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The title compound, [Mo(CH3)(C23H35)(CO)3], has been synthesized and characterized by NMR spectroscopy, elemental analysis, and by an X-ray crystal structure investigation.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802020615/cf6222sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536802020615/cf6222Isup2.hkl
Contains datablock I

CCDC reference: 202311

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.005 Å
  • R factor = 0.034
  • wR factor = 0.062
  • Data-to-parameter ratio = 16.0

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


Red Alert Alert Level A:
DIFF_020 Alert A _diffrn_standards_interval_count and _diffrn_standards_interval_time are missing. Number of measurements between standards or time (min) between standards.
Author response: not applicable due to measurement with area-detector
DIFF_022  Alert A _diffrn_standards_decay_% is missing
          Percentage decrease in standards intensity.


2 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
0 Alert Level C = Please check

Comment top

The title compound, (I), is the first known half-sandwich complex of the 1,2,4-tricyclohexylcyclopentadienyl ligand. The perpendicular distance of Mo from the five-membered ring plane [2.0206 (15) Å] and all Mo—C distances are comparable to the values found for other tricarbonyl(cyclopentadienyl)methylmolybdenum derivatives (El Mouatassim et al., 1995; Lai et al., 1993; Bell et al., 1988). All cyclohexyl (Cy) substituents exhibit a chair conformation. The angles between the cyclopentadienyl ring plane and one plane for each substituent, defined by the cyclopentadienyl ring atom connected to the ipso-C atom and the two nearest methylene C atoms, are 83.17 (13)° for 1-Cy and 68.27 (14)° for 2-Cy. With these two substituents rotated away from each other, a maximum of space is provided for carbonyl C9—O3. The Cy substituent in the 4-position adopts a dihedral angle of 41.91 (18)° with the Cp ring plane, avoiding any close contact with the methyl group bonded to Mo. The absence of steric strain has also been noted for hexa(cyclohexyl)ferrocene, the only other known complex of the 1,2,4-tricyclohexacyclopentadienyl ligand (Burman et al., 1994).

Experimental top

A mixture of lithium tricyclohexylcyclopentadienide (637 mg, 2.0 mmol), molybdenum hexacarbonyl (539 mg, 2.0 mmol), and tetrahydrofuran (50 ml) was stirred at reflux temperature for 5 h and allowed to cool to ambient temperature. Methyl iodide (281 mg, 2.0 mmol) was added and the mixture was heated to reflux temperature for 2 h. The solvent was evaporated and the residue extracted with toluene (30 ml). Evaporation of the filtered toluene solution and recrystallization from hexane–tetrahydrofuran (5:1) at ambient temperature yielded yellow crystalline (I) (712 mg, 1.41 mmol, 70%). C27H38MoO3 (Mr = 506.54), calculated: C 64.02, H 7.56%; found: C 63.31, H 7.64%. 1H NMR (C6D6, 400.13 MHz): 4.75 (s, 2H, ring H), 2.11–0.93 (m, cyclohexyl protons), 0.45 p.p.m. (s, 3H, Mo-methyl). 13C NMR (C6D6, 100.62 MHz): 243.2 (1 C, carbonyl), 229.1 (2 C, carbonyl), 120.9 (s, 1 C, ring C), 117.3 (s, 2 C, ring C), 86.6 (dd, 2 C, J = 163 Hz/5 Hz, ring CH), 37.7 (2 C, methylene), 36.4 (1 C, ipso-CH), 35.7 (2 C, ipso-CH), 35.2 (2 C, cyclohexyl), 34.4 (2 C, cyclohexyl), 27.1 (2 C, cyclohexyl), 27.0 (2 C, cyclohexyl), 26.5 (2 C, cyclohexyl), 26.4 (1 C, cyclohexyl), 26.2 (2 C, cyclohexyl), −14.3 p.p.m. (q, 1 C, J = 136 Hz, Mo-methyl). C,H coupling constants of cyclohexyl carbon signals could not be determined, because of signal superimposition.

