Bis­(tri­phenyl­phosphine)­iminium tri­carbonyl­cyclo­penta­dienyl­molybdate

Evans, C.; Nicholson, B.K.; Oliver, A.G.

doi:10.1107/S1600536801016178

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Bis(triphenylphosphine)iminium tricarbonylcyclopentadienylmolybdate

C. Evans, B. K. Nicholson and A. G. Oliver

The crystal structure of bis(triphenylphosphine)iminium cyclopentadienyltricarbonylmolybdate, [PPN][Mo(CO)₃(η⁵-C₅H₅)] (PPN⁺ = [(PPh₃)₂N]⁺, C₃₆H₃₀NP₂), is reported. The anion is configured in the `piano-stool' arrangement while the cation adopts a bent configuration about the P—N—P bond. An `expanded-phenyl-embrace' supramolecular motif is noted in the packing of the PPN⁺ cation.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536801016178/tk6037sup1.cif Contains datablocks I, global
	Structure factor file (CIF format) https://doi.org/10.1107/S1600536801016178/tk6037Isup2.hkl Contains datablock I

CCDC reference: 175971

checkCIF report

Key indicators

Single-crystal X-ray study
T = 203 K
Mean (C-C) = 0.004 Å
R factor = 0.037
wR factor = 0.090
Data-to-parameter ratio = 17.8

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


 Alert Level C:



WEIGH_01  Alert C Extra text has been found in the
          _refine_ls_weighting_scheme field. This should be in the
          _refine_ls_weighting_details field.
          Weighting scheme given as calc w=1/[\s^2^(Fo^2^)+(0.0305P)^2^+3.4046P
          Weighting scheme identified as calc

PLAT_213  Alert C Atom  C6     has ADP max/min Ratio ...........       3.30

PLAT_213  Alert C Atom  C7     has ADP max/min Ratio ...........       3.70

General Notes



HYDTR_01  Extra text has been found in the _refine_ls_hydrogen_treatment field.
          Explanatory text should be in the _publ_section_refinement field.
          Hydrogen treatment given as riding with tied Uiso
          Hydrogen treatment identified as  riding


 0 Alert Level A = Potentially serious problem

 0 Alert Level B = Potential problem

 3 Alert Level C = Please check

Comment top

Though a commonly used metal carbonyl reagent, the structure of [PPN][Mo(CO)₃(η⁵-C₅H₅)] (I) has not been previously reported.

The anion adopts the classic piano stool type arrangement common for CpML₃ systems. The average Mo—C_CO bond length [1.930 (3) Å] is slightly larger than that reported for the tetrabutyl ammonium salt [1.909 (9) Å] while the average C_CO—Mo—C_CO angle [87 (2)°] and Mo—C_Cp distance [2.37 (2) Å] are similar to those reported] 88.1 (3)° and 2.37 (1) Å respectively; Crotty et al., 1977]. The PPN⁺ cation adopts the typical bent configuration about the P—N—P bond [142.62 (14)°].

A characteristic of triphenyl phosphine related systems is the observance of `phenyl embraces' as a crystal packing motif (Dance & Scudder, 1998). These embraces involve intermolecular phenyl attractions (both edge-face and offset face-face attractions) forming extended networks through the crystal lattice. This type of packing motif is noted in the structure of [PPN][Mo(CO)₃(η⁵-C₅H₅]. The non-bonded P—P distance of 6.8606 (8) Å and N—P—P angle of 72.41 (7)° are characteristic of an `expanded phenyl embrace' crystal packing motif in a compound containing PPN⁺ (Lewis & Dance, 2000).

Experimental top

[Mo(CO)₃(η⁵-C₅H₅)]₂ (0.2 g, 0.41 mmol) was reduced in tetrahydrofuran (20 ml) over a 1% Na/Hg amalgam for 2–3 h. A dichloromethane solution (5 ml) of [PPN]Cl (0.47 g, 0.82 mmol) was added and the reaction mixture stirred for an additional 30 minutes. The pale yellow/orange solution was transferred by syringe and solvent removed under vacuum. Recrystallization from addition of diethyl ether to a dichloromethane solution of the title compound produced a pale yellow powder. Crystals suitable for crystallographic analysis were obtained by liquid–liquid diffusion under a nitrogen atmosphere of diethyl ether and light petroleum spirits into a dichloromethane solution of the compound.

