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Acta Crystallogr Sect E Struct Rep Online. 2008 May 1; 64(Pt 5): m629.
Published online 2008 April 10. doi:  10.1107/S1600536808008635
PMCID: PMC2961270

[1,2-Bis(diphenyl­phosphino)ethane]{2-[bis­(diphenyl­phosphinometh­yl)amino]pyridinium}fluoridohydrazidato­molybdenum(IV) bis­(tetra­fluoridoborate)

Abstract

In the crystal structure of the title compound, [MoF(N2H2)(C31H29N2P2)(C26H24P2)](BF4)2, each Mo atom is surrounded by four P atoms of one 1,2-bis­(diphenyl­phosphino)ethane and one 2-[bis­(diphenyl­phosphinometh­yl)amino]pyridinium ligand. The remaining binding sites of the distorted octa­hedron are occupied by a hydrazidate (NNH2 2−) and a fluoride ligand. Two F atoms of an anion are disordered over two positions; the site occupancy factors are ca 0.7 and 0.3.

Related literature

For related literature, see: Hidai et al. (1976 [triangle]); Stephan et al. (2008 [triangle]).

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Object name is e-64-0m629-scheme1.jpg

Experimental

Crystal data

  • [MoF(N2H2)(C31H29N2P2)(C26H24P2)](BF4)2
  • M r = 1208.49
  • Monoclinic, An external file that holds a picture, illustration, etc.
Object name is e-64-0m629-efi1.jpg
  • a = 12.5791 (6) Å
  • b = 31.2199 (16) Å
  • c = 13.8330 (9) Å
  • β = 94.438 (7)°
  • V = 5416.2 (5) Å3
  • Z = 4
  • Mo Kα radiation
  • μ = 0.43 mm−1
  • T = 170 (2) K
  • 0.2 × 0.08 × 0.06 mm

Data collection

  • Stoe IPDS-1 diffractometer
  • Absorption correction: numerical (X-SHAPE; Stoe & Cie, 1998a [triangle]) T min = 0.949, T max = 0.969
  • 24176 measured reflections
  • 8538 independent reflections
  • 6783 reflections with I > 2σ(I)
  • R int = 0.032
  • θmax = 24.1°

Refinement

  • R[F 2 > 2σ(F 2)] = 0.039
  • wR(F 2) = 0.108
  • S = 1.02
  • 8538 reflections
  • 706 parameters
  • 39 restraints
  • H-atom parameters constrained
  • Δρmax = 0.94 e Å−3
  • Δρmin = −0.54 e Å−3

Data collection: IPDS Program package (Stoe & Cie, 1998b [triangle]); cell refinement: IPDS Program package; data reduction: IPDS Program package; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 [triangle]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 [triangle]); molecular graphics: DIAMOND (Brandenburg, 1999 [triangle]); software used to prepare material for publication: CIFTAB in SHELXTL (Sheldrick, 2008 [triangle]).

Table 1
Selected geometric parameters (Å, °)

Supplementary Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536808008635/bt2688sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808008635/bt2688Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Acknowledgments

This work is supported by the state of Schleswig-Holstein and the DFG (project number: Tu58/13–2, SPP1118).

supplementary crystallographic information

Comment

The structure determination of this compound was undertaken as part of a project on nitrogen fixation on molybdenum(0) centers with PNP co-ligands. The compound was synthesized by protonation of the Mo(0) complex [Mo(N2)2(dppe)(pyNP2)] (Stephan et al., 2008) with HBF4.Et2O in analogy to the known procedure (Hidai et al., 1976). Beside the double protonation of one dinitrogen ligand the complex is secondary protonated at the pyridine N atom of the pyNP2 ligand. The second N2 ligand is exchanged against a fluoride ligand during the protonation.

The crystal structure of the title compound consists of discrete [Mo(F)(NNH2)(P2C26H24)(P2C31H29N2)]2+ cations and tetrafluoroborate anions. Each molybdenum atom is coordinated by four P atoms of one 1,2-bis(diphenylphosphino)ethane and one N,N-bis(diphenylphosphinomethyl)-2-aminopyridinium ligand, one N atom a hydrazido ligand and a fluoro ligand within a distorted octahetral geometry. The bite angles of the phosphine ligands are 79.53 (2)° for the dppe ligand and 89.66 (2)° for the pyHNP2 ligand. The Mo—N distance is 1.755 (2)Å and the N—N distance is 1.326 (4) Å.

