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The title compound, [Mo(C5H9N)3(CO)3], was produced from Mo(CO)6 and tert-butyl isocyanide in the presence of 10 atm of carbon monoxide (1 atm = 101325 Pa). The octa­hedral complex shows a facial arrangement of the ligands, the Mo—C distances of the isocyanide ligands being about 0.15 Å longer than the corresponding bond lengths of the carbonyl ligands. The crystal structure is influenced by one short C—H...·O contact, resulting in infinite chains which are inter­connected by additional weak C—H...·O inter­actions.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806004181/ac2003sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806004181/ac2003Isup2.hkl
Contains datablock I

CCDC reference: 601090

Key indicators

  • Single-crystal X-ray study
  • T = 183 K
  • Mean [sigma](C-C) = 0.007 Å
  • R factor = 0.052
  • wR factor = 0.117
  • Data-to-parameter ratio = 22.2

checkCIF/PLATON results

No syntax errors found



Datablock: I


Alert level B PLAT220_ALERT_2_B Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.92 Ratio PLAT242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C12
Alert level C PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Mo - C11 .. 6.18 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Mo - C17 .. 5.43 su PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C2 PLAT480_ALERT_4_C Long H...A H-Bond Reported H15B .. O3 .. 2.81 Ang. PLAT480_ALERT_4_C Long H...A H-Bond Reported H9B .. O3 .. 2.82 Ang. PLAT480_ALERT_4_C Long H...A H-Bond Reported H8A .. O1 .. 2.85 Ang. PLAT481_ALERT_4_C Long D...A H-Bond Reported C8 .. O1 .. 3.75 Ang.
0 ALERT level A = In general: serious problem 2 ALERT level B = Potentially serious problem 7 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 5 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 4 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: COLLECT, Nonius 1998; cell refinement: DENZO (Otwinowski & Minor, 1997); data reduction: DENZO; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP (Siemens, 1990); software used to prepare material for publication: XP.

fac-Tris(tert-butyl isocyanide)tricarbonylmolybdenum(0) top
Crystal data top
[Mo(C5H9N)3(CO)3]F(000) = 888
Mr = 429.37Dx = 1.280 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P2ynCell parameters from 3828 reflections
a = 9.5070 (3) Åθ = 1.9–27.4°
b = 15.6817 (7) ŵ = 0.61 mm1
c = 15.3422 (6) ÅT = 183 K
β = 103.149 (3)°Quader, light yellow
V = 2227.34 (15) Å30.03 × 0.03 × 0.03 mm
Z = 4
Data collection top
Nonius KappaCCD
diffractometer
3828 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.033
Graphite monochromatorθmax = 27.4°, θmin = 1.9°
φ and ω scansh = 1212
8441 measured reflectionsk = 2018
5027 independent reflectionsl = 1919
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.052Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.117H-atom parameters constrained
S = 1.10 w = 1/[σ2(Fo2) + (0.0275P)2 + 4.4505P]
where P = (Fo2 + 2Fc2)/3
5027 reflections(Δ/σ)max < 0.001
226 parametersΔρmax = 0.59 e Å3
0 restraintsΔρmin = 1.06 e Å3
Special details top

