metal-organic compounds
[1,2-Bis(diphenylphosphino)ethane]{2-[bis(diphenylphosphinomethyl)amino]pyridinium}fluoridohydrazidatomolybdenum(IV) bis(tetrafluoridoborate)
aInstitut für Anorganische Chemie, Christian-Albrechts-Universität Kiel, Olshausenstrasse 40, D-24098 Kiel, Germany
*Correspondence e-mail: cnaether@ac.uni-kiel.de
In the 2H2)(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 (NNH22−) 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.
of the title compound, [MoF(NExperimental
Crystal data
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Refinement
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Data collection: IPDS Program package (Stoe & Cie, 1998b); cell IPDS Program package; data reduction: IPDS Program package; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg, 1999); software used to prepare material for publication: CIFTAB in SHELXTL (Sheldrick, 2008).
Supporting information
10.1107/S1600536808008635/bt2688sup1.cif
contains datablocks I, global. DOI:Structure factors: contains datablock I. DOI: 10.1107/S1600536808008635/bt2688Isup2.hkl
Under an
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)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.
Data collection: IPDS program package (Stoe & Cie, 1998b); cell
IPDS program package; data reduction: IPDS program package; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg, 1999); software used to prepare material for publication: CIFTAB in SHELXTL (Sheldrick, 2008).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. |
[MoF(N2H2)(C31H29N2P2)(C26H24P2)](BF4)2 | F(000) = 2472 |
Mr = 1208.49 | Dx = 1.482 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
a = 12.5791 (6) Å | Cell parameters from 8000 reflections |
b = 31.2199 (16) Å | θ = 10–22° |
c = 13.8330 (9) Å | µ = 0.44 mm−1 |
β = 94.438 (7)° | T = 170 K |
V = 5416.2 (5) Å3 | Needle, colourless |
Z = 4 | 0.2 × 0.08 × 0.06 mm |
Stoe IPDS-1 diffractometer | 8538 independent reflections |
Radiation source: fine-focus sealed tube | 6783 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.032 |
ϕ scans | θmax = 24.1°, θmin = 1.8° |
Absorption correction: numerical (X-SHAPE; Stoe & Cie, 1998a) | h = −14→14 |
Tmin = 0.949, Tmax = 0.969 | k = −35→35 |
24176 measured reflections | l = −15→15 |
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)] = 0.039 | H-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 reflections | Δρmax = 0.94 e Å−3 |
706 parameters | Δρmin = −0.54 e Å−3 |
39 restraints | Extinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0045 (4) |
[MoF(N2H2)(C31H29N2P2)(C26H24P2)](BF4)2 | V = 5416.2 (5) Å3 |
Mr = 1208.49 | Z = 4 |
Monoclinic, P21/n | Mo Kα radiation |
a = 12.5791 (6) Å | µ = 0.44 mm−1 |
b = 31.2199 (16) Å | T = 170 K |
c = 13.8330 (9) Å | 0.2 × 0.08 × 0.06 mm |
β = 94.438 (7)° |
Stoe IPDS-1 diffractometer | 8538 independent reflections |
Absorption correction: numerical (X-SHAPE; Stoe & Cie, 1998a) | 6783 reflections with I > 2σ(I) |
Tmin = 0.949, Tmax = 0.969 | Rint = 0.032 |
24176 measured reflections | θmax = 24.1° |
R[F2 > 2σ(F2)] = 0.039 | 39 restraints |
wR(F2) = 0.108 | H-atom parameters constrained |
S = 1.02 | Δρmax = 0.94 e Å−3 |
8538 reflections | Δρmin = −0.54 e Å−3 |
706 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 | 0.10191 (2) | 0.148150 (8) | 0.284941 (19) | 0.01774 (12) | |
F1 | 0.20855 (15) | 0.17169 (6) | 0.20023 (13) | 0.0234 (4) | |
N1 | 0.0094 (2) | 0.12792 (9) | 0.3620 (2) | 0.0251 (6) | |
N2 | −0.0567 (5) | 0.11290 (17) | 0.4239 (3) | 0.094 (2) | |
H1N2 | −0.0661 | 0.1300 | 0.4759 | 0.13 (3)* | |
