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The crystal structure determination of the title compound, [Mo2(C8H6ClO3)4], confirms the existence of a quadruple bond between the Mo atoms, with an Mo—Mo distance of 2.101 (5) Å. One half of the mol­ecule constitutes the asymmetric unit and the carboxyl­ate ligands define a paddle-wheel structure, with similar O—C—O angles of 122.9 (3) and 123.7 (3)°. The inter­planar angles between the acetate and 4-chloro­phen­oxy planes in the two independent ligands are 135.9 (8) and 91.3 (8)°, which is indicative of a dramatic difference in the orientation of the ligands.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805015795/fl6166sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805015795/fl6166Isup2.hkl
Contains datablock I

CCDC reference: 274396

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.005 Å
  • R factor = 0.026
  • wR factor = 0.063
  • Data-to-parameter ratio = 11.1

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT027_ALERT_3_B _diffrn_reflns_theta_full (too) Low ............ 24.96 Deg. PLAT430_ALERT_2_B Short Inter D...A Contact O2 .. O2 .. 2.75 Ang.
Alert level C PLAT164_ALERT_4_C Nr. of Refined C-H H-Atoms in Heavy-At Struct... 12 PLAT199_ALERT_1_C Check the Reported _cell_measurement_temperature 293 K PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C6 PLAT350_ALERT_3_C Short C-H Bond (0.96A) C4 - H4 ... 0.79 Ang. PLAT350_ALERT_3_C Short C-H Bond (0.96A) C5 - H5 ... 0.82 Ang. PLAT350_ALERT_3_C Short C-H Bond (0.96A) C8 - H8 ... 0.83 Ang.
0 ALERT level A = In general: serious problem 2 ALERT level B = Potentially serious problem 6 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 2 ALERT type 2 Indicator that the structure model may be wrong or deficient 4 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: CAD-4 EXPRESS (Enraf–Nonius, 1994); cell refinement: CAD-4 EXPRESS; data reduction: XCAD4 (Harms & Wocadlo, 1995); program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).