Computing details top

Data collection: SMART (Siemens, 1994); cell refinement: SAINT (Siemens, 1994); data reduction: SADABS (Blessing, 1995); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).

Figures top

Fig. 1. Structure of [PPN][Mo(CO)₃(η⁵-C₅H₅)] showing the atom-labelling scheme. The diagram was drawn at the 50% probability level (Farrugia, 1997)

(I) top

Crystal data top

C₃₆H₃₀NP₂·C₈H₅MoO₃	F(000) = 1608
M_r = 783.61	D_x = 1.401 Mg m⁻³
Monoclinic, P2₁/c	Mo Kα radiation, λ = 0.71073 Å
a = 14.0385 (2) Å	Cell parameters from 7126 reflections
b = 19.1269 (2) Å	θ = 1.5–27.5°
c = 13.8322 (1) Å	µ = 0.48 mm⁻¹
β = 90.728 (1)°	T = 203 K
V = 3713.83 (7) Å³	Prism, yellow
Z = 4	0.26 × 0.24 × 0.20 mm

Data collection top

Siemens SMART CCD diffractometer	8177 independent reflections
Radiation source: fine-focus sealed tube	6724 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.025
multiscan	θ_max = 27.5°, θ_min = 1.5°
Absorption correction: empirical (using intensity measurements) (Blessing, 1995)	h = −18→18
T_min = 0.885, T_max = 0.910	k = 0→24
22556 measured reflections	l = 0→17

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)] = 0.037	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.090	Riding with tied Uiso
S = 1.08	Calculated w = 1/[σ²(F_o²) + (0.0305P)² + 3.4046P] where P = (F_o² + 2F_c²)/3
8177 reflections	(Δ/σ)_max = 0.001
460 parameters	Δρ_max = 0.52 e Å⁻³
0 restraints	Δρ_min = −0.40 e Å⁻³

Crystal data top

C₃₆H₃₀NP₂·C₈H₅MoO₃	V = 3713.83 (7) Å³
M_r = 783.61	Z = 4
Monoclinic, P2₁/c	Mo Kα radiation
a = 14.0385 (2) Å	µ = 0.48 mm⁻¹
b = 19.1269 (2) Å	T = 203 K
c = 13.8322 (1) Å	0.26 × 0.24 × 0.20 mm
β = 90.728 (1)°