H2N2 | −0.0890 | 0.0868 | 0.4206 | 0.11 (2)* | |
C1 | 0.2510 (3) | 0.09669 (10) | 0.4909 (2) | 0.0232 (7) | |
H1A | 0.3011 | 0.0995 | 0.5493 | 0.028* | |
H1B | 0.1817 | 0.0866 | 0.5117 | 0.028* | |
N3 | 0.2925 (2) | 0.06529 (8) | 0.4248 (2) | 0.0250 (6) | |
C2 | 0.2109 (3) | 0.04163 (10) | 0.3656 (2) | 0.0261 (8) | |
H2A | 0.1529 | 0.0339 | 0.4068 | 0.031* | |
H2B | 0.2427 | 0.0146 | 0.3440 | 0.031* | |
P1 | 0.23297 (7) | 0.14991 (2) | 0.43059 (6) | 0.0184 (2) | |
P2 | 0.15116 (7) | 0.07070 (3) | 0.25607 (6) | 0.0205 (2) | |
C11 | 0.1921 (3) | 0.18206 (10) | 0.5315 (2) | 0.0205 (7) | |
C12 | 0.1252 (3) | 0.16457 (12) | 0.5967 (3) | 0.0301 (8) | |
H12 | 0.1071 | 0.1351 | 0.5928 | 0.036* | |
C13 | 0.0849 (3) | 0.19017 (13) | 0.6676 (3) | 0.0376 (10) | |
H13 | 0.0390 | 0.1780 | 0.7116 | 0.045* | |
C14 | 0.1109 (3) | 0.23297 (12) | 0.6747 (3) | 0.0331 (9) | |
H14 | 0.0832 | 0.2502 | 0.7234 | 0.040* | |
C15 | 0.1775 (3) | 0.25078 (11) | 0.6104 (3) | 0.0289 (8) | |
H15 | 0.1961 | 0.2802 | 0.6154 | 0.035* | |
C16 | 0.2171 (3) | 0.22555 (11) | 0.5385 (2) | 0.0249 (7) | |
H16 | 0.2617 | 0.2380 | 0.4938 | 0.030* | |
C21 | 0.3723 (3) | 0.16364 (10) | 0.4168 (2) | 0.0199 (7) | |
C22 | 0.4412 (3) | 0.17702 (11) | 0.4954 (3) | 0.0282 (8) | |
H22 | 0.4140 | 0.1820 | 0.5566 | 0.034* | |
C23 | 0.5490 (3) | 0.18301 (13) | 0.4845 (3) | 0.0391 (10) | |
H23 | 0.5953 | 0.1919 | 0.5383 | 0.047* | |
C24 | 0.5890 (3) | 0.17612 (14) | 0.3955 (3) | 0.0431 (10) | |
H24 | 0.6627 | 0.1803 | 0.3879 | 0.052* | |
C25 | 0.5212 (3) | 0.16314 (14) | 0.3172 (3) | 0.0387 (10) | |
H25 | 0.5489 | 0.1584 | 0.2562 | 0.046* | |
C26 | 0.4132 (3) | 0.15695 (11) | 0.3272 (2) | 0.0279 (8) | |
H26 | 0.3674 | 0.1482 | 0.2730 | 0.034* | |
C31 | 0.3978 (3) | 0.05601 (11) | 0.4229 (3) | 0.0275 (8) | |
N4 | 0.4696 (3) | 0.07235 (9) | 0.4921 (2) | 0.0323 (7) | |
H4 | 0.4453 | 0.0885 | 0.5377 | 0.039* | |
C32 | 0.5761 (3) | 0.06524 (14) | 0.4949 (3) | 0.0443 (10) | |
H32 | 0.6221 | 0.0780 | 0.5445 | 0.053* | |
C33 | 0.6175 (4) | 0.04001 (15) | 0.4273 (4) | 0.0520 (12) | |
H33 | 0.6920 | 0.0348 | 0.4287 | 0.062* | |
C34 | 0.5476 (4) | 0.02198 (13) | 0.3558 (3) | 0.0477 (11) | |
H34 | 0.5751 | 0.0041 | 0.3081 | 0.057* | |
C35 | 0.4399 (3) | 0.02946 (12) | 0.3524 (3) | 0.0382 (9) | |
H35 | 0.3937 | 0.0168 | 0.3028 | 0.046* | |
C41 | 0.2374 (3) | 0.05482 (11) | 0.1619 (2) | 0.0248 (7) | |
C42 | 0.2806 (3) | 0.08551 (12) | 0.1042 (3) | 0.0279 (8) | |
H42 | 0.2661 | 0.1150 | 0.1141 | 0.034* | |
C43 | 0.3453 (3) | 0.07327 (13) | 0.0314 (3) | 0.0348 (9) | |
H43 | 0.3731 | 0.0944 | −0.0091 | 0.042* | |
C44 | 0.3689 (3) | 0.03079 (14) | 0.0183 (3) | 0.0385 (10) | |
H44 | 0.4139 | 0.0227 | −0.0307 | 0.046* | |
C45 | 0.3275 (3) | −0.00026 (13) | 0.0759 (3) | 0.0392 (10) | |
H45 | 0.3447 | −0.0296 | 0.0670 | 0.047* | |
C46 | 0.2603 (3) | 0.01148 (12) | 0.1473 (3) | 0.0337 (9) | |
H46 | 0.2303 | −0.0099 | 0.1858 | 0.040* | |
C51 | 0.0310 (3) | 0.03842 (10) | 0.2289 (2) | 0.0242 (7) | |
C52 | −0.0067 (3) | 0.03302 (11) | 0.1324 (3) | 0.0304 (8) | |
H52 | 0.0346 | 0.0432 | 0.0825 | 0.037* | |
C53 | −0.1037 (3) | 0.01295 (13) | 0.1077 (3) | 0.0388 (9) | |
H53 | −0.1286 | 0.0098 | 0.0415 | 0.047* | |
C54 | −0.1641 (3) | −0.00240 (12) | 0.1797 (3) | 0.0391 (10) | |
H54 | −0.2308 | −0.0158 | 0.1631 | 0.047* | |
C55 | −0.1271 (3) | 0.00183 (13) | 0.2755 (3) | 0.0382 (9) | |
H55 | −0.1678 | −0.0093 | 0.3249 | 0.046* | |
C56 | −0.0302 (3) | 0.02239 (12) | 0.3006 (3) | 0.0337 (9) | |
H56 | −0.0058 | 0.0255 | 0.3670 | 0.040* | |
C61 | −0.0634 (3) | 0.23553 (11) | 0.2013 (2) | 0.0263 (8) | |
