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The structure of the title compound, [W2(C4H9N)4(C7H11N2)(C4H10NO)O], was determined at 150 K. It is an asymmetrical binuclear compound with a μ-oxo bridge linking two tungsten(VI) centers.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805007610/ac6163sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805007610/ac6163Isup2.hkl
Contains datablock I

CCDC reference: 270222

Key indicators

  • Single-crystal X-ray study
  • T = 150 K
  • Mean [sigma](C-C) = 0.007 Å
  • R factor = 0.026
  • wR factor = 0.063
  • Data-to-parameter ratio = 25.4

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.91 Ratio PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.72 Ratio PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) W2 - O2 .. 5.04 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) W2 - N7 .. 7.78 su PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C8
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 5 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 4 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: APEX2 (Bruker, 2004); cell refinement: APEX2; data reduction: APEX2; program(s) used to solve structure: SHELXTL (Sheldrick, 1998); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Bis(tert-butylimido)[2-(dimethylaminomethyl)pyrrol-1-yl]tungsten(VI)-µ-oxo- bis(tert-butylimido)(η2-N,O-tert-butylnitroso)tungsten(VI) top
Crystal data top
[W2(C4H9N)4(C7H11N2)(C4H10NO)O]Z = 2
Mr = 879.50F(000) = 864
Triclinic, P1Dx = 1.656 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 9.6263 (3) ÅCell parameters from 5880 reflections
b = 12.0153 (3) Åθ = 2.3–28.8°
c = 15.6375 (4) ŵ = 6.55 mm1
α = 86.334 (2)°T = 150 K
β = 79.479 (2)°Block, colorless
γ = 83.175 (2)°0.53 × 0.34 × 0.27 mm
V = 1764.02 (8) Å3
Data collection top
Bruker SMART APEX-II
diffractometer
9142 independent reflections
Radiation source: fine-focus sealed tube7668 reflections with I > 2σ
Graphite monochromatorRint = 0.029
ω scansθmax = 28.9°, θmin = 2.2°
Absorption correction: multi-scan
(SADABS; Sheldrick, 2003)
h = 1213
Tmin = 0.080, Tmax = 0.171k = 1616
25718 measured reflectionsl = 2121
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)] = 0.026Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.063H-atom parameters constrained
S = 1.04 w = 1/[σ2(Fo2) + (0.0236P)2 + 3.8003P]
where P = (Fo2 + 2Fc2)/3
9142 reflections(Δ/σ)max = 0.002
360 parametersΔρmax = 3.04 e Å3
0 restraintsΔρmin = 1.90 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
W10.547649 (14)0.291142 (11)0.243471 (9)0.01774 (4)
O10.5664 (3)0.1316 (2)0.25392 (17)0.0253 (6)
N10.3678 (3)0.4023 (3)0.2761 (2)0.0255 (7)