Data collection top

Siemens SMART CCD diffractometer	8177 independent reflections
Absorption correction: empirical (using intensity measurements) (Blessing, 1995)	6724 reflections with I > 2σ(I)
T_min = 0.885, T_max = 0.910	R_int = 0.025
22556 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.037	0 restraints
wR(F²) = 0.090	Riding with tied Uiso
S = 1.08	Δρ_max = 0.52 e Å⁻³
8177 reflections	Δρ_min = −0.40 e Å⁻³
460 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
Mo1	0.782761 (15)	0.133599 (12)	0.965022 (16)	0.03376 (7)
C1	0.7895 (2)	0.19985 (16)	0.8601 (2)	0.0450 (7)
C2	0.7354 (2)	0.07031 (15)	0.8672 (2)	0.0422 (6)
C3	0.65293 (18)	0.16285 (13)	0.98661 (17)	0.0335 (5)
C4	0.8258 (2)	0.1278 (2)	1.1316 (2)	0.0629 (10)
H4	0.7805	0.1392	1.1786	0.075*
C5	0.8875 (3)	0.17303 (19)	1.0911 (3)	0.0650 (10)
H5	0.8931	0.2210	1.1051	0.078*
C6	0.9412 (3)	0.1359 (4)	1.0253 (3)	0.117 (2)
H6	0.9898	0.1538	0.9863	0.140*
C7	0.9091 (5)	0.0665 (4)	1.0280 (5)	0.134 (3)
H7	0.9320	0.0292	0.9908	0.161*
C8	0.8396 (4)	0.0633 (2)	1.0935 (4)	0.102 (2)
H8	0.8058	0.0228	1.1103	0.122*
O1	0.79513 (18)	0.23972 (13)	0.79578 (17)	0.0672 (7)
O2	0.70750 (17)	0.03169 (13)	0.80714 (17)	0.0666 (7)
O3	0.57456 (14)	0.17952 (12)	1.00384 (14)	0.0494 (5)
P2	0.29551 (4)	0.16911 (3)	0.44339 (4)	0.02470 (12)
P1	0.28894 (4)	0.05693 (3)	0.59437 (4)	0.02641 (13)
N1	0.32740 (14)	0.11646 (10)	0.52611 (15)	0.0320 (4)
C11	0.37105 (17)	0.04858 (12)	0.69445 (16)	0.0295 (5)
C12	0.3777 (2)	−0.01346 (14)	0.7472 (2)	0.0437 (6)
H12	0.3422	−0.0528	0.7278	0.052*
C13	0.4365 (2)	−0.01702 (16)	0.8284 (2)	0.0494 (7)
H13	0.4400	−0.0585	0.8648	0.059*
C14	0.4899 (2)	0.04035 (16)	0.8557 (2)	0.0444 (7)
H14	0.5298	0.0378	0.9106	0.053*
C15	0.48520 (19)	0.10140 (16)	0.80301 (19)	0.0424 (6)
H15	0.5225	0.1400	0.8217	0.051*
C16	0.42564 (18)	0.10594 (14)	0.72260 (18)	0.0354 (5)
H16	0.4221	0.1478	0.6871	0.043*
C21	0.17307 (17)	0.07617 (12)	0.64383 (18)	0.0323 (5)
C22	0.09211 (18)	0.07193 (14)	0.5848 (2)	0.0398 (6)
H22	0.0962	0.0532	0.5222	0.048*
C23	0.0050 (2)	0.09559 (17)	0.6191 (3)	0.0559 (8)
H23	−0.0496	0.0930	0.5793	0.067*
C24	−0.0018 (2)	0.12274 (17)	0.7111 (3)	0.0660 (10)
H24	−0.0607	0.1391	0.7334	0.079*
C25	0.0777 (3)	0.12594 (17)	0.7702 (3)	0.0642 (10)
H25	0.0727	0.1437	0.8333	0.077*
C26	0.1653 (2)	0.10300 (16)	0.7370 (2)	0.0466 (7)
H26	0.2195	0.1056	0.7775	0.056*
C31	0.28148 (17)	−0.02674 (12)	0.53423 (17)	0.0294 (5)
C32	0.21688 (18)	−0.07789 (13)	0.56304 (19)	0.0355 (5)
H32	0.1752	−0.0692	0.6143	0.043*
C33	0.2147 (2)	−0.14178 (14)	0.5152 (2)	0.0438 (7)
H33	0.1715	−0.1764	0.5348	0.053*
C34	0.2748 (2)	−0.15502 (15)	0.4398 (2)	0.0476 (7)
H34	0.2724	−0.1984	0.4078	0.057*
C35	0.3389 (2)	−0.10431 (16)	0.4111 (2)	0.0494 (7)
H35	0.3797	−0.1132	0.3591	0.059*
