Two molybdenum penta­carbonyl complexes with electro­neutral phos­phane ligands: [bis­(morpholin-4-yl)(penta­fluoro­ethyl)phosphane-κP]penta­carbonylmolybdenum(0) and penta­carbonyl[(penta­fluoro­ethyl)bis(piperidin-1-yl)phosphane-κP]molybdenum(0)

The crystal structures of the title compounds, [Mo{(C₄H₈NO)₂P(C₂F₅)}(CO)₅], (1a), and [Mo{(C₅H₁₀N)₂P(C₂F₅)}(CO)₅], (2a), were determined as part of a larger project that focuses on the synthesis and coordination chemistry of phosphane ligands possessing moderate (electro­neutral, i.e. neither electron-rich nor electron-deficient) electronic characteristics. Both complexes feature a slightly distorted octa­hedral geometry at the metal center, due to the electronic and steric repulsions between two of the four equatorial CO groups and the penta­fluoro­ethyl group attached to the phosphane ligand. Bond length and angle data for (1a) and (2a) support the conclusion that the free phosphane ligands are electro­neutral. For complex (1a), the Mo—P, Mo—C_ax and Mo—C_eq(ave) bond lengths are 2.5063 (5), 2.018 (2) and 2.048 (2) Å, respectively, and for complex (2a) these values are 2.5274 (5), 2.009 (3) and 2.050 (3) Å, respectively. Geometric data for (1a) and (2a) are compared with similar data reported for analogous Mo(CO)₅ complexes.

Computing details

For both structures, data collection: XSCANS (Bruker, 1996); cell refinement: XSCANS (Bruker, 1996); data reduction: XSCANS (Bruker, 1996); program(s) used to solve structure: SHELXS86 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL/PC (Sheldrick, 2008); software used to prepare material for publication: SHELXTL/PC (Sheldrick, 2008) and SHELXL97 (Sheldrick, 2008).

[Bis(morpholin-4-yl)(pentafluoroethyl)phosphane-κP]pentacarbonylmolybdenum(0) (1a)

Crystal data

[Mo(C10H16F5N2O2P)(CO)5]	Z = 2
Mr = 558.21	F(000) = 556
Triclinic, P1	Dx = 1.723 Mg m^−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 9.4555 (3) Å	Cell parameters from 100 reflections
b = 9.9522 (4) Å	θ = 11.7–25.4°
c = 12.8809 (5) Å	µ = 0.77 mm^−1
α = 82.536 (3)°	T = 295 K
β = 80.868 (3)°	Parallelepiped cut from block, colourless
γ = 64.345 (3)°	0.56 × 0.52 × 0.43 mm
V = 1076.23 (7) Å^3

Data collection

Bruker P4 diffractometer	4616 reflections with I > 2σ(I)
Radiation source: normal-focus sealed tube	Rint = 0.019
Graphite monochromator	θmax = 27.5°, θmin = 2.3°
θ2θ scans	h = −1→12
Absorption correction: integration (XSHELL; Bruker, 1999)	k = −12→12
Tmin = 0.642, Tmax = 0.734	l = −16→16
5836 measured reflections	3 standard reflections every 100 reflections
4932 independent reflections	intensity decay: 1.7%

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.026	H-atom parameters constrained
wR(F^2) = 0.070	w = 1/[σ^2(Fo^2) + (0.031P)^2 + 0.4203P] where P = (Fo^2 + 2Fc^2)/3
S = 1.09	(Δ/σ)max = 0.001
4932 reflections	Δρmax = 0.47 e Å^−3
281 parameters	Δρmin = −0.34 e Å^−3
0 restraints	Extinction correction: SHELXL97 (Sheldrick, 2008), Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0195 (9)

Special details

Geometry. All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'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 > 2σ(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 (Ų)

