metal-organic compounds
Tetracarbonyl[N-(diphenylphosphanyl-κP)-N,N′-diisopropyl-P-phenylphosphorus diamide-κP]molybdenum(0) with an unknown solvent
aLeibniz-Institut für Katalyse e. V. an der Universität Rostock, Albert-Einstein-Str. 29a, 18059 Rostock, Germany
*Correspondence e-mail: uwe.rosenthal@catalysis.de
The title complex, [Mo(C24H30N2P2)(CO)4], contains a molybdenum centre bearing a P,P′-cis-chelating Ph2PN(iPr)P(Ph)NH(iPr) and four carbonyl ligands in a distorted octahedral coordination geometry. This results in a nearly planar four-membered metallacycle. In the crystal, molecules are linked by N—H⋯O and C—H⋯O hydrogen bonds to form layers parallel to the ac plane. For the final the contributions of disordered solvent molecules were removed from the diffraction data with SQUEEZE in PLATON [Spek (2015). Acta Cryst. C71, 9–18]. The given chemical formula and other crystal data do not take into account the unknown solvent molecule(s).
Keywords: crystal structure; molybdenum; diphosphazane.
CCDC reference: 1848117
Structure description
The title complex (Fig. 1) contains a molybdenum centre coordinated to a P,P′-cis-chelating Ph2PN(iPr)P(Ph)NH(iPr) ligand and four carbonyl ligands in a distorted octahedral geometry, forming a nearly planar four-membered Mo—P—N—P metallacycle (r.m.s. deviation for Mo1, P1, N1, P2 = 0.053 Å). The P—Mo—P bite angle amounts to 64.948 (13)° and complies with those in comparable [Mo(CO)4{Ph2PN(R)PPh2}] (R ≠ H) complexes [range from 64.38 (8) to 66.14 (3)°; Al-Masri et al., 2013; Biricik et al., 2003; Gaw et al., 2000, 2002; Majoumo et al., 2004; Majoumo-Mbe et al., 2015; Payne et al., 1965] and is slightly smaller than that found in the analogous chromium complex [P—Cr—P = 67.90 (2), 67.95 (12)°] published by Aluri et al. (2010) and Dulai et al. (2011). As a result of the ring strain, the P—N—P bond angle [103.10 (6)°] is clearly smaller than that observed in the uncoordinated Ph2PN(iPr)P(Ph)NH(iPr) molecule [121.53 (11)°; Peitz et al., 2010] but conforms with comparable [Mo(CO)4{Ph2PN(R)PPh2}] (R ≠ H) complexes (Al-Masri et al., 2013; Biricik et al., 2003; Gaw et al., 2000, 2002; Majoumo et al., 2004; Majoumo-Mbe et al., 2015; Payne et al., 1965). The P—N bond lengths [range from 1.6462 (13) to 1.7185 (13) Å] are noticeably shortened compared to the calculated sum of the covalent radii by Pyykkö [single: Σrcov(P—N) = 1.82 Å; Pyykkö, 2015] and show some multiple-bond character [double: Σrcov(P=N) = 1.62 Å; Pyykkö, 2015]. Consistent with this geometry, the central N1 atom is nearly trigonal planar [Σ(∠N1) = 359°]. The Mo—P distances are slightly different [Mo1—P1 = 2.4731 (5), Mo1—P2 = 2.5056 (6) Å], which might be an effect of the asymmetric P,P′-cis-ligating Ph2PN(iPr)P(Ph)NH(iPr) ligand.
In the crystal, N—H⋯O and C—H⋯O hydrogen bonds (Table 1) link the molecules into layers parallel to the ac plane.
Synthesis and crystallization
Mo(CO)4(pip)2 (pip = piperidine; 0.99 g, 2.617 mmol) and Ph2PN(iPr)P(Ph)NH(iPr) (1.305 g, 3.193 mmol), were dissolved in CH2Cl2 (30 ml) at r.t. After 2 h of refluxing, 20 ml CH2Cl2 was removed in vacuo. Ethanol (15 ml) was added and the solution was cooled. The white solid was washed with n-hexane at −78°C and dried under vacuum. Yield 1.45 g (90%). Crystals were obtained from a saturated CH2Cl2/EtOH solution at −78°C.
