Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807019320/gw2011sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807019320/gw2011Isup2.hkl |
CCDC reference: 646650
Key indicators
- Single-crystal X-ray study
- T = 170 K
- Mean (C-C) = 0.004 Å
- Disorder in main residue
- R factor = 0.037
- wR factor = 0.101
- Data-to-parameter ratio = 17.8
checkCIF/PLATON results
No syntax errors found
Alert level C PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ? PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.63 Ratio PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for N1 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C91 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C91' PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for C93 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for C95 PLAT301_ALERT_3_C Main Residue Disorder ......................... 2.00 Perc. PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 44.90 Deg. C91 -N1 -C91' 1.555 1.555 1.555
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 9 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 5 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 3 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
Under an inert gas atmosphere, 120 mg (0,127 mmol) of the nitrido complex [Mo(N)(Cl)(dppe)2], prepared following literature procedures (George et al., 1978; Chatt et al., 1977), were dissolved in 15 ml thf. Some drops of ethyliodide were added and the solution was stirred for 3 h. Afterwards the reaction mixture was evaporated to dryness and the residue was redissolved in 30 ml of acetonitrile. After addition of 50 mg (0,15 mmol) sodium tetraphenylborate the product crystallizes in rectangular plates.
The hydrogen atoms were positioned with idealized geometry (methyl H atoms allowed to rotate but not to tip) and were refined isotropic with Ueq = 1.2 Ueq(C) for aromatic and methylene H atoms and Ueq = 1.5 Ueq(C) for methyl H atoms using a riding model with C—H = 0.95 Å for aromatic, C—H = 0.99 Å for methylene and C—H = 0.98 Å for methyl H atoms. Both carbon atoms of the ethylimido ligand are disordered in two positions and were refined using a split model.
The structure determination of this compound was undertaken as part of a project on the asymmetric reduction of dinitrogen via the Chatt cycle (Mersmann et al., 2006). Imido complexes are problematic intermediates in this cycle because of their very negative reduction potentials (Alias et al., 1997). For practical reasons it is instructive to study alkylimido complexes. During these investigations we obtained big crystals of the title compound in order to perform polarized absorption spectroscopy. An absoption band at 510 nm possesses unexpected differences in intensity under polarization along the a- and b axis of this molecule. Furthermore a vibrational fine structure of about 530 cm-1 was observed on the absorption band, which is attributed to a Mo—N—C bending vibration.
The crystal structure of the title compound consists of discrete [Mo(Cl)(NC2H5)(P2C26H24)2]+ cations and tetraphenylborate anions. The molybdenum atoms are coordinated by four phosphorous atoms of two crystallographically independent 1,2-bis(diphenylphosphino)ethane ligands, one nitrogen atom of an ethylimido ligand and one chlorine atom within distorted octahedra (Fig. 1). All bond lengths and angles are in good agreement with those retrieved from the CSD database (conquest version 1.8, 2007; Bruno et al., 2002) The Mo1—N1 bond lengths of 1.732 (2) Å strongly indicate that this is a Mo—N triple bond. There are two additional acetonitrile ligands per formula unit within the structure, that are located in holes of the crystal. These solvent molecules exhibit slightly enlarged anisotropic displacement parameters indicating some static or dynamic disorder.
For related literature, see: Alias et al. (1997); Allen & Kennard (1993); Chatt & Dilworth (1977); George & Noble (1978); Mersmann et al. (2006).
Data collection: IPDS Program Package (Stoe & Cie, 1998); cell refinement: IPDS Program Package; data reduction: IPDS Program Package; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP in SHELXTL (Bruker, 1998); software used to prepare material for publication: CIFTAB in SHELXTL.
Fig. 1. : Crystal structure of compound I with labelling and displacement ellipsoids drawn at the 50% probability level. The hydrogen atoms are omitted for clarity. |
[Mo(C2H5N)Cl(C26H24P2)2](C24H20B)·2C2H3N | F(000) = 2864 |
Mr = 1372.56 | Dx = 1.299 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
a = 15.3299 (12) Å | Cell parameters from 8000 reflections |
b = 21.5840 (11) Å | θ = 11.3–24.3° |
c = 21.3439 (16) Å | µ = 0.36 mm−1 |
β = 96.387 (9)° | T = 170 K |
V = 7018.4 (8) Å3 | Block, red |
Z = 4 | 0.2 × 0.15 × 0.1 mm |
Stoe IPDS-1 diffractometer | 15159 independent reflections |