Computing details top

Data collection: EXPOSE in IPDS (Stoe & Cie, 1997); cell refinement: CELL in IPDS; data reduction: INTEGRATE in IPDS; program(s) used to solve structure: SIR97 (Altomare et al., 1998); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1998); software used to prepare material for publication: SHELXTL.

Figures top
[Figure 1] Fig. 1. A view of (I) with the atomic numbering scheme. Displacement ellipsoids are drawn at the 50% probability level.
Tricarbonyl(methyl)(η5-1,2,4-tricyclohexylcyclopentadienyl)molybdenum top
Crystal data top
[Mo(CH3)(C23H35)(CO)3]F(000) = 1064
Mr = 506.51Dx = 1.357 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 1480 reflections
a = 10.8664 (8) Åθ = 2–25°
b = 9.8320 (5) ŵ = 0.55 mm1
c = 23.3279 (17) ÅT = 293 K
β = 95.838 (9)°Transparent block, colourless
V = 2479.4 (3) Å30.25 × 0.13 × 0.08 mm
Z = 4
Data collection top
Stoe IPDS
diffractometer
4495 independent reflections
Radiation source: fine-focus sealed tube2569 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.097
ϕ scansθmax = 25.4°, θmin = 2.8°
Absorption correction: analytical
(ABST in PLATON; Spek, 2000)
h = 1313
Tmin = 0.922, Tmax = 0.979k = 1111
18023 measured reflectionsl = 2828
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)] = 0.034Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.062H-atom parameters constrained
S = 0.80 w = 1/[σ2(Fo2) + (0.001P)2]
where P = (Fo2 + 2Fc2)/3
4495 reflections(Δ/σ)max = 0.001
281 parametersΔρmax = 0.47 e Å3
0 restraintsΔρmin = 0.28 e Å3
Crystal data top
[Mo(CH3)(C23H35)(CO)3]V = 2479.4 (3) Å3
Mr = 506.51Z = 4
Monoclinic, P21/nMo Kα radiation
a = 10.8664 (8) ŵ = 0.55 mm1
b = 9.8320 (5) ÅT = 293 K
c = 23.3279 (17) Å0.25 × 0.13 × 0.08 mm
β = 95.838 (9)°
Data collection top
Stoe IPDS
diffractometer
4495 independent reflections
Absorption correction: analytical
(ABST in PLATON; Spek, 2000)
2569 reflections with I > 2σ(I)
Tmin = 0.922, Tmax = 0.979Rint = 0.097
18023 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0340 restraints
wR(F2) = 0.062H-atom parameters constrained
S = 0.80Δρmax = 0.47 e Å3
4495 reflectionsΔρmin = 0.28 e Å3
281 parameters
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
Mo10.24948 (3)0.78939 (4)0.145882 (14)0.03463 (9)
O10.4447 (3)0.7140 (4)0.24899 (13)0.0813 (10)
O20.2347 (3)1.1055 (4)0.14270 (17)0.0772 (9)
O30.4941 (3)0.8586 (4)0.09410 (13)0.0709 (10)
C10.1616 (3)0.7094 (4)0.05652 (12)0.0280 (7)