C10.3147 (5)0.4615 (3)0.3504 (3)0.0319 (9)
H10.36220.46450.39820.038*
W20.618558 (14)0.016386 (12)0.296263 (9)0.01901 (4)
N20.3673 (3)0.2456 (3)0.1644 (2)0.0265 (7)
C20.1831 (5)0.5150 (4)0.3442 (4)0.0437 (12)
H20.12380.56080.38650.052*
O20.6194 (3)0.0443 (3)0.41870 (19)0.0332 (7)
N30.6414 (3)0.3396 (3)0.1430 (2)0.0245 (7)
C30.1514 (5)0.4895 (4)0.2630 (4)0.0411 (11)
H3A0.06750.51540.24050.049*
N40.6323 (3)0.3249 (3)0.3272 (2)0.0232 (6)
C40.2653 (4)0.4203 (4)0.2231 (3)0.0311 (9)
N50.4787 (3)0.0910 (3)0.2822 (2)0.0250 (7)
C50.2977 (5)0.3578 (4)0.1412 (3)0.0353 (10)
H5A0.20920.35040.11920.042*
H5B0.36200.39730.09580.042*
N60.7761 (3)0.0637 (3)0.2277 (2)0.0278 (7)
C60.2617 (4)0.1793 (4)0.2184 (3)0.0337 (9)
H6A0.21370.22180.26890.050*
H6B0.30980.10840.23830.050*
H6C0.19150.16350.18390.050*
C70.4314 (5)0.1843 (4)0.0847 (3)0.0390 (11)
H7A0.35610.16880.05410.059*
H7B0.48360.11340.10100.059*
H7C0.49690.23020.04660.059*
N70.6449 (3)0.0751 (3)0.4225 (2)0.0243 (7)
H70.56450.10630.45130.029*
C80.7541 (4)0.3937 (4)0.0874 (3)0.0298 (9)
C90.7273 (7)0.5200 (5)0.1017 (4)0.0630 (18)
H9A0.63070.54790.09310.095*
H9B0.79610.55910.06010.095*
H9C0.73780.53380.16120.095*
C100.8955 (5)0.3457 (7)0.1075 (4)0.072 (2)
H10A0.90090.36160.16740.108*
H10B0.97090.37960.06720.108*
H10C0.90750.26430.10100.108*
C110.7461 (6)0.3756 (5)0.0073 (3)0.0450 (12)
H11A0.75720.29500.01700.067*
H11B0.82230.41090.04590.067*
H11C0.65380.40920.01990.067*
C120.7165 (4)0.3531 (3)0.3892 (3)0.0255 (8)
C130.6361 (6)0.3282 (5)0.4808 (3)0.0466 (12)
H13A0.54220.37160.48880.070*
H13B0.68960.34910.52380.070*
H13C0.62500.24800.48840.070*
C140.7380 (5)0.4768 (4)0.3768 (3)0.0393 (11)
H14A0.79170.49130.31840.059*
H14B0.79090.49690.42040.059*
H14C0.64530.52210.38360.059*
C150.8596 (5)0.2794 (4)0.3728 (4)0.0447 (12)
H15A0.84290.20020.37690.067*
H15B0.91610.29330.41640.067*
H15C0.91110.29780.31450.067*
C160.4046 (4)0.1777 (4)0.2548 (3)0.0280 (8)
C170.2565 (4)0.1732 (4)0.3102 (3)0.0362 (10)
H17A0.26430.18000.37200.054*
H17B0.20810.23520.29610.054*
H17C0.20180.10170.29820.054*
C180.3917 (5)0.1527 (5)0.1588 (3)0.0443 (12)
H18A0.33640.07960.15280.066*
H18B0.34360.21110.13900.066*
H18C0.48670.15150.12350.066*
C190.4887 (5)0.2911 (4)0.2677 (4)0.0437 (12)
H19A0.58290.29290.23100.065*
H19B0.43820.35060.25160.065*
H19C0.49910.30290.32890.065*
C200.8819 (4)0.1145 (4)0.1586 (3)0.0341 (10)
C210.8128 (6)0.1239 (6)0.0790 (3)0.0575 (16)
H21A0.73330.16960.09490.086*
H21B0.88320.15940.03250.086*
H21C0.77760.04880.05860.086*
C220.9386 (5)0.2328 (4)0.1894 (3)0.0460 (12)
H22A0.98080.22760.24130.069*
H22B1.01100.26640.14300.069*
H22C0.86020.27970.20350.069*
C231.0035 (5)0.0402 (5)0.1359 (4)0.0492 (13)