	x	y	z	Uiso*/Ueq
Mo1	0.254204 (18)	0.476693 (17)	0.332147 (12)	0.03590 (7)
P1	0.39739 (5)	0.25947 (5)	0.21918 (3)	0.03246 (10)
F1	0.4014 (2)	0.43097 (17)	0.03742 (11)	0.0692 (4)
F2	0.49201 (17)	0.19509 (17)	0.01158 (10)	0.0622 (4)
F3	0.2010 (3)	0.2098 (4)	0.0455 (2)	0.1438 (12)
F4	0.1068 (2)	0.4355 (4)	0.08501 (17)	0.1575 (15)
F5	0.2209 (2)	0.3736 (3)	−0.06765 (13)	0.1063 (8)
O1	0.5722 (2)	0.4846 (3)	0.3758 (2)	0.0801 (6)
O2	0.2233 (3)	0.7230 (2)	0.14061 (17)	0.0901 (7)
O3	−0.0888 (2)	0.5152 (3)	0.3005 (2)	0.0855 (7)
O4	0.2859 (3)	0.2422 (2)	0.52800 (15)	0.0802 (6)
O5	0.0882 (2)	0.7350 (2)	0.48799 (16)	0.0713 (5)
O6	0.9262 (2)	0.0497 (3)	0.2174 (3)	0.1045 (9)
O7	0.3280 (3)	−0.1550 (2)	0.32874 (18)	0.0821 (7)
N1	0.59744 (18)	0.17449 (19)	0.20831 (14)	0.0418 (4)
N2	0.3552 (2)	0.11247 (19)	0.24618 (13)	0.0413 (4)
C1	0.4623 (3)	0.4778 (3)	0.35758 (19)	0.0509 (5)
C2	0.2361 (3)	0.6336 (3)	0.20750 (19)	0.0551 (5)
C3	0.0351 (3)	0.4972 (3)	0.31154 (19)	0.0528 (5)
C4	0.2738 (3)	0.3262 (3)	0.45779 (17)	0.0490 (5)
C5	0.1485 (3)	0.6434 (2)	0.43071 (18)	0.0484 (5)
C6	0.6950 (3)	0.2477 (3)	0.1497 (2)	0.0585 (6)
H6A	0.6978	0.3203	0.1919	0.070*
H6B	0.6515	0.2990	0.0850	0.070*
C7	0.8596 (3)	0.1271 (5)	0.1250 (3)	0.0908 (11)
H7A	0.8552	0.0567	0.0815	0.109*
H7B	0.9264	0.1719	0.0854	0.109*
C8	0.8312 (4)	−0.0174 (4)	0.2758 (4)	0.0927 (11)
H8A	0.8781	−0.0694	0.3394	0.111*
H8B	0.8280	−0.0905	0.2344	0.111*
C9	0.6657 (3)	0.0958 (3)	0.3057 (2)	0.0585 (6)
H9A	0.6026	0.0464	0.3443	0.070*
H9B	0.6669	0.1666	0.3503	0.070*
C10	0.4388 (3)	−0.0263 (3)	0.1910 (2)	0.0566 (6)
H10A	0.5382	−0.0302	0.1542	0.068*
H10B	0.3755	−0.0279	0.1392	0.068*
C11	0.4689 (4)	−0.1597 (3)	0.2690 (2)	0.0693 (7)
H11A	0.5192	−0.2501	0.2313	0.083*
H11B	0.5410	−0.1629	0.3161	0.083*
C12	0.2498 (4)	−0.0218 (3)	0.3834 (2)	0.0736 (8)
H12A	0.3175	−0.0207	0.4322	0.088*
H12B	0.1536	−0.0204	0.4239	0.088*
C13	0.2104 (3)	0.1152 (3)	0.30840 (19)	0.0523 (5)
H13A	0.1377	0.1179	0.2620	0.063*
H13B	0.1597	0.2041	0.3477	0.063*
C14	0.3803 (2)	0.3049 (3)	0.06994 (16)	0.0469 (5)
C15	0.2238 (3)	0.3330 (5)	0.0336 (2)	0.0785 (9)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Mo1	0.03805 (10)	0.03250 (10)	0.03475 (10)	−0.01420 (7)	0.00072 (6)	−0.00257 (6)
P1	0.0301 (2)	0.0345 (2)	0.0311 (2)	−0.01334 (17)	−0.00022 (16)	−0.00165 (16)
F1	0.0875 (11)	0.0625 (9)	0.0474 (8)	−0.0296 (8)	0.0006 (7)	0.0130 (6)
F2	0.0620 (8)	0.0718 (9)	0.0402 (7)	−0.0168 (7)	0.0052 (6)	−0.0168 (6)
F3	0.141 (2)	0.226 (3)	0.130 (2)	−0.132 (2)	−0.0737 (18)	0.039 (2)
F4	0.0485 (10)	0.277 (4)	0.0785 (14)	0.0149 (15)	−0.0199 (9)	−0.0674 (18)
F5	0.0891 (13)	0.156 (2)	0.0453 (9)	−0.0197 (13)	−0.0274 (9)	−0.0015 (10)
O1	0.0642 (12)	0.0917 (15)	0.1007 (16)	−0.0436 (12)	−0.0145 (11)	−0.0166 (12)
O2	0.132 (2)	0.0549 (11)	0.0625 (12)	−0.0287 (12)	0.0005 (12)	0.0152 (9)
O3	0.0449 (10)	0.1161 (18)	0.0919 (16)	−0.0299 (11)	−0.0036 (10)	−0.0146 (13)
O4	0.1179 (18)	0.0718 (13)	0.0523 (11)	−0.0453 (13)	−0.0163 (11)	0.0185 (9)
O5	0.0827 (13)	0.0557 (10)	0.0677 (12)	−0.0262 (9)	0.0214 (10)	−0.0257 (9)
O6	0.0350 (10)	0.1114 (19)	0.157 (3)	−0.0186 (11)	−0.0203 (13)	−0.0099 (18)
O7	0.1128 (17)	0.0522 (10)	0.0904 (15)	−0.0530 (11)	0.0287 (13)	−0.0188 (10)
N1	0.0297 (7)	0.0438 (9)	0.0474 (9)	−0.0132 (7)	−0.0018 (6)	0.0006 (7)
N2	0.0438 (9)	0.0406 (8)	0.0430 (9)	−0.0231 (7)	0.0065 (7)	−0.0095 (7)
C1	0.0542 (12)	0.0468 (11)	0.0549 (12)	−0.0240 (10)	−0.0026 (10)	−0.0086 (9)
C2	0.0666 (14)	0.0422 (11)	0.0469 (12)	−0.0178 (10)	0.0029 (10)	−0.0011 (9)
C3	0.0456 (12)	0.0563 (13)	0.0495 (12)	−0.0164 (10)	0.0019 (9)	−0.0079 (10)
C4	0.0592 (13)	0.0464 (11)	0.0416 (10)	−0.0235 (10)	−0.0025 (9)	−0.0026 (9)
C5	0.0508 (12)	0.0389 (10)	0.0495 (11)	−0.0164 (9)	0.0049 (9)	−0.0043 (8)
C6	0.0419 (11)	0.0694 (15)	0.0664 (15)	−0.0298 (11)	0.0027 (10)	−0.0002 (12)
C7	0.0403 (14)	0.120 (3)	0.110 (3)	−0.0359 (17)	0.0177 (16)	−0.026 (2)
C8	0.0534 (16)	0.0687 (19)	0.141 (3)	−0.0053 (14)	−0.0414 (19)	0.007 (2)
C9	0.0496 (12)	0.0558 (13)	0.0672 (15)	−0.0184 (11)	−0.0217 (11)	0.0105 (11)
C10	0.0687 (15)	0.0486 (12)	0.0558 (13)	−0.0301 (11)	0.0130 (11)	−0.0199 (10)
C11	0.0834 (19)	0.0447 (12)	0.0777 (18)	−0.0296 (13)	0.0110 (14)	−0.0121 (12)
C12	0.099 (2)	0.0568 (15)	0.0714 (17)	−0.0495 (15)	0.0309 (15)	−0.0167 (12)
C13	0.0505 (12)	0.0570 (13)	0.0596 (13)	−0.0349 (11)	0.0107 (10)	−0.0147 (10)
C14	0.0434 (10)	0.0547 (12)	0.0342 (9)	−0.0145 (9)	0.0002 (8)	−0.0028 (8)
C15	0.0545 (15)	0.130 (3)	0.0432 (13)	−0.0298 (17)	−0.0135 (11)	−0.0021 (15)

