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The title cluster compound, [Mo45-C5H4Me)43-Se)4], was synthesized from the reaction of [Mo(η5-C5H4Me)(CO)3]2 with grey selenium in refluxing xylene solution under a nitro­gen atmosphere. The complete cluster is generated by a crystallographic twofold axis and contains an Mo4Se4 cubane-like core surrounded by four η5-methylcyclo­pentadienyl ligands. In the core, the four molybdenum atoms are connected to each other to form a tetra­hedron, with a selenium atom capping each face. The Mo—Mo bond lengths vary from 2.9857 (5) to 3.0083 (3) Å and the Mo—Se separations range from 2.4633 (4) to 2.4693 (5) Å.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S2414314623006570/hb4439sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2414314623006570/hb4439Isup2.hkl
Contains datablock I

CCDC reference: 2285076

Key indicators

Structure: I
  • Single-crystal X-ray study
  • T = 296 K
  • Mean [sigma](C-C) = 0.005 Å
  • R factor = 0.021
  • wR factor = 0.051
  • Data-to-parameter ratio = 19.6

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT910_ALERT_3_C Missing # of FCF Reflection(s) Below Theta(Min). 5 Note PLAT934_ALERT_3_C Number of (Iobs-Icalc)/Sigma(W) > 10 Outliers .. 1 Check
Alert level G PLAT128_ALERT_4_G Alternate Setting for Input Space Group C2/c I2/a Note PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X) Mo1 --Se1 . 6.5 s.u. PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X) Mo1 --Se2 . 9.5 s.u. PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X) Mo1 --Se2_a . 8.8 s.u. PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X) Mo2 --Se1 . 6.5 s.u. PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X) Mo2 --Se2 . 6.5 s.u. PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X) Mo2 --Se1_a . 7.5 s.u. PLAT764_ALERT_4_G Overcomplete CIF Bond List Detected (Rep/Expd) . 1.14 Ratio PLAT912_ALERT_4_G Missing # of FCF Reflections Above STh/L= 0.600 6 Note PLAT941_ALERT_3_G Average HKL Measurement Multiplicity ........... 4.1 Low PLAT978_ALERT_2_G Number C-C Bonds with Positive Residual Density. 0 Info
0 ALERT level A = Most likely a serious problem - resolve or explain 0 ALERT level B = A potentially serious problem, consider carefully 2 ALERT level C = Check. Ensure it is not caused by an omission or oversight 11 ALERT level G = General information/check it is not something unexpected 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 7 ALERT type 2 Indicator that the structure model may be wrong or deficient 3 ALERT type 3 Indicator that the structure quality may be low 3 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: RAPID AUTO (Rigaku, 2006); cell refinement: RAPID AUTO (Rigaku, 2006); data reduction: RAPID AUTO (Rigaku, 2006); program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXL2018/3 (Sheldrick, 2015); molecular graphics: CrystalStructure 4.0 (Rigaku, 2010); software used to prepare material for publication: CrystalStructure 4.0 (Rigaku, 2010).

Tetra-µ3-selenido-1:2:3κ3Se;1:2:4κ3Se;1:3:4κ3Se;2:3:4κ3Se-tetrakis[(η5-methylcyclopentadienyl)molybdenum(III)](6 Mo—Mo) top
Crystal data top
[Mo4(C6H7)4Se4]F(000) = 1904.00
Mr = 1016.09Dx = 2.673 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71075 Å
a = 21.1820 (4) ÅCell parameters from 10275 reflections
b = 8.42496 (16) Åθ = 3.2–27.5°
c = 16.4482 (3) ŵ = 7.72 mm1
β = 120.6613 (7)°T = 296 K
V = 2524.93 (9) Å3Platelet, brown
Z = 40.10 × 0.10 × 0.10 mm
Data collection top
Rigaku R-AXIS RAPID
diffractometer
2617 reflections with F2 > 2.0σ(F2)
Detector resolution: 10.000 pixels mm-1Rint = 0.040
ω scansθmax = 27.5°, θmin = 3.3°
Absorption correction: multi-scan
(ABSCOR; Rigaku, 1995)
h = 2427
Tmin = 0.201, Tmax = 0.462k = 1010
11868 measured reflectionsl = 2121
2878 independent reflections
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.021Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.051H-atom parameters constrained
S = 1.07 w = 1/[σ2(Fo2) + (0.0168P)2 + 4.2366P]
where P = (Fo2 + 2Fc2)/3
2878 reflections(Δ/σ)max = 0.002
147 parametersΔρmax = 0.49 e Å3
0 restraintsΔρmin = 0.79 e Å3
Primary atom site location: structure-invariant direct methods
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Refinement. Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F2. R-factor (gt) are based on F. The threshold expression of F2 > 2.0 sigma(F2) is used only for calculating R-factor (gt).