Radiation source: fine-focus sealed tube | 12034 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.043 |
φ scans | θmax = 27.0°, θmin = 2.1° |
Absorption correction: numerical (X-SHAPE; Stoe & Cie, 1998) | h = −19→18 |
Tmin = 0.929, Tmax = 0.941 | k = −23→27 |
48449 measured reflections | l = −27→27 |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.037 | H-atom parameters constrained |
wR(F2) = 0.101 | w = 1/[σ2(Fo2) + (0.0633P)2 + 1.19P] where P = (Fo2 + 2Fc2)/3 |
S = 1.01 | (Δ/σ)max = 0.005 |
15159 reflections | Δρmax = 0.62 e Å−3 |
850 parameters | Δρmin = −0.68 e Å−3 |
0 restraints | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0024 (2) |
[Mo(C2H5N)Cl(C26H24P2)2](C24H20B)·2C2H3N | V = 7018.4 (8) Å3 |
Mr = 1372.56 | Z = 4 |
Monoclinic, P21/n | Mo Kα radiation |
a = 15.3299 (12) Å | µ = 0.36 mm−1 |
b = 21.5840 (11) Å | T = 170 K |
c = 21.3439 (16) Å | 0.2 × 0.15 × 0.1 mm |
β = 96.387 (9)° |
Stoe IPDS-1 diffractometer | 15159 independent reflections |
Absorption correction: numerical (X-SHAPE; Stoe & Cie, 1998) | 12034 reflections with I > 2σ(I) |
Tmin = 0.929, Tmax = 0.941 | Rint = 0.043 |
48449 measured reflections |
R[F2 > 2σ(F2)] = 0.037 | 0 restraints |
wR(F2) = 0.101 | H-atom parameters constrained |
S = 1.01 | Δρmax = 0.62 e Å−3 |
15159 reflections | Δρmin = −0.68 e Å−3 |
850 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 | Occ. (<1) | |
Mo1 | 0.498959 (11) | 0.407142 (8) | 0.224115 (7) | 0.01628 (6) | |
Cl1 | 0.47025 (4) | 0.40693 (3) | 0.10929 (2) | 0.02676 (12) | |
N1 | 0.52061 (19) | 0.40494 (9) | 0.30548 (9) | 0.0443 (6) | |
C91 | 0.5682 (3) | 0.40422 (19) | 0.37061 (19) | 0.0293 (8) | 0.60 |
H91A | 0.5967 | 0.4447 | 0.3809 | 0.035* | 0.60 |
H91B | 0.6135 | 0.3714 | 0.3747 | 0.035* | 0.60 |
C92 | 0.4978 (4) | 0.3913 (3) | 0.4132 (2) | 0.0538 (13) | 0.60 |
H92A | 0.5243 | 0.3900 | 0.4572 | 0.081* | 0.60 |
H92B | 0.4700 | 0.3513 | 0.4019 | 0.081* | 0.60 |
H92C | 0.4535 | 0.4242 | 0.4083 | 0.081* | 0.60 |
C91' | 0.4942 (4) | 0.3962 (3) | 0.3708 (3) | 0.0281 (12) | 0.40 |
H91C | 0.4728 | 0.3535 | 0.3768 | 0.034* | 0.40 |
H91D | 0.4483 | 0.4261 | 0.3796 | 0.034* | 0.40 |
C92' | 0.5809 (5) | 0.4085 (4) | 0.4127 (3) | 0.050 (2) | 0.40 |
H92D | 0.5714 | 0.4040 | 0.4572 | 0.075* | 0.40 |
H92E | 0.6011 | 0.4506 | 0.4052 | 0.075* | 0.40 |
H92F | 0.6253 | 0.3786 | 0.4025 | 0.075* | 0.40 |
P1 | 0.39118 (3) | 0.49746 (2) | 0.21967 (2) | 0.01916 (11) | |
P2 | 0.35534 (3) | 0.34829 (3) | 0.22543 (2) | 0.02065 (12) | |
C1 | 0.28036 (15) | 0.46342 (11) | 0.21360 (12) | 0.0289 (5) | |
H1A | 0.2385 | 0.4939 | 0.2277 | 0.035* | |
H1B | 0.2610 | 0.4526 | 0.1691 | 0.035* | |
C2 | 0.28130 (15) | 0.40533 (10) | 0.25447 (11) | 0.0270 (5) | |
H2A | 0.2213 | 0.3879 | 0.2527 | 0.032* | |
H2B | 0.3014 | 0.4159 | 0.2989 | 0.032* | |
C3 | 0.38091 (14) | 0.55426 (10) | 0.15561 (9) | 0.0219 (4) | |
C4 | 0.41413 (16) | 0.61398 (11) | 0.16549 (10) | 0.0267 (5) | |
H4 | 0.4416 | 0.6256 | 0.2059 | 0.032* | |
C5 | 0.40713 (19) | 0.65652 (12) | 0.11648 (11) | 0.0377 (6) | |
H5 | 0.4293 | 0.6974 | 0.1235 | 0.045* | |
C6 | 0.3682 (2) | 0.63965 (13) | 0.05778 (11) | 0.0407 (6) | |
H6 | 0.3624 | 0.6691 | 0.0245 | 0.049* | |
C7 | 0.33749 (19) | 0.58018 (13) | 0.04703 (11) | 0.0388 (6) | |
H7 | 0.3122 | 0.5685 | 0.0061 | 0.047* | |
C8 | 0.34333 (16) | 0.53753 (11) | 0.09556 (10) | 0.0305 (5) | |
H8 | 0.3217 | 0.4967 | 0.0880 | 0.037* | |
C9 | 0.39205 (14) | 0.54671 (10) | 0.28972 (9) | 0.0227 (4) | |
C10 | 0.46220 (15) | 0.54570 (11) | 0.33647 (10) | 0.0267 (5) | |
H10 | 0.5111 | 0.5196 | 0.3321 | 0.032* | |
C11 | 0.46172 (18) | 0.58257 (11) | 0.38987 (11) | 0.0336 (5) | |
H11 | 0.5096 | 0.5809 | 0.4222 | 0.040* | |
C12 | 0.39177 (19) | 0.62165 (11) | 0.39600 (11) | 0.0350 (6) | |
H12 | 0.3911 | 0.6463 | 0.4328 | 0.042* | |
C13 | 0.32302 (18) | 0.62475 (12) | 0.34869 (12) | 0.0360 (6) | |
H13 | 0.2758 | 0.6525 | 0.3523 | 0.043* | |
C14 | 0.32282 (16) | 0.58740 (11) | 0.29599 (11) | 0.0296 (5) | |
H14 | 0.2750 | 0.5895 | 0.2637 | 0.036* | |
C15 | 0.29625 (15) | 0.31922 (11) | 0.15219 (10) | 0.0265 (5) | |
C16 | 0.20557 (16) | 0.32541 (13) | 0.13927 (12) | 0.0369 (6) | |
H16 | 0.1734 | 0.3479 | 0.1673 | 0.044* | |
C17 | 0.1625 (2) | 0.29883 (15) | 0.08555 (14) | 0.0498 (8) | |
H17 | 0.1008 | 0.3037 | 0.0766 | 0.060* | |
C18 | 0.2080 (2) | 0.26536 (15) | 0.04495 (13) | 0.0497 (8) | |
H18 | 0.1775 | 0.2469 | 0.0085 | 0.060* | |
C19 | 0.2979 (2) | 0.25859 (14) | 0.05704 (12) | 0.0448 (7) | |
H19 | 0.3294 | 0.2353 | 0.0293 | 0.054* | |
C20 | 0.34173 (17) | 0.28634 (12) | 0.11043 (11) | 0.0340 (5) | |
H20 | 0.4037 | 0.2827 | 0.1184 | 0.041* | |
C21 | 0.34541 (14) | 0.28166 (10) | 0.27740 (10) | 0.0248 (4) | |
C22 | 0.36671 (16) | 0.22305 (11) | 0.25682 (12) | 0.0330 (5) | |
H22 | 0.3863 | 0.2183 | 0.2164 | 0.040* | |
C23 | 0.35970 (17) | 0.17142 (12) | 0.29471 (15) | 0.0429 (7) | |
H23 | 0.3758 | 0.1317 | 0.2807 | 0.051* | |
C24 | 0.3292 (2) | 0.17804 (15) | 0.35267 (15) | 0.0514 (8) | |