H23A0.96540.03590.11950.074*
H23B1.07310.07120.08710.074*
H23C1.04960.03780.18660.074*
C240.7723 (4)0.1219 (3)0.4603 (2)0.0247 (8)
C250.7890 (5)0.2478 (4)0.4466 (3)0.0399 (11)
H25A0.70180.27950.47450.060*
H25B0.86920.28410.47240.060*
H25C0.80680.26070.38410.060*
C260.9026 (4)0.0685 (4)0.4162 (3)0.0337 (10)
H26A0.91860.08000.35350.051*
H26B0.98540.10290.44030.051*
H26C0.88840.01210.42610.051*
C270.7426 (5)0.1000 (5)0.5569 (3)0.0457 (12)
H27A0.71620.01950.56500.069*
H27B0.82810.12460.58180.069*
H27C0.66450.14160.58620.069*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
W10.01895 (7)0.01578 (8)0.01867 (7)0.00371 (5)0.00221 (5)0.00194 (5)
O10.0286 (14)0.0184 (13)0.0303 (14)0.0047 (11)0.0069 (11)0.0031 (11)
N10.0240 (16)0.0204 (16)0.0319 (17)0.0055 (13)0.0025 (13)0.0011 (13)
C10.033 (2)0.020 (2)0.039 (2)0.0045 (17)0.0039 (18)0.0071 (17)
W20.01799 (7)0.01796 (8)0.02240 (8)0.00391 (6)0.00615 (5)0.00028 (6)
N20.0258 (16)0.0292 (18)0.0269 (16)0.0078 (14)0.0079 (13)0.0012 (14)
C20.031 (2)0.028 (2)0.065 (3)0.0000 (19)0.010 (2)0.009 (2)
O20.0373 (16)0.0283 (16)0.0348 (16)0.0004 (13)0.0088 (13)0.0068 (13)
N30.0234 (15)0.0257 (17)0.0234 (15)0.0036 (13)0.0007 (12)0.0021 (13)
C30.023 (2)0.029 (2)0.068 (3)0.0010 (18)0.003 (2)0.004 (2)
N40.0242 (15)0.0218 (17)0.0236 (15)0.0025 (13)0.0032 (12)0.0052 (12)
C40.027 (2)0.024 (2)0.041 (2)0.0041 (16)0.0044 (17)0.0081 (17)
N50.0260 (16)0.0198 (16)0.0307 (17)0.0064 (13)0.0077 (13)0.0030 (13)
C50.030 (2)0.040 (3)0.038 (2)0.0072 (19)0.0144 (18)0.0119 (19)
N60.0229 (16)0.035 (2)0.0237 (16)0.0005 (14)0.0019 (13)0.0005 (14)
C60.027 (2)0.038 (2)0.039 (2)0.0112 (18)0.0090 (18)0.0023 (19)
C70.040 (2)0.050 (3)0.031 (2)0.010 (2)0.0122 (19)0.011 (2)
N70.0204 (15)0.0209 (16)0.0330 (17)0.0047 (13)0.0057 (13)0.0038 (13)
C80.032 (2)0.032 (2)0.0248 (19)0.0112 (17)0.0028 (16)0.0006 (16)
C90.092 (5)0.040 (3)0.053 (3)0.030 (3)0.019 (3)0.013 (3)
C100.030 (3)0.112 (6)0.068 (4)0.018 (3)0.002 (3)0.035 (4)
C110.058 (3)0.046 (3)0.027 (2)0.015 (2)0.005 (2)0.000 (2)
C120.031 (2)0.0216 (19)0.0272 (19)0.0032 (16)0.0121 (16)0.0063 (15)
C130.066 (3)0.050 (3)0.029 (2)0.020 (3)0.011 (2)0.003 (2)
C140.052 (3)0.021 (2)0.050 (3)0.010 (2)0.020 (2)0.0030 (19)
C150.041 (3)0.041 (3)0.057 (3)0.007 (2)0.025 (2)0.014 (2)
C160.0246 (19)0.026 (2)0.035 (2)0.0094 (16)0.0042 (16)0.0062 (17)
C170.027 (2)0.036 (3)0.046 (3)0.0114 (18)0.0029 (18)0.003 (2)
C180.041 (3)0.063 (3)0.035 (2)0.019 (2)0.009 (2)0.014 (2)
C190.032 (2)0.025 (2)0.072 (3)0.0063 (19)0.002 (2)0.010 (2)
C200.0170 (18)0.052 (3)0.030 (2)0.0040 (18)0.0043 (15)0.0050 (19)
C210.039 (3)0.102 (5)0.031 (2)0.005 (3)0.002 (2)0.016 (3)
C220.036 (2)0.044 (3)0.051 (3)0.010 (2)0.004 (2)0.017 (2)