All hydrogen atoms were placed at calculated positions (C—H = 0.96–0.98 Å) and refined using a riding model with Uiso(H) = 1.2Ueq(C).

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Mo10.05709 (2)0.36774 (3)0.77761 (2)0.01956 (7)
Mo20.05898 (2)0.11729 (3)0.85272 (2)0.02062 (7)
Se10.07420 (2)0.07974 (3)0.78522 (2)0.02368 (8)
Se20.07609 (2)0.40514 (3)0.88225 (2)0.02324 (8)
C10.16873 (18)0.4032 (4)0.7760 (2)0.0334 (7)
C20.16199 (18)0.5254 (4)0.7228 (2)0.0317 (7)
H10.1973720.5486210.6563430.038*
C30.1002 (2)0.6197 (4)0.7834 (2)0.0344 (7)
H20.0861450.7196150.7664220.041*
C40.0688 (2)0.5553 (4)0.8753 (2)0.0350 (7)
H30.0282350.6019560.9328770.042*
C50.10922 (19)0.4220 (4)0.8715 (2)0.0332 (7)
H40.1017230.3594190.9259030.040*
C60.0722 (2)0.0631 (4)0.9693 (2)0.0380 (8)
H50.0321420.1083110.9753540.046*
C70.1045 (2)0.1336 (4)0.9208 (2)0.0362 (8)
H60.0905690.2355280.8874980.043*
C80.16702 (18)0.0398 (4)0.9400 (2)0.0335 (7)
C90.1704 (2)0.0874 (4)0.9965 (2)0.0381 (8)
H70.2097540.1664361.0245980.046*
C100.1123 (2)0.0738 (4)1.0150 (2)0.0401 (9)
H80.1054390.1399471.0589220.048*
C110.2285 (2)0.2840 (5)0.7442 (3)0.0524 (10)
H90.2137810.2020410.7910470.063*
H100.2383480.2382120.6854700.063*
H110.2720790.3347780.7357130.063*
C120.2244 (2)0.0779 (5)0.9148 (3)0.0509 (10)
H120.2505620.0170260.9178580.061*
H130.2010800.1204110.8518410.061*
H140.2580690.1547500.9584720.061*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mo10.02236 (13)0.01507 (12)0.01911 (12)0.00142 (9)0.00902 (10)0.00024 (9)
Mo20.02366 (13)0.01577 (12)0.01921 (12)0.00191 (9)0.00860 (10)0.00260 (9)
Se10.02711 (16)0.01821 (15)0.02549 (15)0.00290 (11)0.01325 (12)0.00020 (11)
Se20.02603 (16)0.01916 (14)0.01959 (14)0.00302 (11)0.00805 (12)0.00285 (11)
C10.0301 (17)0.0359 (18)0.0375 (17)0.0050 (14)0.0196 (14)0.0026 (14)
C20.0305 (17)0.0322 (17)0.0314 (16)0.0127 (14)0.0151 (13)0.0036 (14)
C30.042 (2)0.0175 (14)0.0447 (19)0.0097 (14)0.0232 (16)0.0006 (14)
