 (3)	0.3398 (3)	0.0839 (15)
C19A	0.0698 (8)	0.5221 (5)	0.3490 (4)	0.062 (4)	0.53 (2)
F1A	0.2187 (15)	0.5147 (9)	0.2849 (4)	0.083 (2)	0.53 (2)
F2A	0.0044 (9)	0.5763 (7)	0.3220 (5)	0.101 (3)	0.53 (2)
F3A	0.0114 (11)	0.5077 (8)	0.3952 (5)	0.079 (2)	0.53 (2)
C19B	0.1381 (15)	0.5208 (8)	0.3063 (7)	0.095 (6)	0.47 (2)
F1B	0.0424 (15)	0.4886 (11)	0.3827 (7)	0.111 (4)	0.47 (2)
F2B	0.0394 (17)	0.5750 (8)	0.2929 (8)	0.131 (4)	0.47 (2)
F3B	0.232 (2)	0.5232 (11)	0.2663 (5)	0.099 (3)	0.47 (2)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Mo1	0.0487 (2)	0.0475 (2)	0.0433 (2)	−0.00176 (12)	−0.00053 (12)	−0.00180 (12)
P1	0.0500 (5)	0.0443 (5)	0.0458 (5)	0.0052 (4)	−0.0019 (4)	−0.0011 (4)
O1	0.131 (3)	0.054 (2)	0.121 (3)	0.022 (2)	−0.006 (2)	−0.011 (2)
O2	0.114 (2)	0.069 (2)	0.090 (2)	0.017 (2)	0.004 (2)	−0.022 (2)
O3	0.060 (2)	0.150 (3)	0.084 (2)	−0.010 (2)	−0.016 (2)	−0.013 (2)
O4	0.058 (2)	0.104 (2)	0.099 (2)	−0.019 (2)	−0.007 (2)	−0.010 (2)
O5	0.100 (2)	0.108 (2)	0.058 (2)	−0.014 (2)	0.005 (2)	0.017 (2)
C1	0.077 (2)	0.057 (2)	0.062 (2)	0.001 (2)	−0.008 (2)	0.002 (2)
C2	0.063 (2)	0.062 (2)	0.055 (2)	−0.001 (2)	0.002 (2)	−0.001 (2)
C3	0.064 (2)	0.072 (2)	0.051 (2)	0.001 (2)	−0.002 (2)	−0.003 (2)
C4	0.061 (2)	0.056 (2)	0.055 (2)	−0.001 (2)	0.001 (2)	−0.003 (2)
C5	0.062 (2)	0.069 (2)	0.057 (2)	−0.006 (2)	−0.002 (2)	0.000 (2)
C6	0.062 (2)	0.056 (2)	0.045 (2)	0.012 (2)	−0.004 (2)	−0.0029 (15)
C7	0.087 (3)	0.078 (3)	0.054 (2)	−0.010 (2)	−0.001 (2)	−0.014 (2)
C8	0.115 (4)	0.081 (3)	0.075 (3)	−0.011 (3)	−0.011 (3)	−0.028 (2)
C9	0.127 (4)	0.103 (4)	0.069 (3)	0.030 (3)	−0.015 (3)	−0.036 (3)
C10	0.118 (4)	0.127 (4)	0.059 (3)	0.019 (4)	0.024 (3)	−0.026 (3)
C11	0.089 (3)	0.091 (3)	0.069 (3)	0.002 (2)	0.016 (2)	−0.011 (2)
C12	0.057 (2)	0.050 (2)	0.047 (2)	−0.001 (2)	−0.0009 (15)	0.008 (2)
C13	0.059 (2)	0.065 (2)	0.099 (3)	0.004 (2)	0.002 (2)	0.005 (2)
C14	0.055 (2)	0.094 (4)	0.105 (3)	0.005 (2)	0.007 (2)	0.000 (3)