Geometric parameters (Å, º)

Mo1—C5	2.018 (2)	N1—C6	1.473 (3)
Mo1—C4	2.030 (2)	N2—C13	1.464 (2)
Mo1—C3	2.049 (2)	N2—C10	1.473 (3)
Mo1—C1	2.050 (2)	C6—C7	1.513 (4)
Mo1—C2	2.062 (2)	C6—H6A	0.97
Mo1—P1	2.5063 (5)	C6—H6B	0.97
P1—N2	1.6580 (16)	C7—H7A	0.97
P1—N1	1.6954 (16)	C7—H7B	0.97
P1—C14	1.933 (2)	C8—C9	1.504 (4)
F1—C14	1.358 (3)	C8—H8A	0.97
F2—C14	1.355 (2)	C8—H8B	0.97
F3—C15	1.320 (5)	C9—H9A	0.97
F4—C15	1.291 (4)	C9—H9B	0.97
F5—C15	1.315 (3)	C10—C11	1.507 (4)
O1—C1	1.133 (3)	C10—H10A	0.97
O2—C2	1.136 (3)	C10—H10B	0.97
O3—C3	1.136 (3)	C11—H11A	0.97
O4—C4	1.133 (3)	C11—H11B	0.97
O5—C5	1.137 (3)	C12—C13	1.504 (4)
O6—C7	1.409 (5)	C12—H12A	0.97
O6—C8	1.412 (4)	C12—H12B	0.97
O7—C11	1.414 (3)	C13—H13A	0.97
O7—C12	1.424 (3)	C13—H13B	0.97
N1—C9	1.472 (3)	C14—C15	1.521 (3)
C5—Mo1—C4	89.32 (9)	O6—C8—H8A	109.3
C5—Mo1—C3	88.66 (9)	C9—C8—H8A	109.1
C4—Mo1—C3	92.82 (10)	O6—C8—H8B	109.2
C5—Mo1—C1	85.93 (9)	C9—C8—H8B	109.3
C4—Mo1—C1	89.22 (10)	H8A—C8—H8B	107.9
C3—Mo1—C1	174.19 (9)	N1—C9—C8	108.2 (2)
C5—Mo1—C2	89.23 (9)	N1—C9—H9A	110.1
C4—Mo1—C2	178.12 (9)	C8—C9—H9A	110.1
C3—Mo1—C2	88.34 (10)	N1—C9—H9B	109.9
C1—Mo1—C2	89.49 (10)	C8—C9—H9B	110.1
C5—Mo1—P1	176.10 (7)	H9A—C9—H9B	108.4
C4—Mo1—P1	87.57 (6)	N2—C10—C11	109.9 (2)
C3—Mo1—P1	93.84 (7)	N2—C10—H10A	109.7
C1—Mo1—P1	91.68 (6)	C11—C10—H10A	109.9
C2—Mo1—P1	93.83 (7)	N2—C10—H10B	109.6
N2—P1—N1	100.58 (9)	C11—C10—H10B	109.6
N2—P1—C14	103.40 (10)	H10A—C10—H10B	108.2
N1—P1—C14	96.30 (9)	O7—C11—C10	112.0 (2)
N2—P1—Mo1	118.43 (6)	O7—C11—H11A	109.2
N1—P1—Mo1	118.99 (6)	C10—C11—H11A	109.1
C14—P1—Mo1	115.65 (7)	O7—C11—H11B	109.3
C7—O6—C8	110.3 (2)	C10—C11—H11B	109.1
C11—O7—C12	110.53 (19)	H11A—C11—H11B	107.9
C9—N1—C6	109.63 (18)	O7—C12—C13	111.5 (2)
C9—N1—P1	115.35 (14)	O7—C12—H12A	109.2
C6—N1—P1	121.80 (15)	C13—C12—H12A	109.2
C13—N2—C10	110.45 (16)	O7—C12—H12B	109.4
C13—N2—P1	124.36 (14)	C13—C12—H12B	109.5
C10—N2—P1	123.76 (14)	H12A—C12—H12B	108.0
O1—C1—Mo1	175.9 (2)	N2—C13—C12	109.6 (2)
O2—C2—Mo1	178.1 (2)	N2—C13—H13A	109.8
O3—C3—Mo1	177.0 (2)	C12—C13—H13A	109.7
O4—C4—Mo1	179.4 (2)	N2—C13—H13B	109.7
O5—C5—Mo1	178.4 (2)	C12—C13—H13B	109.7
N1—C6—C7	107.4 (2)	H13A—C13—H13B	108.2
N1—C6—H6A	110.3	F2—C14—F1	106.51 (17)
C7—C6—H6A	110.2	F2—C14—C15	105.5 (2)
N1—C6—H6B	110.2	F1—C14—C15	105.0 (2)
C7—C6—H6B	110.2	F2—C14—P1	112.20 (14)