1H NMR (300 MHz, C6D6, 298 K): δ (p.p.m.) 7.95–7.88 (m, 2H, ArH), 7.69–7.53 (m, 4H, ArH), 7.14–6.98 (m, 9H, ArH), 4.17 (m, 1H, CHCH3), 3.31 (m, 1H, CHCH3), 2.19 (t, 1H, NH), 1.22 (d, 3JH,H = 6.5 Hz, 3H, CHCH3), 1.15 (d, 3JH,H = 6.4 Hz, 3H, CHCH3), 0.89 (d, J = 6.7 Hz, 3H, CHCH3), 0.38 (d, 3JH,H = 6.7 Hz, 3H, CHCH3). 13C NMR (100 MHz, C6D6, 298 K): δ (p.p.m.) 219.7 (m, CO), 212.4 (m, CO), 141.7, 141.0, 138.7, 138.2, 136.2, 138.8, 133.8, 131.3, 130.8, 130.0, 128.9, 128.7, 128.5 (ArC), 55.7 (t, 2JP,C = 6.0 Hz, CHCH3), 49.3 (d, 2JP,C = 18.0 Hz, CHCH3), 26.3 (d, 3JP,C = 4.5 Hz, CHCH3), 25.6 (d, 3JP,C = 4.5 Hz, CHCH3), 24.3 (br s, CHCH3) 24.2 (br s, CHCH3). 31P NMR (121 MHz, CD2Cl2, 298 K): δ = 96.7 (d, 2JPP = 8.7 Hz), 80.2 (d, 2JPP = 8.7 Hz). Elemental analysis calcd. (%) for C28H30MoN2O4P2 (616.44): C 54.56, H 4.91, N 4.54. Found: C 55.42, H 4.96, N 4.65. IR (CH2Cl2, cm−1): ν (CO) 1870, 1896, 1918, 2005. M.p. 180°C (dec.).
Refinement
Crystal data, data collection and structure . Six outliers (4 0 10, 6 3 4, 1 2 11, 5 7 4, 1 2 8, 2 3 8) were omitted in the last cycles of For the final the contributions of disordered solvent molecules were removed from the diffraction data with SQUEEZE in PLATON (Spek, 2015). SQUEEZE estimated the electron counts in each of the four voids of 111 and 112 Å3, respectively to be 34.
details are summarized in Table 2Structural data
CCDC reference: 1848117
https://doi.org/10.1107/S2414314618008465/rz4024sup1.cif
contains datablock I. DOI:Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S2414314618008465/rz4024Isup2.hkl
Data collection: X-AREA (Stoe & Cie, 2005); cell
X-AREA (Stoe & Cie, 2005); data reduction: X-AREA (Stoe & Cie, 2005); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL2014 (Sheldrick, 2015); molecular graphics: XP in SHELXTL (Sheldrick, 2008); software used to prepare material for publication: publCIF (Westrip, 2010).[Mo(C24H30N2P2)(CO)4] | Dx = 1.365 Mg m−3 |
Mr = 616.42 | Mo Kα radiation, λ = 0.71073 Å |
Orthorhombic, Pbca | Cell parameters from 11600 reflections |
a = 15.634 (3) Å | θ = 1.8–29.7° |
b = 17.716 (4) Å | µ = 0.58 mm−1 |
c = 21.661 (4) Å | T = 150 K |
V = 5999 (2) Å3 | Prism, colourless |
Z = 8 | 0.46 × 0.38 × 0.36 mm |
F(000) = 2528 |