C20.2209 (3)0.5972 (4)0.08760 (13)0.0285 (8)
C30.1556 (3)0.5740 (4)0.13597 (14)0.0335 (9)
H30.17520.50700.16350.040*
C40.0564 (3)0.6668 (4)0.13684 (14)0.0341 (10)
C50.0634 (3)0.7522 (3)0.08776 (13)0.0324 (11)
H50.01120.82530.07780.039*
C60.1743 (4)0.8694 (5)0.22982 (17)0.0606 (13)
H6A0.23260.93230.24880.091*
H6B0.16290.79430.25500.091*
H6C0.09660.91450.22020.091*
C70.3742 (4)0.7435 (4)0.21102 (18)0.0536 (14)
C80.2432 (4)0.9871 (5)0.1438 (2)0.0472 (10)
C90.4041 (4)0.8313 (4)0.11316 (16)0.0478 (11)
C110.1832 (3)0.7598 (4)0.00255 (13)0.0348 (11)
H110.26110.72040.01250.042*
C120.0802 (3)0.7078 (5)0.04579 (14)0.0460 (9)
H12A0.07800.60930.04370.055*
H12B0.00180.74180.03530.055*
C130.0942 (4)0.7493 (4)0.10733 (15)0.0584 (15)
H13A0.16740.70680.11990.070*
H13B0.02300.71810.13230.070*
C140.1051 (4)0.9030 (5)0.11199 (18)0.0549 (12)
H14A0.12050.92720.15090.066*
H14B0.02780.94490.10400.066*
C150.2076 (4)0.9558 (5)0.07062 (17)0.0539 (12)
H15A0.20981.05420.07310.065*
H15B0.28580.92110.08110.065*
C160.1919 (4)0.9144 (4)0.00900 (16)0.0497 (11)
H16A0.26170.94780.01630.060*
H16B0.11750.95600.00270.060*
C210.3202 (3)0.5079 (4)0.06751 (14)0.0318 (9)
H210.36850.56330.04300.038*
C220.4097 (3)0.4487 (5)0.11552 (16)0.0509 (11)
H22A0.36370.39430.14070.061*
H22B0.44860.52250.13820.061*
C230.5096 (3)0.3611 (5)0.09326 (18)0.0561 (13)
H23A0.56200.41720.07170.067*
H23B0.56070.32180.12560.067*
C240.4535 (4)0.2486 (4)0.0550 (2)0.0566 (14)
H24A0.51890.19920.03860.068*
H24B0.41060.18530.07790.068*
C250.3645 (4)0.3035 (5)0.00722 (18)0.0605 (12)
H25A0.32550.22860.01470.073*
H25B0.40920.35770.01860.073*
C260.2646 (3)0.3916 (4)0.03119 (17)0.0495 (11)
H26A0.20990.42790.00060.059*
H26B0.21560.33540.05440.059*
C410.0433 (3)0.6678 (4)0.17624 (15)0.0389 (10)
H410.04630.75950.19250.047*
C420.1692 (3)0.6404 (5)0.14179 (16)0.0465 (11)
H42A0.18430.70900.11200.056*
H42B0.16700.55240.12310.056*
C430.2740 (4)0.6423 (5)0.1800 (2)0.0682 (15)
H43A0.35070.61870.15730.082*
H43B0.28270.73340.19510.082*
C440.2510 (4)0.5439 (6)0.2294 (2)0.0763 (16)
H44A0.31740.55090.25410.092*
H44B0.25060.45180.21450.092*
C450.1282 (4)0.5730 (6)0.26449 (18)0.0701 (15)
H45A0.11340.50580.29490.084*
H45B0.13110.66190.28230.084*
C460.0244 (3)0.5689 (5)0.22611 (15)0.0463 (11)
H46A0.05290.59000.24890.056*
H46B0.01780.47750.21110.056*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mo10.03622 (15)0.03567 (19)0.03131 (15)0.0015 (2)0.00017 (11)0.0044 (2)