C40.0388 (19)0.0307 (17)0.0322 (16)0.0051 (14)0.0157 (14)0.0109 (14)
C50.0404 (19)0.0358 (18)0.0283 (15)0.0116 (15)0.0210 (14)0.0031 (14)
C60.044 (2)0.0360 (19)0.0345 (17)0.0073 (15)0.0200 (15)0.0200 (15)
C70.046 (2)0.0199 (15)0.0370 (17)0.0100 (14)0.0169 (16)0.0127 (13)
C80.0306 (17)0.0340 (18)0.0287 (15)0.0130 (14)0.0099 (13)0.0145 (14)
C90.0344 (19)0.0376 (19)0.0261 (15)0.0056 (15)0.0036 (14)0.0067 (14)
C100.051 (2)0.041 (2)0.0208 (14)0.0139 (17)0.0122 (15)0.0095 (14)
C110.039 (2)0.055 (2)0.068 (3)0.0036 (19)0.031 (2)0.006 (2)
C120.046 (2)0.052 (2)0.052 (2)0.0155 (19)0.0230 (19)0.0129 (19)
Geometric parameters (Å, º) top
Mo1—C32.332 (3)C2—C31.416 (5)
Mo1—C22.339 (3)C2—H10.9800
Mo1—C42.355 (3)C3—C41.413 (5)
Mo1—C52.356 (3)C3—H20.9800
Mo1—C12.370 (3)C4—C51.394 (5)
Mo1—Se22.4633 (4)C4—H30.9800
Mo1—Se12.4659 (4)C5—H40.9800
Mo1—Se2i2.4689 (3)C6—C101.402 (5)
Mo1—Mo1i2.9857 (5)C6—C71.419 (5)
Mo1—Mo22.9875 (3)C6—H50.9800
Mo1—Mo2i2.9935 (3)C7—C81.432 (5)
Mo2—C102.337 (3)C7—H60.9800
Mo2—C62.350 (3)C8—C91.396 (5)
Mo2—C92.352 (3)C8—C121.506 (5)
Mo2—C72.356 (3)C9—C101.414 (5)
Mo2—C82.387 (3)C9—H70.9800
Mo2—Se22.4635 (4)C10—H80.9800
Mo2—Se12.4691 (4)C11—H90.9600
Mo2—Se1i2.4692 (4)C11—H100.9600
Mo2—Mo2i3.0083 (5)C11—H110.9600
C1—C21.404 (5)C12—H120.9600
C1—C51.435 (5)C12—H130.9600
C1—C111.487 (5)C12—H140.9600
C3—Mo1—C235.30 (12)C7—Mo2—Mo1i145.65 (9)
C3—Mo1—C435.09 (12)C8—Mo2—Mo1i118.70 (8)
C2—Mo1—C458.11 (11)Se2—Mo2—Mo1i52.718 (9)
C3—Mo1—C558.16 (12)Se1—Mo2—Mo1i99.982 (11)
C2—Mo1—C558.09 (11)Se1i—Mo2—Mo1i52.606 (9)
C4—Mo1—C534.41 (12)Mo1—Mo2—Mo1i59.894 (10)
C3—Mo1—C158.43 (12)C10—Mo2—Mo2i157.50 (10)
C2—Mo1—C134.69 (12)C6—Mo2—Mo2i127.01 (9)
C4—Mo1—C158.08 (12)C9—Mo2—Mo2i164.17 (9)
C5—Mo1—C135.36 (11)C7—Mo2—Mo2i115.98 (9)
C3—Mo1—Se2100.84 (9)C8—Mo2—Mo2i131.90 (8)
C2—Mo1—Se2136.14 (9)Se2—Mo2—Mo2i100.132 (8)
C4—Mo1—Se285.36 (9)Se1—Mo2—Mo2i52.472 (10)
C5—Mo1—Se2105.65 (9)Se1i—Mo2—Mo2i52.471 (10)
C1—Mo1—Se2140.55 (8)Mo1—Mo2—Mo2i59.902 (8)
C3—Mo1—Se1145.37 (9)Mo1i—Mo2—Mo2i59.705 (8)