H24 | 0.3233 | 0.1427 | 0.3784 | 0.062* | |
C25 | 0.3075 (2) | 0.23580 (15) | 0.37329 (13) | 0.0479 (7) | |
H25 | 0.2861 | 0.2401 | 0.4132 | 0.057* | |
C26 | 0.31648 (16) | 0.28802 (12) | 0.33636 (11) | 0.0323 (5) | |
H26 | 0.3028 | 0.3279 | 0.3515 | 0.039* | |
P3 | 0.63851 (3) | 0.46729 (2) | 0.21345 (2) | 0.01898 (11) | |
P4 | 0.60205 (3) | 0.31874 (2) | 0.20681 (2) | 0.02002 (11) | |
C31 | 0.72697 (14) | 0.41003 (10) | 0.22556 (11) | 0.0269 (5) | |
H31A | 0.7827 | 0.4284 | 0.2150 | 0.032* | |
H31B | 0.7351 | 0.3968 | 0.2702 | 0.032* | |
C32 | 0.70217 (15) | 0.35445 (11) | 0.18297 (11) | 0.0282 (5) | |
H32A | 0.7506 | 0.3239 | 0.1867 | 0.034* | |
H32B | 0.6918 | 0.3681 | 0.1385 | 0.034* | |
C33 | 0.65835 (14) | 0.50534 (10) | 0.13959 (9) | 0.0232 (4) | |
C34 | 0.74278 (15) | 0.51344 (12) | 0.12320 (11) | 0.0310 (5) | |
H34 | 0.7913 | 0.4959 | 0.1487 | 0.037* | |
C35 | 0.75663 (17) | 0.54724 (13) | 0.06962 (12) | 0.0363 (6) | |
H35 | 0.8146 | 0.5523 | 0.0586 | 0.044* | |
C36 | 0.68722 (18) | 0.57335 (12) | 0.03251 (11) | 0.0346 (6) | |
H36 | 0.6972 | 0.5966 | −0.0038 | 0.041* | |
C37 | 0.60335 (18) | 0.56560 (12) | 0.04823 (11) | 0.0346 (5) | |
H37 | 0.5552 | 0.5836 | 0.0227 | 0.041* | |
C38 | 0.58884 (16) | 0.53159 (12) | 0.10132 (10) | 0.0295 (5) | |
H38 | 0.5306 | 0.5262 | 0.1116 | 0.035* | |
C39 | 0.67054 (13) | 0.52817 (10) | 0.27102 (9) | 0.0211 (4) | |
C40 | 0.71922 (15) | 0.51613 (11) | 0.32870 (10) | 0.0276 (5) | |
H40 | 0.7373 | 0.4750 | 0.3393 | 0.033* | |
C41 | 0.74138 (17) | 0.56396 (13) | 0.37068 (11) | 0.0359 (6) | |
H41 | 0.7747 | 0.5554 | 0.4099 | 0.043* | |
C42 | 0.71564 (18) | 0.62372 (12) | 0.35619 (12) | 0.0367 (6) | |
H42 | 0.7319 | 0.6564 | 0.3850 | 0.044* | |
C43 | 0.66570 (18) | 0.63605 (11) | 0.29926 (12) | 0.0348 (5) | |
H43 | 0.6466 | 0.6771 | 0.2893 | 0.042* | |
C44 | 0.64374 (16) | 0.58848 (11) | 0.25710 (11) | 0.0283 (5) | |
H44 | 0.6099 | 0.5972 | 0.2181 | 0.034* | |
C45 | 0.57533 (14) | 0.25804 (10) | 0.14803 (10) | 0.0242 (4) | |
C46 | 0.57037 (18) | 0.27257 (12) | 0.08388 (11) | 0.0341 (5) | |
H46 | 0.5853 | 0.3130 | 0.0711 | 0.041* | |
C47 | 0.5437 (2) | 0.22822 (13) | 0.03898 (12) | 0.0428 (7) | |
H47 | 0.5408 | 0.2384 | −0.0045 | 0.051* | |
C48 | 0.52136 (19) | 0.16919 (13) | 0.05671 (12) | 0.0405 (6) | |
H48 | 0.5031 | 0.1390 | 0.0256 | 0.049* | |
C49 | 0.52576 (18) | 0.15443 (12) | 0.12001 (12) | 0.0369 (6) | |
H49 | 0.5100 | 0.1141 | 0.1324 | 0.044* | |
C50 | 0.55329 (16) | 0.19857 (11) | 0.16568 (11) | 0.0292 (5) | |
H50 | 0.5570 | 0.1879 | 0.2091 | 0.035* | |
C51 | 0.64005 (15) | 0.27452 (10) | 0.27751 (10) | 0.0253 (5) | |
C52 | 0.58005 (17) | 0.26072 (11) | 0.31972 (10) | 0.0310 (5) | |
H52 | 0.5224 | 0.2773 | 0.3131 | 0.037* | |
C53 | 0.6037 (2) | 0.22294 (12) | 0.37139 (12) | 0.0402 (6) | |
H53 | 0.5621 | 0.2132 | 0.3997 | 0.048* | |
C54 | 0.6877 (2) | 0.19962 (12) | 0.38149 (13) | 0.0492 (8) | |
H54 | 0.7041 | 0.1739 | 0.4170 | 0.059* | |
C55 | 0.7475 (2) | 0.21340 (15) | 0.34061 (15) | 0.0555 (9) | |
H55 | 0.8053 | 0.1971 | 0.3479 | 0.067* | |
C56 | 0.72490 (19) | 0.25093 (14) | 0.28856 (13) | 0.0427 (6) | |
H56 | 0.7671 | 0.2605 | 0.2606 | 0.051* | |
B1 | 0.48127 (15) | −0.08729 (11) | 0.17146 (11) | 0.0203 (4) | |
C61 | 0.50020 (13) | −0.03005 (10) | 0.22225 (10) | 0.0215 (4) | |
C62 | 0.56562 (15) | 0.01470 (10) | 0.22030 (11) | 0.0272 (5) | |
H62 | 0.6006 | 0.0140 | 0.1863 | 0.033* | |
C63 | 0.58165 (17) | 0.06050 (11) | 0.26652 (13) | 0.0366 (6) | |
H63 | 0.6270 | 0.0899 | 0.2634 | 0.044* | |
C64 | 0.53206 (18) | 0.06319 (12) | 0.31651 (12) | 0.0380 (6) | |
H64 | 0.5429 | 0.0942 | 0.3480 | 0.046* | |
C65 | 0.46630 (17) | 0.01994 (12) | 0.32005 (12) | 0.0366 (6) | |
H65 | 0.4311 | 0.0214 | 0.3539 | 0.044* | |
C66 | 0.45152 (15) | −0.02579 (11) | 0.27405 (11) | 0.0289 (5) | |
H66 | 0.4065 | −0.0554 | 0.2779 | 0.035* | |
C67 | 0.38780 (14) | −0.07824 (10) | 0.12653 (9) | 0.0216 (4) | |
C68 | 0.36469 (15) | −0.12151 (11) | 0.07866 (10) | 0.0281 (5) | |
H68 | 0.4037 | −0.1549 | 0.0735 | 0.034* | |
C69 | 0.28697 (17) | −0.11773 (13) | 0.03827 (10) | 0.0345 (6) | |
H69 | 0.2736 | −0.1483 | 0.0066 | 0.041* | |
C70 | 0.22974 (16) | −0.06959 (14) | 0.04446 (11) | 0.0358 (6) | |
H70 | 0.1765 | −0.0668 | 0.0172 | 0.043* | |
C71 | 0.25019 (15) | −0.02557 (13) | 0.09041 (11) | 0.0324 (5) | |
H71 | 0.2110 | 0.0078 | 0.0949 | 0.039* | |
C72 | 0.32856 (14) | −0.02987 (11) | 0.13057 (10) | 0.0246 (4) | |
H72 | 0.3418 | 0.0013 | 0.1616 | 0.030* | |
C73 | 0.55772 (14) | −0.09069 (10) | 0.12310 (10) | 0.0230 (4) | |
C74 | 0.56174 (15) | −0.04456 (11) | 0.07683 (10) | 0.0273 (5) | |
H74 | 0.5204 | −0.0117 | 0.0749 | 0.033* | |
C75 | 0.62368 (16) | −0.04511 (13) | 0.03393 (11) | 0.0339 (5) | |
H75 | 0.6241 | −0.0129 | 0.0036 | 0.041* | |
C76 | 0.68469 (17) | −0.09249 (13) | 0.03532 (12) | 0.0372 (6) | |
H76 | 0.7272 | −0.0932 | 0.0062 | 0.045* | |
C77 | 0.68259 (16) | −0.13894 (13) | 0.07998 (12) | 0.0356 (5) | |