O10.089 (2)0.084 (3)0.0614 (19)0.001 (2)0.0402 (17)0.005 (2)
O20.092 (2)0.042 (2)0.099 (2)0.003 (2)0.0153 (18)0.004 (2)
O30.0519 (18)0.088 (3)0.076 (2)0.0101 (16)0.0215 (16)0.0055 (18)
C10.0279 (16)0.026 (2)0.0290 (17)0.0001 (19)0.0009 (13)0.003 (2)
C20.0288 (18)0.025 (2)0.032 (2)0.0005 (15)0.0019 (15)0.0037 (16)
C30.035 (2)0.038 (3)0.0274 (19)0.0053 (17)0.0004 (15)0.0015 (17)
C40.034 (2)0.035 (3)0.032 (2)0.0007 (16)0.0002 (16)0.0015 (16)
C50.0328 (18)0.030 (3)0.0337 (19)0.0026 (14)0.0010 (15)0.0009 (15)
C60.068 (3)0.066 (4)0.048 (3)0.018 (2)0.008 (2)0.019 (2)
C70.066 (3)0.045 (4)0.049 (3)0.013 (2)0.004 (2)0.007 (2)
C80.050 (2)0.041 (3)0.050 (2)0.005 (3)0.0057 (17)0.003 (3)
C90.060 (3)0.045 (3)0.037 (2)0.003 (2)0.006 (2)0.0097 (18)
C110.0363 (18)0.038 (4)0.0315 (18)0.0078 (15)0.0075 (14)0.0041 (16)
C120.060 (2)0.036 (2)0.040 (2)0.004 (2)0.0067 (16)0.005 (2)
C130.080 (3)0.057 (5)0.035 (2)0.005 (2)0.008 (2)0.0025 (19)
C140.073 (3)0.044 (3)0.047 (3)0.011 (2)0.002 (2)0.014 (2)
C150.059 (3)0.044 (3)0.057 (3)0.003 (2)0.002 (2)0.021 (2)
C160.057 (3)0.044 (3)0.046 (2)0.008 (2)0.0058 (19)0.003 (2)
C210.0277 (18)0.031 (3)0.038 (2)0.0001 (16)0.0061 (15)0.0040 (17)
C220.044 (2)0.062 (3)0.044 (2)0.016 (2)0.0063 (18)0.002 (2)
C230.043 (2)0.064 (4)0.062 (3)0.024 (2)0.005 (2)0.004 (2)
C240.048 (2)0.035 (4)0.089 (3)0.0141 (18)0.020 (2)0.006 (2)
C250.052 (2)0.053 (3)0.075 (3)0.011 (2)0.003 (2)0.023 (3)
C260.044 (2)0.042 (3)0.061 (3)0.009 (2)0.0007 (19)0.014 (2)
C410.035 (2)0.044 (3)0.038 (2)0.0016 (16)0.0043 (16)0.0018 (17)
C420.042 (2)0.055 (3)0.041 (2)0.000 (2)0.0034 (18)0.005 (2)
C430.040 (2)0.082 (4)0.085 (4)0.002 (2)0.015 (2)0.002 (3)
C440.065 (3)0.090 (5)0.080 (4)0.012 (3)0.035 (3)0.006 (3)
C450.066 (3)0.097 (5)0.049 (3)0.001 (3)0.016 (2)0.011 (3)
C460.045 (2)0.057 (3)0.038 (2)0.002 (2)0.0124 (17)0.008 (2)
Geometric parameters (Å, º) top
Mo1—C81.946 (5)C15—H15A0.970
Mo1—C91.958 (5)C15—H15B0.970
Mo1—C71.982 (4)C16—H16A0.970
Mo1—C62.333 (4)C16—H16B0.970
Mo1—C22.330 (3)C21—C221.523 (4)
Mo1—C12.339 (3)C21—C261.512 (5)
Mo1—C52.346 (3)C21—H210.980
Mo1—C32.351 (4)C22—C231.518 (5)
Mo1—C42.411 (3)C22—H22A0.970
O1—C71.148 (4)C22—H22B0.970
O2—C81.168 (4)C23—C241.510 (6)
O3—C91.147 (4)C23—H23A0.970
C1—C51.416 (4)C23—H23B0.970
C1—C21.436 (5)C24—C251.500 (6)
C1—C111.505 (4)C24—H24A0.970
C2—C31.411 (4)C24—H24B0.970
C2—C211.502 (4)C25—C261.538 (5)
C3—C41.414 (5)C25—H25A0.970
C3—H30.930C25—H25B0.970