H6A—C6—H6B	108.5	F1—C14—P1	110.13 (15)
O6—C7—C6	111.7 (3)	C15—C14—P1	116.73 (16)
O6—C7—H7A	109.1	F4—C15—F5	108.5 (3)
C6—C7—H7A	109.3	F4—C15—F3	108.9 (3)
O6—C7—H7B	109.4	F5—C15—F3	105.1 (3)
C6—C7—H7B	109.4	F4—C15—C14	111.3 (3)
H7A—C7—H7B	108.0	F5—C15—C14	111.7 (2)
O6—C8—C9	111.9 (3)	F3—C15—C14	111.1 (3)
C4—Mo1—P1—N2	39.38 (10)	C1—Mo1—C4—O4	−3 (25)
C3—Mo1—P1—N2	−53.28 (10)	C2—Mo1—C4—O4	−49 (26)
C1—Mo1—P1—N2	128.54 (10)	P1—Mo1—C4—O4	89 (25)
C2—Mo1—P1—N2	−141.87 (11)	C4—Mo1—C5—O5	−19 (9)
C5—Mo1—P1—N1	−46.1 (9)	C3—Mo1—C5—O5	74 (9)
C4—Mo1—P1—N1	−83.20 (10)	C1—Mo1—C5—O5	−108 (9)
C3—Mo1—P1—N1	−175.86 (10)	C2—Mo1—C5—O5	162 (9)
C1—Mo1—P1—N1	5.95 (10)	P1—Mo1—C5—O5	−56 (9)
C2—Mo1—P1—N1	95.55 (10)	C9—N1—C6—C7	59.3 (3)
C5—Mo1—P1—C14	−160.0 (9)	P1—N1—C6—C7	−161.5 (2)
C4—Mo1—P1—C14	162.90 (10)	C8—O6—C7—C6	59.3 (4)
C3—Mo1—P1—C14	70.23 (10)	N1—C6—C7—O6	−59.6 (3)
C1—Mo1—P1—C14	−107.95 (10)	C7—O6—C8—C9	−58.5 (4)
C2—Mo1—P1—C14	−18.35 (11)	C6—N1—C9—C8	−59.0 (3)
N2—P1—N1—C9	−64.74 (18)	P1—N1—C9—C8	159.0 (2)
C14—P1—N1—C9	−169.68 (17)	O6—C8—C9—N1	58.3 (4)
Mo1—P1—N1—C9	66.33 (17)	C13—N2—C10—C11	−55.0 (3)
N2—P1—N1—C6	158.26 (18)	P1—N2—C10—C11	138.2 (2)
C14—P1—N1—C6	53.3 (2)	C12—O7—C11—C10	−57.8 (3)
Mo1—P1—N1—C6	−70.66 (19)	N2—C10—C11—O7	56.0 (3)
N1—P1—N2—C13	151.03 (18)	C11—O7—C12—C13	58.8 (3)
C14—P1—N2—C13	−109.81 (19)	C10—N2—C13—C12	56.0 (3)
Mo1—P1—N2—C13	19.6 (2)	P1—N2—C13—C12	−137.23 (19)
N1—P1—N2—C10	−43.9 (2)	O7—C12—C13—N2	−58.0 (3)
C14—P1—N2—C10	55.2 (2)	N2—P1—C14—F2	−65.75 (17)
Mo1—P1—N2—C10	−175.37 (16)	N1—P1—C14—F2	36.74 (17)
C5—Mo1—C1—O1	4 (3)	Mo1—P1—C14—F2	163.17 (13)
C4—Mo1—C1—O1	−85 (3)	N2—P1—C14—F1	175.80 (14)
C3—Mo1—C1—O1	26 (4)	N1—P1—C14—F1	−81.72 (15)
C2—Mo1—C1—O1	94 (3)	Mo1—P1—C14—F1	44.71 (16)
P1—Mo1—C1—O1	−173 (3)	N2—P1—C14—C15	56.2 (2)
C5—Mo1—C2—O2	−13 (8)	N1—P1—C14—C15	158.7 (2)
C4—Mo1—C2—O2	−53 (10)	Mo1—P1—C14—C15	−74.9 (2)
C3—Mo1—C2—O2	76 (8)	F2—C14—C15—F4	179.3 (3)
C1—Mo1—C2—O2	−99 (8)	F1—C14—C15—F4	−68.4 (3)
P1—Mo1—C2—O2	169 (8)	P1—C14—C15—F4	53.9 (4)
C5—Mo1—C3—O3	35 (4)	F2—C14—C15—F5	−59.3 (4)
C4—Mo1—C3—O3	124 (4)	F1—C14—C15—F5	53.0 (3)
C1—Mo1—C3—O3	14 (5)	P1—C14—C15—F5	175.3 (2)
C2—Mo1—C3—O3	−54 (4)	F2—C14—C15—F3	57.7 (3)
P1—Mo1—C3—O3	−148 (4)	F1—C14—C15—F3	170.0 (2)
C5—Mo1—C4—O4	−89 (25)	P1—C14—C15—F3	−67.7 (3)
C3—Mo1—C4—O4	−177 (100)

