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The title complex, [Co4(CH3O)4L4(CH4O)4] (LH = 2-hydroxy­benz­aldehyde, C7H6O2), has a cubane-type structural topology with four Co atoms and four O atoms, each derived from MeO, at alternate corners. Each Co atom is coordinated in a distorted octahedral geometry defined by three bridging O atoms, two O atoms from chelating L, and one O atom from a methanol mol­ecule.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536801010479/tk6029sup1.cif
Contains datablocks I, Co4

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536801010479/tk6029Isup2.hkl
Contains datablock I

CCDC reference: 170751

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.006 Å
  • R factor = 0.037
  • wR factor = 0.103
  • Data-to-parameter ratio = 14.2

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


Yellow Alert Alert Level C:
PLAT_213 Alert C Atom C2 has ADP max/min Ratio ........... 3.60
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
1 Alert Level C = Please check

Comment top

In the past two decades, cubane-type polynuclear complexes have received much attention owing to their magnetic and optical properties, as well their biological relevance. Complexes of the type Mn4O4 and their derivatives have been extensively studied for they are thought to have relevance to the Water Oxidation Center (WOC) in the photosynthetic apparatus of green plants and cyanobacteria (Christou, 1989; Brudrig et al., 1991; Dimitrou et al., 1993; Taft et al., 1993; Wieghardt, 1989). Recently, several cubane-type complexes of cobalt and other transition metals, such as nickel, zinc and cadmium, have been reported. For example, Christou and others have reported biologically relevant cubane complexes, e.g. [Co4O4(OAc)2bpy4(ClO4)2], containing the [Co4O4]+4 core, which is structurally analogous to, but more stable than, that of MnIIIMnIV or MnIV4 species (Dimitrou et al., 1993). Two mixed-valence clusters, [Co8O4(O2CPh)12solv4] (solv = DMF, MeCN, H2O) containing the [CoIII4O4]+4 core, [Co8O4(OH)4(OAc)6L2](ClO4)2 [L = 1,2-bis(2,2'-bipyridyl-6-yl)ethane] containing a [Co8µ4-O43-OH)4]+8 core with an unusual face-sharing triple-cubane architecture, as well as [Co4(2,2-PyC(O)(OH)4(OAc)3(H2O)](ClO4), containing the [CoII4O4]+4 cubane unit, have been also reported (Dimitrou et al., 1995; Grillo et al., 1996; Tong et al., 1999). In an attempt to prepare Schiff base complexes, the unexpected complex, [Co4(OMe)4L4(MeOH)4] (LH = 2-hydroxylbenzaldehyde), was isolated and characterized crystallographically.

As shown in Fig. 1, four Co atoms and four O atoms, each from MeO-, occupy alternate corners of the cubane unit where each Co atom is surrounded by three bridging O atoms derived from MeO-, one from MeOH and two O atoms from chelating 2-formylphenolate so as to form a distorted octahedral geometry. Each of the bridging O atoms has a remarkably distorted tetrahedral geometry. The Co—O(MeOH) bond lengths are longer than those for Co—O(MeO-).

Experimental top

A solution of melamine (0.04 g, 0.33 mmol) and salicylahdehyde (0.12 g, 1 mmol) in methanol solution (20 ml) was heated to 333 K for 3 h with vigorous stirring. After cooling, NaOH (0.04 g, 1 mmol) in methanol (5 ml) was added to the colorless solution. Co(NO3)2·6H2O (0.15 g, 0.5 mmol) was then added and the reaction mixture was stirred for 1 h to give a red solution which was filtered. Deep-red and pale-red crystalline complexes were obtained by keeping the resultant solution open to the air for a week. A deep-red single-crystal was selected for X-ray diffraction.

Refinement top

H-atom positions were generated geometrically and allowed to ride on their respective parent carbon atoms. The O—H atoms were refined with isotropic displacement parameters but fixed in the final cycles of least-squares refinement.

Computing details top

Data collection: SMART (Siemens, 1994); cell refinement: SMART; data reduction: SMART; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXL97; software used to prepare material for publication: SHELXL97.