H61A | −0.1315 | 0.2229 | 0.2191 | 0.032* | |
H61B | −0.0743 | 0.2667 | 0.1916 | 0.032* | |
C62 | −0.0315 (3) | 0.21521 (11) | 0.1075 (2) | 0.0260 (8) | |
H62A | 0.0361 | 0.2280 | 0.0892 | 0.031* | |
H62B | −0.0872 | 0.2208 | 0.0545 | 0.031* | |
P3 | 0.04148 (7) | 0.22633 (3) | 0.30016 (6) | 0.0194 (2) | |
P4 | −0.01447 (7) | 0.15685 (3) | 0.12462 (6) | 0.0210 (2) | |
C71 | 0.1408 (3) | 0.26775 (10) | 0.2819 (2) | 0.0219 (7) | |
C72 | 0.2489 (3) | 0.25795 (11) | 0.2986 (2) | 0.0240 (7) | |
H72 | 0.2701 | 0.2295 | 0.3154 | 0.029* | |
C73 | 0.3259 (3) | 0.28937 (11) | 0.2910 (3) | 0.0297 (8) | |
H73 | 0.3991 | 0.2824 | 0.3038 | 0.036* | |
C74 | 0.2969 (3) | 0.33074 (12) | 0.2649 (3) | 0.0334 (9) | |
H74 | 0.3498 | 0.3521 | 0.2592 | 0.040* | |
C75 | 0.1905 (3) | 0.34069 (11) | 0.2474 (3) | 0.0337 (9) | |
H75 | 0.1704 | 0.3691 | 0.2296 | 0.040* | |
C76 | 0.1119 (3) | 0.30973 (11) | 0.2552 (3) | 0.0288 (8) | |
H76 | 0.0388 | 0.3171 | 0.2425 | 0.035* | |
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) | |
H82 | 0.0382 | 0.3033 | 0.4238 | 0.046* | |
C83 | −0.0724 (4) | 0.29663 (14) | 0.5233 (3) | 0.0476 (11) | |
H83 | −0.0632 | 0.3245 | 0.5501 | 0.057* | |
C84 | −0.1438 (3) | 0.26910 (15) | 0.5600 (3) | 0.0453 (11) | |
H84 | −0.1829 | 0.2776 | 0.6129 | 0.054* | |
C85 | −0.1585 (4) | 0.22907 (16) | 0.5197 (3) | 0.0510 (12) | |
H85 | −0.2075 | 0.2097 | 0.5453 | 0.061* | |
C86 | −0.1020 (3) | 0.21664 (14) | 0.4415 (3) | 0.0441 (11) | |
H86 | −0.1140 | 0.1892 | 0.4133 | 0.053* | |
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 | −0.1479 | 0.1114 | 0.2490 | 0.041* | |
C93 | −0.2950 (3) | 0.09930 (14) | 0.1819 (3) | 0.0464 (11) | |
H93 | −0.3218 | 0.0846 | 0.2350 | 0.056* | |
C94 | −0.3590 (3) | 0.10451 (14) | 0.0970 (4) | 0.0488 (12) | |
H94 | −0.4291 | 0.0930 | 0.0913 | 0.059* | |
C95 | −0.3208 (3) | 0.12639 (13) | 0.0209 (3) | 0.0428 (10) | |
H95 | −0.3649 | 0.1301 | −0.0374 | 0.051* | |
C96 | −0.2178 (3) | 0.14327 (12) | 0.0284 (3) | 0.0323 (9) | |
H96 | −0.1925 | 0.1588 | −0.0243 | 0.039* | |
C101 | 0.0390 (3) | 0.14118 (11) | 0.0102 (2) | 0.0259 (8) | |
C102 | −0.0050 (3) | 0.10789 (12) | −0.0474 (2) | 0.0315 (8) | |
H102 | −0.0669 | 0.0935 | −0.0293 | 0.038* | |
C103 | 0.0417 (4) | 0.09577 (13) | −0.1312 (3) | 0.0426 (10) | |
H103 | 0.0106 | 0.0735 | −0.1707 | 0.051* | |
C104 | 0.1324 (4) | 0.11582 (15) | −0.1572 (3) | 0.0486 (12) | |
H104 | 0.1652 | 0.1068 | −0.2133 | 0.058* | |
C105 | 0.1758 (4) | 0.14918 (15) | −0.1015 (3) | 0.0462 (11) | |
H105 | 0.2377 | 0.1634 | −0.1205 | 0.055* | |
C106 | 0.1299 (3) | 0.16213 (13) | −0.0178 (3) | 0.0348 (9) | |
H106 | 0.1602 | 0.1851 | 0.0200 | 0.042* | |
B1 | 0.8583 (5) | 0.07358 (16) | 0.6061 (4) | 0.0541 (15) | |
F11 | 0.8620 (2) | 0.04255 (7) | 0.53264 (17) | 0.0507 (6) | |
F12 | 0.8016 (3) | 0.10857 (9) | 0.5658 (2) | 0.0746 (9) | |
F13 | 0.9582 (3) | 0.08731 (11) | 0.6351 (2) | 0.0925 (12) | |
F14 | 0.8083 (4) | 0.05738 (10) | 0.6817 (2) | 0.1209 (19) | |
B2 | 0.4315 (4) | 0.09191 (16) | 0.7490 (3) | 0.0497 (14) | |
F21 | 0.3459 (3) | 0.06624 (9) | 0.7323 (3) | 0.0867 (12) | |
F22 | 0.4582 (3) | 0.11052 (11) | 0.66855 (19) | 0.0921 (13) | |
F23 | 0.4439 (5) | 0.11424 (17) | 0.8310 (3) | 0.099 (3) | 0.737 (9) |
F24 | 0.5265 (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) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Mo1 | 0.02013 (18) | 0.01895 (17) | 0.01402 (17) | −0.00276 (11) | 0.00048 (11) | 0.00024 (10) |
F1 | 0.0252 (11) | 0.0248 (9) | 0.0203 (10) | −0.0029 (8) | 0.0036 (8) | 0.0021 (7) |
N1 | 0.0319 (17) | 0.0252 (14) | 0.0188 (14) | −0.0091 (13) | 0.0066 (12) | −0.0024 (11) |
