supporting information&Acta Cryst. (2011). E67, m94-m95&&&&[
Bis[1,3-bis­(2,4,6-trimethyl­phen­yl)-2,3-dihydro-1H-imidazol-2-yl­idene]dinitros­yl(tetra­hydro­borato-2H,H')tungsten(0),
In the title paramagnetic 19-electron neutral complex, [W(BH4)(C21H24N2)2(NO)2], the W(0) atom is coordinated by two 1,3-bis­(2,4,6-trimethyl­phen­yl)imidazol-2-yl­idene (IMes) carbene ligands, two NO groups and two H atoms of an 2-tetra­hydro­borate ligand. Depending on the number of coordination sites (n) assigned to the BH4- ligand, the coordination geometry of the W atom may either be described as approximately trigonal-bipyramidal (n = 1) or as very distorted octa­hedral with the bridging H atoms filling two coordination positions (n = 2). In the latter case, the coplanar NO groups and bridging H atoms (r.m.s. deviation = 0.032&&A) form one octa­hedral plane, with mutually trans-oriented carbene ligands. In the crystal, mol­ecules are connected via C-HO inter­actions.
In the course of our efforts on the synthesis of novel dinitrosyl hydride and
dihydride tungsten derivatives bearing sterically demanding and highly
donating phosphine ligands or N-heterocyclic (NHC) carbene ligands
(Fraga-Hernández, 2007), the title compound, C42H52BN6O2W,
synthesized as an intermediate species.The reaction of the recently reported compound W(NO)2Cl2(IMes)2
(Fraga-Hernández, 2011) with [NBu4][BH4] in THF furnished the
complex W(NO)2(IMes)2(2-BH4). The one-electron reduction of the
starting material to yield the title paramagnetic 19-electron neutral complex
can be explained considering that [NBu4][BH4] can act as a
hydride-transfer reagent, as well as a reducing agent. In (I), the oxidation
number of the W atom is formally –I. Nevertheless, a density functional
theory (DFT) study combined with EPR measurements (Fraga-Hernández,
indicated that the unpaired electron is delocalized on the two N atoms of the
nitrosyl groups (and not on the metal center) which become equivalent and the
oxidation number of the W atom is in fact 0, considering BH4- and
(NO)2+.The W metal center is coordinated by two
1,3-bis(2,4,6-trimethylphenyl)imidazol-2-ylidene (IMes) carbene ligands, two
NO groups and two H atoms of an 2-tetrahydroborate ligand (Fig. 1).
Depending on the number of coordination sites (n) occupied by the
BH4- ligand, the molecular structure of the title compound consists of an
approximately trigonal bipyramidal arrangement of the ligands around the W
atom (n = 1) or might be referred to a very distorted octahedral
environment around the W center with the bridging H atoms filling two
coordination positions (n = 2). In the latter case, the trans
carbene ligands occupy axial positions, and the coplanar NO groups and
bridging H atoms (r.m.s. deviation = 0.032 Å) form the equatorial plane of a
pseudo octahedron. The two nitrosyl ligands with a N(2)—W(1)—N(1)
bond angle of 100.4 (2)° are located trans to the bridging borohydride
moiety. The N(1)—W(1)—C(1) and N(2)—W(1)—C(1) bond angles show that
the carbene ligands are bent toward the bridging borohydride group (98.5 (2)
and 96.1 (2)°) and away from the NO groups. This bending [C(1)—W(1)—C(22)
= 158.4 (2)°] may be due to the electronic effects caused by the strong
-acceptor groups. In comparison with the dichlorido compound
W(NO)2Cl2(IMes)2 (Fraga-Hernández, 2011) where the
five-membered rings
of the carbene ligands are almost perpendicular to each other, they would be
coplanar in (I) without the bending. The W—N—O bond angles [177.1 (5)° for
O(1)—N(1)—W(1), and 176.0 (5)° for O(2)—N(2)—W(1)] are almost linear
and indicate the coordination in form of nitrosonium groups (NO+). In the
structure the two NO ligands are equivalent and the W—N—O bond angles are
not far from linearity (average of 176.6°).In the crystal structure, molecules are connected via C—H···O
interactions (Table 1).