Figures top
[Figure 1] Fig. 1. The structure of [Co4(OMe)4L4(MeOH)4]. Displacement ellipsoids are plotted at the 50% probability level (Sheldrick, 1997)
Tetra-u3methanolate tetra-u2(2-hydroxylatebenzaldehyde) tetra-methanol tetracobalt(II) [Co4OMe4L4(MeOH)4] (L=2-hydroxylatebenzaldehyde) top
Crystal data top
[Co4(CH3O)4(C7H5O2)4(CH4O)4]F(000) = 2000
Mr = 972.46Dx = 1.518 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
a = 14.6546 (5) ÅCell parameters from 154 reflections
b = 14.7082 (5) Åθ = 3.1–20.7°
c = 20.3235 (7) ŵ = 1.60 mm1
β = 103.789 (1)°T = 293 K
V = 4254.3 (3) Å3Block, dark-red
Z = 40.50 × 0.45 × 0.45 mm
Data collection top
Siemens SMART CCD
diffractometer
7411 independent reflections
Radiation source: fine-focus sealed tube5377 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.039
ω scansθmax = 24.9°, θmin = 1.6°
Absorption correction: empirical (using intensity measurements)
(SADABS; Sheldrick, 1996)
h = 1717
Tmin = 0.454, Tmax = 0.487k = 1217
15156 measured reflectionsl = 1024
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)] = 0.037Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.103H-atom parameters constrained
S = 1.01 w = 1/[σ2(Fo2) + (0.0537P)2 + 0.6296P]
where P = (Fo2 + 2Fc2)/3
7411 reflections(Δ/σ)max = 0.001
521 parametersΔρmax = 0.58 e Å3
0 restraintsΔρmin = 0.37 e Å3
Crystal data top
[Co4(CH3O)4(C7H5O2)4(CH4O)4]V = 4254.3 (3) Å3
Mr = 972.46Z = 4
Monoclinic, P21/nMo Kα radiation
a = 14.6546 (5) ŵ = 1.60 mm1
b = 14.7082 (5) ÅT = 293 K
c = 20.3235 (7) Å0.50 × 0.45 × 0.45 mm
β = 103.789 (1)°
Data collection top
Siemens SMART CCD
diffractometer
7411 independent reflections
Absorption correction: empirical (using intensity measurements)
(SADABS; Sheldrick, 1996)
5377 reflections with I > 2σ(I)
Tmin = 0.454, Tmax = 0.487Rint = 0.039
15156 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0370 restraints
wR(F2) = 0.103H-atom parameters constrained
S = 1.01Δρmax = 0.58 e Å3
7411 reflectionsΔρmin = 0.37 e Å3
521 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
Co10.61010 (3)0.26149 (3)0.03310 (2)0.03916 (14)
Co20.70158 (3)0.24802 (3)0.08950 (2)0.03774 (13)
Co30.82178 (3)0.30894 (3)0.05690 (2)0.03873 (13)
Co40.75875 (3)0.10739 (3)0.02696 (2)0.03858 (13)
O10.6129 (2)0.36420 (19)0.10860 (13)0.0554 (7)
H0A0.664 (3)0.381 (2)0.1210 (18)0.046 (12)*