N2 | 0.137 (5) | 0.091 (4) | 0.063 (3) | −0.066 (3) | 0.062 (3) | −0.020 (3) |
C1 | 0.027 (2) | 0.0224 (17) | 0.0201 (17) | −0.0012 (14) | 0.0023 (14) | 0.0033 (13) |
N3 | 0.0283 (18) | 0.0211 (14) | 0.0250 (16) | −0.0007 (12) | −0.0015 (12) | −0.0007 (11) |
C2 | 0.031 (2) | 0.0235 (16) | 0.0233 (18) | −0.0019 (15) | −0.0013 (15) | 0.0011 (14) |
P1 | 0.0201 (5) | 0.0209 (4) | 0.0141 (4) | −0.0019 (3) | 0.0004 (3) | 0.0007 (3) |
P2 | 0.0250 (5) | 0.0196 (4) | 0.0169 (4) | −0.0027 (3) | 0.0016 (3) | −0.0010 (3) |
C11 | 0.0166 (17) | 0.0289 (17) | 0.0155 (16) | 0.0003 (14) | −0.0027 (13) | −0.0003 (13) |
C12 | 0.030 (2) | 0.0307 (18) | 0.030 (2) | 0.0013 (16) | 0.0106 (16) | 0.0008 (15) |
C13 | 0.039 (2) | 0.045 (2) | 0.031 (2) | 0.0063 (18) | 0.0168 (18) | 0.0038 (17) |
C14 | 0.035 (2) | 0.036 (2) | 0.029 (2) | 0.0121 (17) | 0.0058 (17) | −0.0061 (16) |
C15 | 0.029 (2) | 0.0280 (18) | 0.029 (2) | 0.0034 (15) | −0.0028 (16) | −0.0059 (15) |
C16 | 0.0246 (19) | 0.0280 (18) | 0.0220 (18) | −0.0012 (14) | 0.0016 (14) | −0.0010 (14) |
C21 | 0.0189 (18) | 0.0209 (15) | 0.0200 (17) | 0.0010 (13) | 0.0009 (13) | 0.0017 (13) |
C22 | 0.024 (2) | 0.0356 (19) | 0.0248 (19) | −0.0012 (15) | 0.0017 (15) | −0.0049 (15) |
C23 | 0.025 (2) | 0.050 (2) | 0.041 (2) | −0.0065 (18) | −0.0040 (17) | −0.0108 (19) |
C24 | 0.025 (2) | 0.061 (3) | 0.045 (3) | −0.0055 (19) | 0.0092 (19) | −0.004 (2) |
C25 | 0.031 (2) | 0.056 (2) | 0.030 (2) | 0.0044 (19) | 0.0115 (18) | −0.0018 (18) |
C26 | 0.027 (2) | 0.037 (2) | 0.0198 (18) | 0.0027 (16) | 0.0016 (15) | 0.0005 (15) |
C31 | 0.031 (2) | 0.0244 (17) | 0.0263 (19) | 0.0024 (15) | −0.0007 (15) | 0.0067 (14) |
N4 | 0.0311 (19) | 0.0309 (16) | 0.0340 (18) | 0.0045 (14) | −0.0024 (14) | 0.0025 (13) |
C32 | 0.032 (2) | 0.047 (2) | 0.052 (3) | 0.0032 (19) | −0.008 (2) | 0.012 (2) |
C33 | 0.035 (3) | 0.055 (3) | 0.067 (3) | 0.011 (2) | 0.005 (2) | 0.010 (2) |
C34 | 0.051 (3) | 0.039 (2) | 0.055 (3) | 0.014 (2) | 0.015 (2) | 0.001 (2) |
C35 | 0.044 (3) | 0.035 (2) | 0.036 (2) | 0.0047 (18) | 0.0039 (18) | −0.0032 (17) |
C41 | 0.0238 (19) | 0.0290 (17) | 0.0211 (17) | 0.0008 (14) | −0.0021 (14) | −0.0029 (14) |
C42 | 0.024 (2) | 0.0333 (19) | 0.0266 (19) | 0.0006 (15) | 0.0009 (15) | 0.0007 (15) |
C43 | 0.027 (2) | 0.050 (2) | 0.028 (2) | −0.0006 (18) | 0.0044 (16) | −0.0005 (17) |
C44 | 0.028 (2) | 0.060 (3) | 0.028 (2) | 0.0065 (19) | 0.0032 (16) | −0.0080 (19) |
C45 | 0.041 (3) | 0.040 (2) | 0.037 (2) | 0.0110 (18) | −0.0002 (18) | −0.0117 (18) |
C46 | 0.042 (2) | 0.0311 (19) | 0.028 (2) | 0.0027 (17) | 0.0016 (17) | −0.0041 (16) |
C51 | 0.027 (2) | 0.0181 (16) | 0.0275 (19) | −0.0019 (14) | 0.0017 (15) | −0.0029 (13) |
C52 | 0.028 (2) | 0.0332 (19) | 0.029 (2) | −0.0045 (16) | −0.0004 (16) | −0.0050 (15) |
C53 | 0.035 (2) | 0.043 (2) | 0.037 (2) | −0.0061 (18) | −0.0040 (18) | −0.0131 (18) |
C54 | 0.025 (2) | 0.035 (2) | 0.057 (3) | −0.0069 (17) | 0.0002 (18) | −0.0109 (19) |
C55 | 0.031 (2) | 0.040 (2) | 0.044 (2) | −0.0077 (18) | 0.0096 (18) | 0.0010 (18) |
C56 | 0.034 (2) | 0.037 (2) | 0.031 (2) | −0.0071 (17) | 0.0044 (17) | −0.0010 (16) |
C61 | 0.026 (2) | 0.0261 (17) | 0.0256 (18) | 0.0020 (15) | −0.0032 (15) | 0.0012 (14) |
C62 | 0.029 (2) | 0.0288 (18) | 0.0195 (18) | −0.0007 (15) | −0.0033 (15) | 0.0051 (14) |
P3 | 0.0191 (5) | 0.0207 (4) | 0.0184 (4) | −0.0002 (3) | 0.0024 (3) | −0.0002 (3) |
P4 | 0.0211 (5) | 0.0264 (4) | 0.0152 (4) | −0.0011 (4) | −0.0001 (3) | −0.0007 (3) |
C71 | 0.0247 (19) | 0.0226 (16) | 0.0191 (17) | −0.0020 (14) | 0.0055 (14) | −0.0007 (13) |