C4—C51.428 (4)C26—H26A0.970
C4—C411.490 (5)C26—H26B0.970
C5—H50.930C41—C461.514 (5)
C6—H6A0.960C41—C421.538 (5)
C6—H6B0.960C41—H410.980
C6—H6C0.960C42—C431.516 (5)
C11—C161.531 (5)C42—H42A0.970
C11—C121.517 (5)C42—H42B0.970
C11—H110.980C43—C441.506 (6)
C12—C131.515 (5)C43—H43A0.970
C12—H12A0.970C43—H43B0.970
C12—H12B0.970C44—C451.520 (6)
C13—C141.521 (6)C44—H44A0.970
C13—H13A0.970C44—H44B0.970
C13—H13B0.970C45—C461.511 (5)
C14—C151.490 (5)C45—H45A0.970
C14—H14A0.970C45—H45B0.970
C14—H14B0.970C46—H46A0.970
C15—C161.520 (5)C46—H46B0.970
C8—Mo1—C979.00 (18)H13A—C13—H13B108.1
C8—Mo1—C7105.43 (19)C15—C14—C13111.0 (3)
C9—Mo1—C778.46 (16)C15—C14—H14A109.4
C8—Mo1—C670.73 (18)C13—C14—H14A109.4
C9—Mo1—C6130.04 (15)C15—C14—H14B109.4
C7—Mo1—C672.77 (16)C13—C14—H14B109.4
C8—Mo1—C2142.50 (16)H14A—C14—H14B108.0
C9—Mo1—C290.68 (13)C14—C15—C16111.8 (3)
C7—Mo1—C2107.63 (15)C14—C15—H15A109.3
C6—Mo1—C2136.53 (13)C16—C15—H15A109.3
C8—Mo1—C1107.66 (17)C14—C15—H15B109.3
C9—Mo1—C190.68 (13)C16—C15—H15B109.3
C7—Mo1—C1142.36 (15)H15A—C15—H15B107.9
C6—Mo1—C1135.67 (12)C11—C16—C15111.9 (3)
C2—Mo1—C135.83 (12)C11—C16—H16A109.2
C8—Mo1—C596.60 (16)C15—C16—H16A109.2
C9—Mo1—C5122.05 (13)C11—C16—H16B109.2
C7—Mo1—C5152.81 (14)C15—C16—H16B109.2
C6—Mo1—C5100.54 (13)H16A—C16—H16B107.9
C2—Mo1—C558.71 (11)C2—C21—C22114.8 (3)
C1—Mo1—C535.20 (10)C2—C21—C26111.0 (3)
C8—Mo1—C3152.06 (16)C22—C21—C26108.2 (3)
C9—Mo1—C3122.14 (14)C2—C21—H21107.5
C7—Mo1—C397.27 (15)C22—C21—H21107.5
C6—Mo1—C3101.58 (14)C26—C21—H21107.5
C2—Mo1—C335.08 (11)C21—C22—C23113.0 (3)
C1—Mo1—C358.40 (13)C21—C22—H22A109.0
C5—Mo1—C357.53 (12)C23—C22—H22A109.0
C8—Mo1—C4117.99 (16)C21—C22—H22B109.0
C9—Mo1—C4147.64 (13)C23—C22—H22B109.0
C7—Mo1—C4118.33 (15)H22A—C22—H22B107.8
C6—Mo1—C482.31 (13)C24—C23—C22111.0 (3)
C2—Mo1—C458.69 (11)C24—C23—H23A109.4
C1—Mo1—C458.75 (11)C22—C23—H23A109.4
C5—Mo1—C434.92 (11)C24—C23—H23B109.4
C3—Mo1—C434.52 (11)C22—C23—H23B109.4
C5—C1—C2106.9 (3)H23A—C23—H23B108.0
C5—C1—C11124.7 (3)C25—C24—C23111.5 (4)
C2—C1—C11127.7 (3)C25—C24—H24A109.3
C5—C1—Mo172.67 (18)C23—C24—H24A109.3
C2—C1—Mo171.77 (17)C25—C24—H24B109.3
C11—C1—Mo1128.2 (2)C23—C24—H24B109.3
C3—C2—C1106.9 (3)H24A—C24—H24B108.0
C3—C2—C21126.2 (3)C24—C25—C26111.0 (3)
C1—C2—C21126.2 (3)C24—C25—H25A109.4
C3—C2—Mo173.3 (2)C26—C25—H25A109.4
C1—C2—Mo172.4 (2)C24—C25—H25B109.4
C21—C2—Mo1126.8 (2)C26—C25—H25B109.4
C4—C3—C2110.7 (3)H25A—C25—H25B108.0
C4—C3—Mo175.0 (2)C21—C26—C25111.9 (3)