Stoe IPDS II diffractometer | 6886 independent reflections |
Radiation source: fine-focus sealed tube | 5657 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.041 |
ω scans | θmax = 27.5°, θmin = 1.9° |
Absorption correction: numerical (X-SHAPE and X-RED32; Stoe & Cie, 2005) | h = −20→20 |
Tmin = 0.75, Tmax = 0.89 | k = −22→23 |
95647 measured reflections | l = −28→28 |
Refinement on F2 | 1 restraint |
Least-squares matrix: full | Hydrogen site location: mixed |
R[F2 > 2σ(F2)] = 0.022 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.050 | w = 1/[σ2(Fo2) + (0.0338P)2] where P = (Fo2 + 2Fc2)/3 |
S = 0.92 | (Δ/σ)max = 0.002 |
6886 reflections | Δρmax = 0.38 e Å−3 |
342 parameters | Δρmin = −0.31 e Å−3 |
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. |
Refinement. The N-bound H atom was located in a difference Fourier map and refined with the N–H distance constrained to be 0.87 Å. All other H atoms were placed geometrically and refined using a riding atom approximation, with C–H = 0.95–1.00 Å, and with Uiso(H) = 1.2Ueq(C) or 1.5Ueq(C) for methyl H atoms. A rotating model was used for the methyl groups. |
x | y | z | Uiso*/Ueq | ||
C1 | 0.34111 (9) | 0.15827 (8) | 0.28181 (6) | 0.0269 (3) | |
C2 | 0.28472 (9) | 0.07619 (8) | 0.38433 (7) | 0.0271 (3) | |
C3 | 0.44531 (9) | 0.01870 (8) | 0.40890 (7) | 0.0262 (3) | |
C4 | 0.40591 (9) | 0.01114 (9) | 0.28804 (7) | 0.0288 (3) | |
C5 | 0.40138 (9) | 0.22378 (9) | 0.48935 (7) | 0.0287 (3) | |
C6 | 0.39750 (10) | 0.15799 (10) | 0.52376 (7) | 0.0343 (3) | |
H6 | 0.4040 | 0.1106 | 0.5037 | 0.041* | |
C7 | 0.38431 (11) | 0.16021 (11) | 0.58705 (8) | 0.0416 (4) | |
H7 | 0.3828 | 0.1147 | 0.6102 | 0.050* | |
C8 | 0.37339 (12) | 0.22824 (12) | 0.61608 (8) | 0.0450 (4) | |
H8 | 0.3645 | 0.2299 | 0.6594 | 0.054* | |
C9 | 0.37530 (12) | 0.29434 (12) | 0.58244 (9) | 0.0487 (5) | |
H9 | 0.3665 | 0.3413 | 0.6026 | 0.058* | |
C10 | 0.38998 (11) | 0.29266 (10) | 0.51939 (8) | 0.0399 (4) | |
H10 | 0.3923 | 0.3384 | 0.4966 | 0.048* | |
C11 | 0.37638 (9) | 0.29940 (8) | 0.37296 (7) | 0.0271 (3) | |
C12 | 0.29425 (10) | 0.32308 (9) | 0.38861 (7) | 0.0314 (3) | |
H12 | 0.2642 | 0.2987 | 0.4211 | 0.038* | |
C13 | 0.25641 (11) | 0.38204 (9) | 0.35696 (8) | 0.0372 (4) | |