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) top
xyzUiso*/Ueq
Mo0.45122 (4)0.18065 (2)0.74608 (2)0.03286 (11)
O10.4080 (5)0.3620 (2)0.8238 (3)0.0778 (12)
O20.5498 (4)0.2804 (2)0.5920 (2)0.0520 (8)
O30.7652 (4)0.1790 (2)0.8693 (2)0.0591 (9)
C10.2311 (4)0.1786 (3)0.6725 (3)0.0415 (9)
C60.3673 (4)0.1059 (3)0.8407 (3)0.0388 (9)
C110.4953 (4)0.0601 (3)0.6913 (3)0.0396 (9)
N10.1092 (4)0.1776 (3)0.6383 (2)0.0501 (9)
C20.0436 (5)0.1668 (3)0.5978 (3)0.0422 (10)
C30.0556 (8)0.0875 (3)0.5396 (4)0.084 (2)
H3A0.00410.09690.49190.126*
H3B0.15750.07560.51320.126*
H3C0.01270.03890.57630.126*
C40.1215 (5)0.1545 (4)0.6721 (4)0.0636 (14)
H4A0.11170.20610.70900.095*
H4B0.07930.10590.70920.095*
H4C0.22400.14340.64640.095*
C50.0956 (5)0.2456 (3)0.5431 (3)0.0572 (13)
H5A0.04270.25160.49560.086*
H5B0.07870.29600.58190.086*
H5C0.19920.24030.51630.086*
N20.3159 (4)0.0615 (2)0.8841 (2)0.0410 (8)
C70.2372 (4)0.0010 (3)0.9265 (3)0.0386 (9)
C80.0806 (5)0.0006 (4)0.8747 (4)0.0621 (14)
H8A0.07550.01770.81260.093*
H8B0.04060.05690.87570.093*
H8C0.02480.04070.90240.093*
C90.2534 (6)0.0249 (3)1.0245 (3)0.0531 (12)
H9A0.35580.02381.05510.080*
H9B0.19970.01511.05380.080*
H9C0.21510.08261.02730.080*
C100.3055 (5)0.0879 (3)0.9211 (3)0.0523 (12)
H10A0.29350.10430.85820.078*
H10B0.25840.13030.95190.078*
H10C0.40870.08530.94980.078*
N30.5261 (4)0.0057 (2)0.6662 (2)0.0455 (9)
C120.5805 (5)0.0906 (3)0.6518 (3)0.0452 (10)
C130.4613 (7)0.1539 (4)0.6554 (6)0.109 (3)
H13A0.43940.15210.71480.164*
H13B0.49300.21150.64400.164*
H13C0.37450.13910.60990.164*
C140.6197 (12)0.0918 (5)0.5631 (4)0.143 (4)
H14A0.69740.05060.56340.215*
H14B0.53510.07640.51620.215*
H14C0.65250.14900.55150.215*
C150.7075 (6)0.1071 (3)0.7273 (4)0.0727 (17)
H15A0.78510.06700.72390.109*
H15B0.74160.16560.72320.109*
H15C0.67910.09950.78430.109*
C160.4205 (5)0.2940 (3)0.7974 (3)0.0486 (11)
C170.5143 (4)0.2431 (3)0.6486 (3)0.0369 (9)
C180.6501 (5)0.1790 (3)0.8241 (3)0.0396 (9)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mo0.03171 (18)0.03277 (18)0.03727 (19)0.00371 (16)0.01448 (13)0.00626 (15)
O10.125 (4)0.051 (2)0.068 (2)0.021 (2)0.044 (2)0.0032 (18)
O20.060 (2)0.0528 (19)0.0504 (18)0.0041 (16)0.0270 (16)0.0168 (15)
O30.048 (2)0.066 (2)0.057 (2)0.0107 (18)0.0023 (16)0.0186 (17)
C10.036 (2)0.049 (2)0.044 (2)0.009 (2)0.0180 (18)0.011 (2)
C60.033 (2)0.044 (2)0.042 (2)0.0003 (18)0.0135 (17)0.0038 (19)
C110.036 (2)0.042 (2)0.041 (2)0.0013 (19)0.0102 (18)0.0068 (18)
N10.035 (2)0.064 (3)0.053 (2)0.0120 (19)0.0129 (17)0.0114 (19)
C20.037 (2)0.042 (2)0.044 (2)0.0053 (19)0.0018 (18)0.0048 (18)
C30.123 (6)0.051 (3)0.068 (4)0.014 (3)0.002 (4)0.014 (3)
C40.046 (3)0.066 (3)0.084 (4)0.006 (3)0.026 (3)0.004 (3)
C50.049 (3)0.049 (3)0.066 (3)0.007 (2)0.003 (2)0.005 (2)
N20.0393 (19)0.045 (2)0.0428 (19)0.0015 (16)0.0172 (16)0.0050 (16)
C70.037 (2)0.039 (2)0.045 (2)0.0047 (18)0.0190 (18)0.0036 (18)
C80.041 (3)0.064 (3)0.079 (4)0.006 (2)0.008 (2)0.012 (3)
C90.069 (3)0.048 (3)0.051 (3)0.010 (2)0.031 (2)0.000 (2)
C100.051 (3)0.042 (3)0.068 (3)0.003 (2)0.022 (2)0.002 (2)
N30.047 (2)0.040 (2)0.049 (2)0.0051 (17)0.0106 (17)0.0006 (17)
C120.058 (3)0.032 (2)0.043 (2)0.008 (2)0.006 (2)0.0033 (18)