Pentacarbonyl[(pentafluoroethyl)bis(piperidin-1-yl)phosphane-κP]molybdenum(0) (2a)

Crystal data

[Mo(C12H20F5N2P)(CO)5]	F(000) = 1112
Mr = 554.26	Dx = 1.643 Mg m^−3
Monoclinic, P21/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 100 reflections
a = 10.4472 (3) Å	θ = 10.1–26.3°
b = 15.8563 (6) Å	µ = 0.73 mm^−1
c = 14.0067 (6) Å	T = 295 K
β = 105.110 (3)°	Parallelepiped cut from larger block, colourless
V = 2240.05 (14) Å^3	0.58 × 0.42 × 0.40 mm
Z = 4

Data collection

Bruker P4 diffractometer	4324 reflections with I > 2σ(I)
Radiation source: normal-focus sealed tube	Rint = 0.027
Graphite monochromator	θmax = 27.5°, θmin = 2.0°
θ/2θ scans	h = −1→13
Absorption correction: integration (XSHELL; Bruker, 1999)	k = −20→1
Tmin = 0.744, Tmax = 0.774	l = −18→17
6372 measured reflections	3 standard reflections every 100 reflections
5120 independent reflections	intensity decay: 1.1%

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.028	H-atom parameters constrained
wR(F^2) = 0.072	w = 1/[σ^2(Fo^2) + (0.0276P)^2 + 0.7523P] where P = (Fo^2 + 2Fc^2)/3
S = 1.05	(Δ/σ)max = 0.001
5120 reflections	Δρmax = 0.27 e Å^−3
281 parameters	Δρmin = −0.38 e Å^−3
0 restraints	Extinction correction: SHELXL97 (Sheldrick, 2008), Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0122 (4)

Special details

Geometry. All s.u.'s (except the s.u.'s in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'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 > 2σ(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 (Ų)