O20.56573 (19)0.2969 (2)0.14293 (13)0.0632 (8)
H0B0.536 (3)0.310 (3)0.112 (2)0.095 (18)*
O30.94220 (17)0.2422 (2)0.12119 (13)0.0546 (8)
H0C0.937 (3)0.191 (2)0.1168 (18)0.034 (12)*
O40.7689 (2)0.0147 (2)0.05559 (15)0.0576 (7)
H0D0.754 (3)0.041 (3)0.086 (2)0.081 (18)*
O50.69698 (14)0.34157 (15)0.01468 (10)0.0379 (5)
O60.63723 (14)0.15938 (15)0.03310 (10)0.0381 (5)
O70.73533 (13)0.21335 (15)0.09075 (9)0.0366 (5)
O80.82575 (14)0.21275 (15)0.01710 (10)0.0370 (5)
O110.52403 (16)0.18250 (18)0.07986 (12)0.0557 (7)
O120.49213 (15)0.30573 (17)0.03334 (11)0.0499 (6)
O210.76493 (17)0.33054 (16)0.15137 (11)0.0509 (6)
O220.71430 (17)0.14363 (15)0.15242 (10)0.0481 (6)
O310.91173 (17)0.40862 (18)0.03044 (11)0.0546 (7)
O320.80070 (16)0.39746 (17)0.12793 (11)0.0514 (6)
O410.68988 (17)0.00369 (18)0.06603 (12)0.0536 (6)
O420.88034 (15)0.06955 (17)0.09166 (11)0.0503 (6)
C10.5456 (3)0.4347 (3)0.1060 (2)0.0766 (13)
H1A0.56360.47180.14580.115*
H1B0.48500.40840.10390.115*
H1C0.54270.47140.06650.115*
C20.5078 (5)0.2866 (7)0.2050 (3)0.208 (5)
H2A0.45130.32080.20760.311*
H2B0.49250.22340.21280.311*
H2C0.53860.30810.23880.311*
C31.0405 (2)0.2581 (3)0.1278 (2)0.0695 (12)
H3A1.07640.21640.16010.104*
H3B1.05560.31930.14290.104*
H3C1.05530.24940.08470.104*
C40.8537 (3)0.0334 (3)0.0574 (3)0.0854 (15)
H4A0.84340.06950.09780.128*
H4B0.87120.07210.01840.128*
H4C0.90320.00950.05710.128*
C50.6783 (3)0.4354 (3)0.03076 (18)0.0556 (10)
H5A0.67890.46870.01000.083*
H5B0.61790.44130.06160.083*
H5C0.72580.45920.05140.083*
C60.5617 (2)0.0999 (3)0.06551 (18)0.0520 (9)
H6A0.51070.13550.09140.078*
H6B0.54050.06600.03170.078*
H6C0.58370.05880.09500.078*
C70.7481 (2)0.1963 (3)0.16190 (15)0.0523 (10)
H7A0.81060.17420.18020.078*
H7B0.70340.15160.16860.078*
H7C0.73870.25170.18440.078*
C80.9097 (2)0.2004 (3)0.03997 (18)0.0501 (9)
H8A0.90000.15370.07400.075*
H8B0.96000.18290.00250.075*
H8C0.92580.25630.05890.075*
C110.4378 (3)0.1822 (3)0.06512 (18)0.0577 (10)
H11A0.40980.14330.09050.069*
C120.3741 (2)0.2341 (3)0.01376 (17)0.0483 (9)
C130.2762 (3)0.2229 (3)0.0092 (2)0.0679 (12)
H13A0.25710.18460.03970.082*
C140.2099 (3)0.2665 (4)0.0386 (3)0.0818 (15)
H14A0.14650.26010.03960.098*
C150.2385 (3)0.3206 (3)0.0856 (3)0.0763 (13)
H15A0.19330.34920.11910.092*
C160.3320 (3)0.3331 (3)0.0841 (2)0.0635 (11)
H16A0.34860.36940.11680.076*
C170.4035 (2)0.2917 (3)0.03349 (17)0.0477 (9)