H77 | 0.7242 | −0.1717 | 0.0816 | 0.043* | |
C78 | 0.61981 (15) | −0.13791 (11) | 0.12256 (11) | 0.0279 (5) | |
H78 | 0.6193 | −0.1706 | 0.1523 | 0.034* | |
C79 | 0.47921 (13) | −0.15040 (10) | 0.21425 (9) | 0.0205 (4) | |
C80 | 0.54757 (15) | −0.16243 (11) | 0.26222 (10) | 0.0275 (5) | |
H80 | 0.5954 | −0.1342 | 0.2681 | 0.033* | |
C81 | 0.54804 (16) | −0.21383 (12) | 0.30136 (11) | 0.0331 (5) | |
H81 | 0.5958 | −0.2203 | 0.3330 | 0.040* | |
C82 | 0.47913 (17) | −0.25576 (12) | 0.29447 (12) | 0.0353 (5) | |
H82 | 0.4793 | −0.2910 | 0.3211 | 0.042* | |
C83 | 0.41032 (16) | −0.24545 (11) | 0.24836 (11) | 0.0309 (5) | |
H83 | 0.3622 | −0.2734 | 0.2435 | 0.037* | |
C84 | 0.41126 (14) | −0.19410 (10) | 0.20891 (10) | 0.0239 (4) | |
H84 | 0.3636 | −0.1885 | 0.1769 | 0.029* | |
N2 | 0.2933 (3) | 0.2066 (3) | 0.54874 (19) | 0.1073 (15) | |
C93 | 0.3490 (3) | 0.2388 (2) | 0.53754 (18) | 0.0772 (12) | |
C94 | 0.4213 (3) | 0.2788 (3) | 0.5230 (3) | 0.1022 (16) | |
H94A | 0.4523 | 0.2948 | 0.5623 | 0.153* | |
H94B | 0.3979 | 0.3134 | 0.4966 | 0.153* | |
H94C | 0.4621 | 0.2548 | 0.5003 | 0.153* | |
N3 | 0.5099 (5) | 0.1161 (4) | 0.4785 (2) | 0.178 (3) | |
C95 | 0.4699 (4) | 0.0975 (3) | 0.5157 (2) | 0.0936 (16) | |
C96 | 0.4198 (4) | 0.0808 (3) | 0.5645 (3) | 0.121 (2) | |
H96A | 0.4565 | 0.0831 | 0.6050 | 0.182* | |
H96B | 0.3980 | 0.0384 | 0.5576 | 0.182* | |
H96C | 0.3700 | 0.1093 | 0.5648 | 0.182* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Mo1 | 0.01982 (9) | 0.01424 (9) | 0.01485 (9) | 0.00141 (7) | 0.00219 (6) | −0.00022 (6) |
Cl1 | 0.0357 (3) | 0.0260 (3) | 0.0177 (2) | −0.0009 (2) | −0.00102 (19) | −0.00043 (19) |
N1 | 0.0904 (19) | 0.0166 (10) | 0.0249 (10) | 0.0166 (11) | 0.0015 (11) | −0.0020 (8) |
C91 | 0.031 (2) | 0.031 (2) | 0.026 (2) | 0.0033 (17) | 0.0032 (16) | 0.0022 (16) |
C92 | 0.060 (3) | 0.071 (4) | 0.033 (3) | −0.011 (3) | 0.014 (2) | 0.005 (2) |
C91' | 0.040 (4) | 0.028 (3) | 0.016 (3) | −0.001 (3) | 0.003 (2) | 0.005 (2) |
C92' | 0.051 (4) | 0.076 (6) | 0.022 (3) | −0.009 (4) | −0.008 (3) | 0.004 (3) |
P1 | 0.0214 (3) | 0.0154 (3) | 0.0211 (2) | 0.0021 (2) | 0.00404 (19) | 0.00153 (19) |
P2 | 0.0205 (3) | 0.0159 (3) | 0.0263 (3) | 0.0004 (2) | 0.0058 (2) | 0.0011 (2) |
C1 | 0.0241 (11) | 0.0187 (11) | 0.0441 (13) | 0.0015 (9) | 0.0046 (9) | 0.0048 (9) |
C2 | 0.0247 (11) | 0.0187 (11) | 0.0398 (12) | 0.0025 (9) | 0.0130 (9) | 0.0026 (9) |
C3 | 0.0230 (10) | 0.0192 (10) | 0.0238 (10) | 0.0026 (8) | 0.0044 (8) | 0.0013 (8) |
C4 | 0.0360 (12) | 0.0213 (11) | 0.0238 (10) | −0.0013 (10) | 0.0071 (9) | 0.0007 (8) |
C5 | 0.0609 (17) | 0.0218 (12) | 0.0325 (12) | −0.0044 (12) | 0.0150 (11) | 0.0029 (9) |
C6 | 0.0618 (18) | 0.0324 (14) | 0.0295 (12) | 0.0070 (13) | 0.0117 (12) | 0.0122 (10) |
C7 | 0.0539 (16) | 0.0381 (15) | 0.0228 (11) | 0.0070 (12) | −0.0026 (10) | 0.0033 (10) |
C8 | 0.0377 (13) | 0.0250 (12) | 0.0276 (11) | 0.0023 (10) | −0.0019 (9) | 0.0000 (9) |
C9 | 0.0297 (11) | 0.0174 (10) | 0.0224 (9) | 0.0020 (9) | 0.0093 (8) | 0.0022 (8) |
C10 | 0.0318 (12) | 0.0212 (11) | 0.0280 (10) | 0.0019 (9) | 0.0071 (9) | −0.0018 (8) |
C11 | 0.0438 (14) | 0.0272 (13) | 0.0297 (11) | −0.0033 (11) | 0.0034 (10) | −0.0026 (9) |
C12 | 0.0565 (16) | 0.0229 (12) | 0.0284 (11) | −0.0003 (11) | 0.0169 (11) | −0.0036 (9) |
C13 | 0.0465 (15) | 0.0273 (13) | 0.0376 (13) | 0.0116 (11) | 0.0191 (11) | 0.0003 (10) |
C14 | 0.0344 (12) | 0.0269 (12) | 0.0287 (11) | 0.0089 (10) | 0.0083 (9) | 0.0033 (9) |
C15 | 0.0263 (11) | 0.0213 (11) | 0.0314 (11) | −0.0042 (9) | 0.0010 (9) | 0.0036 (9) |
C16 | 0.0279 (12) | 0.0377 (15) | 0.0439 (14) | −0.0041 (11) | −0.0009 (10) | 0.0093 (11) |
C17 | 0.0376 (15) | 0.060 (2) | 0.0479 (16) | −0.0145 (14) | −0.0142 (12) | 0.0151 (14) |
C18 | 0.0580 (18) | 0.0558 (19) | 0.0316 (13) | −0.0279 (15) | −0.0111 (13) | 0.0091 (12) |
C19 | 0.0565 (18) | 0.0440 (16) | 0.0337 (13) | −0.0173 (14) | 0.0035 (12) | −0.0068 (11) |
C20 | 0.0329 (12) | 0.0339 (14) | 0.0345 (12) | −0.0068 (11) | 0.0008 (10) | −0.0054 (10) |
C21 | 0.0183 (10) | 0.0223 (11) | 0.0338 (11) | −0.0011 (9) | 0.0022 (8) | 0.0056 (9) |
C22 | 0.0280 (12) | 0.0222 (12) | 0.0490 (14) | 0.0004 (10) | 0.0058 (10) | 0.0047 (10) |
C23 | 0.0314 (13) | 0.0207 (13) | 0.0739 (19) | −0.0018 (11) | −0.0050 (12) | 0.0114 (12) |
C24 | 0.0483 (17) | 0.0387 (17) | 0.0651 (19) | −0.0092 (14) | −0.0028 (14) | 0.0293 (14) |
C25 | 0.0494 (17) | 0.0516 (19) | 0.0428 (14) | −0.0097 (14) | 0.0055 (12) | 0.0212 (13) |
C26 | 0.0311 (12) | 0.0338 (13) | 0.0322 (11) | −0.0037 (10) | 0.0052 (9) | 0.0076 (10) |
P3 | 0.0181 (2) | 0.0159 (3) | 0.0224 (2) | 0.0006 (2) | 0.00004 (19) | −0.00067 (19) |
P4 | 0.0214 (3) | 0.0157 (3) | 0.0230 (2) | 0.0019 (2) | 0.00261 (19) | −0.00274 (19) |
C31 | 0.0201 (10) | 0.0193 (11) | 0.0403 (12) | 0.0006 (9) | −0.0004 (9) | −0.0030 (9) |
C32 | 0.0239 (11) | 0.0211 (11) | 0.0406 (12) | 0.0015 (9) | 0.0074 (9) | −0.0041 (9) |