For the synthesis, characterization and reactivity of dinitrosyl tungsten
complexes in various oxidation states, see: Fraga-Hernández (2007).
related complex with the W(NO)(2-BH4) core, see: van der Zeijden et
al. (1991). For tungsten complexes with N-heterocyclic (NHC)
carbenes, see: Nonnenmacher et al. (2005); Hahn et al.
Wu et al. (2007); Fraga-Hernández et al.
(2011). For an
overview of the first organometallic nitrosyls known, see: Enemark & Feltham
(1974); Richter-Addo & Legzdins (1988); Berke & Burger
A mixture of [W(NO)2Cl2(IMes)2] (90 mg, 0.097 mmol) (Fraga-Hernández,
2011) and [NBu4]BH4 (49.7 mg, 0.195 mmol) in 10 ml ether and 5 ml
stirred for 21 h. After this time, the black green solution was filtered over
celite and dried under vacuum. The residue was extracted with 15 ml of
ether/pentane (1:2) and filtered over celite again. Removal of the solvent
left a dark green solid, which was extracted with pentane (3 x 8 ml)
and dried under vacuum, affording 62 mg of the title compound (0.071 mmol,
74%). Green crystals were obtained from a pentane solution at room
temperature. IR (ATR, 22°C, cm-1): 1597 (NO), 1537 (NO). Elemental analysis
(%) calculated for C42H52BN6O2W: C (58.14), H (6.04), N (9.68);
found: C (58.40), H (5.86), N (9.78).
The H atoms of the tetrahydroborate group were located in difference Fourier
maps. Their coordinates were freely refined, except for H1D, with
Uiso(H) = 1.2Ueq(B). All other H positions were calculated
after each cycle of refinement using a riding model with C—H = 0.93 Å and
Uiso(H) = 1.2Ueq(C) for aromatic H atoms, and with C—H =
0.96 Å and Uiso(H) = 1.5Ueq(C) for methyl H atoms.
Data collection: EXPOSE in IPDS Software (Stoe & Cie, 1999); cell refinement: CELL in IPDS Software (Stoe & Cie, 1999); data reduction: INTEGRATE in IPDS Software (Stoe & Cie, 1999); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008), WinGX (Farrugia, 1999) and publCIF
(Westrip, 2010).
View of the title compound showing the labeling of the non-H atoms and
30% probability ellipsoids.
[W(BH4)(C21H24N2)2(NO)2]F(000) = 1764Mr = 867.56Dx = 1.392 Mg m3Monoclinic, P21/cMo K radiation,
= 0.71073 ÅHall symbol:
-P 2ybcCell parameters from 7998 reflectionsa = 24.7322 (13) Å = 2.5b = 11.2183 (5) ŵ = 2.83 mm1c = 15.0522 (8) ÅT = 183 K = 97.643 (6)°Irregular, dark greenV = )
Å30.3 × 0.2 × 0.18 mmZ = 4
Stoe IPDS diffractometer9946 independent reflectionsRadiation source: fine-focus sealed tube5931 reflections with I > 2(I)Graphite monochromatorRint = 0.072 oscillation scanmax = 28.0°, min = 2.5°Absorption correction: numerical (Coppens et al., 1965)h = 3232Tmin = 0.551, Tmax = 0.725k = 01448806 measured reflectionsl = 019
Refinement on F20 restraintsLeast-squares matrix: fullH atoms treated by a mixture of independent and constrained refinementR[F2 > 2(F2)] = 0.037
w = 1/[2(Fo2) + (0.0497P)2]
where P = (Fo2 + 2Fc2)/3wR(F2) = 0.113(Δ/)max = 0.001S = 1.02Δmax = 2.07 e Å39946 reflectionsΔmin = 0.60 e Å3490 parameters
[W(BH4)(C21H24N2)2(NO)2]V = )
Å3Mr = 867.56Z = 4Monoclinic, P21/cMo K radiationa = 24.7322 (13) ŵ = 2.83 mm1b = 11.2183 (5) ÅT = 183 Kc = 15.0522 (8) Å0.3 × 0.2 × 0.18 mm = 97.643 (6)°
Stoe IPDS diffractometer9946 independent reflectionsAbsorption correction: numerical (Coppens et al., 1965)5931 reflections with I > 2(I)Tmin = 0.551, Tmax = 0.725Rint = 0.07248806 measured reflections
R[F2 > 2(F2)] = 0.0370 restraintswR(F2) = 0.113H atoms treated by a mixture of independent and constrained refinementS = 1.02Δmax = 2.07 e Å39946 reflectionsΔmin = 0.60 e Å3490 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
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.