Experimental

Under an inert gas atmosphere 0.115 ml HBF4*Et2O were added to 300 mg of [Mo(N2)2(dppe)(pyNP2)] in 8 ml Dichloromethane at -15°C. The brown solution was stirred for 15 min and 15 ml of n-Hexane were added. The brown solid was filtered off, washed four times with diethylether and dried under vacuum. Yield: 270 mg (82%). Single crystals were obtained by diffusion of diethylether into a methanolic solution of the complex over a period of one week. 31P NMR (CD2Cl2, 20°C): 43.5 (2 P, dppe), 16.9 (2 P, pyHNP2), 2JPP,trans= 132.0 Hz (P1—P4, P2—P4), 2JPP,cis= -26.5 Hz (P2—P3, P1—P4), 2JPP,cis= -33.0 Hz (P1—P2), 2JPP,cis= 3.0 Hz (P3—P4), 2JPF,cis= -31.0 Hz. 19F NMR (CD2Cl2, 20°C) 148.1 (Mo—F), q, 31 Hz), 149.5 (BF4-, s)

Refinement

The C—H H atoms and the N—H H atom of the 6-membered ring were positioned with idealized geometry and refined using a riding model with Uiso(H)=1.2Ueq(carrier atom) and with C—H = 0.95–0.99 Å and N—H = 0.88 Å or N—H= 0.99 Å. Two of the four F atoms of the tetrafluoroborate anion are disordered over two positions with site occupation factors of 0.737 (9) and 0.263 (9). The minor occupied sites were refined isotropically. The bond lengths and angles of the disordered BF4 anion were restrained to be equal to those of the not disordered one.

Figures

Fig. 1.
: Crystal structure of the title compound with labelling and displacement ellipsoids drawn at the 50% probability level. The H atoms are omitted for clarity.

Crystal data

[MoF(N2H2)(C31H29N2P2)(C26H24P2)](BF4)2F000 = 2472
Mr = 1208.49Dx = 1.482 Mg m3
Monoclinic, P21/nMo Kα radiation λ = 0.71073 Å
a = 12.5791 (6) ÅCell parameters from 8000 reflections
b = 31.2199 (16) Åθ = 10–22º
c = 13.8330 (9) ŵ = 0.44 mm1
β = 94.438 (7)ºT = 170 (2) K
V = 5416.2 (5) Å3Needle, colourless
Z = 40.2 × 0.08 × 0.06 mm

Data collection

Stoe IPDS-1 diffractometer8538 independent reflections
Radiation source: fine-focus sealed tube6783 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.032
T = 170(2) Kθmax = 24.1º
[var phi] scansθmin = 1.8º
Absorption correction: numerical(X-SHAPE; Stoe & Cie, 1998a)h = −14→14
Tmin = 0.949, Tmax = 0.969k = −35→35
24176 measured reflectionsl = −15→15

Refinement

Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.039H-atom parameters constrained
wR(F2) = 0.108  w = 1/[σ2(Fo2) + (0.0748P)2] where P = (Fo2 + 2Fc2)/3
S = 1.02(Δ/σ)max = 0.001
8538 reflectionsΔρmax = 0.94 e Å3
706 parametersΔρmin = −0.54 e Å3
39 restraintsExtinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0045 (4)

Special details

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)