C33 | 0.0254 (11) | 0.0202 (11) | 0.0245 (10) | −0.0051 (9) | 0.0048 (8) | −0.0046 (8) |
C34 | 0.0260 (11) | 0.0339 (13) | 0.0335 (12) | −0.0064 (10) | 0.0046 (9) | −0.0047 (10) |
C35 | 0.0352 (13) | 0.0388 (15) | 0.0374 (13) | −0.0126 (11) | 0.0158 (10) | −0.0047 (11) |
C36 | 0.0504 (15) | 0.0298 (13) | 0.0248 (11) | −0.0124 (11) | 0.0103 (10) | −0.0032 (9) |
C37 | 0.0418 (14) | 0.0341 (14) | 0.0275 (11) | −0.0033 (11) | 0.0025 (10) | 0.0045 (10) |
C38 | 0.0295 (12) | 0.0321 (13) | 0.0275 (11) | −0.0013 (10) | 0.0054 (9) | 0.0044 (9) |
C39 | 0.0176 (9) | 0.0203 (10) | 0.0253 (10) | −0.0012 (8) | 0.0026 (8) | −0.0017 (8) |
C40 | 0.0299 (11) | 0.0275 (12) | 0.0249 (10) | 0.0067 (10) | 0.0005 (9) | −0.0023 (9) |
C41 | 0.0369 (13) | 0.0421 (15) | 0.0269 (11) | 0.0070 (12) | −0.0044 (10) | −0.0099 (10) |
C42 | 0.0406 (14) | 0.0338 (14) | 0.0353 (12) | −0.0036 (11) | 0.0025 (10) | −0.0162 (10) |
C43 | 0.0459 (14) | 0.0197 (11) | 0.0390 (13) | 0.0011 (11) | 0.0055 (11) | −0.0042 (9) |
C44 | 0.0325 (12) | 0.0219 (11) | 0.0294 (11) | 0.0012 (9) | −0.0014 (9) | −0.0010 (9) |
C45 | 0.0251 (10) | 0.0201 (11) | 0.0280 (10) | 0.0025 (9) | 0.0058 (8) | −0.0062 (8) |
C46 | 0.0494 (15) | 0.0270 (12) | 0.0287 (11) | −0.0083 (11) | 0.0171 (10) | −0.0072 (9) |
C47 | 0.0626 (18) | 0.0392 (15) | 0.0291 (12) | −0.0108 (14) | 0.0165 (12) | −0.0130 (11) |
C48 | 0.0524 (16) | 0.0319 (14) | 0.0386 (13) | −0.0087 (12) | 0.0111 (12) | −0.0176 (11) |
C49 | 0.0449 (15) | 0.0214 (12) | 0.0440 (14) | −0.0041 (11) | 0.0034 (11) | −0.0065 (10) |
C50 | 0.0350 (12) | 0.0204 (11) | 0.0318 (11) | −0.0002 (10) | 0.0020 (9) | −0.0031 (9) |
C51 | 0.0296 (11) | 0.0168 (10) | 0.0276 (10) | 0.0031 (9) | −0.0049 (8) | −0.0041 (8) |
C52 | 0.0369 (13) | 0.0241 (12) | 0.0301 (11) | −0.0002 (10) | −0.0048 (9) | 0.0043 (9) |
C53 | 0.0628 (18) | 0.0246 (13) | 0.0309 (12) | −0.0033 (12) | −0.0057 (11) | 0.0051 (10) |
C54 | 0.080 (2) | 0.0257 (13) | 0.0349 (13) | 0.0163 (14) | −0.0223 (14) | 0.0003 (10) |
C55 | 0.0589 (19) | 0.0484 (19) | 0.0532 (17) | 0.0296 (16) | −0.0195 (15) | −0.0048 (14) |
C56 | 0.0395 (14) | 0.0445 (16) | 0.0420 (14) | 0.0175 (13) | −0.0045 (11) | −0.0025 (12) |
B1 | 0.0185 (11) | 0.0177 (11) | 0.0252 (11) | −0.0002 (9) | 0.0043 (8) | 0.0006 (8) |
C61 | 0.0185 (9) | 0.0161 (10) | 0.0293 (10) | 0.0013 (8) | 0.0005 (8) | 0.0000 (8) |
C62 | 0.0242 (11) | 0.0195 (11) | 0.0368 (12) | −0.0025 (9) | −0.0012 (9) | 0.0029 (9) |
C63 | 0.0338 (13) | 0.0196 (12) | 0.0530 (15) | −0.0059 (10) | −0.0107 (11) | −0.0011 (10) |
C64 | 0.0413 (14) | 0.0243 (13) | 0.0445 (14) | 0.0063 (11) | −0.0120 (11) | −0.0127 (10) |
C65 | 0.0403 (14) | 0.0330 (14) | 0.0366 (13) | 0.0053 (11) | 0.0050 (10) | −0.0103 (10) |
C66 | 0.0272 (11) | 0.0238 (12) | 0.0362 (12) | −0.0026 (9) | 0.0065 (9) | −0.0066 (9) |
C67 | 0.0210 (10) | 0.0234 (11) | 0.0212 (9) | −0.0035 (8) | 0.0064 (8) | 0.0012 (8) |
C68 | 0.0286 (11) | 0.0288 (12) | 0.0271 (11) | −0.0002 (10) | 0.0036 (9) | −0.0035 (9) |
C69 | 0.0370 (13) | 0.0426 (15) | 0.0229 (10) | −0.0090 (12) | −0.0012 (9) | −0.0042 (10) |
C70 | 0.0233 (11) | 0.0559 (17) | 0.0276 (11) | −0.0025 (11) | −0.0003 (9) | 0.0059 (11) |
C71 | 0.0257 (11) | 0.0433 (15) | 0.0293 (11) | 0.0079 (11) | 0.0074 (9) | 0.0055 (10) |
C72 | 0.0229 (10) | 0.0271 (12) | 0.0250 (10) | 0.0019 (9) | 0.0073 (8) | −0.0003 (8) |
C73 | 0.0213 (10) | 0.0208 (11) | 0.0272 (10) | −0.0028 (8) | 0.0045 (8) | −0.0019 (8) |
C74 | 0.0242 (11) | 0.0272 (12) | 0.0309 (11) | −0.0033 (9) | 0.0054 (9) | 0.0012 (9) |
C75 | 0.0339 (13) | 0.0396 (14) | 0.0291 (11) | −0.0113 (11) | 0.0077 (10) | 0.0013 (10) |
C76 | 0.0315 (12) | 0.0476 (16) | 0.0355 (12) | −0.0091 (12) | 0.0169 (10) | −0.0090 (11) |
C77 | 0.0289 (12) | 0.0366 (14) | 0.0431 (13) | 0.0029 (11) | 0.0122 (10) | −0.0082 (11) |
C78 | 0.0261 (11) | 0.0247 (12) | 0.0342 (11) | 0.0000 (9) | 0.0085 (9) | −0.0016 (9) |
C79 | 0.0203 (10) | 0.0173 (10) | 0.0250 (10) | −0.0009 (8) | 0.0077 (8) | −0.0037 (8) |
C80 | 0.0256 (11) | 0.0230 (12) | 0.0331 (11) | −0.0064 (9) | −0.0001 (9) | 0.0030 (9) |
C81 | 0.0321 (12) | 0.0304 (13) | 0.0356 (12) | 0.0024 (10) | −0.0010 (10) | 0.0058 (10) |
C82 | 0.0430 (14) | 0.0219 (12) | 0.0427 (13) | −0.0012 (11) | 0.0127 (11) | 0.0098 (10) |
C83 | 0.0318 (12) | 0.0180 (11) | 0.0441 (13) | −0.0054 (9) | 0.0096 (10) | 0.0011 (9) |
C84 | 0.0219 (10) | 0.0191 (11) | 0.0310 (10) | −0.0031 (8) | 0.0050 (8) | −0.0026 (8) |
N2 | 0.090 (3) | 0.153 (5) | 0.077 (2) | −0.033 (3) | −0.001 (2) | 0.018 (3) |
C93 | 0.075 (3) | 0.094 (3) | 0.059 (2) | 0.000 (3) | −0.007 (2) | 0.002 (2) |
C94 | 0.086 (3) | 0.096 (4) | 0.119 (4) | −0.018 (3) | −0.015 (3) | 0.004 (3) |
N3 | 0.176 (6) | 0.278 (9) | 0.083 (3) | −0.106 (6) | 0.030 (3) | −0.022 (4) |
C95 | 0.095 (3) | 0.107 (4) | 0.078 (3) | −0.044 (3) | 0.002 (3) | 0.004 (3) |
C96 | 0.107 (4) | 0.115 (5) | 0.145 (5) | 0.001 (4) | 0.035 (4) | 0.051 (4) |
Mo1—N1 | 1.732 (2) | C37—C38 | 1.389 (3) |