C36	0.34329 (19)	−0.04028 (14)	0.45873 (19)	0.0396 (6)
H36	0.3878	−0.0063	0.4400	0.047*
C41	0.26851 (17)	0.25448 (12)	0.49123 (17)	0.0282 (5)
C42	0.19943 (18)	0.26024 (13)	0.56327 (18)	0.0340 (5)
H42	0.1705	0.2198	0.5880	0.041*
C43	0.17386 (19)	0.32511 (14)	0.59789 (19)	0.0396 (6)
H43	0.1268	0.3288	0.6454	0.048*
C44	0.2170 (2)	0.38459 (14)	0.5632 (2)	0.0446 (7)
H44	0.1990	0.4287	0.5867	0.054*
C45	0.2864 (2)	0.37958 (14)	0.4941 (2)	0.0478 (7)
H45	0.3166	0.4202	0.4717	0.057*
C46	0.31212 (19)	0.31436 (13)	0.45693 (19)	0.0376 (6)
H46	0.3587	0.3112	0.4090	0.045*
C51	0.19083 (16)	0.14147 (12)	0.37544 (16)	0.0278 (5)
C52	0.10658 (17)	0.18037 (14)	0.37214 (18)	0.0357 (6)
H52	0.1043	0.2246	0.4016	0.043*
C53	0.02607 (18)	0.15379 (17)	0.3254 (2)	0.0439 (7)
H53	−0.0305	0.1801	0.3232	0.053*
C54	0.02929 (19)	0.08857 (16)	0.28221 (19)	0.0425 (7)
H54	−0.0255	0.0702	0.2517	0.051*
C55	0.11263 (19)	0.05044 (14)	0.28380 (18)	0.0373 (6)
H55	0.1145	0.0064	0.2537	0.045*
C56	0.19384 (17)	0.07649 (13)	0.32945 (17)	0.0314 (5)
H56	0.2507	0.0505	0.3294	0.038*
C61	0.39327 (16)	0.17898 (12)	0.36196 (16)	0.0265 (5)
C62	0.37850 (18)	0.19020 (14)	0.26333 (18)	0.0357 (6)
H62	0.3163	0.1901	0.2373	0.043*
C63	0.45566 (19)	0.20152 (16)	0.20361 (19)	0.0423 (6)
H63	0.4458	0.2082	0.1369	0.051*
C64	0.54692 (18)	0.20298 (14)	0.2421 (2)	0.0392 (6)
H64	0.5990	0.2112	0.2016	0.047*
C65	0.56193 (18)	0.19243 (15)	0.3400 (2)	0.0400 (6)
H65	0.6242	0.1939	0.3658	0.048*
C66	0.48586 (17)	0.17977 (14)	0.40010 (18)	0.0354 (5)
H66	0.4964	0.1717	0.4664	0.043*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Mo1	0.03072 (12)	0.03717 (13)	0.03335 (12)	0.00392 (9)	−0.00132 (8)	−0.00387 (9)
C1	0.0385 (15)	0.0515 (17)	0.0451 (16)	0.0022 (12)	0.0071 (12)	−0.0039 (13)
C2	0.0413 (15)	0.0457 (16)	0.0394 (15)	0.0158 (12)	−0.0019 (12)	−0.0079 (12)
C3	0.0393 (14)	0.0381 (14)	0.0231 (11)	0.0029 (11)	−0.0013 (10)	−0.0024 (10)
C4	0.0473 (18)	0.098 (3)	0.0433 (18)	0.0086 (18)	−0.0113 (14)	0.0099 (18)
C5	0.076 (2)	0.055 (2)	0.063 (2)	−0.0076 (18)	−0.035 (2)	0.0002 (17)
C6	0.0278 (18)	0.268 (8)	0.054 (2)	−0.017 (3)	−0.0077 (16)	0.003 (4)
C7	0.113 (4)	0.169 (6)	0.119 (4)	0.112 (5)	−0.083 (4)	−0.096 (4)
C8	0.131 (4)	0.046 (2)	0.127 (4)	−0.012 (2)	−0.091 (4)	0.026 (3)
O1	0.0780 (17)	0.0685 (16)	0.0557 (14)	−0.0004 (13)	0.0196 (12)	0.0174 (12)
O2	0.0682 (15)	0.0683 (15)	0.0630 (15)	0.0188 (12)	−0.0135 (12)	−0.0334 (12)
O3	0.0406 (11)	0.0682 (14)	0.0396 (11)	0.0130 (10)	0.0073 (9)	−0.0011 (10)
P2	0.0246 (3)	0.0256 (3)	0.0239 (3)	−0.0002 (2)	0.0009 (2)	0.0005 (2)
P1	0.0275 (3)	0.0261 (3)	0.0256 (3)	−0.0017 (2)	0.0009 (2)	0.0019 (2)
N1	0.0324 (11)	0.0328 (11)	0.0308 (11)	−0.0036 (8)	−0.0020 (8)	0.0078 (8)