	x	y	z	Uiso*/Ueq
Mo1	0.627795 (17)	0.186603 (12)	0.121533 (13)	0.03928 (7)
P1	0.59219 (5)	0.10762 (3)	0.26923 (4)	0.03384 (11)
F1	0.67228 (17)	−0.03824 (9)	0.37343 (11)	0.0646 (4)
F2	0.72419 (14)	−0.03160 (9)	0.23285 (11)	0.0555 (3)
F3	0.90586 (17)	0.09292 (14)	0.31104 (17)	0.0952 (6)
F4	0.86178 (18)	0.07793 (16)	0.45014 (14)	0.1002 (7)
F5	0.93360 (19)	−0.02587 (13)	0.38368 (16)	0.0946 (6)
O1	0.8253 (2)	0.05210 (15)	0.06894 (17)	0.0781 (6)
O2	0.6404 (3)	0.2894 (2)	−0.06732 (19)	0.1064 (10)
O3	0.3930 (2)	0.09352 (15)	−0.03070 (14)	0.0725 (6)
O4	0.4227 (2)	0.32204 (13)	0.15979 (19)	0.0785 (6)
O5	0.8894 (2)	0.28279 (14)	0.23930 (16)	0.0742 (6)
N1	0.44739 (17)	0.05461 (11)	0.25583 (13)	0.0407 (4)
N2	0.60008 (18)	0.15990 (12)	0.37300 (13)	0.0418 (4)
C1	0.7549 (2)	0.09839 (17)	0.08988 (18)	0.0519 (5)
C2	0.6380 (3)	0.2523 (2)	0.0011 (2)	0.0642 (7)
C3	0.4749 (2)	0.12454 (15)	0.02803 (17)	0.0480 (5)
C4	0.4978 (2)	0.27448 (15)	0.14772 (19)	0.0511 (5)
C5	0.7946 (3)	0.24952 (15)	0.20067 (19)	0.0507 (5)
C6	0.7122 (2)	0.01533 (14)	0.31138 (16)	0.0447 (5)
C7	0.8561 (3)	0.04111 (19)	0.3652 (2)	0.0609 (7)
C8	0.3305 (2)	0.11055 (15)	0.2331 (2)	0.0498 (5)
H8A	0.3077	0.1252	0.1635	0.060*
H8B	0.3515	0.1622	0.2711	0.060*
C9	0.2133 (3)	0.06811 (19)	0.2575 (2)	0.0646 (7)
H9A	0.1369	0.1052	0.2402	0.078*
H9B	0.2336	0.0571	0.3280	0.078*
C10	0.1811 (3)	−0.0144 (2)	0.2009 (2)	0.0693 (8)
H10A	0.1112	−0.0435	0.2217	0.083*
H10B	0.1495	−0.0028	0.1307	0.083*
C11	0.3023 (3)	−0.06952 (17)	0.2196 (2)	0.0659 (7)
H11A	0.2822	−0.1196	0.1787	0.079*
H11B	0.3264	−0.0872	0.2882	0.079*
C12	0.4192 (2)	−0.02368 (15)	0.19698 (18)	0.0498 (5)
H12A	0.4967	−0.0599	0.2127	0.060*
H12B	0.3987	−0.0102	0.1271	0.060*
C13	0.5724 (3)	0.12005 (17)	0.46079 (18)	0.0562 (6)
H13A	0.6554	0.1092	0.5097	0.067*
H13B	0.5284	0.0664	0.4420	0.067*
C14	0.4860 (3)	0.1755 (2)	0.5054 (2)	0.0707 (8)
H14A	0.4742	0.1493	0.5650	0.085*
H14B	0.3994	0.1811	0.4591	0.085*
C15	0.5465 (3)	0.2620 (2)	0.5300 (2)	0.0750 (9)
H15A	0.6281	0.2574	0.5822	0.090*
H15B	0.4858	0.2978	0.5535	0.090*
C16	0.5751 (3)	0.30102 (18)	0.4386 (2)	0.0684 (8)
H16A	0.4922	0.3116	0.3895	0.082*
H16B	0.6198	0.3546	0.4560	0.082*
C17	0.6609 (2)	0.24344 (15)	0.39500 (18)	0.0493 (5)
H17A	0.6731	0.2683	0.3347	0.059*
H17B	0.7474	0.2377	0.4414	0.059*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Mo1	0.03713 (10)	0.04104 (11)	0.03945 (11)	−0.00276 (7)	0.00958 (7)	0.00438 (7)
P1	0.0317 (2)	0.0325 (2)	0.0362 (2)	−0.00124 (19)	0.00681 (19)	−0.00008 (19)
F1	0.0778 (10)	0.0517 (8)	0.0638 (9)	0.0077 (7)	0.0176 (8)	0.0208 (7)
F2	0.0573 (8)	0.0464 (7)	0.0599 (8)	0.0084 (6)	0.0102 (7)	−0.0094 (6)
F3	0.0443 (9)	0.1108 (15)	0.1160 (16)	−0.0136 (10)	−0.0051 (9)	0.0253 (13)
F4	0.0655 (11)	0.1353 (18)	0.0780 (12)	0.0265 (12)	−0.0203 (9)	−0.0426 (12)
F5	0.0674 (11)	0.0856 (13)	0.1098 (15)	0.0391 (10)	−0.0143 (10)	−0.0043 (11)
O1	0.0715 (13)	0.0824 (14)	0.0911 (15)	0.0097 (12)	0.0402 (12)	−0.0134 (12)
O2	0.0867 (17)	0.148 (2)	0.0845 (16)	−0.0076 (17)	0.0219 (13)	0.0653 (17)
O3	0.0624 (12)	0.0897 (15)	0.0567 (11)	−0.0136 (11)	−0.0001 (9)	−0.0168 (10)
O4	0.0752 (14)	0.0584 (12)	0.1050 (17)	0.0189 (11)	0.0287 (13)	0.0037 (11)
O5	0.0592 (12)	0.0701 (12)	0.0880 (15)	−0.0258 (10)	0.0097 (11)	−0.0059 (11)
N1	0.0357 (8)	0.0379 (9)	0.0485 (10)	−0.0049 (7)	0.0108 (7)	−0.0021 (8)
N2	0.0469 (10)	0.0395 (9)	0.0398 (9)	−0.0058 (8)	0.0127 (8)	−0.0034 (7)
C1	0.0491 (13)	0.0573 (14)	0.0512 (13)	−0.0061 (11)	0.0166 (10)	−0.0032 (11)
C2	0.0533 (15)	0.0785 (18)	0.0608 (16)	−0.0053 (13)	0.0150 (12)	0.0223 (14)
C3	0.0471 (12)	0.0544 (13)	0.0432 (11)	0.0017 (10)	0.0127 (10)	0.0009 (10)
C4	0.0498 (13)	0.0434 (12)	0.0586 (14)	−0.0008 (11)	0.0115 (11)	0.0058 (11)
C5	0.0509 (13)	0.0446 (12)	0.0569 (14)	−0.0051 (10)	0.0149 (11)	0.0021 (10)
C6	0.0471 (12)	0.0388 (11)	0.0455 (11)	0.0042 (9)	0.0071 (9)	0.0020 (9)
C7	0.0472 (14)	0.0633 (16)	0.0615 (15)	0.0175 (12)	−0.0051 (12)	−0.0031 (13)
C8	0.0362 (11)	0.0497 (13)	0.0641 (14)	−0.0023 (10)	0.0141 (10)	−0.0029 (11)
C9	0.0436 (13)	0.0780 (19)	0.0781 (18)	−0.0105 (13)	0.0263 (13)	−0.0063 (15)
C10	0.0485 (14)	0.0770 (19)	0.0841 (19)	−0.0246 (14)	0.0201 (13)	−0.0043 (16)
C11	0.0662 (17)	0.0522 (15)	0.0769 (18)	−0.0257 (13)	0.0142 (14)	−0.0013 (13)
C12	0.0473 (12)	0.0424 (12)	0.0577 (13)	−0.0088 (10)	0.0100 (10)	−0.0092 (10)
C13	0.0683 (16)	0.0588 (14)	0.0450 (12)	−0.0069 (13)	0.0208 (11)	−0.0001 (11)
C14	0.0682 (17)	0.092 (2)	0.0619 (16)	−0.0103 (16)	0.0349 (14)	−0.0097 (15)
C15	0.080 (2)	0.080 (2)	0.0759 (19)	0.0034 (17)	0.0388 (16)	−0.0263 (16)
C16	0.0733 (18)	0.0535 (15)	0.082 (2)	0.0025 (13)	0.0271 (16)	−0.0188 (14)
C17	0.0475 (12)	0.0488 (12)	0.0515 (12)	−0.0094 (10)	0.0129 (10)	−0.0136 (10)