xyzUiso*/UeqOcc. (<1)
Mo10.10191 (2)0.148150 (8)0.284941 (19)0.01774 (12)
F10.20855 (15)0.17169 (6)0.20023 (13)0.0234 (4)
N10.0094 (2)0.12792 (9)0.3620 (2)0.0251 (6)
N2−0.0567 (5)0.11290 (17)0.4239 (3)0.094 (2)
H1N2−0.06610.13000.47590.13 (3)*
H2N2−0.08900.08680.42060.11 (2)*
C10.2510 (3)0.09669 (10)0.4909 (2)0.0232 (7)
H1A0.30110.09950.54930.028*
H1B0.18170.08660.51170.028*
N30.2925 (2)0.06529 (8)0.4248 (2)0.0250 (6)
C20.2109 (3)0.04163 (10)0.3656 (2)0.0261 (8)
H2A0.15290.03390.40680.031*
H2B0.24270.01460.34400.031*
P10.23297 (7)0.14991 (2)0.43059 (6)0.0184 (2)
P20.15116 (7)0.07070 (3)0.25607 (6)0.0205 (2)
C110.1921 (3)0.18206 (10)0.5315 (2)0.0205 (7)
C120.1252 (3)0.16457 (12)0.5967 (3)0.0301 (8)
H120.10710.13510.59280.036*
C130.0849 (3)0.19017 (13)0.6676 (3)0.0376 (10)
H130.03900.17800.71160.045*
C140.1109 (3)0.23297 (12)0.6747 (3)0.0331 (9)
H140.08320.25020.72340.040*
C150.1775 (3)0.25078 (11)0.6104 (3)0.0289 (8)
H150.19610.28020.61540.035*
C160.2171 (3)0.22555 (11)0.5385 (2)0.0249 (7)
H160.26170.23800.49380.030*
C210.3723 (3)0.16364 (10)0.4168 (2)0.0199 (7)
C220.4412 (3)0.17702 (11)0.4954 (3)0.0282 (8)
H220.41400.18200.55660.034*
C230.5490 (3)0.18301 (13)0.4845 (3)0.0391 (10)
H230.59530.19190.53830.047*
C240.5890 (3)0.17612 (14)0.3955 (3)0.0431 (10)
H240.66270.18030.38790.052*
C250.5212 (3)0.16314 (14)0.3172 (3)0.0387 (10)
H250.54890.15840.25620.046*
C260.4132 (3)0.15695 (11)0.3272 (2)0.0279 (8)
H260.36740.14820.27300.034*
C310.3978 (3)0.05601 (11)0.4229 (3)0.0275 (8)
N40.4696 (3)0.07235 (9)0.4921 (2)0.0323 (7)
H40.44530.08850.53770.039*
C320.5761 (3)0.06524 (14)0.4949 (3)0.0443 (10)
H320.62210.07800.54450.053*
C330.6175 (4)0.04001 (15)0.4273 (4)0.0520 (12)
H330.69200.03480.42870.062*
C340.5476 (4)0.02198 (13)0.3558 (3)0.0477 (11)
H340.57510.00410.30810.057*
C350.4399 (3)0.02946 (12)0.3524 (3)0.0382 (9)
H350.39370.01680.30280.046*
C410.2374 (3)0.05482 (11)0.1619 (2)0.0248 (7)
C420.2806 (3)0.08551 (12)0.1042 (3)0.0279 (8)
H420.26610.11500.11410.034*
C430.3453 (3)0.07327 (13)0.0314 (3)0.0348 (9)
H430.37310.0944−0.00910.042*
C440.3689 (3)0.03079 (14)0.0183 (3)0.0385 (10)
H440.41390.0227−0.03070.046*
C450.3275 (3)−0.00026 (13)0.0759 (3)0.0392 (10)
H450.3447−0.02960.06700.047*
C460.2603 (3)0.01148 (12)0.1473 (3)0.0337 (9)
H460.2303−0.00990.18580.040*
C510.0310 (3)0.03842 (10)0.2289 (2)0.0242 (7)
C52−0.0067 (3)0.03302 (11)0.1324 (3)0.0304 (8)
H520.03460.04320.08250.037*
C53−0.1037 (3)0.01295 (13)0.1077 (3)0.0388 (9)
H53−0.12860.00980.04150.047*
C54−0.1641 (3)−0.00240 (12)0.1797 (3)0.0391 (10)
H54−0.2308−0.01580.16310.047*
C55−0.1271 (3)0.00183 (13)0.2755 (3)0.0382 (9)
H55−0.1678−0.00930.32490.046*
C56−0.0302 (3)0.02239 (12)0.3006 (3)0.0337 (9)