C11	0.0314 (12)	0.0318 (12)	0.0253 (11)	0.0001 (9)	−0.0010 (9)	0.0010 (9)
C12	0.0571 (17)	0.0337 (14)	0.0399 (15)	−0.0059 (12)	−0.0106 (13)	0.0042 (11)
C13	0.067 (2)	0.0419 (16)	0.0393 (15)	0.0027 (14)	−0.0131 (14)	0.0103 (12)
C14	0.0434 (15)	0.0567 (18)	0.0329 (14)	0.0037 (13)	−0.0097 (11)	0.0019 (12)
C15	0.0404 (14)	0.0496 (16)	0.0373 (14)	−0.0094 (12)	−0.0035 (12)	−0.0046 (12)
C16	0.0395 (14)	0.0341 (13)	0.0327 (13)	−0.0046 (11)	−0.0015 (11)	0.0030 (10)
C21	0.0317 (12)	0.0274 (12)	0.0378 (13)	−0.0014 (10)	0.0075 (10)	0.0022 (10)
C22	0.0336 (13)	0.0385 (14)	0.0473 (15)	−0.0013 (11)	0.0034 (11)	0.0078 (12)
C23	0.0306 (14)	0.0525 (19)	0.085 (2)	0.0031 (13)	0.0068 (15)	0.0162 (17)
C24	0.0464 (19)	0.0482 (19)	0.104 (3)	0.0050 (14)	0.038 (2)	−0.0008 (18)
C25	0.068 (2)	0.054 (2)	0.071 (2)	−0.0030 (17)	0.0338 (19)	−0.0180 (17)
C26	0.0476 (16)	0.0493 (17)	0.0433 (16)	−0.0065 (13)	0.0122 (13)	−0.0074 (13)
C31	0.0320 (12)	0.0287 (12)	0.0275 (11)	0.0025 (9)	−0.0024 (9)	0.0007 (9)
C32	0.0357 (13)	0.0328 (13)	0.0380 (14)	−0.0024 (10)	0.0003 (11)	0.0000 (10)
C33	0.0446 (16)	0.0316 (14)	0.0550 (18)	−0.0032 (11)	−0.0104 (13)	−0.0018 (12)
C34	0.0581 (18)	0.0344 (14)	0.0499 (17)	0.0093 (13)	−0.0101 (14)	−0.0117 (12)
C35	0.0590 (18)	0.0515 (18)	0.0380 (15)	0.0173 (15)	0.0078 (13)	−0.0058 (13)
C36	0.0407 (14)	0.0395 (15)	0.0385 (14)	0.0039 (11)	0.0049 (11)	0.0029 (11)
C41	0.0328 (12)	0.0251 (11)	0.0266 (11)	0.0028 (9)	−0.0030 (9)	−0.0020 (9)
C42	0.0348 (13)	0.0351 (13)	0.0324 (13)	−0.0012 (10)	0.0040 (10)	−0.0012 (10)
C43	0.0415 (14)	0.0462 (16)	0.0311 (13)	0.0077 (12)	0.0034 (11)	−0.0067 (11)
C44	0.0605 (18)	0.0321 (14)	0.0413 (15)	0.0114 (12)	−0.0012 (13)	−0.0096 (11)
C45	0.0633 (19)	0.0292 (14)	0.0510 (17)	−0.0036 (12)	0.0070 (15)	0.0010 (12)
C46	0.0456 (15)	0.0308 (13)	0.0365 (14)	0.0001 (11)	0.0089 (11)	0.0010 (10)
C51	0.0270 (11)	0.0324 (12)	0.0240 (11)	−0.0021 (9)	0.0020 (9)	0.0025 (9)
C52	0.0343 (13)	0.0398 (14)	0.0330 (13)	0.0038 (11)	0.0003 (10)	−0.0010 (11)
C53	0.0276 (13)	0.0656 (19)	0.0386 (15)	0.0044 (12)	0.0005 (11)	0.0028 (13)
C54	0.0321 (13)	0.0621 (19)	0.0332 (14)	−0.0166 (13)	−0.0012 (11)	0.0050 (13)
C55	0.0435 (15)	0.0383 (14)	0.0301 (13)	−0.0131 (11)	−0.0010 (11)	0.0022 (11)
C56	0.0314 (12)	0.0323 (13)	0.0304 (12)	−0.0021 (10)	−0.0002 (10)	0.0009 (10)
C61	0.0268 (11)	0.0258 (11)	0.0271 (11)	0.0003 (9)	0.0013 (9)	−0.0003 (9)
C62	0.0314 (13)	0.0469 (15)	0.0287 (12)	0.0003 (11)	−0.0003 (10)	0.0012 (11)
C63	0.0426 (15)	0.0572 (18)	0.0272 (13)	0.0023 (13)	0.0062 (11)	0.0013 (12)
C64	0.0324 (13)	0.0437 (15)	0.0416 (15)	0.0013 (11)	0.0130 (11)	−0.0038 (12)
C65	0.0253 (12)	0.0508 (16)	0.0440 (15)	0.0000 (11)	0.0014 (11)	−0.0027 (12)
C66	0.0319 (13)	0.0463 (15)	0.0281 (12)	0.0019 (11)	−0.0004 (10)	−0.0006 (11)