Tetrakis(µ-4-chlorophenoxyacetato-κ2O,O')dimolybdenum(II) top
Crystal data top
[Mo2(C8H6ClO3)4]Z = 1
Mr = 934.19F(000) = 464
Triclinic, P1Dx = 1.797 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71069 Å
a = 5.668 (1) ÅCell parameters from 25 reflections
b = 11.549 (1) Åθ = 10–15°
c = 13.743 (2) ŵ = 1.10 mm1
α = 91.95 (1)°T = 293 K
β = 101.74 (1)°Prism, pale red
γ = 100.64 (1)°0.3 × 0.1 × 0.1 mm
V = 863.3 (2) Å3
Data collection top
Enraf–Nonius TurboCAD-4
diffractometer
Rint = 0.016
non–profiled ω/2θ scansθmax = 25.0°, θmin = 1.5°
Absorption correction: ψ scan
(North et al., 1968)
h = 06
Tmin = 0.856, Tmax = 0.895k = 1313
3374 measured reflectionsl = 1615
3036 independent reflections3 standard reflections every 166 min
2657 reflections with I > 2σ(I) intensity decay: none
Refinement top
Refinement on F20 restraints
Least-squares matrix: fullAll H-atom parameters refined
R[F2 > 2σ(F2)] = 0.026 w = 1/[σ2(Fo2) + (0.0257P)2 + 0.59P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.063(Δ/σ)max = 0.004
S = 1.04Δρmax = 0.62 e Å3
3036 reflectionsΔρmin = 0.47 e Å3
274 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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
C10.3199 (5)0.1942 (2)0.0341 (2)0.0334 (6)
C20.4872 (6)0.3051 (3)0.0510 (3)0.0422 (8)
C30.7827 (5)0.3718 (3)0.1468 (2)0.0364 (7)
C40.7985 (7)0.4885 (3)0.1170 (3)0.0505 (9)
C50.9518 (7)0.5762 (3)0.1528 (3)0.0588 (10)
C61.0877 (6)0.5472 (3)0.2171 (3)0.0492 (8)
C71.0712 (7)0.4314 (3)0.2489 (3)0.0547 (9)
C80.9188 (7)0.3437 (3)0.2135 (3)0.0491 (8)
C90.1150 (6)0.0730 (3)0.1957 (2)0.0381 (7)
C100.1788 (8)0.1210 (3)0.3041 (3)0.0518 (9)
C110.0945 (6)0.0535 (3)0.3872 (2)0.0434 (7)
C120.1502 (6)0.0770 (3)0.3399 (3)0.0490 (8)
C130.3061 (8)0.1723 (4)0.3645 (3)0.0600 (10)
C140.2193 (8)0.2435 (3)0.4344 (3)0.0637 (11)
C150.0253 (9)0.2221 (4)0.4813 (3)0.0626 (11)
C160.1819 (8)0.1271 (4)0.4582 (3)0.0535 (9)
O40.2364 (4)0.00369 (18)0.16549 (15)0.0382 (5)
O50.0604 (4)0.10905 (18)0.13974 (15)0.0378 (5)
O60.2654 (4)0.0395 (2)0.37040 (16)0.0515 (6)
O10.1003 (3)0.20143 (17)0.03518 (15)0.0357 (5)
O20.4019 (3)0.09980 (17)0.01690 (15)0.0343 (4)
O30.6387 (4)0.27830 (18)0.11428 (17)0.0444 (5)
Cl11.2911 (2)0.65818 (10)0.25803 (10)0.0864 (4)
Cl20.4170 (3)0.36302 (12)0.46626 (13)0.1121 (5)
Mo10.14071 (4)0.04903 (2)0.011244 (19)0.02837 (9)
H40.730 (7)0.507 (3)0.076 (3)0.058 (12)*
H50.961 (8)0.646 (4)0.135 (3)0.080 (14)*
H71.175 (7)0.416 (3)0.293 (3)0.070 (12)*
H80.906 (6)0.273 (3)0.232 (3)0.047 (10)*
H120.213 (6)0.026 (3)0.294 (3)0.048 (10)*
H130.458 (8)0.186 (3)0.332 (3)0.062 (12)*
H140.094 (8)0.274 (4)0.524 (3)0.075 (13)*
H150.334 (8)0.110 (4)0.488 (3)0.069 (13)*
H2A0.583 (6)0.341 (3)0.015 (3)0.045 (9)*
H2B0.399 (7)0.358 (3)0.079 (3)0.053 (10)*
H10A0.309 (7)0.186 (3)0.312 (3)0.053 (10)*
H10B0.036 (7)0.148 (3)0.321 (3)0.058 (11)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.0288 (15)0.0302 (15)0.0436 (16)0.0058 (12)0.0130 (13)0.0060 (12)
C20.0359 (17)0.0327 (16)0.064 (2)0.0066 (14)0.0232 (16)0.0095 (16)
C30.0327 (15)0.0338 (16)0.0431 (17)0.0033 (12)0.0114 (13)0.0088 (13)
C40.049 (2)0.0381 (19)0.073 (2)0.0048 (15)0.0344 (19)0.0055 (17)
C50.057 (2)0.035 (2)0.089 (3)0.0036 (17)0.031 (2)0.0109 (19)
C60.0429 (19)0.049 (2)0.058 (2)0.0035 (15)0.0174 (16)0.0214 (17)
C70.056 (2)0.065 (2)0.049 (2)0.0054 (18)0.0279 (18)0.0084 (18)