C72 | 0.028 (2) | 0.0237 (17) | 0.0208 (17) | 0.0033 (15) | 0.0051 (14) | 0.0025 (13) |
C73 | 0.023 (2) | 0.037 (2) | 0.029 (2) | −0.0033 (16) | 0.0066 (15) | 0.0008 (16) |
C74 | 0.037 (2) | 0.033 (2) | 0.031 (2) | −0.0112 (17) | 0.0091 (17) | 0.0015 (16) |
C75 | 0.040 (2) | 0.0245 (18) | 0.037 (2) | −0.0011 (17) | 0.0070 (18) | 0.0071 (16) |
C76 | 0.029 (2) | 0.0268 (18) | 0.0307 (19) | 0.0021 (15) | 0.0020 (16) | 0.0048 (15) |
C81 | 0.0196 (18) | 0.0315 (18) | 0.0201 (17) | 0.0045 (14) | 0.0007 (14) | −0.0002 (14) |
C82 | 0.047 (3) | 0.035 (2) | 0.033 (2) | 0.0011 (18) | 0.0119 (19) | −0.0032 (17) |
C83 | 0.064 (3) | 0.045 (2) | 0.035 (2) | 0.016 (2) | 0.012 (2) | −0.0095 (19) |
C84 | 0.037 (3) | 0.069 (3) | 0.031 (2) | 0.022 (2) | 0.0100 (19) | 0.001 (2) |
C85 | 0.035 (3) | 0.077 (3) | 0.044 (3) | −0.010 (2) | 0.020 (2) | −0.005 (2) |
C86 | 0.039 (3) | 0.052 (2) | 0.045 (3) | −0.012 (2) | 0.019 (2) | −0.012 (2) |
C91 | 0.0223 (19) | 0.0250 (17) | 0.0282 (19) | 0.0020 (14) | 0.0001 (15) | −0.0078 (14) |
C92 | 0.024 (2) | 0.042 (2) | 0.036 (2) | 0.0008 (17) | 0.0035 (16) | −0.0002 (17) |
C93 | 0.031 (2) | 0.052 (3) | 0.058 (3) | −0.0053 (19) | 0.015 (2) | 0.005 (2) |
C94 | 0.021 (2) | 0.046 (2) | 0.080 (4) | −0.0039 (18) | 0.003 (2) | −0.011 (2) |
C95 | 0.030 (2) | 0.043 (2) | 0.052 (3) | 0.0058 (19) | −0.0138 (19) | −0.013 (2) |
C96 | 0.030 (2) | 0.034 (2) | 0.032 (2) | 0.0044 (16) | −0.0054 (16) | −0.0035 (16) |
C101 | 0.0238 (19) | 0.0367 (19) | 0.0169 (17) | 0.0055 (15) | 0.0001 (14) | 0.0027 (14) |
C102 | 0.037 (2) | 0.036 (2) | 0.0211 (19) | 0.0094 (17) | −0.0016 (16) | −0.0006 (15) |
C103 | 0.057 (3) | 0.044 (2) | 0.027 (2) | 0.017 (2) | −0.0007 (19) | −0.0054 (17) |
C104 | 0.065 (3) | 0.059 (3) | 0.023 (2) | 0.024 (2) | 0.014 (2) | 0.0039 (19) |
C105 | 0.040 (3) | 0.070 (3) | 0.030 (2) | 0.009 (2) | 0.0145 (19) | 0.015 (2) |
C106 | 0.035 (2) | 0.047 (2) | 0.0225 (19) | 0.0027 (18) | 0.0051 (16) | 0.0057 (16) |
B1 | 0.090 (5) | 0.032 (2) | 0.042 (3) | −0.023 (3) | 0.015 (3) | −0.006 (2) |
F11 | 0.0766 (19) | 0.0377 (12) | 0.0389 (13) | −0.0116 (12) | 0.0123 (13) | −0.0034 (10) |
F12 | 0.093 (2) | 0.0527 (17) | 0.083 (2) | 0.0031 (16) | 0.0340 (19) | −0.0054 (15) |
F13 | 0.112 (3) | 0.089 (2) | 0.070 (2) | −0.045 (2) | −0.037 (2) | 0.0137 (18) |
F14 | 0.247 (5) | 0.0607 (19) | 0.067 (2) | −0.070 (3) | 0.088 (3) | −0.0181 (16) |
B2 | 0.062 (4) | 0.056 (3) | 0.033 (3) | −0.027 (3) | 0.016 (2) | −0.009 (2) |
F21 | 0.071 (2) | 0.0651 (18) | 0.131 (3) | −0.0384 (16) | 0.055 (2) | −0.0372 (19) |
F22 | 0.133 (3) | 0.111 (3) | 0.0303 (15) | −0.076 (2) | −0.0069 (17) | 0.0020 (15) |
F23 | 0.175 (6) | 0.090 (4) | 0.041 (3) | −0.075 (4) | 0.059 (3) | −0.037 (2) |
F24 | 0.102 (5) | 0.062 (3) | 0.200 (7) | 0.015 (3) | −0.088 (4) | −0.012 (4) |
Mo1—N1 | 1.755 (3) | C53—H53 | 0.9500 |
Mo1—F1 | 1.9889 (18) | C54—C55 | 1.377 (6) |
Mo1—P1 | 2.5032 (9) | C54—H54 | 0.9500 |
Mo1—P2 | 2.5353 (9) | C55—C56 | 1.398 (6) |
Mo1—P3 | 2.5698 (8) | C55—H55 | 0.9500 |
Mo1—P4 | 2.5754 (9) | C56—H56 | 0.9500 |
N1—N2 | 1.325 (5) | C61—C62 | 1.526 (5) |
N2—H1N2 | 0.9101 | C61—P3 | 1.848 (4) |
N2—H2N2 | 0.9100 | C61—H61A | 0.9900 |
C1—N3 | 1.464 (4) | C61—H61B | 0.9900 |
C1—P1 | 1.865 (3) | C62—P4 | 1.847 (3) |
C1—H1A | 0.9900 | C62—H62A | 0.9900 |
C1—H1B | 0.9900 | C62—H62B | 0.9900 |
N3—C31 | 1.358 (5) | P3—C71 | 1.829 (3) |
N3—C2 | 1.463 (4) | P3—C81 | 1.832 (3) |
C2—P2 | 1.873 (3) | P4—C91 | 1.826 (4) |
C2—H2A | 0.9900 | P4—C101 | 1.833 (3) |
C2—H2B | 0.9900 | C71—C72 | 1.396 (5) |
P1—C11 | 1.826 (3) | C71—C76 | 1.402 (5) |
P1—C21 | 1.828 (3) | C72—C73 | 1.388 (5) |