C130.059 (4)0.053 (4)0.197 (9)0.004 (3)0.009 (5)0.011 (4)
C140.302 (13)0.080 (5)0.070 (4)0.085 (7)0.087 (6)0.019 (4)
C150.070 (4)0.053 (3)0.081 (4)0.023 (3)0.014 (3)0.015 (3)
C160.063 (3)0.049 (3)0.040 (2)0.009 (2)0.025 (2)0.007 (2)
C170.035 (2)0.035 (2)0.042 (2)0.0068 (17)0.0125 (17)0.0025 (18)
C180.044 (2)0.036 (2)0.040 (2)0.002 (2)0.0139 (18)0.0104 (18)
Geometric parameters (Å, º) top
Mo—C161.992 (5)C7—C101.521 (6)
Mo—C171.991 (4)C7—C81.520 (6)
Mo—C181.994 (4)C7—C91.531 (6)
Mo—C12.140 (4)C8—H8A0.9800
Mo—C112.148 (4)C8—H8B0.9800
Mo—C62.156 (4)C8—H8C0.9800
O1—C161.157 (5)C9—H9A0.9800
O2—C171.158 (5)C9—H9B0.9800
O3—C181.155 (5)C9—H9C0.9800
C1—N11.159 (5)C10—H10A0.9800
C6—N21.146 (5)C10—H10B0.9800
C11—N31.162 (5)C10—H10C0.9800
N1—C21.454 (5)N3—C121.464 (5)
C2—C51.513 (6)C12—C141.490 (7)
C2—C41.506 (6)C12—C151.494 (6)
C2—C31.520 (6)C12—C131.517 (8)
C3—H3A0.9800C13—H13A0.9800
C3—H3B0.9800C13—H13B0.9800
C3—H3C0.9800C13—H13C0.9800
C4—H4A0.9800C14—H14A0.9800
C4—H4B0.9800C14—H14B0.9800
C4—H4C0.9800C14—H14C0.9800
C5—H5A0.9800C15—H15A0.9800
C5—H5B0.9800C15—H15B0.9800
C5—H5C0.9800C15—H15C0.9800
N2—C71.471 (5)
C16—Mo—C1787.39 (16)C10—C7—C9110.0 (4)
C16—Mo—C1888.80 (19)C8—C7—C9112.4 (4)
C17—Mo—C1892.91 (16)C7—C8—H8A109.5
C16—Mo—C190.45 (19)C7—C8—H8B109.5
C17—Mo—C192.12 (16)H8A—C8—H8B109.5
C18—Mo—C1174.88 (15)C7—C8—H8C109.5
C16—Mo—C11177.20 (18)H8A—C8—H8C109.5
C17—Mo—C1191.16 (15)H8B—C8—H8C109.5
C18—Mo—C1188.87 (17)C7—C9—H9A109.5
C1—Mo—C1192.01 (17)C7—C9—H9B109.5
C16—Mo—C696.26 (16)H9A—C9—H9B109.5
C17—Mo—C6173.97 (17)C7—C9—H9C109.5
C18—Mo—C691.97 (15)H9A—C9—H9C109.5
C1—Mo—C683.09 (15)H9B—C9—H9C109.5
C11—Mo—C685.38 (15)C7—C10—H10A109.5
N1—C1—Mo175.3 (4)C7—C10—H10B109.5
N2—C6—Mo173.4 (4)H10A—C10—H10B109.5
N3—C11—Mo175.8 (4)C7—C10—H10C109.5
C1—N1—C2173.9 (5)H10A—C10—H10C109.5
N1—C2—C5108.1 (4)H10B—C10—H10C109.5
N1—C2—C4107.9 (4)C11—N3—C12169.3 (4)
C5—C2—C4111.7 (4)N3—C12—C14108.7 (4)
N1—C2—C3106.3 (4)N3—C12—C15106.9 (4)
C5—C2—C3111.8 (4)C14—C12—C15112.4 (6)
C4—C2—C3110.9 (4)N3—C12—C13107.3 (4)
C2—C3—H3A109.5C14—C12—C13111.7 (6)
C2—C3—H3B109.5C15—C12—C13109.7 (5)
H3A—C3—H3B109.5C12—C13—H13A109.5
C2—C3—H3C109.5C12—C13—H13B109.5
H3A—C3—H3C109.5H13A—C13—H13B109.5
H3B—C3—H3C109.5C12—C13—H13C109.5
C2—C4—H4A109.5H13A—C13—H13C109.5
C2—C4—H4B109.5H13B—C13—H13C109.5
H4A—C4—H4B109.5C12—C14—H14A109.5
C2—C4—H4C109.5C12—C14—H14B109.5
H4A—C4—H4C109.5H14A—C14—H14B109.5
H4B—C4—H4C109.5C12—C14—H14C109.5
C2—C5—H5A109.5H14A—C14—H14C109.5
C2—C5—H5B109.5H14B—C14—H14C109.5
H5A—C5—H5B109.5C12—C15—H15A109.5
C2—C5—H5C109.5C12—C15—H15B109.5
H5A—C5—H5C109.5H15A—C15—H15B109.5
H5B—C5—H5C109.5C12—C15—H15C109.5
C6—N2—C7171.0 (4)H15A—C15—H15C109.5
N2—C7—C10107.9 (3)H15B—C15—H15C109.5
N2—C7—C8107.6 (4)O1—C16—Mo175.7 (4)
C10—C7—C8110.8 (4)O2—C17—Mo179.0 (4)
N2—C7—C9108.0 (3)O3—C18—Mo179.2 (4)
Hydrogen-bond geometry (Å, º) top
D—H···AH···AD···AD—H···A
C3—H3A···O1i2.603.345 (8)133
C15—H15B···O3ii2.813.701 (9)151
C9—H9B···O3iii2.823.611 (9)139
C8—H8A···O1iv2.853.754 (10)154
Symmetry codes: (i) x1/2, y+1/2, z1/2; (ii) x+3/2, y1/2, z+3/2; (iii) x+1, y, z+2; (iv) x+1/2, y1/2, z+3/2.
 

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