Geometric parameters (Å, º)

Mo1—C2	2.009 (3)	C8—H8B	0.97
Mo1—C3	2.036 (2)	C9—C10	1.521 (4)
Mo1—C4	2.045 (3)	C9—H9A	0.97
Mo1—C1	2.055 (3)	C9—H9B	0.97
Mo1—C5	2.062 (3)	C10—C11	1.505 (4)
Mo1—P1	2.5274 (5)	C10—H10A	0.97
P1—N2	1.6566 (18)	C10—H10B	0.97
P1—N1	1.6977 (17)	C11—C12	1.523 (3)
P1—C6	1.917 (2)	C11—H11A	0.97
F1—C6	1.356 (3)	C11—H11B	0.97
F2—C6	1.361 (3)	C12—H12A	0.97
F3—C7	1.314 (3)	C12—H12B	0.97
F4—C7	1.312 (3)	C13—C14	1.507 (4)
F5—C7	1.320 (3)	C13—H13A	0.97
O1—C1	1.130 (3)	C13—H13B	0.97
O2—C2	1.131 (3)	C14—C15	1.512 (4)
O3—C3	1.133 (3)	C14—H14A	0.97
O4—C4	1.132 (3)	C14—H14B	0.97
O5—C5	1.128 (3)	C15—C16	1.521 (4)
N1—C8	1.475 (3)	C15—H15A	0.97
N1—C12	1.477 (3)	C15—H15B	0.97
N2—C17	1.467 (3)	C16—C17	1.515 (3)
N2—C13	1.476 (3)	C16—H16A	0.97
C6—C7	1.551 (3)	C16—H16B	0.97
C8—C9	1.511 (3)	C17—H17A	0.97
C8—H8A	0.97	C17—H17B	0.97
C2—Mo1—C3	85.12 (11)	C10—C9—H9A	109.6
C2—Mo1—C4	88.89 (11)	C8—C9—H9B	109.6
C3—Mo1—C4	89.91 (10)	C10—C9—H9B	109.6
C2—Mo1—C1	89.59 (11)	H9A—C9—H9B	108.1
C3—Mo1—C1	88.56 (10)	C11—C10—C9	110.3 (2)
C4—Mo1—C1	177.93 (10)	C11—C10—H10A	109.6
C2—Mo1—C5	88.74 (11)	C9—C10—H10A	109.6
C3—Mo1—C5	172.27 (9)	C11—C10—H10B	109.6
C4—Mo1—C5	94.68 (10)	C9—C10—H10B	109.6
C1—Mo1—C5	86.68 (10)	H10A—C10—H10B	108.1
C2—Mo1—P1	174.64 (8)	C10—C11—C12	111.7 (2)
C3—Mo1—P1	91.66 (7)	C10—C11—H11A	109.3
C4—Mo1—P1	86.82 (7)	C12—C11—H11A	109.3
C1—Mo1—P1	94.62 (7)	C10—C11—H11B	109.2
C5—Mo1—P1	94.81 (7)	C12—C11—H11B	109.2
N2—P1—N1	100.59 (9)	H11A—C11—H11B	107.9
N2—P1—C6	103.46 (10)	N1—C12—C11	109.8 (2)
N1—P1—C6	98.54 (9)	N1—C12—H12A	109.7
N2—P1—Mo1	119.07 (7)	C11—C12—H12A	109.7
N1—P1—Mo1	118.16 (7)	N1—C12—H12B	109.7
C6—P1—Mo1	113.97 (7)	C11—C12—H12B	109.7
C8—N1—C12	110.58 (18)	H12A—C12—H12B	108.2
C8—N1—P1	112.95 (14)	N2—C13—C14	111.3 (2)
C12—N1—P1	121.35 (15)	N2—C13—H13A	109.4
C17—N2—C13	112.31 (18)	C14—C13—H13A	109.4
C17—N2—P1	123.78 (15)	N2—C13—H13B	109.4
C13—N2—P1	122.73 (16)	C14—C13—H13B	109.3
O1—C1—Mo1	176.9 (2)	H13A—C13—H13B	108.0
O2—C2—Mo1	178.2 (3)	C13—C14—C15	111.4 (2)
O3—C3—Mo1	173.9 (2)	C13—C14—H14A	109.4
O4—C4—Mo1	177.8 (2)	C15—C14—H14A	109.3
O5—C5—Mo1	175.7 (2)	C13—C14—H14B	109.4
F1—C6—F2	106.50 (18)	C15—C14—H14B	109.4