Geometric parameters (Å, º) top

Mo1—C2	1.928 (3)	C21—C26	1.392 (4)
Mo1—C1	1.930 (3)	C21—C22	1.394 (4)
Mo1—C3	1.933 (3)	C22—C23	1.393 (4)
Mo1—C7	2.347 (4)	C23—C24	1.378 (5)
Mo1—C8	2.359 (4)	C24—C25	1.377 (6)
Mo1—C6	2.366 (4)	C25—C26	1.389 (4)
Mo1—C4	2.377 (3)	C31—C36	1.390 (3)
Mo1—C5	2.390 (3)	C31—C32	1.396 (3)
C1—O1	1.175 (4)	C32—C33	1.390 (4)
C2—O2	1.175 (3)	C33—C34	1.373 (4)
C3—O3	1.173 (3)	C34—C35	1.385 (4)
C4—C5	1.351 (5)	C35—C36	1.392 (4)
C4—C8	1.356 (6)	C41—C46	1.385 (3)
C5—C6	1.385 (7)	C41—C42	1.404 (3)
C6—C7	1.403 (8)	C42—C43	1.379 (4)
C7—C8	1.341 (8)	C43—C44	1.378 (4)
P2—N1	1.584 (2)	C44—C45	1.376 (4)
P2—C61	1.796 (2)	C45—C46	1.398 (4)
P2—C41	1.804 (2)	C51—C56	1.397 (3)
P2—C51	1.813 (2)	C51—C52	1.398 (3)
P1—N1	1.579 (2)	C52—C53	1.391 (4)
P1—C11	1.797 (2)	C53—C54	1.384 (4)
P1—C31	1.806 (2)	C54—C55	1.379 (4)
P1—C21	1.810 (2)	C55—C56	1.389 (3)
C11—C16	1.391 (3)	C61—C62	1.394 (3)
C11—C12	1.396 (3)	C61—C66	1.397 (3)
C12—C13	1.388 (4)	C62—C63	1.388 (4)
C13—C14	1.378 (4)	C63—C64	1.382 (4)
C14—C15	1.377 (4)	C64—C65	1.382 (4)
C15—C16	1.386 (4)	C65—C66	1.383 (3)