C2—Mo1—Se1116.29 (9)Mo1—Se1—Mo274.510 (12)
C4—Mo1—Se1123.79 (9)Mo1—Se1—Mo2i74.684 (11)
C5—Mo1—Se191.58 (9)Mo2—Se1—Mo2i75.060 (13)
C1—Mo1—Se187.30 (8)Mo1—Se2—Mo274.656 (12)
Se2—Mo1—Se1103.651 (13)Mo1—Se2—Mo1i74.507 (12)
C3—Mo1—Se2i94.16 (9)Mo2—Se2—Mo1i74.730 (11)
C2—Mo1—Se2i84.87 (8)C2—C1—C5106.8 (3)
C4—Mo1—Se2i128.63 (9)C2—C1—C11128.0 (3)
C5—Mo1—Se2i142.82 (8)C5—C1—C11125.1 (3)
C1—Mo1—Se2i110.62 (8)C2—C1—Mo171.44 (19)
Se2—Mo1—Se2i103.560 (13)C5—C1—Mo171.77 (18)
Se1—Mo1—Se2i103.372 (13)C11—C1—Mo1125.8 (2)
C3—Mo1—Mo1i114.04 (9)C1—C2—C3108.9 (3)
C2—Mo1—Mo1i129.84 (8)C1—C2—Mo173.87 (18)
C4—Mo1—Mo1i126.24 (9)C3—C2—Mo172.07 (17)
C5—Mo1—Mo1i157.28 (9)C1—C2—H1125.4
C1—Mo1—Mo1i162.73 (8)C3—C2—H1125.4
Se2—Mo1—Mo1i52.834 (10)Mo1—C2—H1125.4
Se1—Mo1—Mo1i100.268 (9)C4—C3—C2107.4 (3)
Se2i—Mo1—Mo1i52.659 (10)C4—C3—Mo173.37 (18)
C3—Mo1—Mo2152.01 (9)C2—C3—Mo172.64 (17)
C2—Mo1—Mo2168.55 (9)C4—C3—H2126.0
C4—Mo1—Mo2122.87 (8)C2—C3—H2126.0
C5—Mo1—Mo2115.34 (8)Mo1—C3—H2126.0
C1—Mo1—Mo2134.39 (8)C5—C4—C3108.5 (3)
Se2—Mo1—Mo252.676 (10)C5—C4—Mo172.81 (18)
Se1—Mo1—Mo252.794 (10)C3—C4—Mo171.54 (17)
Se2i—Mo1—Mo2100.565 (11)C5—C4—H3125.6
Mo1i—Mo1—Mo260.153 (8)C3—C4—H3125.6
C3—Mo1—Mo2i143.92 (9)Mo1—C4—H3125.6
C2—Mo1—Mo2i117.47 (8)C4—C5—C1108.4 (3)
C4—Mo1—Mo2i173.63 (9)C4—C5—Mo172.78 (18)
C5—Mo1—Mo2i140.04 (9)C1—C5—Mo172.87 (17)
C1—Mo1—Mo2i115.58 (8)C4—C5—H4125.6
Se2—Mo1—Mo2i100.539 (11)C1—C5—H4125.6
Se1—Mo1—Mo2i52.709 (9)Mo1—C5—H4125.6
Se2i—Mo1—Mo2i52.551 (9)C10—C6—C7108.1 (3)
Mo1i—Mo1—Mo2i59.954 (8)C10—C6—Mo272.11 (18)
Mo2—Mo1—Mo2i60.394 (10)C7—C6—Mo272.68 (17)
C10—Mo2—C634.82 (13)C10—C6—H5125.8
C10—Mo2—C935.10 (13)C7—C6—H5125.8
C6—Mo2—C957.92 (13)Mo2—C6—H5125.8
C10—Mo2—C758.26 (13)C6—C7—C8107.6 (3)
C6—Mo2—C735.11 (12)C6—C7—Mo272.22 (18)
C9—Mo2—C757.88 (13)C8—C7—Mo273.65 (18)
C10—Mo2—C857.94 (12)C6—C7—H6126.0
C6—Mo2—C858.10 (12)C8—C7—H6126.0
C9—Mo2—C834.26 (12)Mo2—C7—H6126.0
C7—Mo2—C835.14 (12)C9—C8—C7107.3 (3)
C10—Mo2—Se289.56 (9)C9—C8—C12125.0 (3)