Mo1—Cl1 | 2.4413 (5) | C37—H37 | 0.9500 |
Mo1—P4 | 2.5308 (6) | C38—H38 | 0.9500 |
Mo1—P3 | 2.5342 (6) | C39—C44 | 1.387 (3) |
Mo1—P2 | 2.5447 (6) | C39—C40 | 1.391 (3) |
Mo1—P1 | 2.5503 (6) | C40—C41 | 1.384 (3) |
N1—C91 | 1.496 (4) | C40—H40 | 0.9500 |
N1—C91' | 1.507 (6) | C41—C42 | 1.374 (4) |
C91—C92 | 1.513 (6) | C41—H41 | 0.9500 |
C91—H91A | 0.9900 | C42—C43 | 1.388 (4) |
C91—H91B | 0.9900 | C42—H42 | 0.9500 |
C92—H92A | 0.9800 | C43—C44 | 1.382 (3) |
C92—H92B | 0.9800 | C43—H43 | 0.9500 |
C92—H92C | 0.9800 | C44—H44 | 0.9500 |
C91'—C92' | 1.540 (9) | C45—C50 | 1.390 (3) |
C91'—H91C | 0.9900 | C45—C46 | 1.399 (3) |
C91'—H91D | 0.9900 | C46—C47 | 1.384 (3) |
C92'—H92D | 0.9800 | C46—H46 | 0.9500 |
C92'—H92E | 0.9800 | C47—C48 | 1.383 (4) |
C92'—H92F | 0.9800 | C47—H47 | 0.9500 |
P1—C3 | 1.830 (2) | C48—C49 | 1.382 (4) |
P1—C9 | 1.833 (2) | C48—H48 | 0.9500 |
P1—C1 | 1.842 (2) | C49—C50 | 1.394 (3) |
P2—C15 | 1.828 (2) | C49—H49 | 0.9500 |
P2—C2 | 1.829 (2) | C50—H50 | 0.9500 |
P2—C21 | 1.833 (2) | C51—C52 | 1.389 (3) |
C1—C2 | 1.527 (3) | C51—C56 | 1.392 (3) |
C1—H1A | 0.9900 | C52—C53 | 1.387 (3) |
C1—H1B | 0.9900 | C52—H52 | 0.9500 |
C2—H2A | 0.9900 | C53—C54 | 1.376 (4) |
C2—H2B | 0.9900 | C53—H53 | 0.9500 |
C3—C8 | 1.393 (3) | C54—C55 | 1.367 (5) |
C3—C4 | 1.393 (3) | C54—H54 | 0.9500 |
C4—C5 | 1.387 (3) | C55—C56 | 1.388 (4) |
C4—H4 | 0.9500 | C55—H55 | 0.9500 |
C5—C6 | 1.376 (4) | C56—H56 | 0.9500 |
C5—H5 | 0.9500 | B1—C79 | 1.642 (3) |
C6—C7 | 1.378 (4) | B1—C67 | 1.645 (3) |
C6—H6 | 0.9500 | B1—C73 | 1.647 (3) |
C7—C8 | 1.381 (3) | B1—C61 | 1.648 (3) |
C7—H7 | 0.9500 | C61—C62 | 1.396 (3) |
C8—H8 | 0.9500 | C61—C66 | 1.404 (3) |
C9—C10 | 1.383 (3) | C62—C63 | 1.399 (3) |
C9—C14 | 1.395 (3) | C62—H62 | 0.9500 |
C10—C11 | 1.391 (3) | C63—C64 | 1.378 (4) |
C10—H10 | 0.9500 | C63—H63 | 0.9500 |
C11—C12 | 1.382 (4) | C64—C65 | 1.382 (4) |
C11—H11 | 0.9500 | C64—H64 | 0.9500 |
C12—C13 | 1.378 (4) | C65—C66 | 1.393 (3) |
C12—H12 | 0.9500 | C65—H65 | 0.9500 |
C13—C14 | 1.384 (3) | C66—H66 | 0.9500 |
C13—H13 | 0.9500 | C67—C72 | 1.393 (3) |
C14—H14 | 0.9500 | C67—C68 | 1.400 (3) |
C15—C20 | 1.386 (3) | C68—C69 | 1.393 (3) |
C15—C16 | 1.393 (3) | C68—H68 | 0.9500 |
C16—C17 | 1.382 (4) | C69—C70 | 1.376 (4) |
C16—H16 | 0.9500 | C69—H69 | 0.9500 |
C17—C18 | 1.376 (5) | C70—C71 | 1.376 (4) |
C17—H17 | 0.9500 | C70—H70 | 0.9500 |
C18—C19 | 1.381 (4) | C71—C72 | 1.399 (3) |
C18—H18 | 0.9500 | C71—H71 | 0.9500 |
C19—C20 | 1.392 (3) | C72—H72 | 0.9500 |
C19—H19 | 0.9500 | C73—C78 | 1.395 (3) |
C20—H20 | 0.9500 | C73—C74 | 1.409 (3) |
C21—C26 | 1.387 (3) | C74—C75 | 1.391 (3) |
C21—C22 | 1.390 (3) | C74—H74 | 0.9500 |
C22—C23 | 1.388 (4) | C75—C76 | 1.384 (4) |
C22—H22 | 0.9500 | C75—H75 | 0.9500 |
C23—C24 | 1.378 (5) | C76—C77 | 1.386 (4) |
C23—H23 | 0.9500 | C76—H76 | 0.9500 |
C24—C25 | 1.375 (5) | C77—C78 | 1.395 (3) |
C24—H24 | 0.9500 | C77—H77 | 0.9500 |
C25—C26 | 1.391 (4) | C78—H78 | 0.9500 |
C25—H25 | 0.9500 | C79—C84 | 1.401 (3) |
C26—H26 | 0.9500 | C79—C80 | 1.405 (3) |
P3—C39 | 1.829 (2) | C80—C81 | 1.388 (3) |
P3—C31 | 1.832 (2) | C80—H80 | 0.9500 |
P3—C33 | 1.833 (2) | C81—C82 | 1.386 (4) |
P4—C51 | 1.825 (2) | C81—H81 | 0.9500 |
P4—C45 | 1.828 (2) | C82—C83 | 1.378 (4) |
P4—C32 | 1.839 (2) | C82—H82 | 0.9500 |
C31—C32 | 1.528 (3) | C83—C84 | 1.393 (3) |
C31—H31A | 0.9900 | C83—H83 | 0.9500 |
C31—H31B | 0.9900 | C84—H84 | 0.9500 |
C32—H32A | 0.9900 | N2—C93 | 1.147 (6) |
C32—H32B | 0.9900 | C93—C94 | 1.465 (7) |
C33—C38 | 1.389 (3) | C94—H94A | 0.9800 |
C33—C34 | 1.389 (3) | C94—H94B | 0.9800 |
C34—C35 | 1.392 (3) | C94—H94C | 0.9800 |
C34—H34 | 0.9500 | N3—C95 | 1.129 (6) |
C35—C36 | 1.375 (4) | C95—C96 | 1.408 (7) |
C35—H35 | 0.9500 | C96—H96A | 0.9800 |
C36—C37 | 1.375 (4) | C96—H96B | 0.9800 |
C36—H36 | 0.9500 | C96—H96C | 0.9800 |
N1—Mo1—Cl1 | 178.20 (7) | C38—C33—P3 | 119.92 (17) |
N1—Mo1—P4 | 94.16 (8) | C34—C33—P3 | 121.44 (17) |
Cl1—Mo1—P4 | 84.136 (19) | C33—C34—C35 | 120.3 (2) |
N1—Mo1—P3 | 91.98 (10) | C33—C34—H34 | 119.9 |
Cl1—Mo1—P3 | 88.31 (2) | C35—C34—H34 | 119.9 |
P4—Mo1—P3 | 79.981 (19) | C36—C35—C34 | 120.6 (2) |
N1—Mo1—P2 | 92.57 (10) | C36—C35—H35 | 119.7 |
Cl1—Mo1—P2 | 87.16 (2) | C34—C35—H35 | 119.7 |
P4—Mo1—P2 | 100.388 (19) | C35—C36—C37 | 119.6 (2) |
P3—Mo1—P2 | 175.395 (18) | C35—C36—H36 | 120.2 |
N1—Mo1—P1 | 96.28 (8) | C37—C36—H36 | 120.2 |
Cl1—Mo1—P1 | 85.432 (19) | C36—C37—C38 | 120.2 (2) |
P4—Mo1—P1 | 169.537 (17) | C36—C37—H37 | 119.9 |
P3—Mo1—P1 | 98.915 (18) | C38—C37—H37 | 119.9 |
P2—Mo1—P1 | 79.879 (18) | C37—C38—C33 | 120.9 (2) |
C91—N1—C91' | 44.9 (3) | C37—C38—H38 | 119.6 |
C91—N1—Mo1 | 162.0 (3) | C33—C38—H38 | 119.6 |
C91'—N1—Mo1 | 152.9 (3) | C44—C39—C40 | 118.8 (2) |
N1—C91—C92 | 104.7 (3) | C44—C39—P3 | 118.66 (16) |
N1—C91—H91A | 110.8 | C40—C39—P3 | 122.54 (17) |
C92—C91—H91A | 110.8 | C41—C40—C39 | 120.1 (2) |
N1—C91—H91B | 110.8 | C41—C40—H40 | 119.9 |
C92—C91—H91B | 110.8 | C39—C40—H40 | 119.9 |