C80.053 (2)0.043 (2)0.053 (2)0.0027 (16)0.0224 (17)0.0009 (16)
C90.0389 (17)0.0381 (16)0.0373 (16)0.0010 (14)0.0135 (14)0.0072 (13)
C100.059 (2)0.052 (2)0.0410 (19)0.0004 (19)0.0136 (17)0.0037 (16)
C110.0486 (19)0.0507 (19)0.0324 (16)0.0077 (15)0.0146 (14)0.0002 (14)
C120.044 (2)0.062 (2)0.0421 (19)0.0111 (17)0.0116 (16)0.0043 (17)
C130.050 (2)0.067 (3)0.063 (2)0.003 (2)0.019 (2)0.000 (2)
C140.079 (3)0.049 (2)0.071 (3)0.005 (2)0.042 (2)0.0027 (19)
C150.085 (3)0.059 (2)0.057 (2)0.028 (2)0.030 (2)0.0161 (19)
C160.057 (2)0.068 (3)0.0379 (19)0.019 (2)0.0089 (18)0.0026 (17)
O40.0351 (11)0.0437 (12)0.0373 (11)0.0094 (9)0.0091 (9)0.0078 (9)
O50.0379 (11)0.0372 (11)0.0421 (12)0.0082 (9)0.0162 (10)0.0038 (9)
O60.0466 (13)0.0644 (15)0.0372 (12)0.0010 (12)0.0047 (10)0.0068 (11)
O10.0297 (11)0.0306 (10)0.0517 (12)0.0087 (8)0.0159 (9)0.0115 (9)
O20.0254 (10)0.0324 (10)0.0499 (12)0.0080 (8)0.0158 (9)0.0105 (9)
O30.0427 (12)0.0305 (11)0.0665 (15)0.0026 (9)0.0306 (11)0.0059 (10)
Cl10.0746 (7)0.0733 (7)0.1229 (10)0.0022 (6)0.0518 (7)0.0493 (7)
Cl20.1253 (12)0.0721 (8)0.1529 (14)0.0008 (8)0.0756 (11)0.0330 (8)
Mo10.02287 (13)0.02914 (13)0.03674 (14)0.00697 (9)0.01212 (9)0.00842 (9)
Geometric parameters (Å, º) top
C1—O11.260 (3)C10—H10A0.94 (4)
C1—O21.273 (3)C10—H10B0.98 (4)
C1—C21.502 (4)C11—O61.367 (4)
C2—O31.405 (4)C11—C121.379 (5)
C2—H2A0.99 (3)C11—C161.391 (5)
C2—H2B0.91 (4)C12—C131.376 (5)
C3—O31.374 (3)C12—H120.93 (3)
C3—C41.377 (5)C13—C141.360 (6)
C3—C81.379 (4)C13—H130.87 (4)
C4—C51.380 (5)C14—C151.378 (6)
C4—H40.80 (4)C14—Cl21.739 (4)
C5—C61.356 (5)C15—C161.368 (6)
C5—H50.83 (4)C15—H140.94 (4)
C6—C71.373 (5)C16—H150.86 (4)
C6—Cl11.748 (3)O4—Mo12.117 (2)
C7—C81.375 (5)O5—Mo1i2.096 (2)
C7—H70.96 (4)O1—Mo12.0991 (19)
C8—H80.84 (3)O2—Mo1i2.1529 (19)
C9—O41.258 (4)Mo1—O5i2.096 (2)
C9—O51.272 (4)Mo1—Mo1i2.1007 (5)
C9—C101.519 (5)Mo1—O2i2.1529 (19)
C10—O61.415 (4)
O1—C1—O2122.9 (3)H10A—C10—H10B109 (3)
O1—C1—C2116.5 (3)O6—C11—C12124.9 (3)
O2—C1—C2120.6 (2)O6—C11—C16115.4 (3)
O3—C2—C1109.8 (3)C12—C11—C16119.7 (3)
O3—C2—H2A112.1 (19)C13—C12—C11119.6 (4)
C1—C2—H2A107.4 (19)C13—C12—H12120 (2)
O3—C2—H2B109 (2)C11—C12—H12121 (2)
C1—C2—H2B111 (2)C14—C13—C12120.3 (4)
H2A—C2—H2B107 (3)C14—C13—H13122 (3)
O3—C3—C4124.5 (3)C12—C13—H13117 (3)
O3—C3—C8116.1 (3)C13—C14—C15120.9 (4)
C4—C3—C8119.4 (3)C13—C14—Cl2120.2 (4)
C3—C4—C5120.1 (3)C15—C14—Cl2118.9 (3)
C3—C4—H4121 (3)C16—C15—C14119.5 (4)
C5—C4—H4118 (3)C16—C15—H14118 (3)
C6—C5—C4119.9 (4)C14—C15—H14123 (3)
C6—C5—H5120 (3)C15—C16—C11120.1 (4)
C4—C5—H5120 (3)C15—C16—H15122 (3)
C5—C6—C7120.7 (3)C11—C16—H15118 (3)
C5—C6—Cl1119.7 (3)C9—O4—Mo1116.22 (19)
C7—C6—Cl1119.6 (3)C9—O5—Mo1i116.47 (19)
C6—C7—C8119.6 (3)C11—O6—C10116.8 (3)
C6—C7—H7117 (2)C1—O1—Mo1118.00 (18)
C8—C7—H7123 (2)C1—O2—Mo1i115.71 (17)
C7—C8—C3120.2 (3)C3—O3—C2117.1 (2)
C7—C8—H8121 (2)O5i—Mo1—O187.74 (8)
C3—C8—H8119 (2)O5i—Mo1—Mo1i92.03 (6)
O4—C9—O5123.7 (3)O1—Mo1—Mo1i92.07 (5)
O4—C9—C10120.1 (3)O5i—Mo1—O4176.38 (8)
O5—C9—C10116.1 (3)O1—Mo1—O491.45 (8)
O6—C10—C9113.0 (3)Mo1i—Mo1—O491.52 (6)
O6—C10—H10A106 (2)O5i—Mo1—O2i90.34 (8)
C9—C10—H10A108 (2)O1—Mo1—O2i176.22 (7)
O6—C10—H10B112 (2)Mo1i—Mo1—O2i91.25 (5)
C9—C10—H10B109 (2)O4—Mo1—O2i90.27 (8)
Symmetry code: (i) x, y, z.
 

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