H56−0.00580.02550.36700.040*
C61−0.0634 (3)0.23553 (11)0.2013 (2)0.0263 (8)
H61A−0.13150.22290.21910.032*
H61B−0.07430.26670.19160.032*
C62−0.0315 (3)0.21521 (11)0.1075 (2)0.0260 (8)
H62A0.03610.22800.08920.031*
H62B−0.08720.22080.05450.031*
P30.04148 (7)0.22633 (3)0.30016 (6)0.0194 (2)
P4−0.01447 (7)0.15685 (3)0.12462 (6)0.0210 (2)
C710.1408 (3)0.26775 (10)0.2819 (2)0.0219 (7)
C720.2489 (3)0.25795 (11)0.2986 (2)0.0240 (7)
H720.27010.22950.31540.029*
C730.3259 (3)0.28937 (11)0.2910 (3)0.0297 (8)
H730.39910.28240.30380.036*
C740.2969 (3)0.33074 (12)0.2649 (3)0.0334 (9)
H740.34980.35210.25920.040*
C750.1905 (3)0.34069 (11)0.2474 (3)0.0337 (9)
H750.17040.36910.22960.040*
C760.1119 (3)0.30973 (11)0.2552 (3)0.0288 (8)
H760.03880.31710.24250.035*
C81−0.0282 (3)0.24415 (11)0.4045 (2)0.0238 (7)
C82−0.0130 (3)0.28421 (12)0.4469 (3)0.0380 (9)
H820.03820.30330.42380.046*
C83−0.0724 (4)0.29663 (14)0.5233 (3)0.0476 (11)
H83−0.06320.32450.55010.057*
C84−0.1438 (3)0.26910 (15)0.5600 (3)0.0453 (11)
H84−0.18290.27760.61290.054*
C85−0.1585 (4)0.22907 (16)0.5197 (3)0.0510 (12)
H85−0.20750.20970.54530.061*
C86−0.1020 (3)0.21664 (14)0.4415 (3)0.0441 (11)
H86−0.11400.18920.41330.053*
C91−0.1518 (3)0.13741 (11)0.1137 (3)0.0252 (8)
C92−0.1915 (3)0.11545 (12)0.1905 (3)0.0342 (9)
H92−0.14790.11140.24900.041*
C93−0.2950 (3)0.09930 (14)0.1819 (3)0.0464 (11)
H93−0.32180.08460.23500.056*
C94−0.3590 (3)0.10451 (14)0.0970 (4)0.0488 (12)
H94−0.42910.09300.09130.059*
C95−0.3208 (3)0.12639 (13)0.0209 (3)0.0428 (10)
H95−0.36490.1301−0.03740.051*
C96−0.2178 (3)0.14327 (12)0.0284 (3)0.0323 (9)
H96−0.19250.1588−0.02430.039*
C1010.0390 (3)0.14118 (11)0.0102 (2)0.0259 (8)
C102−0.0050 (3)0.10789 (12)−0.0474 (2)0.0315 (8)
H102−0.06690.0935−0.02930.038*
C1030.0417 (4)0.09577 (13)−0.1312 (3)0.0426 (10)
H1030.01060.0735−0.17070.051*
C1040.1324 (4)0.11582 (15)−0.1572 (3)0.0486 (12)
H1040.16520.1068−0.21330.058*
C1050.1758 (4)0.14918 (15)−0.1015 (3)0.0462 (11)
H1050.23770.1634−0.12050.055*
C1060.1299 (3)0.16213 (13)−0.0178 (3)0.0348 (9)
H1060.16020.18510.02000.042*
B10.8583 (5)0.07358 (16)0.6061 (4)0.0541 (15)
F110.8620 (2)0.04255 (7)0.53264 (17)0.0507 (6)
F120.8016 (3)0.10857 (9)0.5658 (2)0.0746 (9)
F130.9582 (3)0.08731 (11)0.6351 (2)0.0925 (12)
F140.8083 (4)0.05738 (10)0.6817 (2)0.1209 (19)
B20.4315 (4)0.09191 (16)0.7490 (3)0.0497 (14)
F210.3459 (3)0.06624 (9)0.7323 (3)0.0867 (12)
F220.4582 (3)0.11052 (11)0.66855 (19)0.0921 (13)
F230.4439 (5)0.11424 (17)0.8310 (3)0.099 (3)0.737 (9)
F240.5265 (4)0.06407 (15)0.7551 (6)0.127 (3)0.737 (9)
F23'0.3739 (10)0.1356 (3)0.7658 (10)0.080 (5)*0.263 (9)
F24'0.4862 (11)0.0855 (5)0.8262 (9)0.104 (6)*0.263 (9)