H91A—C91—H91B | 108.9 | C42—C41—C40 | 120.7 (2) |
C91—C92—H92A | 109.5 | C42—C41—H41 | 119.6 |
C91—C92—H92B | 109.5 | C40—C41—H41 | 119.6 |
H92A—C92—H92B | 109.5 | C41—C42—C43 | 119.6 (2) |
C91—C92—H92C | 109.5 | C41—C42—H42 | 120.2 |
H92A—C92—H92C | 109.5 | C43—C42—H42 | 120.2 |
H92B—C92—H92C | 109.5 | C44—C43—C42 | 119.9 (2) |
N1—C91'—C92' | 102.3 (5) | C44—C43—H43 | 120.1 |
N1—C91'—H91C | 111.3 | C42—C43—H43 | 120.1 |
C92'—C91'—H91C | 111.3 | C43—C44—C39 | 120.9 (2) |
N1—C91'—H91D | 111.3 | C43—C44—H44 | 119.6 |
C92'—C91'—H91D | 111.3 | C39—C44—H44 | 119.6 |
H91C—C91'—H91D | 109.2 | C50—C45—C46 | 118.9 (2) |
C91'—C92'—H92D | 109.5 | C50—C45—P4 | 121.23 (17) |
C91'—C92'—H92E | 109.5 | C46—C45—P4 | 119.65 (17) |
H92D—C92'—H92E | 109.5 | C47—C46—C45 | 120.2 (2) |
C91'—C92'—H92F | 109.5 | C47—C46—H46 | 119.9 |
H92D—C92'—H92F | 109.5 | C45—C46—H46 | 119.9 |
H92E—C92'—H92F | 109.5 | C46—C47—C48 | 120.7 (2) |
C3—P1—C9 | 102.30 (10) | C46—C47—H47 | 119.6 |
C3—P1—C1 | 102.27 (10) | C48—C47—H47 | 119.6 |
C9—P1—C1 | 102.22 (11) | C49—C48—C47 | 119.5 (2) |
C3—P1—Mo1 | 122.78 (7) | C49—C48—H48 | 120.2 |
C9—P1—Mo1 | 117.84 (7) | C47—C48—H48 | 120.2 |
C1—P1—Mo1 | 106.64 (7) | C48—C49—C50 | 120.3 (2) |
C15—P2—C2 | 104.69 (11) | C48—C49—H49 | 119.9 |
C15—P2—C21 | 100.46 (10) | C50—C49—H49 | 119.9 |
C2—P2—C21 | 103.10 (10) | C45—C50—C49 | 120.4 (2) |
C15—P2—Mo1 | 120.59 (8) | C45—C50—H50 | 119.8 |
C2—P2—Mo1 | 103.77 (8) | C49—C50—H50 | 119.8 |
C21—P2—Mo1 | 121.91 (7) | C52—C51—C56 | 119.0 (2) |
C2—C1—P1 | 109.72 (15) | C52—C51—P4 | 118.34 (17) |
C2—C1—H1A | 109.7 | C56—C51—P4 | 122.5 (2) |
P1—C1—H1A | 109.7 | C53—C52—C51 | 120.5 (2) |
C2—C1—H1B | 109.7 | C53—C52—H52 | 119.7 |
P1—C1—H1B | 109.7 | C51—C52—H52 | 119.7 |
H1A—C1—H1B | 108.2 | C54—C53—C52 | 119.8 (3) |
C1—C2—P2 | 109.03 (15) | C54—C53—H53 | 120.1 |
C1—C2—H2A | 109.9 | C52—C53—H53 | 120.1 |
P2—C2—H2A | 109.9 | C55—C54—C53 | 120.2 (2) |
C1—C2—H2B | 109.9 | C55—C54—H54 | 119.9 |
P2—C2—H2B | 109.9 | C53—C54—H54 | 119.9 |
H2A—C2—H2B | 108.3 | C54—C55—C56 | 120.8 (3) |
C8—C3—C4 | 119.1 (2) | C54—C55—H55 | 119.6 |
C8—C3—P1 | 120.41 (17) | C56—C55—H55 | 119.6 |
C4—C3—P1 | 120.47 (16) | C55—C56—C51 | 119.6 (3) |
C5—C4—C3 | 120.1 (2) | C55—C56—H56 | 120.2 |
C5—C4—H4 | 119.9 | C51—C56—H56 | 120.2 |
C3—C4—H4 | 119.9 | C79—B1—C67 | 110.70 (17) |
C6—C5—C4 | 120.1 (2) | C79—B1—C73 | 111.75 (17) |
C6—C5—H5 | 120.0 | C67—B1—C73 | 105.93 (16) |
C4—C5—H5 | 120.0 | C79—B1—C61 | 105.59 (16) |
C5—C6—C7 | 120.3 (2) | C67—B1—C61 | 111.88 (17) |
C5—C6—H6 | 119.9 | C73—B1—C61 | 111.11 (17) |
C7—C6—H6 | 119.9 | C62—C61—C66 | 115.1 (2) |
C6—C7—C8 | 120.2 (2) | C62—C61—B1 | 124.99 (19) |
C6—C7—H7 | 119.9 | C66—C61—B1 | 119.80 (19) |
C8—C7—H7 | 119.9 | C61—C62—C63 | 122.6 (2) |
C7—C8—C3 | 120.2 (2) | C61—C62—H62 | 118.7 |
C7—C8—H8 | 119.9 | C63—C62—H62 | 118.7 |
C3—C8—H8 | 119.9 | C64—C63—C62 | 120.5 (2) |
C10—C9—C14 | 118.6 (2) | C64—C63—H63 | 119.8 |
C10—C9—P1 | 120.90 (16) | C62—C63—H63 | 119.8 |
C14—C9—P1 | 120.43 (17) | C63—C64—C65 | 118.8 (2) |
C9—C10—C11 | 120.5 (2) | C63—C64—H64 | 120.6 |
C9—C10—H10 | 119.8 | C65—C64—H64 | 120.6 |
C11—C10—H10 | 119.8 | C64—C65—C66 | 120.2 (2) |
C12—C11—C10 | 120.1 (2) | C64—C65—H65 | 119.9 |
C12—C11—H11 | 119.9 | C66—C65—H65 | 119.9 |
C10—C11—H11 | 119.9 | C65—C66—C61 | 122.8 (2) |
C13—C12—C11 | 119.9 (2) | C65—C66—H66 | 118.6 |
C13—C12—H12 | 120.0 | C61—C66—H66 | 118.6 |
C11—C12—H12 | 120.0 | C72—C67—C68 | 115.5 (2) |
C12—C13—C14 | 120.0 (2) | C72—C67—B1 | 125.79 (19) |
C12—C13—H13 | 120.0 | C68—C67—B1 | 118.65 (19) |
C14—C13—H13 | 120.0 | C69—C68—C67 | 122.8 (2) |
C13—C14—C9 | 120.8 (2) | C69—C68—H68 | 118.6 |
C13—C14—H14 | 119.6 | C67—C68—H68 | 118.6 |
C9—C14—H14 | 119.6 | C70—C69—C68 | 119.7 (2) |
C20—C15—C16 | 118.9 (2) | C70—C69—H69 | 120.2 |
C20—C15—P2 | 119.25 (17) | C68—C69—H69 | 120.2 |
C16—C15—P2 | 121.66 (19) | C69—C70—C71 | 119.5 (2) |
C17—C16—C15 | 119.9 (3) | C69—C70—H70 | 120.2 |
C17—C16—H16 | 120.1 | C71—C70—H70 | 120.2 |
C15—C16—H16 | 120.1 | C70—C71—C72 | 120.2 (2) |
C18—C17—C16 | 120.7 (3) | C70—C71—H71 | 119.9 |
C18—C17—H17 | 119.6 | C72—C71—H71 | 119.9 |
C16—C17—H17 | 119.6 | C67—C72—C71 | 122.2 (2) |
C17—C18—C19 | 120.2 (3) | C67—C72—H72 | 118.9 |
C17—C18—H18 | 119.9 | C71—C72—H72 | 118.9 |
C19—C18—H18 | 119.9 | C78—C73—C74 | 115.3 (2) |
C18—C19—C20 | 119.2 (3) | C78—C73—B1 | 124.84 (19) |
C18—C19—H19 | 120.4 | C74—C73—B1 | 119.84 (19) |
C20—C19—H19 | 120.4 | C75—C74—C73 | 122.8 (2) |
C15—C20—C19 | 121.0 (2) | C75—C74—H74 | 118.6 |
C15—C20—H20 | 119.5 | C73—C74—H74 | 118.6 |
C19—C20—H20 | 119.5 | C76—C75—C74 | 120.1 (2) |
C26—C21—C22 | 119.1 (2) | C76—C75—H75 | 119.9 |
C26—C21—P2 | 121.87 (18) | C74—C75—H75 | 120.0 |
C22—C21—P2 | 118.99 (18) | C75—C76—C77 | 118.8 (2) |
C23—C22—C21 | 120.7 (3) | C75—C76—H76 | 120.6 |
C23—C22—H22 | 119.7 | C77—C76—H76 | 120.6 |
C21—C22—H22 | 119.7 | C76—C77—C78 | 120.4 (2) |
C24—C23—C22 | 119.7 (3) | C76—C77—H77 | 119.8 |