C230.032 (2)0.058 (3)0.055 (3)0.014 (2)0.002 (2)0.006 (3)
C240.0213 (17)0.026 (2)0.0267 (19)0.0009 (15)0.0042 (14)0.0034 (15)
C250.042 (3)0.027 (2)0.051 (3)0.0035 (19)0.014 (2)0.000 (2)
C260.0236 (19)0.044 (3)0.037 (2)0.0095 (18)0.0099 (17)0.0005 (19)
C270.034 (2)0.069 (4)0.032 (2)0.008 (2)0.0041 (19)0.013 (2)
Geometric parameters (Å, º) top
W1—N41.754 (3)C12—C141.521 (6)
W1—N31.765 (3)C12—C131.528 (6)
W1—O11.903 (3)C12—C151.535 (6)
W1—N12.063 (3)C13—H13A0.9800
W1—N22.437 (3)C13—H13B0.9800
O1—W21.901 (3)C13—H13C0.9800
N1—C11.385 (5)C14—H14A0.9800
N1—C41.390 (5)C14—H14B0.9800
C1—C21.367 (6)C14—H14C0.9800
C1—H10.9500C15—H15A0.9800
W2—N61.747 (3)C15—H15B0.9800
W2—N51.757 (3)C15—H15C0.9800
W2—O22.094 (3)C16—C191.521 (6)
W2—N72.102 (3)C16—C171.524 (6)
N2—C61.475 (5)C16—C181.536 (6)
N2—C71.484 (6)C17—H17A0.9800
N2—C51.486 (5)C17—H17B0.9800
C2—C31.418 (8)C17—H17C0.9800
C2—H20.9500C18—H18A0.9800
O2—N71.426 (4)C18—H18B0.9800
N3—C81.451 (5)C18—H18C0.9800
C3—C41.372 (6)C19—H19A0.9800
C3—H3A0.9500C19—H19B0.9800
N4—C121.451 (5)C19—H19C0.9800
C4—C51.491 (7)C20—C211.530 (6)
N5—C161.457 (5)C20—C231.533 (6)
C5—H5A0.9900C20—C221.541 (7)
C5—H5B0.9900C21—H21A0.9800
N6—C201.454 (5)C21—H21B0.9800
C6—H6A0.9800C21—H21C0.9800
C6—H6B0.9800C22—H22A0.9800
C6—H6C0.9800C22—H22B0.9800
C7—H7A0.9800C22—H22C0.9800
C7—H7B0.9800C23—H23A0.9800
C7—H7C0.9800C23—H23B0.9800
N7—C241.492 (5)C23—H23C0.9800
N7—H70.9300C24—C261.510 (6)
C8—C101.493 (7)C24—C271.519 (6)
C8—C111.528 (6)C24—C251.527 (6)
C8—C91.534 (7)C25—H25A0.9800
C9—H9A0.9800C25—H25B0.9800
C9—H9B0.9800C25—H25C0.9800
C9—H9C0.9800C26—H26A0.9800
C10—H10A0.9800C26—H26B0.9800
C10—H10B0.9800C26—H26C0.9800
C10—H10C0.9800C27—H27A0.9800
C11—H11A0.9800C27—H27B0.9800
C11—H11B0.9800C27—H27C0.9800
C11—H11C0.9800
N4—W1—N3108.77 (15)N4—C12—C13108.1 (3)
N4—W1—O1101.78 (13)C14—C12—C13110.3 (4)
N3—W1—O1111.49 (13)N4—C12—C15107.8 (3)
N4—W1—N195.83 (14)C14—C12—C15110.8 (4)
N3—W1—N1107.55 (14)C13—C12—C15110.4 (4)
O1—W1—N1128.59 (12)C12—C13—H13A109.5
N4—W1—N2162.12 (13)C12—C13—H13B109.5
N3—W1—N287.56 (13)H13A—C13—H13B109.5
O1—W1—N277.92 (11)C12—C13—H13C109.5
N1—W1—N271.62 (12)H13A—C13—H13C109.5
W2—O1—W1159.69 (16)H13B—C13—H13C109.5
C1—N1—C4106.7 (3)C12—C14—H14A109.5
C1—N1—W1131.9 (3)C12—C14—H14B109.5
C4—N1—W1121.0 (3)H14A—C14—H14B109.5
C2—C1—N1109.4 (4)C12—C14—H14C109.5
C2—C1—H1125.3H14A—C14—H14C109.5
N1—C1—H1125.3H14B—C14—H14C109.5
N6—W2—N5110.91 (16)C12—C15—H15A109.5
N6—W2—O1105.59 (14)C12—C15—H15B109.5
N5—W2—O1103.99 (13)H15A—C15—H15B109.5
N6—W2—O2121.55 (14)C12—C15—H15C109.5
N5—W2—O2119.23 (14)H15A—C15—H15C109.5
O1—W2—O290.09 (11)H15B—C15—H15C109.5
N6—W2—N7105.79 (14)N5—C16—C19108.5 (3)