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
Mo10.02013 (18)0.01895 (17)0.01402 (17)−0.00276 (11)0.00048 (11)0.00024 (10)
F10.0252 (11)0.0248 (9)0.0203 (10)−0.0029 (8)0.0036 (8)0.0021 (7)
N10.0319 (17)0.0252 (14)0.0188 (14)−0.0091 (13)0.0066 (12)−0.0024 (11)
N20.137 (5)0.091 (4)0.063 (3)−0.066 (3)0.062 (3)−0.020 (3)
C10.027 (2)0.0224 (17)0.0201 (17)−0.0012 (14)0.0023 (14)0.0033 (13)
N30.0283 (18)0.0211 (14)0.0250 (16)−0.0007 (12)−0.0015 (12)−0.0007 (11)
C20.031 (2)0.0235 (16)0.0233 (18)−0.0019 (15)−0.0013 (15)0.0011 (14)
P10.0201 (5)0.0209 (4)0.0141 (4)−0.0019 (3)0.0004 (3)0.0007 (3)
P20.0250 (5)0.0196 (4)0.0169 (4)−0.0027 (3)0.0016 (3)−0.0010 (3)
C110.0166 (17)0.0289 (17)0.0155 (16)0.0003 (14)−0.0027 (13)−0.0003 (13)
C120.030 (2)0.0307 (18)0.030 (2)0.0013 (16)0.0106 (16)0.0008 (15)
C130.039 (2)0.045 (2)0.031 (2)0.0063 (18)0.0168 (18)0.0038 (17)
C140.035 (2)0.036 (2)0.029 (2)0.0121 (17)0.0058 (17)−0.0061 (16)
C150.029 (2)0.0280 (18)0.029 (2)0.0034 (15)−0.0028 (16)−0.0059 (15)
C160.0246 (19)0.0280 (18)0.0220 (18)−0.0012 (14)0.0016 (14)−0.0010 (14)
C210.0189 (18)0.0209 (15)0.0200 (17)0.0010 (13)0.0009 (13)0.0017 (13)
C220.024 (2)0.0356 (19)0.0248 (19)−0.0012 (15)0.0017 (15)−0.0049 (15)
C230.025 (2)0.050 (2)0.041 (2)−0.0065 (18)−0.0040 (17)−0.0108 (19)
C240.025 (2)0.061 (3)0.045 (3)−0.0055 (19)0.0092 (19)−0.004 (2)
C250.031 (2)0.056 (2)0.030 (2)0.0044 (19)0.0115 (18)−0.0018 (18)
C260.027 (2)0.037 (2)0.0198 (18)0.0027 (16)0.0016 (15)0.0005 (15)
C310.031 (2)0.0244 (17)0.0263 (19)0.0024 (15)−0.0007 (15)0.0067 (14)
N40.0311 (19)0.0309 (16)0.0340 (18)0.0045 (14)−0.0024 (14)0.0025 (13)
C320.032 (2)0.047 (2)0.052 (3)0.0032 (19)−0.008 (2)0.012 (2)
C330.035 (3)0.055 (3)0.067 (3)0.011 (2)0.005 (2)0.010 (2)
C340.051 (3)0.039 (2)0.055 (3)0.014 (2)0.015 (2)0.001 (2)
C350.044 (3)0.035 (2)0.036 (2)0.0047 (18)0.0039 (18)−0.0032 (17)
C410.0238 (19)0.0290 (17)0.0211 (17)0.0008 (14)−0.0021 (14)−0.0029 (14)
C420.024 (2)0.0333 (19)0.0266 (19)0.0006 (15)0.0009 (15)0.0007 (15)
C430.027 (2)0.050 (2)0.028 (2)−0.0006 (18)0.0044 (16)−0.0005 (17)
C440.028 (2)0.060 (3)0.028 (2)0.0065 (19)0.0032 (16)−0.0080 (19)
C450.041 (3)0.040 (2)0.037 (2)0.0110 (18)−0.0002 (18)−0.0117 (18)
C460.042 (2)0.0311 (19)0.028 (2)0.0027 (17)0.0016 (17)−0.0041 (16)
C510.027 (2)0.0181 (16)0.0275 (19)−0.0019 (14)0.0017 (15)−0.0029 (13)
C520.028 (2)0.0332 (19)0.029 (2)−0.0045 (16)−0.0004 (16)−0.0050 (15)
C530.035 (2)0.043 (2)0.037 (2)−0.0061 (18)−0.0040 (18)−0.0131 (18)
C540.025 (2)0.035 (2)0.057 (3)−0.0069 (17)0.0002 (18)−0.0109 (19)
C550.031 (2)0.040 (2)0.044 (2)−0.0077 (18)0.0096 (18)0.0010 (18)