C2—C3—Mo171.6 (2)C21—C26—H26A109.2
C4—C3—H3124.6C25—C26—H26A109.2
C2—C3—H3124.6C21—C26—H26B109.2
Mo1—C3—H3120.3C25—C26—H26B109.2
C3—C4—C5105.3 (3)H26A—C26—H26B107.9
C3—C4—C41128.0 (3)C4—C41—C46114.8 (3)
C5—C4—C41126.3 (3)C4—C41—C42109.9 (3)
C3—C4—Mo170.4 (2)C46—C41—C42109.5 (3)
C5—C4—Mo170.05 (18)C4—C41—H41107.5
C41—C4—Mo1128.6 (2)C46—C41—H41107.5
C1—C5—C4110.0 (3)C42—C41—H41107.5
C1—C5—Mo172.13 (17)C43—C42—C41111.8 (3)
C4—C5—Mo175.03 (18)C43—C42—H42A109.3
C1—C5—H5125.0C41—C42—H42A109.3
C4—C5—H5125.0C43—C42—H42B109.3
Mo1—C5—H5119.5C41—C42—H42B109.3
Mo1—C6—H6A109.5H42A—C42—H42B107.9
Mo1—C6—H6B109.5C42—C43—C44111.5 (4)
H6A—C6—H6B109.5C42—C43—H43A109.3
Mo1—C6—H6C109.5C44—C43—H43A109.3
H6A—C6—H6C109.5C42—C43—H43B109.3
H6B—C6—H6C109.5C44—C43—H43B109.3
O1—C7—Mo1178.2 (4)H43A—C43—H43B108.0
O2—C8—Mo1177.5 (4)C45—C44—C43111.1 (4)
O3—C9—Mo1178.7 (4)C45—C44—H44A109.4
C1—C11—C16115.7 (3)C43—C44—H44A109.4
C1—C11—C12109.0 (3)C45—C44—H44B109.4
C16—C11—C12108.5 (3)C43—C44—H44B109.4
C1—C11—H11107.8H44A—C44—H44B108.0
C16—C11—H11107.8C44—C45—C46110.1 (4)
C12—C11—H11107.8C44—C45—H45A109.6
C13—C12—C11113.7 (3)C46—C45—H45A109.6
C13—C12—H12A108.8C44—C45—H45B109.6
C11—C12—H12A108.8C46—C45—H45B109.6
C13—C12—H12B108.8H45A—C45—H45B108.2
C11—C12—H12B108.8C41—C46—C45112.8 (3)
H12A—C12—H12B107.7C41—C46—H46A109.0
C14—C13—C12110.6 (3)C45—C46—H46A109.0
C14—C13—H13A109.5C41—C46—H46B109.0
C12—C13—H13A109.5C45—C46—H46B109.0
C14—C13—H13B109.5H46A—C46—H46B107.8
C12—C13—H13B109.5

Experimental details

Crystal data
Chemical formula[Mo(CH3)(C23H35)(CO)3]
Mr506.51
Crystal system, space groupMonoclinic, P21/n
Temperature (K)293
a, b, c (Å)10.8664 (8), 9.8320 (5), 23.3279 (17)
β (°) 95.838 (9)
V3)2479.4 (3)
Z4
Radiation typeMo Kα
µ (mm1)0.55
Crystal size (mm)0.25 × 0.13 × 0.08
Data collection
DiffractometerStoe IPDS
diffractometer
Absorption correctionAnalytical
(ABST in PLATON; Spek, 2000)
Tmin, Tmax0.922, 0.979
No. of measured, independent and
observed [I > 2σ(I)] reflections
18023, 4495, 2569
Rint0.097
(sin θ/λ)max1)0.602
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.034, 0.062, 0.80
No. of reflections4495
No. of parameters281
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.47, 0.28

Computer programs: EXPOSE in IPDS (Stoe & Cie, 1997), CELL in IPDS, INTEGRATE in IPDS, SIR97 (Altomare et al., 1998), SHELXL97 (Sheldrick, 1997), SHELXTL (Bruker, 1998), SHELXTL.

 

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