H13 | 0.2006 | 0.3983 | 0.3681 | 0.045* | |
C14 | 0.29902 (12) | 0.41738 (9) | 0.30934 (9) | 0.0417 (4) | |
H14 | 0.2726 | 0.4578 | 0.2878 | 0.050* | |
C15 | 0.38000 (12) | 0.39387 (10) | 0.29309 (9) | 0.0432 (4) | |
H15 | 0.4095 | 0.4182 | 0.2603 | 0.052* | |
C16 | 0.41847 (10) | 0.33487 (9) | 0.32456 (8) | 0.0354 (4) | |
H16 | 0.4741 | 0.3186 | 0.3129 | 0.042* | |
C17 | 0.63680 (9) | 0.09612 (8) | 0.37610 (6) | 0.0241 (3) | |
C18 | 0.64070 (10) | 0.08548 (8) | 0.43972 (7) | 0.0290 (3) | |
H18 | 0.5987 | 0.1080 | 0.4655 | 0.035* | |
C19 | 0.70499 (11) | 0.04247 (9) | 0.46573 (8) | 0.0361 (3) | |
H19 | 0.7077 | 0.0364 | 0.5093 | 0.043* | |
C20 | 0.76512 (11) | 0.00839 (9) | 0.42858 (8) | 0.0394 (4) | |
H20 | 0.8094 | −0.0210 | 0.4466 | 0.047* | |
C21 | 0.76123 (11) | 0.01667 (10) | 0.36556 (8) | 0.0394 (4) | |
H21 | 0.8025 | −0.0074 | 0.3401 | 0.047* | |
C22 | 0.69701 (10) | 0.06027 (9) | 0.33895 (7) | 0.0310 (3) | |
H22 | 0.6943 | 0.0656 | 0.2954 | 0.037* | |
C23 | 0.54833 (10) | 0.19268 (10) | 0.21953 (7) | 0.0363 (4) | |
H23 | 0.4871 | 0.2051 | 0.2283 | 0.044* | |
C24 | 0.55048 (17) | 0.12180 (16) | 0.18082 (10) | 0.0691 (7) | |
H24A | 0.6100 | 0.1082 | 0.1720 | 0.104* | |
H24B | 0.5201 | 0.1307 | 0.1419 | 0.104* | |
H24C | 0.5228 | 0.0806 | 0.2034 | 0.104* | |
C25 | 0.58778 (15) | 0.25923 (16) | 0.18724 (11) | 0.0718 (8) | |
H25A | 0.5816 | 0.3043 | 0.2130 | 0.108* | |
H25B | 0.5589 | 0.2674 | 0.1477 | 0.108* | |
H25C | 0.6486 | 0.2494 | 0.1800 | 0.108* | |
C26 | 0.58322 (10) | 0.28343 (9) | 0.41876 (9) | 0.0395 (4) | |
H26 | 0.5443 | 0.3277 | 0.4244 | 0.047* | |
C27 | 0.62182 (13) | 0.26694 (12) | 0.48171 (10) | 0.0537 (5) | |
H27A | 0.5774 | 0.2472 | 0.5093 | 0.081* | |
H27B | 0.6454 | 0.3135 | 0.4991 | 0.081* | |
H27C | 0.6675 | 0.2295 | 0.4774 | 0.081* | |
C28 | 0.65060 (13) | 0.30750 (11) | 0.37253 (11) | 0.0554 (5) | |
H28A | 0.6886 | 0.2648 | 0.3637 | 0.083* | |
H28B | 0.6841 | 0.3493 | 0.3897 | 0.083* | |
H28C | 0.6227 | 0.3239 | 0.3343 | 0.083* | |
N1 | 0.52898 (7) | 0.22025 (7) | 0.39514 (6) | 0.0271 (3) | |
N2 | 0.59168 (8) | 0.18048 (8) | 0.27863 (6) | 0.0332 (3) | |
O1 | 0.30266 (7) | 0.18956 (7) | 0.24502 (5) | 0.0397 (3) | |
O2 | 0.22161 (7) | 0.06770 (8) | 0.41024 (6) | 0.0427 (3) | |