N5—W2—N7100.27 (14)N5—C16—C17108.4 (3)
O1—W2—N7129.66 (12)C19—C16—C17110.6 (4)
O2—W2—N739.72 (12)N5—C16—C18108.3 (4)
C6—N2—C7109.0 (3)C19—C16—C18111.5 (4)
C6—N2—C5109.8 (3)C17—C16—C18109.3 (4)
C7—N2—C5110.7 (3)C16—C17—H17A109.5
C6—N2—W1112.6 (2)C16—C17—H17B109.5
C7—N2—W1111.8 (2)H17A—C17—H17B109.5
C5—N2—W1102.9 (2)C16—C17—H17C109.5
C1—C2—C3107.6 (4)H17A—C17—H17C109.5
C1—C2—H2126.2H17B—C17—H17C109.5
C3—C2—H2126.2C16—C18—H18A109.5
N7—O2—W270.46 (18)C16—C18—H18B109.5
C8—N3—W1154.8 (3)H18A—C18—H18B109.5
C4—C3—C2106.8 (4)C16—C18—H18C109.5
C4—C3—H3A126.6H18A—C18—H18C109.5
C2—C3—H3A126.6H18B—C18—H18C109.5
C12—N4—W1173.7 (3)C16—C19—H19A109.5
C3—C4—N1109.5 (4)C16—C19—H19B109.5
C3—C4—C5134.8 (4)H19A—C19—H19B109.5
N1—C4—C5115.5 (4)C16—C19—H19C109.5
C16—N5—W2160.0 (3)H19A—C19—H19C109.5
N2—C5—C4105.9 (3)H19B—C19—H19C109.5
N2—C5—H5A110.6N6—C20—C21109.1 (3)
C4—C5—H5A110.6N6—C20—C23108.5 (4)
N2—C5—H5B110.6C21—C20—C23110.4 (4)
C4—C5—H5B110.6N6—C20—C22109.6 (4)
H5A—C5—H5B108.7C21—C20—C22109.1 (4)
C20—N6—W2165.1 (3)C23—C20—C22110.1 (4)
N2—C6—H6A109.5C20—C21—H21A109.5
N2—C6—H6B109.5C20—C21—H21B109.5
H6A—C6—H6B109.5H21A—C21—H21B109.5
N2—C6—H6C109.5C20—C21—H21C109.5
H6A—C6—H6C109.5H21A—C21—H21C109.5
H6B—C6—H6C109.5H21B—C21—H21C109.5
N2—C7—H7A109.5C20—C22—H22A109.5
N2—C7—H7B109.5C20—C22—H22B109.5
H7A—C7—H7B109.5H22A—C22—H22B109.5
N2—C7—H7C109.5C20—C22—H22C109.5
H7A—C7—H7C109.5H22A—C22—H22C109.5
H7B—C7—H7C109.5H22B—C22—H22C109.5
O2—N7—C24115.1 (3)C20—C23—H23A109.5
O2—N7—W269.81 (17)C20—C23—H23B109.5
C24—N7—W2132.7 (2)H23A—C23—H23B109.5
O2—N7—H7110.5C20—C23—H23C109.5
C24—N7—H7110.5H23A—C23—H23C109.5
W2—N7—H7110.5H23B—C23—H23C109.5
N3—C8—C10110.3 (4)N7—C24—C26111.0 (3)
N3—C8—C11108.4 (4)N7—C24—C27108.4 (3)
C10—C8—C11110.5 (4)C26—C24—C27109.9 (4)
N3—C8—C9108.2 (4)N7—C24—C25105.5 (3)
C10—C8—C9111.3 (5)C26—C24—C25111.5 (4)
C11—C8—C9108.2 (4)C27—C24—C25110.3 (4)
C8—C9—H9A109.5C24—C25—H25A109.5
C8—C9—H9B109.5C24—C25—H25B109.5
H9A—C9—H9B109.5H25A—C25—H25B109.5
C8—C9—H9C109.5C24—C25—H25C109.5
H9A—C9—H9C109.5H25A—C25—H25C109.5
H9B—C9—H9C109.5H25B—C25—H25C109.5
C8—C10—H10A109.5C24—C26—H26A109.5
C8—C10—H10B109.5C24—C26—H26B109.5
H10A—C10—H10B109.5H26A—C26—H26B109.5
C8—C10—H10C109.5C24—C26—H26C109.5
H10A—C10—H10C109.5H26A—C26—H26C109.5
H10B—C10—H10C109.5H26B—C26—H26C109.5
C8—C11—H11A109.5C24—C27—H27A109.5
C8—C11—H11B109.5C24—C27—H27B109.5
H11A—C11—H11B109.5H27A—C27—H27B109.5
C8—C11—H11C109.5C24—C27—H27C109.5
H11A—C11—H11C109.5H27A—C27—H27C109.5
H11B—C11—H11C109.5H27B—C27—H27C109.5
N4—C12—C14109.4 (3)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N7—H7···O2i0.932.533.220 (4)132
Symmetry code: (i) x+1, y, z+1.
 

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