P2—C41 | 1.827 (3) | C72—H72 | 0.9500 |
P2—C51 | 1.831 (3) | C73—C74 | 1.382 (5) |
C11—C12 | 1.392 (5) | C73—H73 | 0.9500 |
C11—C16 | 1.396 (5) | C74—C75 | 1.377 (6) |
C12—C13 | 1.390 (5) | C74—H74 | 0.9500 |
C12—H12 | 0.9500 | C75—C76 | 1.393 (5) |
C13—C14 | 1.377 (6) | C75—H75 | 0.9500 |
C13—H13 | 0.9500 | C76—H76 | 0.9500 |
C14—C15 | 1.384 (5) | C81—C82 | 1.388 (5) |
C14—H14 | 0.9500 | C81—C86 | 1.391 (5) |
C15—C16 | 1.391 (5) | C82—C83 | 1.395 (6) |
C15—H15 | 0.9500 | C82—H82 | 0.9500 |
C16—H16 | 0.9500 | C83—C84 | 1.369 (6) |
C21—C26 | 1.395 (5) | C83—H83 | 0.9500 |
C21—C22 | 1.401 (5) | C84—C85 | 1.375 (7) |
C22—C23 | 1.388 (5) | C84—H84 | 0.9500 |
C22—H22 | 0.9500 | C85—C86 | 1.394 (6) |
C23—C24 | 1.383 (6) | C85—H85 | 0.9500 |
C23—H23 | 0.9500 | C86—H86 | 0.9500 |
C24—C25 | 1.385 (6) | C91—C92 | 1.389 (5) |
C24—H24 | 0.9500 | C91—C96 | 1.401 (5) |
C25—C26 | 1.389 (5) | C92—C93 | 1.393 (6) |
C25—H25 | 0.9500 | C92—H92 | 0.9500 |
C26—H26 | 0.9500 | C93—C94 | 1.382 (7) |
C31—N4 | 1.363 (5) | C93—H93 | 0.9500 |
C31—C35 | 1.413 (5) | C94—C95 | 1.372 (7) |
N4—C32 | 1.356 (5) | C94—H94 | 0.9500 |
N4—H4 | 0.8800 | C95—C96 | 1.395 (6) |
C32—C33 | 1.357 (6) | C95—H95 | 0.9500 |
C32—H32 | 0.9500 | C96—H96 | 0.9500 |
C33—C34 | 1.391 (7) | C101—C106 | 1.397 (5) |
C33—H33 | 0.9500 | C101—C102 | 1.398 (5) |
C34—C35 | 1.372 (6) | C102—C103 | 1.392 (5) |
C34—H34 | 0.9500 | C102—H102 | 0.9500 |
C35—H35 | 0.9500 | C103—C104 | 1.374 (7) |
C41—C42 | 1.385 (5) | C103—H103 | 0.9500 |
C41—C46 | 1.401 (5) | C104—C105 | 1.383 (7) |
C42—C43 | 1.396 (5) | C104—H104 | 0.9500 |
C42—H42 | 0.9500 | C105—C106 | 1.393 (6) |
C43—C44 | 1.374 (6) | C105—H105 | 0.9500 |
C43—H43 | 0.9500 | C106—H106 | 0.9500 |
C44—C45 | 1.383 (6) | B1—F14 | 1.358 (6) |
C44—H44 | 0.9500 | B1—F13 | 1.359 (7) |
C45—C46 | 1.397 (5) | B1—F12 | 1.397 (7) |
C45—H45 | 0.9500 | B1—F11 | 1.407 (6) |
C46—H46 | 0.9500 | B2—F24' | 1.241 (10) |
C51—C52 | 1.393 (5) | B2—F22 | 1.322 (5) |
C51—C56 | 1.394 (5) | B2—F23 | 1.330 (6) |
C52—C53 | 1.391 (5) | B2—F21 | 1.348 (5) |
C52—H52 | 0.9500 | B2—F24 | 1.475 (7) |
C53—C54 | 1.384 (6) | B2—F23' | 1.570 (10) |
N1—Mo1—F1 | 178.70 (11) | C55—C54—C53 | 119.8 (4) |
N1—Mo1—P1 | 86.88 (10) | C55—C54—H54 | 120.1 |
F1—Mo1—P1 | 91.94 (6) | C53—C54—H54 | 120.1 |
N1—Mo1—P2 | 86.22 (9) | C54—C55—C56 | 120.4 (4) |
F1—Mo1—P2 | 94.33 (6) | C54—C55—H55 | 119.8 |
P1—Mo1—P2 | 89.65 (3) | C56—C55—H55 | 119.8 |
N1—Mo1—P3 | 94.46 (9) | C51—C56—C55 | 120.5 (4) |
F1—Mo1—P3 | 85.10 (5) | C51—C56—H56 | 119.8 |
P1—Mo1—P3 | 95.38 (3) | C55—C56—H56 | 119.8 |
P2—Mo1—P3 | 174.95 (3) | C62—C61—P3 | 110.1 (2) |
N1—Mo1—P4 | 101.62 (10) | C62—C61—H61A | 109.6 |
F1—Mo1—P4 | 79.52 (6) | P3—C61—H61A | 109.6 |
P1—Mo1—P4 | 170.35 (3) | C62—C61—H61B | 109.6 |
P2—Mo1—P4 | 95.42 (3) | P3—C61—H61B | 109.6 |
P3—Mo1—P4 | 79.53 (3) | H61A—C61—H61B | 108.1 |
N2—N1—Mo1 | 177.1 (3) | C61—C62—P4 | 109.7 (2) |
N1—N2—H1N2 | 115.4 | C61—C62—H62A | 109.7 |
N1—N2—H2N2 | 125.8 | P4—C62—H62A | 109.7 |
H1N2—N2—H2N2 | 118.7 | C61—C62—H62B | 109.7 |
N3—C1—P1 | 110.7 (2) | P4—C62—H62B | 109.7 |
N3—C1—H1A | 109.5 | H62A—C62—H62B | 108.2 |
P1—C1—H1A | 109.5 | C71—P3—C81 | 105.51 (15) |
N3—C1—H1B | 109.5 | C71—P3—C61 | 104.13 (16) |
P1—C1—H1B | 109.5 | C81—P3—C61 | 100.27 (16) |
H1A—C1—H1B | 108.1 | C71—P3—Mo1 | 116.78 (11) |
C31—N3—C2 | 121.6 (3) | C81—P3—Mo1 | 121.04 (11) |
C31—N3—C1 | 123.4 (3) | C61—P3—Mo1 | 106.61 (11) |
C2—N3—C1 | 114.7 (3) | C91—P4—C101 | 104.34 (16) |
N3—C2—P2 | 115.4 (2) | C91—P4—C62 | 102.59 (16) |
N3—C2—H2A | 108.4 | C101—P4—C62 | 101.48 (16) |
P2—C2—H2A | 108.4 | C91—P4—Mo1 | 120.50 (12) |