xyzUiso*/UeqW10.)0.46192 (2)0.)0.03782 (8)B10.2475 (4)0.5990 (9)0.6041 (6)0.058 (2)H1A0.257 (3)0.567 (7)0.539 (5)0.07*H1B0.208 (3)0.538 (8)0.629 (5)0.07*H1C0.244 (3)0.698 (8)0.618 (5)0.07*H1D0.27980.56320.65640.07*N10.3114 (2)0.4285 (5)0.8134 (3)0.0415 (12)O10.34901 (19)0.4039 (4)0.8701 (3)0.0474 (11)N20.2018 (2)0.3667 (5)0.7721 (3)0.0433 (13)O20.1703 (2)0.3013 (5)0.8032 (3)0.0550 (13)N30.3202 (2)0.3248 (5)0.5926 (3)0.0419 (12)N40.2357 (2)0.2813 (5)0.5619 (3)0.0425 (13)C10.2711 (3)0.3409 (5)0.6230 (4)0.0370 (14)C20.3145 (3)0.2579 (6)0.5145 (4)0.0492 (17)H20.34230.23530.48210.059*C30.2621 (3)0.2324 (7)0.4950 (4)0.0498 (18)H30.2460.18960.44560.06*C40.3720 (3)0.3646 (6)0.6380 (4)0.0447 (15)C50.3978 (3)0.4602 (8)0.6032 (5)0.0566 (17)C60.4463 (4)0.4984 (8)0.6517 (7)0.072 (2)H60.46420.56350.63080.086*C70.4687 (3)0.4438 (8)0.7288 (6)0.069 (2)C80.4441 (3)0.3442 (8)0.7580 (5)0.059 (2)H80.46040.30420.80870.071*C90.3949 (3)0.3021 (7)0.7126 (5)0.0484 (16)C100.3752 (4)0.5222 (8)0.5180 (6)0.075 (2)H10A0.39690.50290.47180.112*H10B0.33830.49670.50020.112*H10C0.37580.60680.52770.112*C110.5211 (4)0.4909 (10)0.7822 (8)0.105 (4)H11A0.51510.57030.80260.157*H11B0.53150.44010.83290.157*H11C0.54960.49190.74470.157*C120.3676 (3)0.1923 (7)0.7442 (5)0.0548 (18)H12A0.33320.21410.76270.082*H12B0.36160.13560.69620.082*H12C0.39060.15760.79390.082*C130.1794 (3)0.2590 (7)0.5674 (4)0.0476 (16)C140.1395 (3)0.3205 (7)0.5122 (5)0.0569 (19)C150.0857 (3)0.2897 (9)0.5158 (6)0.071 (2)H150.05850.33120.47990.085*C160.0707 (3)0.2005 (9)0.5702 (7)0.076 (2)C170.1120 (4)0.1411 (8)0.6236 (5)0.068 (2)H170.10260.08140.66170.081*C180.1665 (3)0.1669 (7)0.6226 (5)0.0541 (18)C190.1535 (3)0.4164 (8)0.4485 (5)0.066 (2)H19A0.13370.48790.45820.099*H19B0.19190.43220.45890.099*H19C0.14360.390.38780.099*C200.0121 (4)0.1635 (13)0.5706 (9)0.117 (4)H20A0.01060.23310.56810.176*H20B0.00090.1140.51940.176*H20C0.00890.11970.62440.176*C210.2104 (3)0.0944 (7)0.6778 (5)0.062 (2)H21A0.230.14430.72290.092*H21B0.19390.02960.70610.092*H21C0.23510.06330.63950.092*N50.2647 (3)0.7156 (5)0.8370 (3)0.0529 (15)N60.1797 (3)0.6770 (6)0.7943 (4)0.0559 (16)C220.2305 (3)0.6296 (6)0.7970 (4)0.0448 (16)C230.2356 (5)0.8127 (8)0.8591 (5)0.077 (3)H230.24980.88140.88780.092*C240.1834 (4)0.7903 (8)0.8319 (5)0.074 (3)H240.15440.84140.83710.089*C250.3226 (3)0.7031 (6)0.8652 (4)0.0523 (18)C260.3584 (4)0.7573 (7)0.8163 (5)0.060 (2)C270.4138 (4)0.7520 (8)0.8493 (5)0.067 (2)H270.43890.78610.8160.08*C280.4325 (4)0.6977 (8)0.9301 (5)0.063 (2)C290.3953 (3)0.6464 (7)0.9765 (4)0.058 (2)H290.40780.60941.03070.07*C300.3397 (3)0.6459 (6)0.9476 (4)0.0510 (18)C310.3403 (4)0.8205 (9)0.7283 (6)0.081 (3)H31A0.30330.79890.70680.122*H31B0.34260.90520.73740.122*H31C0.36360.79760.68510.122*C320.4925 (4)0.7018 (10)0.9671 (6)0.084 (3)H32A0.51360.71650.91910.127*H32B0.49870.76461.01060.127*H32C0.50320.6270.9950.127*C330.2994 (4)0.5898 (7)1.0002 (4)0.062 (2)H33A0.31840.54941.05130.093*H33B0.27630.65031.02010.093*H33C0.27760.53350.96320.093*C340.1293 (3)0.6155 (8)0.7676 (5)0.0575 (19)C350.0990 (4)0.6413 (9)0.6850 (6)0.074 (3)C360.0511 (4)0.5790 (11)0.6639 (7)0.089 (3)H360.03020.59410.6090.106*C370.0321 (4)0.4949 (11)0.7199 (8)0.092 (3)C380.0629 (4)0.4782 (10)0.8025 (7)0.082 (3)H380.05040.42470.84230.098*C390.1115 (3)0.5372 (10)0.8290 (5)0.068 (2)C400.1164 (4)0.7322 (10)0.6218 (6)0.089 (3)H40A0.11780.80930.64970.133*H40B0.15180.71180.60710.133*H40C0.09070.73370.56810.133*C410.0214 (5)0.4306 (13)0.6941 (10)0.129 (5)H41A0.05060.47730.71210.193*H41B0.02740.41930.63030.193*H41C0.02020.35450.72340.193*C420.1424 (4)0.5191 (10)0.9213 (5)0.080 (3)H42A0.13960.58960.95650.12*H42B0.12710.45260.94960.12*H42C0.180.50350.91650.12*
U11U22U33U12U13U23W10.04481 (14)0.03601 (12)0.03189 (11)0.00153 (16)0.00228 (8)0.00023 (13)B10.080 (7)0.055 (5)0.037 (4)0.007 (5)0.000 (4)0.012 (4)N10.051 (3)0.037 (3)0.037 (3)0.004 (2)0.010 (2)0.003 (2)O10.053 (3)0.051 (3)0.036 (2)0.005 (2)0.005 (2)0.002 (2)N20.045 (3)0.046 (3)0.036 (3)0.012 (3)0.004 (2)0.000 (2)O20.053 (3)0.063 (3)0.050 (3)0.011 (3)0.012 (2)0.007 (2)N30.045 (3)0.042 (3)0.039 (3)0.003 (2)0.007 (2)0.004 (2)N40.052 (3)0.042 (3)0.032 (3)0.006 (3)0.002 (2)0.004 (2)C10.042 (4)0.035 (3)0.034 (3)0.004 (3)0.006 (3)0.001 (2)C20.062 (5)0.049 (4)0.038 (3)0.002 (4)0.015 (3)0.008 (3)C30.059 (5)0.055 (5)0.034 (3)0.005 (4)0.003 (3)0.010 (3)C40.043 (4)0.047 (4)0.045 (3)0.004 (3)0.011 (3)0.009 (3)C50.053 (4)0.049 (4)0.070 (4)0.001 (4)0.017 (3)0.002 (4)C60.055 (5)0.058 (5)0.105 (7)0.012 (4)0.020 (5)0.011 (4)C70.046 (4)0.062 (6)0.098 (6)0.003 (4)0.006 (4)0.017 (5)C80.045 (4)0.069 (5)0.063 (4)0.009 (4)0.000 (3)0.012 (4)C90.045 (4)0.046 (4)0.054 (4)0.002 (3)0.009 (3)0.006 (3)C100.083 (6)0.061 (6)0.084 (6)0.010 (5)0.023 (5)0.020 (5)C110.051 (5)0.100 (9)0.154 (10)0.011 (5)0.019 (5)0.037 (7)C120.059 (5)0.047 (4)0.057 (4)0.011 (4)0.000 (3)0.005 (3)C130.048 (4)0.051 (4)0.043 (4)0.014 (3)0.004 (3)0.012 (3)C140.051 (4)0.062 (5)0.054 (4)0.005 (4)0.005 (3)0.003 (4)C150.045 (5)0.088 (7)0.076 (5)0.007 (4)0.007 (4)0.005 (5)C160.049 (5)0.084 (7)0.093 (6)0.015 (5)0.004 (4)0.004 (5)C170.081 (6)0.063 (5)0.062 (5)0.026 (5)0.021 (4)0.002 (4)C180.060 (5)0.050 (4)0.053 (4)0.013 (4)0.010 (3)0.005 (3)C190.069 (5)0.059 (5)0.065 (5)0.002 (4)0.013 (4)0.011 (4)C200.059 (6)0.133 (12)0.160 (11)0.030 (7)0.016 (6)0.008 (9)C210.073 (5)0.046 (4)0.067 (5)0.009 (4)0.014 (4)0.009 (4)N50.075 (4)0.038 (3)0.042 (3)0.005 (3)0.007 (3)0.010 (2)N60.072 (4)0.049 (4)0.044 (3)0.022 (3)0.004 (3)0.007 (3)C220.064 (4)0.038 (4)0.033 (3)0.012 (3)0.007 (3)0.001 (3)C230.118 (8)0.051 (5)0.055 (5)0.024 (5)0.009 (5)0.016 (4)C240.096 (7)0.059 (5)0.062 (5)0.039 (5)0.006 (5)0.012 (4)C250.067 (5)0.039 (4)0.046 (4)0.004 (4)0.009 (3)0.009 (3)C260.081 (6)0.046 (4)0.048 (4)0.013 (4)0.014 (4)0.002 (3)C270.083 (6)0.060 (5)0.054 (4)0.020 (5)0.001 (4)0.004 (4)C280.073 (5)0.060 (5)0.051 (4)0.011 (4)0.011 (4)0.007 (4)C290.080 (6)0.051 (5)0.038 (4)0.007 (4)0.013 (4)0.006 (3)C300.076 (5)0.039 (4)0.035 (3)0.000 (4)0.002 (3)0.007 (3)C310.091 (7)0.075 (6)0.070 (5)0.023 (5)0.017 (5)0.024 (5)C320.077 (6)0.091 (7)0.078 (6)0.011 (6)0.014 (5)0.006 (5)C330.089 (6)0.060 (5)0.034 (3)0.010 (4)0.003 (3)0.005 (3)C340.051 (4)0.060 (5)0.061 (4)0.023 (4)0.005 (3)0.003 (4)C350.067 (6)0.083 (7)0.067 (5)0.027 (5)0.003 (4)0.003 (5)C360.064 (6)0.110 (9)0.086 (6)0.021 (6)0.013 (5)0.011 (6)C370.052 (5)0.101 (9)0.120 (9)0.023 (5)0.003 (5)0.007 (7)C380.067 (6)0.089 (7)0.094 (6)0.029 (6)0.026 (5)0.014 (6)C390.054 (5)0.086 (6)0.065 (5)0.032 (5)0.013 (4)0.002 (5)C400.085 (7)0.100 (8)0.075 (6)0.028 (6)0.016 (5)0.016 (5)C410.068 (7)0.136 (14)0.177 (12)0.001 (7)0.001 (7)0.010 (9)C420.085 (6)0.104 (8)0.055 (4)0.027 (6)0.025 (4)0.012 (5)
W1—N11.813 (5)C20—H20A0.96W1—N21.814 (6)C20—H20B0.96W1—C12.221 (6)C20—H20C0.96W1—C222.223 (6)C21—H21A0.96W1—B12.451 (8)C21—H21B0.96W1—H1B1.98 (8)C21—H21C0.96W1—H1D1.8N5—C221.371 (9)B1—H1A1.11 (8)N5—C231.371 (10)B1—H1B1.29 (8)N5—C251.443 (10)B1—H1C1.13 (9)N6—C221.358 (9)B1—H1D1.12N6—C241.389 (10)N1—O11.209 (6)N6—C341.436 (10)N2—O21.207 (7)C23—C241.324 (13)N3—C11.366 (8)C23—H230.93N3—C21.385 (8)C24—H240.93N3—C41.440 (8)C25—C261.368 (11)N4—C11.359 (8)C25—C301.411 (9)N4—C31.384 (9)C26—C271.395 (12)N4—C131.428 (9)C26—C311.516 (10)C2—C31.322 (10)C27—C281.383 (11)C2—H20.93C27—H270.93C3—H30.93C28—C291.356 (12)C4—C91.379 (10)C28—C321.515 (12)C4—C51.386 (10)C29—C301.387 (11)C5—C61.386 (11)C29—H290.93C5—C101.500 (11)C30—C331.492 (11)C6—C71.363 (13)C31—H31A0.96C6—H60.93C31—H31B0.96C7—C81.372 (12)C31—H31C0.96C7—C111.526 (11)C32—H32A0.96C8—C91.396 (10)C32—H32B0.96C8—H80.93C32—H32C0.96C9—C121.512 (10)C33—H33A0.96C10—H10A0.96C33—H33B0.96C10—H10B0.96C33—H33C0.96C10—H10C0.96C34—C391.387 (12)C11—H11A0.96C34—C351.394 (11)C11—H11B0.96C35—C361.377 (14)C11—H11C0.96C35—C401.496 (14)C12—H12A0.96C36—C371.387 (15)C12—H12B0.96C36—H360.93C12—H12C0.96C37—C381.382 (14)C13—C141.386 (10)C37—C411.512 (15)C13—C181.389 (10)C38—C391.384 (13)C14—C151.380 (11)C38—H380.93C14—C191.512 (11)C39—C421.507 (11)C15—C161.375 (13)C40—H40A0.96C15—H150.93C40—H40B0.96C16—C171.384 (13)C40—H40C0.96C16—C201.508 (13)C41—H41A0.96C17—C181.382 (11)C41—H41B0.96C17—H170.93C41—H41C0.96C18—C211.514 (11)C42—H42A0.96C19—H19A0.96C42—H42B0.96C19—H19B0.96C42—H42C0.96C19—H19C0.96
N1N2100.4 (2)H19AH19C109.5N1C198.5 (2)H19BH19C109.5N2C196.1 (2)C16H20A109.5N1C2295.6 (2)C16H20B109.5N2C2297.3 (3)H20AH20B109.5C1C22158.4 (2)C16H20C109.5N1B1127.9 (3)H20AH20C109.5N2B1131.7 (3)H20BH20C109.5C1B178.4 (3)C18H21A109.5C22B180.0 (3)C18H21B109.5N1H1B159 (2)H21AH21B109.5N2H1B100 (2)C18H21C109.5C1H1B80 (2)H21AH21C109.5C22H1B81 (2)H21BH21C109.5N1H1D103C22C23110.5 (7)N2H1D156C22C25126.3 (6)C1H1D78C23C25122.6 (7)C22H1D83C22C24109.7 (7)H1BH1D57C22C34125.8 (6)W1H1A120 (4)C24C34124.1 (7)H1AH1B110 (5)N6N5104.6 (6)W1H1C118 (4)N6W1126.8 (5)H1AH1C121 (6)N5W1128.0 (5)H1BH1C112 (6)C24N5107.3 (8)H1AH1D107C24H23126.3H1BH1D96N5H23126.3H1CH1D107C23N6107.9 (7)O1W1177.1 (5)C23H24126.1O2W1176.0 (5)N6H24126.1C1C2111.2 (5)C26C30122.4 (7)C1C4125.0 (5)C26N5119.1 (6)C2C4123.7 (5)C30N5118.2 (7)C1C3111.3 (5)C25C27117.7 (7)C1C13126.3 (5)C25C31122.8 (8)C3C13122.1 (5)C27C31119.5 (8)N4N3103.3 (5)C28C26122.0 (8)N4W1128.5 (5)C28H27119N3W1127.4 (4)C26H27119C3N3107.0 (6)C29C27118.0 (8)C3H2126.5C29C32121.4 (7)N3H2126.5C27C32120.5 (8)C2N4107.3 (6)C28C30123.5 (7)C2H3126.4C28H29118.2N4H3126.4C30H29118.2C9C5122.8 (6)C29C25116.3 (7)C9N3118.2 (6)C29C33122.7 (6)C5N3119.0 (6)C25C33121.0 (7)C6C4116.7 (7)C26H31A109.5C6C10120.3 (8)C26H31B109.5C4C10122.9 (7)H31AH31B109.5C7C5122.3 (8)C26H31C109.5C7H6118.9H31AH31C109.5C5H6118.9H31BH31C109.5C6C8119.5 (8)C28H32A109.5C6C11120.9 (9)C28H32B109.5C8C11119.7 (9)H32AH32B109.5C7C9120.8 (8)C28H32C109.5C7H8119.6H32AH32C109.5C9H8119.6H32BH32C109.5C4C8117.6 (7)C30H33A109.5C4C12121.2 (6)C30H33B109.5C8C12121.2 (7)H33AH33B109.5C5H10A109.5C30H33C109.5C5H10B109.5H33AH33C109.5H10AH10B109.5H33BH33C109.5C5H10C109.5C39C35123.1 (8)H10AH10C109.5C39N6117.2 (7)H10BH10C109.5C35N6119.6 (8)C7H11A109.5C36C34116.3 (9)C7H11B109.5C36C40120.8 (8)H11AH11B109.5C34C40122.9 (9)C7H11C109.5C35C37123.7 (9)H11AH11C109.5C35H36118.1H11BH11C109.5C37H36118.1C9H12A109.5C38C36116.6 (10)C9H12B109.5C38C41121.7 (12)H12AH12B109.5C36C41121.5 (11)C9H12C109.5C37C39123.3 (10)H12AH12C109.5C37H38118.4H12BH12C109.5C39H38118.4C14C18121.7 (7)C38C34116.8 (8)C14N4120.0 (6)C38C42121.0 (9)C18N4117.9 (6)C34C42122.3 (9)C15C13117.7 (8)C35H40A109.5C15C19120.3 (7)C35H40B109.5C13C19121.9 (7)H40AH40B109.5C16C14122.9 (8)C35H40C109.5C16H15118.6H40AH40C109.5C14H15118.6H40BH40C109.5C15C17117.4 (8)C37H41A109.5C15C20122.6 (9)C37H41B109.5C17C20120.0 (10)H41AH41B109.5C18C16122.5 (8)C37H41C109.5C18H17118.7H41AH41C109.5C16H17118.7H41BH41C109.5C17C13117.7 (7)C39H42A109.5C17C21120.7 (7)C39H42B109.5C13C21121.5 (7)H42AH42B109.5C14H19A109.5C39H42C109.5C14H19B109.5H42AH42C109.5H19AH19B109.5H42BH42C109.5C14H19C109.5
D—H···AD—HH···AD···AD—H···AC2··O1i0.932.323.040 (8)134Symmetry code:
(i) x, y1/2, z1/2.
Crystal dataChemical formula[W(BH4)(C21H24N2)2(NO)2]Mr867.56Crystal system, space groupMonoclinic, P21/cTemperature (K)183a, b, c (Å)24.7322 (13), 11.2183 (5), 15.0522 (8) (°) 97.643 (6)V (Å3))Z4Radiation typeMo Kµ (mm1)2.83Crystal size (mm)0.3 × 0.2 × 0.18 Data collectionDiffractometerStoe IPDS diffractometerAbsorption correctionNumerical (Coppens et al., 1965)
Tmin, Tmax0.551, 0.725No. of measured, independent and observed [I > 2(I)] reflections4, 5931
Rint0.072(sin /)max (Å1)0.661 RefinementR[F2 > 2(F2)], wR(F2), S 0.037,
1.02No. of reflections9946No. of parameters490H-atom treatmentH atoms treated by a mixture of independent and constrained refinementΔmax, Δmin (e Å3)2.07, 0.60
-->Hydrogen-bond geometry (Å, º)
D—H···AD—HH···AD···AD—H···AC2··O1i0.932.323.040 (8)134Symmetry code:
(i) x, y1/2, z1/2.
Financial support by the University of Zurich is gratefully acknowledged.