C6—Mo2—Se2122.11 (9)C7—C8—C12127.4 (3)
C9—Mo2—Se286.33 (9)C9—C8—Mo271.47 (18)
C7—Mo2—Se2143.71 (9)C7—C8—Mo271.21 (18)
C8—Mo2—Se2115.33 (9)C12—C8—Mo2127.8 (2)
C10—Mo2—Se1105.64 (10)C8—C9—C10109.1 (3)
C6—Mo2—Se185.26 (9)C8—C9—Mo274.27 (18)
C9—Mo2—Se1140.23 (9)C10—C9—Mo271.88 (18)
C7—Mo2—Se1101.27 (9)C8—C9—H7125.3
C8—Mo2—Se1136.41 (9)C10—C9—H7125.3
Se2—Mo2—Se1103.549 (13)Mo2—C9—H7125.3
C10—Mo2—Se1i144.67 (10)C6—C10—C9107.9 (3)
C6—Mo2—Se1i130.55 (9)C6—C10—Mo273.08 (18)
C9—Mo2—Se1i112.09 (9)C9—C10—Mo273.01 (18)
C7—Mo2—Se1i96.22 (9)C6—C10—H8125.8
C8—Mo2—Se1i86.98 (8)C9—C10—H8125.8
Se2—Mo2—Se1i103.434 (13)Mo2—C10—H8125.8
Se1—Mo2—Se1i103.004 (13)C1—C11—H9109.5
C10—Mo2—Mo1113.56 (9)C1—C11—H10109.5
C6—Mo2—Mo1121.66 (9)H9—C11—H10109.5
C9—Mo2—Mo1133.12 (9)C1—C11—H11109.5
C7—Mo2—Mo1151.79 (9)H9—C11—H11109.5
C8—Mo2—Mo1167.07 (9)H10—C11—H11109.5
Se2—Mo2—Mo152.668 (10)C8—C12—H12109.5
Se1—Mo2—Mo152.696 (9)C8—C12—H13109.5
Se1i—Mo2—Mo1100.141 (11)H12—C12—H13109.5
C10—Mo2—Mo1i138.65 (10)C8—C12—H14109.5
C6—Mo2—Mo1i173.27 (10)H12—C12—H14109.5
C9—Mo2—Mo1i115.84 (9)H13—C12—H14109.5
C5—C1—C2—C30.5 (4)C10—C6—C7—C81.8 (4)
C11—C1—C2—C3174.6 (3)Mo2—C6—C7—C865.7 (2)
Mo1—C1—C2—C364.0 (2)C10—C6—C7—Mo263.8 (2)
C5—C1—C2—Mo163.5 (2)C6—C7—C8—C92.0 (3)
C11—C1—C2—Mo1121.4 (4)Mo2—C7—C8—C962.8 (2)
C1—C2—C3—C40.5 (4)C6—C7—C8—C12171.5 (3)
Mo1—C2—C3—C465.7 (2)Mo2—C7—C8—C12123.7 (3)
C1—C2—C3—Mo165.2 (2)C6—C7—C8—Mo264.7 (2)
C2—C3—C4—C51.3 (4)C7—C8—C9—C101.3 (3)
Mo1—C3—C4—C563.9 (2)C12—C8—C9—C10172.4 (3)
C2—C3—C4—Mo165.2 (2)Mo2—C8—C9—C1063.9 (2)
C3—C4—C5—C11.6 (4)C7—C8—C9—Mo262.6 (2)
Mo1—C4—C5—C164.7 (2)C12—C8—C9—Mo2123.7 (3)
C3—C4—C5—Mo163.0 (2)C7—C6—C10—C91.0 (4)
C2—C1—C5—C41.3 (4)Mo2—C6—C10—C965.2 (2)
C11—C1—C5—C4173.9 (3)C7—C6—C10—Mo264.2 (2)
Mo1—C1—C5—C464.6 (2)C8—C9—C10—C60.2 (4)
C2—C1—C5—Mo163.3 (2)Mo2—C9—C10—C665.3 (2)
C11—C1—C5—Mo1121.4 (3)C8—C9—C10—Mo265.5 (2)
Symmetry code: (i) x, y, z+3/2.
 

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