C2—Mo1—C1	84.49 (12)	C11—P1—C31	108.00 (11)
C2—Mo1—C3	88.43 (11)	N1—P1—C21	113.27 (11)
C1—Mo1—C3	88.93 (11)	C11—P1—C21	107.31 (11)
C2—Mo1—C7	99.75 (15)	C31—P1—C21	107.88 (11)
C1—Mo1—C7	126.4 (3)	P1—N1—P2	142.62 (14)
C3—Mo1—C7	144.1 (2)	C16—C11—C12	119.4 (2)
C2—Mo1—C8	106.34 (14)	C16—C11—P1	119.42 (18)
C1—Mo1—C8	157.12 (17)	C12—C11—P1	121.07 (19)
C3—Mo1—C8	111.04 (19)	C13—C12—C11	120.0 (3)
C7—Mo1—C8	33.1 (2)	C14—C13—C12	119.9 (3)
C2—Mo1—C6	124.99 (19)	C15—C14—C13	120.6 (3)
C1—Mo1—C6	101.43 (17)	C14—C15—C16	120.1 (3)
C3—Mo1—C6	145.50 (17)	C15—C16—C11	120.0 (2)
C7—Mo1—C6	34.6 (2)	C26—C21—C22	119.4 (2)
C8—Mo1—C6	55.79 (19)	C26—C21—P1	120.4 (2)
C2—Mo1—C4	137.09 (13)	C22—C21—P1	119.8 (2)
C1—Mo1—C4	138.18 (14)	C23—C22—C21	119.6 (3)
C3—Mo1—C4	95.29 (11)	C24—C23—C22	120.6 (3)
C7—Mo1—C4	55.50 (16)	C25—C24—C23	120.0 (3)
C8—Mo1—C4	33.29 (15)	C24—C25—C26	120.3 (3)
C6—Mo1—C4	55.47 (14)	C25—C26—C21	120.2 (3)
C2—Mo1—C5	156.10 (12)	C36—C31—C32	119.9 (2)
C1—Mo1—C5	107.84 (13)	C36—C31—P1	118.54 (19)
C3—Mo1—C5	111.64 (13)	C32—C31—P1	121.58 (19)
C7—Mo1—C5	56.40 (16)	C33—C32—C31	119.4 (3)
C8—Mo1—C5	55.30 (13)	C34—C33—C32	120.9 (3)
C6—Mo1—C5	33.86 (17)	C33—C34—C35	119.8 (3)
C4—Mo1—C5	32.92 (12)	C34—C35—C36	120.3 (3)
O1—C1—Mo1	178.8 (3)	C31—C36—C35	119.7 (3)
O2—C2—Mo1	179.3 (3)	C46—C41—C42	119.4 (2)
O3—C3—Mo1	177.0 (2)	C46—C41—P2	121.80 (19)
C5—C4—C8	109.0 (4)	C42—C41—P2	118.80 (18)
C5—C4—Mo1	74.05 (19)	C43—C42—C41	120.2 (2)
C8—C4—Mo1	72.6 (2)	C44—C43—C42	120.3 (2)
C4—C5—C6	107.6 (4)	C45—C44—C43	120.2 (2)
C4—C5—Mo1	73.03 (19)	C44—C45—C46	120.4 (3)
C6—C5—Mo1	72.1 (2)	C41—C46—C45	119.6 (2)
C5—C6—C7	106.8 (4)	C56—C51—C52	119.3 (2)
C5—C6—Mo1	74.0 (2)	C56—C51—P2	117.80 (18)
C7—C6—Mo1	72.0 (2)	C52—C51—P2	122.80 (19)
C8—C7—C6	107.3 (4)	C53—C52—C51	120.2 (3)
C8—C7—Mo1	73.9 (2)	C54—C53—C52	119.9 (3)
C6—C7—Mo1	73.4 (3)	C55—C54—C53	120.2 (2)
C7—C8—C4	109.3 (5)	C54—C55—C56	120.6 (3)
C7—C8—Mo1	73.0 (3)	C55—C56—C51	119.8 (2)
C4—C8—Mo1	74.1 (2)	C62—C61—C66	119.6 (2)
N1—P2—C61	107.97 (11)	C62—C61—P2	121.64 (18)
N1—P2—C41	111.66 (11)	C66—C61—P2	118.62 (18)
C61—P2—C41	107.49 (11)	C63—C62—C61	119.9 (2)
N1—P2—C51	114.13 (11)	C64—C63—C62	120.0 (2)
C61—P2—C51	109.04 (10)	C63—C64—C65	120.3 (2)
C41—P2—C51	106.34 (11)	C64—C65—C66	120.3 (2)
N1—P1—C11	107.69 (11)	C65—C66—C61	119.8 (2)
N1—P1—C31	112.45 (11)

Experimental details

Crystal data
Chemical formula	C₃₆H₃₀NP₂·C₈H₅MoO₃
M_r	783.61
Crystal system, space group	Monoclinic, P2₁/c
Temperature (K)	203
a, b, c (Å)	14.0385 (2), 19.1269 (2), 13.8322 (1)
β (°)	90.728 (1)
V (Å³)	3713.83 (7)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	0.48
Crystal size (mm)	0.26 × 0.24 × 0.20

Data collection
Diffractometer	Siemens SMART CCD diffractometer
Absorption correction	Empirical (using intensity measurements) (Blessing, 1995)
T_min, T_max	0.885, 0.910
No. of measured, independent and observed [I > 2σ(I)] reflections	22556, 8177, 6724
R_int	0.025
(sin θ/λ)_max (Å⁻¹)	0.650

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.037, 0.090, 1.08
No. of reflections	8177
No. of parameters	460
H-atom treatment	Riding with tied Uiso
Δρ_max, Δρ_min (e Å⁻³)	0.52, −0.40

Computer programs: SMART (Siemens, 1994), SAINT (Siemens, 1994), SADABS (Blessing, 1995), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), ORTEP-3 for Windows (Farrugia, 1997), WinGX (Farrugia, 1999).

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