C15	0.070 (3)	0.098 (4)	0.079 (3)	−0.026 (3)	0.004 (2)	0.001 (3)
C16	0.092 (3)	0.062 (3)	0.100 (3)	−0.020 (2)	0.010 (3)	−0.003 (2)
C17	0.064 (2)	0.058 (2)	0.075 (2)	−0.004 (2)	0.004 (2)	−0.002 (2)
C18	0.088 (4)	0.065 (3)	0.099 (4)	0.022 (3)	−0.042 (3)	−0.007 (3)
C19A	0.050 (5)	0.072 (6)	0.065 (7)	0.009 (4)	−0.005 (5)	0.011 (5)
F1A	0.108 (5)	0.099 (5)	0.041 (5)	0.029 (4)	0.022 (5)	0.042 (5)
F2A	0.087 (4)	0.111 (4)	0.103 (6)	0.042 (3)	−0.002 (4)	0.045 (5)
F3A	0.068 (5)	0.090 (6)	0.079 (5)	0.027 (4)	0.011 (4)	0.012 (4)
C19B	0.107 (11)	0.090 (9)	0.089 (12)	0.011 (8)	−0.008 (10)	0.007 (8)
F1B	0.099 (8)	0.112 (8)	0.123 (10)	0.058 (5)	0.039 (6)	0.034 (7)
F2B	0.137 (9)	0.114 (6)	0.144 (10)	0.042 (6)	−0.051 (8)	0.060 (8)
F3B	0.142 (7)	0.104 (6)	0.049 (7)	0.023 (5)	0.022 (7)	0.037 (6)

Geometric parameters (Å, º)

Mo1—P1	2.5168 (9)	C12—C17	1.378 (5)
Mo1—C1	2.042 (4)	C13—C14	1.391 (6)
Mo1—C2	2.057 (4)	C13—H13A	0.96
Mo1—C3	2.055 (4)	C14—C15	1.360 (6)
Mo1—C4	2.044 (4)	C14—H14A	0.96
Mo1—C5	1.996 (4)	C15—C16	1.354 (6)
P1—C6	1.834 (3)	C15—H15A	0.96
P1—C12	1.818 (3)	C16—C17	1.372 (6)
P1—C18	1.814 (5)	C16—H16A	0.96
O1—C1	1.126 (4)	C17—H17A	0.96
O2—C2	1.130 (4)	C18—C19B	1.043 (13)
O3—C3	1.130 (4)	C18—C19A	1.173 (9)
O4—C4	1.131 (4)	C18—F1A	1.529 (10)
O5—C5	1.150 (4)	C18—F1B	1.643 (15)
C6—C7	1.377 (5)	C19A—F1B	1.03 (2)
C6—C11	1.379 (5)	C19A—C19B	1.26 (2)
C7—C8	1.380 (5)	C19A—F2A	1.285 (14)
C7—H7A	0.96	C19A—F3A	1.30 (2)
C8—C9	1.334 (7)	C19A—F2B	1.65 (2)
C8—H8A	0.96	F1A—C19B	0.98 (2)
C9—C10	1.383 (7)	F2A—F2B	0.798 (15)
C9—H9A	0.96	F2A—C19B	1.68 (2)
C10—C11	1.379 (6)	F3A—F1B	0.537 (14)
C10—H10A	0.96	C19B—F3B	1.37 (2)
C11—H11A	0.96	C19B—F2B	1.38 (2)
C12—C13	1.378 (5)
P1—Mo1—C1	90.02 (11)	C16—C15—C14	119.9 (4)
P1—Mo1—C2	91.43 (10)	C16—C15—H15A	119.5
P1—Mo1—C3	90.86 (10)	C14—C15—H15A	120.6
P1—Mo1—C4	90.85 (10)	C15—C16—C17	120.8 (4)
P1—Mo1—C5	178.72 (11)	C15—C16—H16A	119.8
C1—Mo1—C2	176.24 (14)	C17—C16—H16A	119.4
C1—Mo1—C3	88.23 (15)	C16—C17—C12	120.6 (4)