O3 | 0.46686 (8) | −0.03061 (7) | 0.43865 (5) | 0.0418 (3) | |
O4 | 0.41082 (8) | −0.03731 (7) | 0.25315 (6) | 0.0459 (3) | |
P1 | 0.42203 (2) | 0.21436 (2) | 0.40705 (2) | 0.02325 (7) | |
P2 | 0.54809 (2) | 0.14920 (2) | 0.34291 (2) | 0.02225 (7) | |
Mo1 | 0.39963 (2) | 0.09633 (2) | 0.34827 (2) | 0.01978 (4) | |
H2 | 0.6430 (9) | 0.1912 (10) | 0.2777 (8) | 0.035 (5)* |
U11 | U22 | U33 | U12 | U13 | U23 | |
C1 | 0.0232 (7) | 0.0302 (8) | 0.0274 (7) | −0.0046 (6) | −0.0005 (6) | 0.0038 (6) |
C2 | 0.0247 (7) | 0.0285 (7) | 0.0282 (7) | 0.0004 (6) | −0.0026 (6) | 0.0055 (6) |
C3 | 0.0255 (7) | 0.0273 (7) | 0.0257 (7) | −0.0001 (6) | 0.0015 (6) | 0.0007 (6) |
C4 | 0.0266 (7) | 0.0304 (7) | 0.0294 (7) | −0.0012 (6) | −0.0011 (6) | −0.0013 (6) |
C5 | 0.0259 (7) | 0.0305 (8) | 0.0295 (7) | 0.0043 (6) | −0.0041 (6) | −0.0062 (6) |
C6 | 0.0389 (8) | 0.0350 (8) | 0.0291 (7) | 0.0049 (7) | −0.0004 (7) | −0.0050 (6) |
C7 | 0.0453 (10) | 0.0508 (11) | 0.0286 (8) | 0.0027 (8) | 0.0016 (7) | −0.0017 (7) |
C8 | 0.0393 (9) | 0.0657 (13) | 0.0301 (8) | 0.0075 (9) | −0.0017 (7) | −0.0139 (8) |
C9 | 0.0477 (10) | 0.0526 (12) | 0.0458 (10) | 0.0118 (9) | −0.0071 (8) | −0.0274 (9) |
C10 | 0.0431 (9) | 0.0341 (9) | 0.0425 (9) | 0.0051 (7) | −0.0070 (7) | −0.0109 (7) |
C11 | 0.0258 (7) | 0.0204 (7) | 0.0349 (7) | 0.0008 (5) | −0.0041 (6) | −0.0011 (6) |
C12 | 0.0273 (7) | 0.0270 (7) | 0.0399 (8) | 0.0027 (6) | −0.0009 (6) | −0.0010 (6) |
C13 | 0.0295 (8) | 0.0307 (8) | 0.0515 (10) | 0.0083 (6) | −0.0031 (7) | −0.0012 (7) |
C14 | 0.0414 (9) | 0.0284 (8) | 0.0552 (10) | 0.0087 (7) | −0.0069 (8) | 0.0095 (7) |
C15 | 0.0405 (9) | 0.0364 (9) | 0.0528 (10) | 0.0021 (7) | 0.0022 (8) | 0.0156 (8) |
C16 | 0.0277 (8) | 0.0313 (8) | 0.0471 (9) | 0.0032 (6) | 0.0017 (7) | 0.0065 (7) |
C17 | 0.0213 (6) | 0.0214 (6) | 0.0297 (7) | −0.0012 (6) | −0.0017 (5) | 0.0022 (6) |
C18 | 0.0285 (7) | 0.0285 (8) | 0.0302 (7) | 0.0021 (6) | −0.0009 (6) | 0.0021 (6) |
C19 | 0.0391 (9) | 0.0347 (8) | 0.0345 (8) | 0.0026 (7) | −0.0082 (7) | 0.0071 (7) |
C20 | 0.0328 (8) | 0.0316 (8) | 0.0540 (10) | 0.0085 (7) | −0.0092 (7) | 0.0082 (8) |
C21 | 0.0334 (8) | 0.0338 (8) | 0.0510 (10) | 0.0109 (7) | 0.0071 (7) | 0.0024 (7) |
C22 | 0.0312 (8) | 0.0291 (8) | 0.0325 (8) | 0.0028 (6) | 0.0032 (6) | 0.0015 (6) |