C210.7779 (2)0.3085 (2)0.20756 (16)0.0452 (9)
H21A0.80170.35410.23040.054*
C220.7615 (2)0.2234 (2)0.24203 (15)0.0369 (7)
C230.7787 (2)0.2180 (3)0.30763 (16)0.0448 (8)
H23A0.79990.26930.32620.054*
C240.7651 (3)0.1397 (3)0.34414 (17)0.0532 (10)
H24A0.77730.13730.38700.064*
C250.7326 (3)0.0633 (3)0.31676 (18)0.0580 (10)
H25A0.72200.00980.34180.070*
C260.7161 (3)0.0658 (3)0.25292 (18)0.0556 (10)
H26A0.69500.01330.23560.067*
C270.7299 (2)0.1449 (2)0.21295 (15)0.0388 (8)
C310.9500 (3)0.4691 (3)0.06939 (18)0.0576 (10)
H31A0.99490.50330.05490.069*
C320.9343 (2)0.4940 (2)0.13429 (17)0.0465 (9)
C330.9944 (3)0.5610 (3)0.1717 (2)0.0659 (11)
H33A1.04060.58690.15330.079*
C340.9861 (3)0.5885 (3)0.2341 (2)0.0794 (14)
H34A1.02600.63270.25800.095*
C350.9168 (3)0.5493 (3)0.2618 (2)0.0766 (14)
H35A0.91210.56600.30500.092*
C360.8556 (3)0.4865 (3)0.22591 (18)0.0621 (11)
H36A0.80860.46290.24480.075*
C370.8617 (2)0.4564 (2)0.16106 (16)0.0450 (9)
C410.7273 (3)0.0537 (3)0.10748 (17)0.0525 (9)
H41A0.68770.09840.11730.063*
C420.8247 (3)0.0612 (2)0.14293 (16)0.0493 (9)
C430.8490 (4)0.1332 (3)0.1902 (2)0.0726 (12)
H43A0.80240.17330.19600.087*
C440.9383 (4)0.1454 (4)0.2273 (2)0.0900 (16)
H44A0.95280.19360.25760.108*
C451.0071 (3)0.0855 (4)0.2197 (2)0.0864 (16)
H45A1.06820.09370.24530.104*
C460.9876 (3)0.0133 (3)0.1748 (2)0.0679 (12)
H46A1.03560.02620.17110.082*
C470.8957 (2)0.0012 (3)0.13453 (16)0.0487 (9)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co10.0316 (2)0.0468 (3)0.0380 (2)0.0009 (2)0.00628 (18)0.0036 (2)
Co20.0417 (2)0.0391 (3)0.0308 (2)0.0032 (2)0.00539 (18)0.00050 (19)
Co30.0354 (2)0.0461 (3)0.0342 (2)0.0082 (2)0.00738 (17)0.0046 (2)
Co40.0350 (2)0.0402 (3)0.0392 (2)0.0000 (2)0.00617 (18)0.0055 (2)
O10.0461 (16)0.060 (2)0.0610 (16)0.0014 (15)0.0154 (13)0.0109 (13)
O20.0547 (16)0.088 (2)0.0403 (14)0.0088 (15)0.0009 (12)0.0099 (14)
O30.0336 (13)0.067 (2)0.0573 (16)0.0087 (14)0.0011 (11)0.0007 (15)
O40.0767 (19)0.0441 (19)0.0573 (17)0.0048 (14)0.0263 (14)0.0057 (14)
O50.0379 (12)0.0376 (15)0.0373 (11)0.0009 (10)0.0070 (9)0.0023 (10)
O60.0336 (11)0.0402 (14)0.0368 (11)0.0065 (10)0.0008 (9)0.0009 (10)
O70.0327 (11)0.0467 (15)0.0291 (10)0.0026 (10)0.0046 (8)0.0050 (10)
O80.0330 (11)0.0428 (14)0.0363 (11)0.0039 (10)0.0103 (9)0.0005 (10)
O110.0420 (14)0.070 (2)0.0548 (14)0.0020 (13)0.0117 (11)0.0152 (13)