C1—Mo1—C4	91.34 (14)	C16—C17—H17A	119.3
C1—Mo1—C5	89.9 (2)	C12—C17—H17A	120.1
C2—Mo1—C3	88.27 (15)	C19B—C18—C19A	69.0 (10)
C2—Mo1—C4	92.11 (14)	C19A—C18—F1A	107.8 (9)
C2—Mo1—C5	88.73 (14)	C19B—C18—F1B	106.0 (13)
C3—Mo1—C4	178.24 (14)	F1A—C18—F1B	145.6 (9)
C3—Mo1—C5	90.41 (15)	C19B—C18—P1	146.8 (12)
C4—Mo1—C5	87.88 (15)	C19A—C18—P1	144.0 (8)
Mo1—P1—C6	118.28 (11)	F1A—C18—P1	108.2 (6)
Mo1—P1—C12	112.66 (10)	F1B—C18—P1	106.0 (7)
Mo1—P1—C18	117.4 (2)	F1B—C19A—C18	96.5 (11)
C6—P1—C12	105.4 (2)	F1B—C19A—C19B	144.3 (13)
C6—P1—C18	98.6 (2)	C18—C19A—C19B	50.7 (7)
C12—P1—C18	102.2 (2)	F1B—C19A—F2A	129.1 (12)
O1—C1—Mo1	178.3 (3)	C18—C19A—F2A	133.3 (11)
O2—C2—Mo1	177.0 (3)	C19B—C19A—F2A	82.7 (11)
O3—C3—Mo1	177.8 (4)	C18—C19A—F3A	117.4 (9)
O4—C4—Mo1	178.4 (3)	C19B—C19A—F3A	167.3 (11)
O5—C5—Mo1	178.3 (3)	F2A—C19A—F3A	109.3 (9)
C7—C6—C11	118.0 (3)	F1B—C19A—F2B	153.2 (13)
C7—C6—P1	118.4 (3)	C18—C19A—F2B	105.2 (11)
C11—C6—P1	123.3 (3)	C19B—C19A—F2B	54.6 (12)
C6—C7—C8	121.2 (4)	F3A—C19A—F2B	137.0 (11)
C6—C7—H7A	118.5	F2B—F2A—C19A	102.0 (15)
C8—C7—H7A	120.2	F2B—F2A—C19B	54.3 (13)
C9—C8—C7	120.5 (5)	C19A—F2A—C19B	48.0 (7)
C9—C8—H8A	119.1	F1A—C19B—C18	97.9 (16)
C7—C8—H8A	120.4	F1A—C19B—C19A	155.8 (17)
C8—C9—C10	119.7 (4)	C18—C19B—C19A	60.4 (10)
C8—C9—H9A	119.9	C18—C19B—F3B	112.9 (14)
C10—C9—H9A	120.4	C19A—C19B—F3B	169.0 (15)
C11—C10—C9	120.3 (4)	F1A—C19B—F2B	123.6 (16)
C11—C10—H10A	121.4	C18—C19B—F2B	137.6 (18)
C9—C10—H10A	118.3	C19A—C19B—F2B	77.3 (14)
C10—C11—C6	120.2 (4)	F3B—C19B—F2B	109.0 (15)
C10—C11—H11A	119.7	F1A—C19B—F2A	149.3 (14)
C6—C11—H11A	120.1	C18—C19B—F2A	109.7 (14)
C13—C12—C17	118.4 (3)	C19A—C19B—F2A	49.3 (9)
C13—C12—P1	119.1 (3)	F3B—C19B—F2A	135.9 (13)
C17—C12—P1	121.9 (3)	F3A—F1B—C19A	109 (4)
C12—C13—C14	120.3 (4)	F3A—F1B—C18	147 (4)
C12—C13—H13A	119.7	C19A—F1B—C18	45.2 (6)
C14—C13—H13A	120.0	F2A—F2B—C19B	97.6 (15)
C15—C14—C13	120.0 (4)	F2A—F2B—C19A	49.7 (11)
C15—C14—H14A	119.8	C19B—F2B—C19A	48.2 (8)
C13—C14—H14A	120.2