N3—C2—H2B | 108.4 | C101—P4—Mo1 | 119.52 (12) |
P2—C2—H2B | 108.4 | C62—P4—Mo1 | 105.48 (11) |
H2A—C2—H2B | 107.5 | C72—C71—C76 | 118.6 (3) |
C11—P1—C21 | 106.26 (15) | C72—C71—P3 | 119.3 (2) |
C11—P1—C1 | 100.35 (15) | C76—C71—P3 | 122.1 (3) |
C21—P1—C1 | 99.87 (15) | C73—C72—C71 | 120.6 (3) |
C11—P1—Mo1 | 114.87 (11) | C73—C72—H72 | 119.7 |
C21—P1—Mo1 | 119.87 (11) | C71—C72—H72 | 119.7 |
C1—P1—Mo1 | 112.95 (11) | C74—C73—C72 | 120.6 (4) |
C41—P2—C51 | 103.36 (15) | C74—C73—H73 | 119.7 |
C41—P2—C2 | 102.80 (16) | C72—C73—H73 | 119.7 |
C51—P2—C2 | 99.92 (16) | C75—C74—C73 | 119.4 (3) |
C41—P2—Mo1 | 122.48 (11) | C75—C74—H74 | 120.3 |
C51—P2—Mo1 | 110.44 (11) | C73—C74—H74 | 120.3 |
C2—P2—Mo1 | 114.99 (11) | C74—C75—C76 | 121.0 (3) |
C12—C11—C16 | 118.8 (3) | C74—C75—H75 | 119.5 |
C12—C11—P1 | 120.0 (3) | C76—C75—H75 | 119.5 |
C16—C11—P1 | 120.8 (2) | C75—C76—C71 | 119.9 (3) |
C13—C12—C11 | 120.2 (3) | C75—C76—H76 | 120.1 |
C13—C12—H12 | 119.9 | C71—C76—H76 | 120.1 |
C11—C12—H12 | 119.9 | C82—C81—C86 | 118.3 (3) |
C14—C13—C12 | 120.7 (3) | C82—C81—P3 | 123.3 (3) |
C14—C13—H13 | 119.7 | C86—C81—P3 | 118.4 (3) |
C12—C13—H13 | 119.7 | C81—C82—C83 | 120.4 (4) |
C13—C14—C15 | 119.7 (3) | C81—C82—H82 | 119.8 |
C13—C14—H14 | 120.1 | C83—C82—H82 | 119.8 |
C15—C14—H14 | 120.1 | C84—C83—C82 | 120.8 (4) |
C14—C15—C16 | 120.0 (3) | C84—C83—H83 | 119.6 |
C14—C15—H15 | 120.0 | C82—C83—H83 | 119.6 |
C16—C15—H15 | 120.0 | C83—C84—C85 | 119.4 (4) |
C15—C16—C11 | 120.6 (3) | C83—C84—H84 | 120.3 |
C15—C16—H16 | 119.7 | C85—C84—H84 | 120.3 |
C11—C16—H16 | 119.7 | C84—C85—C86 | 120.5 (4) |
C26—C21—C22 | 119.1 (3) | C84—C85—H85 | 119.8 |
C26—C21—P1 | 118.7 (3) | C86—C85—H85 | 119.8 |
C22—C21—P1 | 122.0 (3) | C81—C86—C85 | 120.5 (4) |
C23—C22—C21 | 120.4 (3) | C81—C86—H86 | 119.7 |
C23—C22—H22 | 119.8 | C85—C86—H86 | 119.7 |
C21—C22—H22 | 119.8 | C92—C91—C96 | 118.9 (3) |
C24—C23—C22 | 120.1 (4) | C92—C91—P4 | 119.6 (3) |
C24—C23—H23 | 119.9 | C96—C91—P4 | 121.5 (3) |
C22—C23—H23 | 119.9 | C91—C92—C93 | 120.2 (4) |
C23—C24—C25 | 119.8 (4) | C91—C92—H92 | 119.9 |
C23—C24—H24 | 120.1 | C93—C92—H92 | 119.9 |
C25—C24—H24 | 120.1 | C94—C93—C92 | 120.6 (4) |
C24—C25—C26 | 120.7 (4) | C94—C93—H93 | 119.7 |
C24—C25—H25 | 119.6 | C92—C93—H93 | 119.7 |
C26—C25—H25 | 119.6 | C95—C94—C93 | 119.6 (4) |
C25—C26—C21 | 119.9 (3) | C95—C94—H94 | 120.2 |
C25—C26—H26 | 120.1 | C93—C94—H94 | 120.2 |
C21—C26—H26 | 120.1 | C94—C95—C96 | 120.6 (4) |
N3—C31—N4 | 120.0 (3) | C94—C95—H95 | 119.7 |
N3—C31—C35 | 123.8 (3) | C96—C95—H95 | 119.7 |
N4—C31—C35 | 116.2 (3) | C95—C96—C91 | 120.0 (4) |
C32—N4—C31 | 123.9 (4) | C95—C96—H96 | 120.0 |
C32—N4—H4 | 118.0 | C91—C96—H96 | 120.0 |
C31—N4—H4 | 118.0 | C106—C101—C102 | 119.1 (3) |
N4—C32—C33 | 120.4 (4) | C106—C101—P4 | 118.5 (3) |
N4—C32—H32 | 119.8 | C102—C101—P4 | 122.3 (3) |
C33—C32—H32 | 119.8 | C103—C102—C101 | 120.2 (4) |
C32—C33—C34 | 118.0 (4) | C103—C102—H102 | 119.9 |
C32—C33—H33 | 121.0 | C101—C102—H102 | 119.9 |
C34—C33—H33 | 121.0 | C104—C103—C102 | 120.4 (4) |
C35—C34—C33 | 121.6 (4) | C104—C103—H103 | 119.8 |
C35—C34—H34 | 119.2 | C102—C103—H103 | 119.8 |
C33—C34—H34 | 119.2 | C103—C104—C105 | 119.9 (4) |
C34—C35—C31 | 119.9 (4) | C103—C104—H104 | 120.1 |
C34—C35—H35 | 120.1 | C105—C104—H104 | 120.1 |
C31—C35—H35 | 120.1 | C104—C105—C106 | 120.7 (4) |
C42—C41—C46 | 119.4 (3) | C104—C105—H105 | 119.7 |
C42—C41—P2 | 120.3 (3) | C106—C105—H105 | 119.7 |
C46—C41—P2 | 120.3 (3) | C105—C106—C101 | 119.7 (4) |
C41—C42—C43 | 120.2 (3) | C105—C106—H106 | 120.1 |
C41—C42—H42 | 119.9 | C101—C106—H106 | 120.1 |