O120.0355 (12)0.0565 (17)0.0551 (14)0.0012 (11)0.0058 (10)0.0138 (12)
O210.0682 (16)0.0409 (16)0.0444 (13)0.0107 (12)0.0153 (12)0.0029 (11)
O220.0712 (16)0.0379 (15)0.0368 (12)0.0098 (12)0.0163 (11)0.0015 (10)
O310.0608 (15)0.0595 (18)0.0469 (13)0.0230 (14)0.0194 (12)0.0107 (13)
O320.0485 (14)0.0604 (18)0.0484 (13)0.0159 (13)0.0177 (11)0.0145 (12)
O410.0499 (14)0.0536 (18)0.0556 (14)0.0053 (12)0.0090 (12)0.0142 (13)
O420.0389 (12)0.0564 (17)0.0535 (14)0.0053 (12)0.0068 (10)0.0179 (12)
C10.075 (3)0.065 (3)0.097 (3)0.016 (3)0.033 (3)0.004 (3)
C20.103 (5)0.455 (15)0.048 (3)0.084 (7)0.014 (3)0.001 (5)
C30.0338 (19)0.089 (4)0.079 (3)0.007 (2)0.0002 (18)0.001 (2)
C40.087 (3)0.062 (3)0.126 (4)0.008 (3)0.064 (3)0.000 (3)
C50.069 (3)0.041 (3)0.056 (2)0.0014 (19)0.0143 (19)0.0072 (18)
C60.0427 (19)0.050 (3)0.058 (2)0.0135 (17)0.0009 (16)0.0071 (18)
C70.049 (2)0.072 (3)0.0354 (17)0.0032 (19)0.0101 (15)0.0055 (17)
C80.0404 (18)0.060 (3)0.053 (2)0.0049 (17)0.0169 (16)0.0072 (18)
C110.057 (2)0.069 (3)0.052 (2)0.013 (2)0.0216 (18)0.0003 (19)
C120.0410 (18)0.053 (3)0.052 (2)0.0042 (17)0.0126 (16)0.0146 (18)
C130.045 (2)0.090 (3)0.071 (3)0.017 (2)0.020 (2)0.023 (2)
C140.040 (2)0.103 (4)0.098 (4)0.001 (2)0.008 (2)0.029 (3)
C150.044 (2)0.070 (3)0.101 (3)0.011 (2)0.011 (2)0.008 (3)
C160.045 (2)0.052 (3)0.085 (3)0.0052 (19)0.000 (2)0.003 (2)
C170.0387 (18)0.045 (2)0.055 (2)0.0020 (16)0.0034 (16)0.0079 (17)
C210.0468 (19)0.045 (2)0.0436 (19)0.0080 (17)0.0099 (15)0.0063 (17)
C220.0350 (16)0.038 (2)0.0355 (16)0.0006 (15)0.0042 (13)0.0006 (15)
C230.0444 (19)0.052 (2)0.0394 (18)0.0002 (17)0.0123 (14)0.0068 (17)
C240.062 (2)0.063 (3)0.0366 (18)0.008 (2)0.0150 (16)0.0010 (19)
C250.078 (3)0.046 (3)0.051 (2)0.000 (2)0.0172 (19)0.0135 (19)
C260.076 (3)0.041 (2)0.052 (2)0.007 (2)0.0191 (19)0.0023 (18)
C270.0411 (18)0.038 (2)0.0350 (16)0.0004 (15)0.0051 (13)0.0018 (15)
C310.054 (2)0.061 (3)0.059 (2)0.018 (2)0.0149 (18)0.003 (2)
C320.0423 (19)0.044 (2)0.052 (2)0.0034 (17)0.0075 (16)0.0124 (17)
C330.046 (2)0.064 (3)0.084 (3)0.012 (2)0.008 (2)0.023 (2)
C340.055 (3)0.084 (4)0.091 (3)0.004 (2)0.002 (2)0.051 (3)
C350.068 (3)0.094 (4)0.062 (3)0.006 (3)0.004 (2)0.039 (3)
C360.063 (2)0.073 (3)0.053 (2)0.001 (2)0.0173 (19)0.020 (2)
C370.0421 (19)0.045 (2)0.0447 (18)0.0018 (17)0.0039 (15)0.0072 (17)
C410.063 (2)0.047 (3)0.049 (2)0.010 (2)0.0171 (18)0.0034 (19)