C560.034 (2)0.037 (2)0.031 (2)−0.0071 (17)0.0044 (17)−0.0010 (16)
C610.026 (2)0.0261 (17)0.0256 (18)0.0020 (15)−0.0032 (15)0.0012 (14)
C620.029 (2)0.0288 (18)0.0195 (18)−0.0007 (15)−0.0033 (15)0.0051 (14)
P30.0191 (5)0.0207 (4)0.0184 (4)−0.0002 (3)0.0024 (3)−0.0002 (3)
P40.0211 (5)0.0264 (4)0.0152 (4)−0.0011 (4)−0.0001 (3)−0.0007 (3)
C710.0247 (19)0.0226 (16)0.0191 (17)−0.0020 (14)0.0055 (14)−0.0007 (13)
C720.028 (2)0.0237 (17)0.0208 (17)0.0033 (15)0.0051 (14)0.0025 (13)
C730.023 (2)0.037 (2)0.029 (2)−0.0033 (16)0.0066 (15)0.0008 (16)
C740.037 (2)0.033 (2)0.031 (2)−0.0112 (17)0.0091 (17)0.0015 (16)
C750.040 (2)0.0245 (18)0.037 (2)−0.0011 (17)0.0070 (18)0.0071 (16)
C760.029 (2)0.0268 (18)0.0307 (19)0.0021 (15)0.0020 (16)0.0048 (15)
C810.0196 (18)0.0315 (18)0.0201 (17)0.0045 (14)0.0007 (14)−0.0002 (14)
C820.047 (3)0.035 (2)0.033 (2)0.0011 (18)0.0119 (19)−0.0032 (17)
C830.064 (3)0.045 (2)0.035 (2)0.016 (2)0.012 (2)−0.0095 (19)
C840.037 (3)0.069 (3)0.031 (2)0.022 (2)0.0100 (19)0.001 (2)
C850.035 (3)0.077 (3)0.044 (3)−0.010 (2)0.020 (2)−0.005 (2)
C860.039 (3)0.052 (2)0.045 (3)−0.012 (2)0.019 (2)−0.012 (2)
C910.0223 (19)0.0250 (17)0.0282 (19)0.0020 (14)0.0001 (15)−0.0078 (14)
C920.024 (2)0.042 (2)0.036 (2)0.0008 (17)0.0035 (16)−0.0002 (17)
C930.031 (2)0.052 (3)0.058 (3)−0.0053 (19)0.015 (2)0.005 (2)
C940.021 (2)0.046 (2)0.080 (4)−0.0039 (18)0.003 (2)−0.011 (2)
C950.030 (2)0.043 (2)0.052 (3)0.0058 (19)−0.0138 (19)−0.013 (2)
C960.030 (2)0.034 (2)0.032 (2)0.0044 (16)−0.0054 (16)−0.0035 (16)
C1010.0238 (19)0.0367 (19)0.0169 (17)0.0055 (15)0.0001 (14)0.0027 (14)
C1020.037 (2)0.036 (2)0.0211 (19)0.0094 (17)−0.0016 (16)−0.0006 (15)
C1030.057 (3)0.044 (2)0.027 (2)0.017 (2)−0.0007 (19)−0.0054 (17)
C1040.065 (3)0.059 (3)0.023 (2)0.024 (2)0.014 (2)0.0039 (19)
C1050.040 (3)0.070 (3)0.030 (2)0.009 (2)0.0145 (19)0.015 (2)
C1060.035 (2)0.047 (2)0.0225 (19)0.0027 (18)0.0051 (16)0.0057 (16)
B10.090 (5)0.032 (2)0.042 (3)−0.023 (3)0.015 (3)−0.006 (2)
F110.0766 (19)0.0377 (12)0.0389 (13)−0.0116 (12)0.0123 (13)−0.0034 (10)
F120.093 (2)0.0527 (17)0.083 (2)0.0031 (16)0.0340 (19)−0.0054 (15)
F130.112 (3)0.089 (2)0.070 (2)−0.045 (2)−0.037 (2)0.0137 (18)
F140.247 (5)0.0607 (19)0.067 (2)−0.070 (3)0.088 (3)−0.0181 (16)
B20.062 (4)0.056 (3)0.033 (3)−0.027 (3)0.016 (2)−0.009 (2)
F210.071 (2)0.0651 (18)0.131 (3)−0.0384 (16)0.055 (2)−0.0372 (19)
F220.133 (3)0.111 (3)0.0303 (15)−0.076 (2)−0.0069 (17)0.0020 (15)
F230.175 (6)0.090 (4)0.041 (3)−0.075 (4)0.059 (3)−0.037 (2)
F240.102 (5)0.062 (3)0.200 (7)0.015 (3)−0.088 (4)−0.012 (4)