C43—C42—H42 | 119.9 | F14—B1—F13 | 111.3 (5) |
C44—C43—C42 | 120.2 (4) | F14—B1—F12 | 110.2 (5) |
C44—C43—H43 | 119.9 | F13—B1—F12 | 107.7 (4) |
C42—C43—H43 | 119.9 | F14—B1—F11 | 110.0 (4) |
C43—C44—C45 | 120.3 (4) | F13—B1—F11 | 110.5 (5) |
C43—C44—H44 | 119.8 | F12—B1—F11 | 107.1 (4) |
C45—C44—H44 | 119.8 | F24'—B2—F22 | 129.4 (8) |
C44—C45—C46 | 120.0 (4) | F24'—B2—F23 | 47.9 (8) |
C44—C45—H45 | 120.0 | F22—B2—F23 | 117.8 (4) |
C46—C45—H45 | 120.0 | F24'—B2—F21 | 115.8 (8) |
C45—C46—C41 | 119.8 (4) | F22—B2—F21 | 111.7 (4) |
C45—C46—H46 | 120.1 | F23—B2—F21 | 119.8 (4) |
C41—C46—H46 | 120.1 | F24'—B2—F24 | 57.5 (8) |
C52—C51—C56 | 118.2 (3) | F22—B2—F24 | 92.9 (5) |
C52—C51—P2 | 118.5 (3) | F23—B2—F24 | 102.6 (5) |
C56—C51—P2 | 123.0 (3) | F21—B2—F24 | 107.0 (4) |
C53—C52—C51 | 121.1 (4) | F24'—B2—F23' | 104.1 (9) |
C53—C52—H52 | 119.4 | F22—B2—F23' | 83.9 (6) |
C51—C52—H52 | 119.4 | F23—B2—F23' | 56.2 (5) |
C54—C53—C52 | 120.0 (4) | F21—B2—F23' | 99.8 (6) |
C54—C53—H53 | 120.0 | F24—B2—F23' | 152.2 (6) |
C52—C53—H53 | 120.0 |
Experimental details
Crystal data | |
Chemical formula | [MoF(N2H2)(C31H29N2P2)(C26H24P2)](BF4)2 |
Mr | 1208.49 |
Crystal system, space group | Monoclinic, P21/n |
Temperature (K) | 170 |
a, b, c (Å) | 12.5791 (6), 31.2199 (16), 13.8330 (9) |
β (°) | 94.438 (7) |
V (Å3) | 5416.2 (5) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 0.44 |
Crystal size (mm) | 0.2 × 0.08 × 0.06 |
Data collection | |
Diffractometer | Stoe IPDS1 diffractometer |
Absorption correction | Numerical (X-SHAPE; Stoe & Cie, 1998a) |
Tmin, Tmax | 0.949, 0.969 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 24176, 8538, 6783 |
Rint | 0.032 |
θmax (°) | 24.1 |
(sin θ/λ)max (Å−1) | 0.575 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.039, 0.108, 1.02 |
No. of reflections | 8538 |
No. of parameters | 706 |
No. of restraints | 39 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.94, −0.54 |
Computer programs: IPDS program package (Stoe & Cie, 1998b), IPDS program package, SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), DIAMOND (Brandenburg, 1999), CIFTAB in SHELXTL (Sheldrick, 2008).
Mo1—N1 | 1.755 (3) | Mo1—P2 | 2.5353 (9) |
Mo1—F1 | 1.9889 (18) | Mo1—P3 | 2.5698 (8) |
Mo1—P1 | 2.5032 (9) | Mo1—P4 | 2.5754 (9) |
N1—Mo1—F1 | 178.70 (11) | P1—Mo1—P3 | 95.38 (3) |
N1—Mo1—P1 | 86.88 (10) | P2—Mo1—P3 | 174.95 (3) |
F1—Mo1—P1 | 91.94 (6) | N1—Mo1—P4 | 101.62 (10) |
N1—Mo1—P2 | 86.22 (9) | F1—Mo1—P4 | 79.52 (6) |
F1—Mo1—P2 | 94.33 (6) | P1—Mo1—P4 | 170.35 (3) |
P1—Mo1—P2 | 89.65 (3) | P2—Mo1—P4 | 95.42 (3) |
N1—Mo1—P3 | 94.46 (9) | P3—Mo1—P4 | 79.53 (3) |
F1—Mo1—P3 | 85.10 (5) | N2—N1—Mo1 | 177.1 (3) |
Acknowledgements
This work is supported by the state of Schleswig-Holstein and the DFG (project number: Tu58/13–2, SPP1118).
References
Brandenburg, K. (1999). DIAMOND. Crystal Impact GbR, Bonn, Germany. Google Scholar
Hidai, M., Kodama, T., Sato, M., Harakawa, M. & Uchida, Y. (1976). Inorg. Chem. 15, 2694–2697. CSD CrossRef CAS Web of Science Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Stephan, G. C., Näther, C., Sivasankar, C. & Tuczek, F. (2008). Inorg. Chim. Acta, 361, 1008–1019. Web of Science CSD CrossRef CAS Google Scholar
Stoe & Cie (1998a). X-SHAPE. Stoe & Cie, Darmstadt, Germany. Google Scholar
Stoe & Cie (1998b). IPDS Program package. Stoe & Cie, Darmstadt, Germany Google Scholar
This is an open-access article distributed under the terms of the Creative Commons Attribution (CC-BY) Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.
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.