Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536801016178/tk6037sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536801016178/tk6037Isup2.hkl |
CCDC reference: 175971
[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.
Hydrogen atoms were placed in calculated positions, with Uiso values 1.2 times the Uiso values of the atoms to which they are attached.
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).
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) |
C36H30NP2·C8H5MoO3 | F(000) = 1608 |
Mr = 783.61 | Dx = 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 |
Siemens SMART CCD diffractometer | 8177 independent reflections |
Radiation source: fine-focus sealed tube | 6724 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.025 |
multiscan | θmax = 27.5°, θmin = 1.5° |
Absorption correction: empirical (using intensity measurements) (Blessing, 1995) | h = −18→18 |
Tmin = 0.885, Tmax = 0.910 | k = 0→24 |
22556 measured reflections | l = 0→17 |
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(Fo2) + (0.0305P)2 + 3.4046P] where P = (Fo2 + 2Fc2)/3 |
8177 reflections | (Δ/σ)max = 0.001 |
460 parameters | Δρmax = 0.52 e Å−3 |
0 restraints | Δρmin = −0.40 e Å−3 |
C36H30NP2·C8H5MoO3 | V = 3713.83 (7) Å3 |
Mr = 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)° |
Siemens SMART CCD diffractometer | 8177 independent reflections |
Absorption correction: empirical (using intensity measurements) (Blessing, 1995) | 6724 reflections with I > 2σ(I) |
Tmin = 0.885, Tmax = 0.910 | Rint = 0.025 |
22556 measured reflections |
R[F2 > 2σ(F2)] = 0.037 | 0 restraints |
wR(F2) = 0.090 | Riding with tied Uiso |
S = 1.08 | Δρmax = 0.52 e Å−3 |
8177 reflections | Δρmin = −0.40 e Å−3 |
460 parameters |
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. |
x | y | z | Uiso*/Ueq | ||
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* |
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) |
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 |
Mr | 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) |
Tmin, Tmax | 0.885, 0.910 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 22556, 8177, 6724 |
Rint | 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 |
Δρmax, Δρmin (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).
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—CCO bond length [1.930 (3) Å] is slightly larger than that reported for the tetrabutyl ammonium salt [1.909 (9) Å] while the average CCO—Mo—CCO angle [87 (2)°] and Mo—CCp 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).