Geometric parameters (Å, °)

Mo1—N11.755 (3)C53—H530.9500
Mo1—F11.9889 (18)C54—C551.377 (6)
Mo1—P12.5032 (9)C54—H540.9500
Mo1—P22.5353 (9)C55—C561.398 (6)
Mo1—P32.5698 (8)C55—H550.9500
Mo1—P42.5754 (9)C56—H560.9500
N1—N21.325 (5)C61—C621.526 (5)
N2—H1N20.9101C61—P31.848 (4)
N2—H2N20.9100C61—H61A0.9900
C1—N31.464 (4)C61—H61B0.9900
C1—P11.865 (3)C62—P41.847 (3)
C1—H1A0.9900C62—H62A0.9900
C1—H1B0.9900C62—H62B0.9900
N3—C311.358 (5)P3—C711.829 (3)
N3—C21.463 (4)P3—C811.832 (3)
C2—P21.873 (3)P4—C911.826 (4)
C2—H2A0.9900P4—C1011.833 (3)
C2—H2B0.9900C71—C721.396 (5)
P1—C111.826 (3)C71—C761.402 (5)
P1—C211.828 (3)C72—C731.388 (5)
P2—C411.827 (3)C72—H720.9500
P2—C511.831 (3)C73—C741.382 (5)
C11—C121.392 (5)C73—H730.9500
C11—C161.396 (5)C74—C751.377 (6)
C12—C131.390 (5)C74—H740.9500
C12—H120.9500C75—C761.393 (5)
C13—C141.377 (6)C75—H750.9500
C13—H130.9500C76—H760.9500
C14—C151.384 (5)C81—C821.388 (5)
C14—H140.9500C81—C861.391 (5)
C15—C161.391 (5)C82—C831.395 (6)
C15—H150.9500C82—H820.9500
C16—H160.9500C83—C841.369 (6)
C21—C261.395 (5)C83—H830.9500
C21—C221.401 (5)C84—C851.375 (7)
C22—C231.388 (5)C84—H840.9500
C22—H220.9500C85—C861.394 (6)
C23—C241.383 (6)C85—H850.9500
C23—H230.9500C86—H860.9500
C24—C251.385 (6)C91—C921.389 (5)
C24—H240.9500C91—C961.401 (5)
C25—C261.389 (5)C92—C931.393 (6)
C25—H250.9500C92—H920.9500
C26—H260.9500C93—C941.382 (7)
C31—N41.363 (5)C93—H930.9500
C31—C351.413 (5)C94—C951.372 (7)
N4—C321.356 (5)C94—H940.9500
N4—H40.8800C95—C961.395 (6)
C32—C331.357 (6)C95—H950.9500
C32—H320.9500C96—H960.9500
C33—C341.391 (7)C101—C1061.397 (5)
C33—H330.9500C101—C1021.398 (5)
C34—C351.372 (6)C102—C1031.392 (5)
C34—H340.9500C102—H1020.9500
C35—H350.9500C103—C1041.374 (7)
C41—C421.385 (5)C103—H1030.9500
C41—C461.401 (5)C104—C1051.383 (7)
C42—C431.396 (5)C104—H1040.9500
C42—H420.9500C105—C1061.393 (6)
C43—C441.374 (6)C105—H1050.9500
C43—H430.9500C106—H1060.9500
C44—C451.383 (6)B1—F141.358 (6)
C44—H440.9500B1—F131.359 (7)
C45—C461.397 (5)B1—F121.397 (7)
C45—H450.9500B1—F111.407 (6)
C46—H460.9500B2—F24'1.241 (10)
C51—C521.393 (5)B2—F221.322 (5)
C51—C561.394 (5)B2—F231.330 (6)
C52—C531.391 (5)B2—F211.348 (5)
C52—H520.9500B2—F241.475 (7)
C53—C541.384 (6)B2—F23'1.570 (10)
N1—Mo1—F1178.70 (11)C55—C54—C53119.8 (4)
N1—Mo1—P186.88 (10)C55—C54—H54120.1
F1—Mo1—P191.94 (6)C53—C54—H54120.1
N1—Mo1—P286.22 (9)C54—C55—C56120.4 (4)
F1—Mo1—P294.33 (6)C54—C55—H55119.8
P1—Mo1—P289.65 (3)C56—C55—H55119.8
N1—Mo1—P394.46 (9)C51—C56—C55120.5 (4)
F1—Mo1—P385.10 (5)C51—C56—H56119.8
P1—Mo1—P395.38 (3)C55—C56—H56119.8
P2—Mo1—P3174.95 (3)C62—C61—P3110.1 (2)
N1—Mo1—P4101.62 (10)C62—C61—H61A109.6
F1—Mo1—P479.52 (6)P3—C61—H61A109.6
P1—Mo1—P4170.35 (3)C62—C61—H61B109.6
P2—Mo1—P495.42 (3)P3—C61—H61B109.6
P3—Mo1—P479.53 (3)H61A—C61—H61B108.1
N2—N1—Mo1177.1 (3)C61—C62—P4109.7 (2)
N1—N2—H1N2115.4C61—C62—H62A109.7
N1—N2—H2N2125.8P4—C62—H62A109.7
H1N2—N2—H2N2118.7C61—C62—H62B109.7
N3—C1—P1110.7 (2)P4—C62—H62B109.7
N3—C1—H1A109.5H62A—C62—H62B108.2
P1—C1—H1A109.5C71—P3—C81105.51 (15)
N3—C1—H1B109.5C71—P3—C61104.13 (16)
P1—C1—H1B109.5C81—P3—C61100.27 (16)
H1A—C1—H1B108.1C71—P3—Mo1116.78 (11)
C31—N3—C2121.6 (3)C81—P3—Mo1121.04 (11)
C31—N3—C1123.4 (3)C61—P3—Mo1106.61 (11)
C2—N3—C1114.7 (3)C91—P4—C101104.34 (16)
N3—C2—P2115.4 (2)C91—P4—C62102.59 (16)
N3—C2—H2A108.4C101—P4—C62101.48 (16)
P2—C2—H2A108.4C91—P4—Mo1120.50 (12)
N3—C2—H2B108.4C101—P4—Mo1119.52 (12)
P2—C2—H2B108.4C62—P4—Mo1105.48 (11)
H2A—C2—H2B107.5C72—C71—C76118.6 (3)
C11—P1—C21106.26 (15)C72—C71—P3119.3 (2)
C11—P1—C1100.35 (15)C76—C71—P3122.1 (3)
C21—P1—C199.87 (15)C73—C72—C71120.6 (3)
C11—P1—Mo1114.87 (11)C73—C72—H72119.7
C21—P1—Mo1119.87 (11)C71—C72—H72119.7
C1—P1—Mo1112.95 (11)C74—C73—C72120.6 (4)
C41—P2—C51103.36 (15)C74—C73—H73119.7
C41—P2—C2102.80 (16)C72—C73—H73119.7