C23 | 0.0271 (8) | 0.0521 (10) | 0.0297 (8) | 0.0028 (7) | 0.0024 (6) | 0.0148 (7) |
C24 | 0.0814 (17) | 0.0884 (18) | 0.0377 (11) | 0.0139 (14) | 0.0051 (11) | −0.0063 (11) |
C25 | 0.0556 (13) | 0.0973 (19) | 0.0625 (14) | −0.0232 (12) | −0.0123 (10) | 0.0524 (14) |
C26 | 0.0307 (8) | 0.0263 (8) | 0.0616 (11) | −0.0042 (6) | −0.0097 (7) | −0.0082 (8) |
C27 | 0.0471 (11) | 0.0448 (11) | 0.0692 (13) | −0.0016 (9) | −0.0272 (10) | −0.0155 (10) |
C28 | 0.0385 (10) | 0.0386 (10) | 0.0891 (16) | −0.0155 (8) | −0.0037 (10) | −0.0024 (10) |
N1 | 0.0214 (6) | 0.0224 (6) | 0.0375 (7) | −0.0001 (5) | −0.0035 (5) | −0.0027 (5) |
N2 | 0.0200 (6) | 0.0465 (8) | 0.0330 (7) | −0.0036 (6) | 0.0010 (5) | 0.0143 (6) |
O1 | 0.0351 (6) | 0.0473 (7) | 0.0368 (6) | −0.0053 (5) | −0.0095 (5) | 0.0157 (5) |
O2 | 0.0257 (6) | 0.0557 (8) | 0.0465 (7) | −0.0005 (5) | 0.0076 (5) | 0.0122 (6) |
O3 | 0.0477 (7) | 0.0373 (6) | 0.0404 (6) | 0.0068 (5) | −0.0008 (5) | 0.0144 (5) |
O4 | 0.0517 (8) | 0.0420 (7) | 0.0440 (7) | −0.0003 (6) | 0.0014 (6) | −0.0174 (6) |
P1 | 0.02145 (16) | 0.02076 (17) | 0.02755 (17) | 0.00172 (13) | −0.00178 (13) | −0.00073 (14) |
P2 | 0.01931 (16) | 0.02283 (16) | 0.02462 (16) | −0.00003 (13) | −0.00046 (13) | 0.00359 (14) |
Mo1 | 0.01891 (6) | 0.02026 (6) | 0.02017 (6) | −0.00123 (4) | −0.00037 (4) | 0.00138 (4) |
C1—O1 | 1.1417 (17) | C15—C16 | 1.385 (2) |
C1—Mo1 | 2.0282 (15) | C17—C22 | 1.392 (2) |
C2—O2 | 1.1450 (18) | C17—C18 | 1.392 (2) |
C2—Mo1 | 1.9912 (15) | C17—P2 | 1.8234 (14) |
C3—O3 | 1.1366 (18) | C18—C19 | 1.381 (2) |
C3—Mo1 | 2.0313 (15) | C19—C20 | 1.377 (2) |
C4—O4 | 1.1463 (19) | C20—C21 | 1.374 (3) |
C4—Mo1 | 1.9973 (15) | C21—C22 | 1.392 (2) |
C5—C6 | 1.385 (2) | C23—N2 | 1.4646 (19) |
C5—C10 | 1.394 (2) | C23—C25 | 1.503 (3) |
C5—P1 | 1.8194 (15) | C23—C24 | 1.510 (3) |
C6—C7 | 1.387 (2) | C26—N1 | 1.4946 (19) |
C7—C8 | 1.370 (3) | C26—C28 | 1.515 (3) |
C8—C9 | 1.380 (3) | C26—C27 | 1.520 (3) |
C9—C10 | 1.385 (3) | N1—P1 | 1.6949 (13) |
C11—C16 | 1.388 (2) | N1—P2 | 1.7185 (13) |
C11—C12 | 1.393 (2) | N2—P2 | 1.6462 (13) |
C11—P1 | 1.8232 (15) | P1—Mo1 | 2.4731 (5) |
C12—C13 | 1.382 (2) | P1—P2 | 2.6733 (6) |
C13—C14 | 1.378 (3) | P2—Mo1 | 2.5056 (6) |
C14—C15 | 1.378 (3) | ||