C420.070 (2)0.041 (2)0.0380 (17)0.0015 (19)0.0141 (17)0.0036 (16)
C430.103 (4)0.055 (3)0.057 (2)0.006 (3)0.013 (2)0.013 (2)
C440.111 (4)0.082 (4)0.071 (3)0.031 (3)0.009 (3)0.028 (3)
C450.069 (3)0.112 (5)0.073 (3)0.042 (3)0.007 (2)0.029 (3)
C460.049 (2)0.089 (4)0.064 (2)0.019 (2)0.0107 (19)0.019 (2)
C470.053 (2)0.056 (3)0.0379 (18)0.0177 (19)0.0122 (15)0.0065 (17)
Geometric parameters (Å, º) top
Co1—O12.147 (3)C5—H5C0.9600
Co1—O52.131 (2)C6—H6A0.9600
Co1—O62.116 (2)C6—H6B0.9600
Co1—O72.054 (2)C6—H6C0.9600
Co1—O112.101 (2)C7—H7A0.9600
Co1—O122.030 (2)C7—H7B0.9600
Co2—O22.152 (3)C7—H7C0.9600
Co2—O52.064 (2)C8—H8A0.9600
Co2—O62.102 (2)C8—H8B0.9600
Co2—O82.114 (2)C8—H8C0.9600
Co2—O212.115 (2)C11—C121.442 (5)
Co2—O222.035 (2)C11—H11A0.9300
Co3—O32.165 (3)C12—C171.422 (5)
Co3—O52.103 (2)C12—C131.425 (5)
Co3—O72.114 (2)C13—C141.359 (6)
Co3—O82.076 (2)C13—H13A0.9300
Co3—O312.125 (2)C14—C151.382 (6)
Co3—O322.022 (2)C14—H14A0.9300
Co4—O42.194 (3)C15—C161.376 (6)
Co4—O62.052 (2)C15—H15A0.9300
Co4—O72.107 (2)C16—C171.419 (5)
Co4—O82.141 (2)C16—H16A0.9300
Co4—O412.088 (2)C21—C221.426 (5)
Co4—O422.024 (2)C21—H21A0.9300
O1—C11.423 (5)C22—C231.417 (4)
O1—H0A0.77 (4)C22—C271.424 (4)
O2—C21.351 (6)C23—C241.359 (5)
O2—H0B0.86 (5)C23—H23A0.9300
O3—C31.434 (4)C24—C251.387 (5)
O3—H0C0.75 (3)C24—H24A0.9300
O4—C41.438 (5)C25—C261.376 (5)
O4—H0D0.72 (4)C25—H25A0.9300
O5—C51.430 (4)C26—C271.406 (5)
O6—C61.440 (4)C26—H26A0.9300
O7—C71.435 (3)C31—C321.439 (5)
O8—C81.427 (4)C31—H31A0.9300
O11—C111.227 (4)C32—C371.417 (5)
O12—C171.314 (4)C32—C331.417 (5)
O21—C211.244 (4)C33—C341.364 (6)
O22—C271.304 (3)C33—H33A0.9300
O31—C311.233 (4)C34—C351.397 (6)
O32—C371.310 (4)C34—H34A0.9300
O41—C411.226 (4)C35—C361.370 (6)
O42—C471.315 (4)C35—H35A0.9300
C1—H1A0.9600C36—C371.413 (5)
C1—H1B0.9600C36—H36A0.9300
C1—H1C0.9600C41—C421.441 (5)
C2—H2A0.9600C41—H41A0.9300
C2—H2B0.9600C42—C431.417 (5)
C2—H2C0.9600C42—C471.428 (5)
C3—H3A0.9600C43—C441.358 (7)
C3—H3B0.9600C43—H43A0.9300
C3—H3C0.9600C44—C451.375 (7)
C4—H4A0.9600C44—H44A0.9300
C4—H4B0.9600C45—C461.384 (6)
C4—H4C0.9600C45—H45A0.9300
C5—H5A0.9600C46—C471.416 (5)
C5—H5B0.9600C46—H46A0.9300
O12—Co1—O591.51 (8)H3A—C3—H3B109.5
O12—Co1—O693.66 (9)O3—C3—H3C109.5
O12—Co1—O7173.41 (9)H3A—C3—H3C109.5
O12—Co1—O1188.30 (9)H3B—C3—H3C109.5
O5—Co1—O191.44 (10)O4—C4—H4A109.5
O6—Co1—O1168.34 (9)O4—C4—H4B109.5