C51—P2—C299.92 (16)C75—C74—C73119.4 (3)
C41—P2—Mo1122.48 (11)C75—C74—H74120.3
C51—P2—Mo1110.44 (11)C73—C74—H74120.3
C2—P2—Mo1114.99 (11)C74—C75—C76121.0 (3)
C12—C11—C16118.8 (3)C74—C75—H75119.5
C12—C11—P1120.0 (3)C76—C75—H75119.5
C16—C11—P1120.8 (2)C75—C76—C71119.9 (3)
C13—C12—C11120.2 (3)C75—C76—H76120.1
C13—C12—H12119.9C71—C76—H76120.1
C11—C12—H12119.9C82—C81—C86118.3 (3)
C14—C13—C12120.7 (3)C82—C81—P3123.3 (3)
C14—C13—H13119.7C86—C81—P3118.4 (3)
C12—C13—H13119.7C81—C82—C83120.4 (4)
C13—C14—C15119.7 (3)C81—C82—H82119.8
C13—C14—H14120.1C83—C82—H82119.8
C15—C14—H14120.1C84—C83—C82120.8 (4)
C14—C15—C16120.0 (3)C84—C83—H83119.6
C14—C15—H15120.0C82—C83—H83119.6
C16—C15—H15120.0C83—C84—C85119.4 (4)
C15—C16—C11120.6 (3)C83—C84—H84120.3
C15—C16—H16119.7C85—C84—H84120.3
C11—C16—H16119.7C84—C85—C86120.5 (4)
C26—C21—C22119.1 (3)C84—C85—H85119.8
C26—C21—P1118.7 (3)C86—C85—H85119.8
C22—C21—P1122.0 (3)C81—C86—C85120.5 (4)
C23—C22—C21120.4 (3)C81—C86—H86119.7
C23—C22—H22119.8C85—C86—H86119.7
C21—C22—H22119.8C92—C91—C96118.9 (3)
C24—C23—C22120.1 (4)C92—C91—P4119.6 (3)
C24—C23—H23119.9C96—C91—P4121.5 (3)
C22—C23—H23119.9C91—C92—C93120.2 (4)
C23—C24—C25119.8 (4)C91—C92—H92119.9
C23—C24—H24120.1C93—C92—H92119.9
C25—C24—H24120.1C94—C93—C92120.6 (4)
C24—C25—C26120.7 (4)C94—C93—H93119.7
C24—C25—H25119.6C92—C93—H93119.7
C26—C25—H25119.6C95—C94—C93119.6 (4)
C25—C26—C21119.9 (3)C95—C94—H94120.2
C25—C26—H26120.1C93—C94—H94120.2
C21—C26—H26120.1C94—C95—C96120.6 (4)
N3—C31—N4120.0 (3)C94—C95—H95119.7
N3—C31—C35123.8 (3)C96—C95—H95119.7
N4—C31—C35116.2 (3)C95—C96—C91120.0 (4)
C32—N4—C31123.9 (4)C95—C96—H96120.0
C32—N4—H4118.0C91—C96—H96120.0
C31—N4—H4118.0C106—C101—C102119.1 (3)
N4—C32—C33120.4 (4)C106—C101—P4118.5 (3)
N4—C32—H32119.8C102—C101—P4122.3 (3)
C33—C32—H32119.8C103—C102—C101120.2 (4)
C32—C33—C34118.0 (4)C103—C102—H102119.9
C32—C33—H33121.0C101—C102—H102119.9
C34—C33—H33121.0C104—C103—C102120.4 (4)
C35—C34—C33121.6 (4)C104—C103—H103119.8
C35—C34—H34119.2C102—C103—H103119.8
C33—C34—H34119.2C103—C104—C105119.9 (4)
C34—C35—C31119.9 (4)C103—C104—H104120.1
C34—C35—H35120.1C105—C104—H104120.1
C31—C35—H35120.1C104—C105—C106120.7 (4)
C42—C41—C46119.4 (3)C104—C105—H105119.7
C42—C41—P2120.3 (3)C106—C105—H105119.7
C46—C41—P2120.3 (3)C105—C106—C101119.7 (4)
C41—C42—C43120.2 (3)C105—C106—H106120.1
C41—C42—H42119.9C101—C106—H106120.1
C43—C42—H42119.9F14—B1—F13111.3 (5)
C44—C43—C42120.2 (4)F14—B1—F12110.2 (5)
C44—C43—H43119.9F13—B1—F12107.7 (4)
C42—C43—H43119.9F14—B1—F11110.0 (4)
C43—C44—C45120.3 (4)F13—B1—F11110.5 (5)
C43—C44—H44119.8F12—B1—F11107.1 (4)
C45—C44—H44119.8F24'—B2—F22129.4 (8)
C44—C45—C46120.0 (4)F24'—B2—F2347.9 (8)
C44—C45—H45120.0F22—B2—F23117.8 (4)
C46—C45—H45120.0F24'—B2—F21115.8 (8)
C45—C46—C41119.8 (4)F22—B2—F21111.7 (4)
C45—C46—H46120.1F23—B2—F21119.8 (4)
C41—C46—H46120.1F24'—B2—F2457.5 (8)
C52—C51—C56118.2 (3)F22—B2—F2492.9 (5)
C52—C51—P2118.5 (3)F23—B2—F24102.6 (5)
C56—C51—P2123.0 (3)F21—B2—F24107.0 (4)
C53—C52—C51121.1 (4)F24'—B2—F23'104.1 (9)
C53—C52—H52119.4F22—B2—F23'83.9 (6)
C51—C52—H52119.4F23—B2—F23'56.2 (5)
C54—C53—C52120.0 (4)F21—B2—F23'99.8 (6)
C54—C53—H53120.0F24—B2—F23'152.2 (6)
C52—C53—H53120.0

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: BT2688).

References

  • Brandenburg, K. (1999). DIAMOND Crystal Impact GbR, Bonn, Germany.
  • Hidai, M., Kodama, T., Sato, M., Harakawa, M. & Uchida, Y. (1976). Inorg. Chem.15, 2694–2697.
  • Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. [PubMed]
  • Stephan, G. C., Näther, C., Sivasankar, C. & Tuczek, F. (2008). Inorg. Chim. Acta, 361, 1008–1019.
  • Stoe & Cie (1998a). X-SHAPE Stoe & Cie, Darmstadt, Germany.
  • Stoe & Cie (1998b). IPDS Program package Stoe & Cie, Darmstadt, Germany

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