O1—C1—Mo1 | 174.59 (12) | C23—N2—P2 | 126.68 (11) |
O2—C2—Mo1 | 173.34 (13) | N1—P1—C5 | 108.58 (6) |
O3—C3—Mo1 | 172.36 (13) | N1—P1—C11 | 105.88 (7) |
O4—C4—Mo1 | 178.85 (14) | C5—P1—C11 | 104.57 (7) |
C6—C5—C10 | 118.67 (14) | N1—P1—Mo1 | 96.51 (4) |
C6—C5—P1 | 117.26 (11) | C5—P1—Mo1 | 123.84 (5) |
C10—C5—P1 | 124.07 (13) | C11—P1—Mo1 | 115.77 (5) |
C5—C6—C7 | 120.99 (16) | N1—P1—P2 | 38.76 (4) |
C8—C7—C6 | 119.81 (18) | C5—P1—P2 | 132.82 (5) |
C7—C8—C9 | 120.10 (16) | C11—P1—P2 | 115.78 (5) |
C8—C9—C10 | 120.40 (17) | Mo1—P1—P2 | 58.112 (14) |
C9—C10—C5 | 120.01 (17) | N2—P2—N1 | 112.48 (7) |
C16—C11—C12 | 118.98 (14) | N2—P2—C17 | 101.08 (7) |
C16—C11—P1 | 119.63 (11) | N1—P2—C17 | 104.50 (6) |
C12—C11—P1 | 120.75 (12) | N2—P2—Mo1 | 123.27 (5) |
C13—C12—C11 | 120.10 (15) | N1—P2—Mo1 | 94.72 (4) |
C14—C13—C12 | 120.49 (15) | C17—P2—Mo1 | 119.57 (5) |
C13—C14—C15 | 119.85 (15) | N2—P2—P1 | 126.83 (5) |
C14—C15—C16 | 120.07 (16) | N1—P2—P1 | 38.13 (4) |
C15—C16—C11 | 120.49 (15) | C17—P2—P1 | 125.34 (5) |
C22—C17—C18 | 118.74 (13) | Mo1—P2—P1 | 56.940 (15) |
C22—C17—P2 | 121.45 (11) | C2—Mo1—C4 | 99.51 (6) |
C18—C17—P2 | 119.57 (11) | C2—Mo1—C1 | 88.19 (6) |
C19—C18—C17 | 120.68 (15) | C4—Mo1—C1 | 88.13 (6) |
C20—C19—C18 | 120.02 (15) | C2—Mo1—C3 | 86.69 (6) |
C21—C20—C19 | 120.23 (15) | C4—Mo1—C3 | 83.89 (6) |
C20—C21—C22 | 120.17 (15) | C1—Mo1—C3 | 169.67 (6) |
C21—C22—C17 | 120.11 (14) | C2—Mo1—P1 | 94.44 (5) |
N2—C23—C25 | 109.43 (15) | C4—Mo1—P1 | 165.51 (4) |
N2—C23—C24 | 110.63 (15) | C1—Mo1—P1 | 88.39 (4) |
C25—C23—C24 | 112.62 (18) | C3—Mo1—P1 | 100.94 (4) |
N1—C26—C28 | 112.27 (15) | C2—Mo1—P2 | 157.06 (4) |
N1—C26—C27 | 112.87 (15) | C4—Mo1—P2 | 101.93 (4) |
C28—C26—C27 | 111.79 (16) | C1—Mo1—P2 | 100.52 (4) |
C26—N1—P1 | 123.61 (10) | C3—Mo1—P2 | 87.56 (4) |
C26—N1—P2 | 132.47 (11) | P1—Mo1—P2 | 64.948 (13) |
P1—N1—P2 | 103.10 (6) |
D—H···A | D—H | H···A | D···A | D—H···A |
C8—H8···O1i | 0.95 | 2.53 | 3.338 (2) | 143 |
N2—H2···O1ii | 0.83 (1) | 2.54 (1) | 3.3419 (18) | 163 (1) |
Symmetry codes: (i) x, −y+1/2, z+1/2; (ii) x+1/2, y, −z+1/2. |
Funding information
Funding for this research was provided by: Open Access Fund of the Leibniz Association.
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