C24—C23—H23 | 120.1 | C78—C77—H77 | 119.8 |
C22—C23—H23 | 120.1 | C73—C78—C77 | 122.5 (2) |
C25—C24—C23 | 120.0 (3) | C73—C78—H78 | 118.7 |
C25—C24—H24 | 120.0 | C77—C78—H78 | 118.7 |
C23—C24—H24 | 120.0 | C84—C79—C80 | 115.0 (2) |
C24—C25—C26 | 120.7 (3) | C84—C79—B1 | 125.00 (18) |
C24—C25—H25 | 119.7 | C80—C79—B1 | 119.97 (18) |
C26—C25—H25 | 119.7 | C81—C80—C79 | 122.7 (2) |
C21—C26—C25 | 119.7 (3) | C81—C80—H80 | 118.7 |
C21—C26—H26 | 120.1 | C79—C80—H80 | 118.7 |
C25—C26—H26 | 120.1 | C82—C81—C80 | 120.3 (2) |
C39—P3—C31 | 104.53 (10) | C82—C81—H81 | 119.8 |
C39—P3—C33 | 101.42 (10) | C80—C81—H81 | 119.8 |
C31—P3—C33 | 103.45 (11) | C83—C82—C81 | 118.9 (2) |
C39—P3—Mo1 | 118.30 (7) | C83—C82—H82 | 120.5 |
C31—P3—Mo1 | 105.12 (8) | C81—C82—H82 | 120.5 |
C33—P3—Mo1 | 121.96 (7) | C82—C83—C84 | 120.1 (2) |
C51—P4—C45 | 102.66 (10) | C82—C83—H83 | 120.0 |
C51—P4—C32 | 104.39 (11) | C84—C83—H83 | 120.0 |
C45—P4—C32 | 103.92 (10) | C83—C84—C79 | 123.0 (2) |
C51—P4—Mo1 | 114.87 (7) | C83—C84—H84 | 118.5 |
C45—P4—Mo1 | 122.99 (7) | C79—C84—H84 | 118.5 |
C32—P4—Mo1 | 106.16 (8) | N2—C93—C94 | 178.7 (6) |
C32—C31—P3 | 108.33 (15) | C93—C94—H94A | 109.5 |
C32—C31—H31A | 110.0 | C93—C94—H94B | 109.5 |
P3—C31—H31A | 110.0 | H94A—C94—H94B | 109.5 |
C32—C31—H31B | 110.0 | C93—C94—H94C | 109.5 |
P3—C31—H31B | 110.0 | H94A—C94—H94C | 109.5 |
H31A—C31—H31B | 108.4 | H94B—C94—H94C | 109.5 |
C31—C32—P4 | 108.95 (16) | N3—C95—C96 | 173.9 (7) |
C31—C32—H32A | 109.9 | C95—C96—H96A | 109.5 |
P4—C32—H32A | 109.9 | C95—C96—H96B | 109.5 |
C31—C32—H32B | 109.9 | H96A—C96—H96B | 109.5 |
P4—C32—H32B | 109.9 | C95—C96—H96C | 109.5 |
H32A—C32—H32B | 108.3 | H96A—C96—H96C | 109.5 |
C38—C33—C34 | 118.4 (2) | H96B—C96—H96C | 109.5 |
Experimental details
Crystal data | |
Chemical formula | [Mo(C2H5N)Cl(C26H24P2)2](C24H20B)·2C2H3N |
Mr | 1372.56 |
Crystal system, space group | Monoclinic, P21/n |
Temperature (K) | 170 |
a, b, c (Å) | 15.3299 (12), 21.5840 (11), 21.3439 (16) |
β (°) | 96.387 (9) |
V (Å3) | 7018.4 (8) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 0.36 |
Crystal size (mm) | 0.2 × 0.15 × 0.1 |
Data collection | |
Diffractometer | Stoe IPDS1 |
Absorption correction | Numerical (X-SHAPE; Stoe & Cie, 1998) |
Tmin, Tmax | 0.929, 0.941 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 48449, 15159, 12034 |
Rint | 0.043 |
(sin θ/λ)max (Å−1) | 0.639 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.037, 0.101, 1.01 |
No. of reflections | 15159 |
No. of parameters | 850 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.62, −0.68 |
Computer programs: IPDS Program Package (Stoe & Cie, 1998), IPDS Program Package, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), XP in SHELXTL (Bruker, 1998), CIFTAB in SHELXTL.
Mo1—N1 | 1.732 (2) | Mo1—P3 | 2.5342 (6) |
Mo1—Cl1 | 2.4413 (5) | Mo1—P2 | 2.5447 (6) |
Mo1—P4 | 2.5308 (6) | Mo1—P1 | 2.5503 (6) |
N1—Mo1—Cl1 | 178.20 (7) | P4—Mo1—P2 | 100.388 (19) |
N1—Mo1—P4 | 94.16 (8) | P3—Mo1—P2 | 175.395 (18) |
Cl1—Mo1—P4 | 84.136 (19) | N1—Mo1—P1 | 96.28 (8) |
N1—Mo1—P3 | 91.98 (10) | Cl1—Mo1—P1 | 85.432 (19) |
Cl1—Mo1—P3 | 88.31 (2) | P4—Mo1—P1 | 169.537 (17) |
P4—Mo1—P3 | 79.981 (19) | P3—Mo1—P1 | 98.915 (18) |
N1—Mo1—P2 | 92.57 (10) | P2—Mo1—P1 | 79.879 (18) |
Cl1—Mo1—P2 | 87.16 (2) |
The structure determination of this compound was undertaken as part of a project on the asymmetric reduction of dinitrogen via the Chatt cycle (Mersmann et al., 2006). Imido complexes are problematic intermediates in this cycle because of their very negative reduction potentials (Alias et al., 1997). For practical reasons it is instructive to study alkylimido complexes. During these investigations we obtained big crystals of the title compound in order to perform polarized absorption spectroscopy. An absoption band at 510 nm possesses unexpected differences in intensity under polarization along the a- and b axis of this molecule. Furthermore a vibrational fine structure of about 530 cm-1 was observed on the absorption band, which is attributed to a Mo—N—C bending vibration.
The crystal structure of the title compound consists of discrete [Mo(Cl)(NC2H5)(P2C26H24)2]+ cations and tetraphenylborate anions. The molybdenum atoms are coordinated by four phosphorous atoms of two crystallographically independent 1,2-bis(diphenylphosphino)ethane ligands, one nitrogen atom of an ethylimido ligand and one chlorine atom within distorted octahedra (Fig. 1). All bond lengths and angles are in good agreement with those retrieved from the CSD database (conquest version 1.8, 2007; Bruno et al., 2002) The Mo1—N1 bond lengths of 1.732 (2) Å strongly indicate that this is a Mo—N triple bond. There are two additional acetonitrile ligands per formula unit within the structure, that are located in holes of the crystal. These solvent molecules exhibit slightly enlarged anisotropic displacement parameters indicating some static or dynamic disorder.