F1—C6—C7	105.9 (2)	H14A—C14—H14B	108.0
F2—C6—C7	104.82 (19)	C14—C15—C16	109.8 (2)
F1—C6—P1	112.92 (15)	C14—C15—H15A	109.7
F2—C6—P1	111.04 (14)	C16—C15—H15A	109.7
C7—C6—P1	114.95 (16)	C14—C15—H15B	109.7
F4—C7—F3	108.3 (3)	C16—C15—H15B	109.7
F4—C7—F5	107.5 (2)	H15A—C15—H15B	108.2
F3—C7—F5	107.5 (2)	C17—C16—C15	111.2 (2)
F4—C7—C6	111.5 (2)	C17—C16—H16A	109.4
F3—C7—C6	111.3 (2)	C15—C16—H16A	109.4
F5—C7—C6	110.5 (2)	C17—C16—H16B	109.4
N1—C8—C9	110.9 (2)	C15—C16—H16B	109.4
N1—C8—H8A	109.4	H16A—C16—H16B	108.0
C9—C8—H8A	109.4	N2—C17—C16	111.1 (2)
N1—C8—H8B	109.5	N2—C17—H17A	109.4
C9—C8—H8B	109.5	C16—C17—H17A	109.4
H8A—C8—H8B	108.1	N2—C17—H17B	109.5
C8—C9—C10	110.4 (2)	C16—C17—H17B	109.5
C8—C9—H9A	109.6	H17A—C17—H17B	108.0
C3—Mo1—P1—N2	−137.45 (10)	Mo1—P1—C6—F2	−45.21 (17)
C4—Mo1—P1—N2	−47.64 (11)	N2—P1—C6—C7	−57.24 (19)
C1—Mo1—P1—N2	133.85 (10)	N1—P1—C6—C7	−160.37 (18)
C5—Mo1—P1—N2	46.80 (11)	Mo1—P1—C6—C7	73.54 (18)
C3—Mo1—P1—N1	−15.04 (10)	F1—C6—C7—F4	−59.5 (3)
C4—Mo1—P1—N1	74.78 (10)	F2—C6—C7—F4	−171.9 (2)
C1—Mo1—P1—N1	−103.73 (10)	P1—C6—C7—F4	65.9 (3)
C5—Mo1—P1—N1	169.22 (10)	F1—C6—C7—F3	179.4 (2)
C3—Mo1—P1—C6	99.95 (10)	F2—C6—C7—F3	67.0 (3)
C4—Mo1—P1—C6	−170.24 (10)	P1—C6—C7—F3	−55.2 (3)
C1—Mo1—P1—C6	11.26 (10)	F1—C6—C7—F5	60.0 (3)
C5—Mo1—P1—C6	−75.80 (11)	F2—C6—C7—F5	−52.4 (3)
N2—P1—N1—C8	68.32 (17)	P1—C6—C7—F5	−174.6 (2)
C6—P1—N1—C8	173.84 (16)	C12—N1—C8—C9	60.6 (3)
Mo1—P1—N1—C8	−63.03 (17)	P1—N1—C8—C9	−159.72 (18)
N2—P1—N1—C12	−156.86 (17)	N1—C8—C9—C10	−57.5 (3)
C6—P1—N1—C12	−51.33 (18)	C8—C9—C10—C11	54.0 (3)
Mo1—P1—N1—C12	71.79 (18)	C9—C10—C11—C12	−54.1 (3)
N1—P1—N2—C17	−148.01 (18)	C8—N1—C12—C11	−59.2 (3)
C6—P1—N2—C17	110.45 (19)	P1—N1—C12—C11	165.03 (18)
Mo1—P1—N2—C17	−17.2 (2)	C10—C11—C12—N1	56.6 (3)
N1—P1—N2—C13	45.3 (2)	C17—N2—C13—C14	56.3 (3)
C6—P1—N2—C13	−56.2 (2)	P1—N2—C13—C14	−135.7 (2)
Mo1—P1—N2—C13	176.11 (16)	N2—C13—C14—C15	−55.5 (3)
N2—P1—C6—F1	64.46 (17)	C13—C14—C15—C16	54.8 (4)
N1—P1—C6—F1	−38.67 (17)	C14—C15—C16—C17	−54.8 (3)
Mo1—P1—C6—F1	−164.76 (13)	C13—N2—C17—C16	−56.3 (3)
N2—P1—C6—F2	−176.00 (15)	P1—N2—C17—C16	135.8 (2)
N1—P1—C6—F2	80.88 (16)	C15—C16—C17—N2	55.7 (3)