O6—Co1—O583.07 (8)H4A—C4—H4B109.5
O7—Co1—O188.44 (10)O4—C4—H4C109.5
O7—Co1—O584.30 (8)H4A—C4—H4C109.5
O7—Co1—O680.81 (8)H4B—C4—H4C109.5
O7—Co1—O1195.88 (9)O5—C5—H5A109.5
O11—Co1—O188.68 (10)O5—C5—H5B109.5
O11—Co1—O5179.78 (9)H5A—C5—H5B109.5
O11—Co1—O696.84 (9)O5—C5—H5C109.5
O12—Co1—O196.77 (10)H5A—C5—H5C109.5
O5—Co2—O287.72 (10)H5B—C5—H5C109.5
O5—Co2—O685.07 (8)O6—C6—H6A109.5
O5—Co2—O879.89 (8)O6—C6—H6B109.5
O5—Co2—O2198.71 (9)H6A—C6—H6B109.5
O6—Co2—O290.07 (10)O6—C6—H6C109.5
O6—Co2—O883.79 (8)H6A—C6—H6C109.5
O6—Co2—O21176.18 (8)H6B—C6—H6C109.5
O8—Co2—O2166.58 (10)O7—C7—H7A109.5
O8—Co2—O2197.34 (9)O7—C7—H7B109.5
O21—Co2—O289.57 (10)H7A—C7—H7B109.5
O22—Co2—O298.48 (11)O7—C7—H7C109.5
O22—Co2—O5171.91 (9)H7A—C7—H7C109.5
O22—Co2—O689.70 (9)H7B—C7—H7C109.5
O22—Co2—O893.42 (9)O8—C8—H8A109.5
O22—Co2—O2186.59 (9)O8—C8—H8B109.5
O5—Co3—O3166.01 (11)H8A—C8—H8B109.5
O5—Co3—O783.52 (8)O8—C8—H8C109.5
O5—Co3—O3199.04 (9)H8A—C8—H8C109.5
O7—Co3—O388.13 (10)H8B—C8—H8C109.5
O7—Co3—O31175.72 (8)O11—C11—C12128.8 (3)
O8—Co3—O388.19 (10)O11—C11—H11A115.6
O8—Co3—O579.88 (8)C12—C11—H11A115.6
O8—Co3—O784.54 (8)C17—C12—C13119.2 (4)
O8—Co3—O3199.25 (9)C17—C12—C11123.7 (3)
O31—Co3—O390.01 (11)C13—C12—C11117.1 (4)
O32—Co3—O395.88 (11)C14—C13—C12121.9 (4)
O32—Co3—O595.24 (9)C14—C13—H13A119.0
O32—Co3—O789.46 (9)C12—C13—H13A119.0
O32—Co3—O8172.64 (9)C13—C14—C15118.8 (4)
O32—Co3—O3186.90 (9)C13—C14—H14A120.6
O6—Co4—O489.08 (10)C15—C14—H14A120.6
O6—Co4—O781.07 (8)C16—C15—C14121.7 (4)
O6—Co4—O884.32 (8)C16—C15—H15A119.1
O6—Co4—O4193.95 (9)C14—C15—H15A119.1
O7—Co4—O4168.73 (10)C15—C16—C17121.2 (4)
O7—Co4—O883.12 (8)C15—C16—H16A119.4
O8—Co4—O490.50 (9)C17—C16—H16A119.4
O41—Co4—O487.92 (10)O12—C17—C16119.5 (3)
O41—Co4—O798.16 (9)O12—C17—C12123.4 (3)
O41—Co4—O8177.67 (9)C16—C17—C12117.0 (3)
O42—Co4—O496.68 (11)O21—C21—C22129.4 (3)
O42—Co4—O6173.63 (10)O21—C21—H21A115.3
O42—Co4—O792.92 (9)C22—C21—H21A115.3
O42—Co4—O892.88 (8)C23—C22—C27119.5 (3)
O42—Co4—O4189.00 (9)C23—C22—C21117.7 (3)
C1—O1—Co1126.2 (3)C27—C22—C21122.7 (3)
C1—O1—H0A113 (3)C24—C23—C22121.7 (3)
Co1—O1—H0A108 (3)C24—C23—H23A119.1
C2—O2—Co2137.1 (4)C22—C23—H23A119.1
C2—O2—H0B113 (3)C23—C24—C25119.2 (3)
Co2—O2—H0B106 (3)C23—C24—H24A120.4
C3—O3—Co3129.7 (3)C25—C24—H24A120.4
C3—O3—H0C104 (3)C26—C25—C24120.8 (4)
Co3—O3—H0C109 (3)C26—C25—H25A119.6
C4—O4—Co4122.8 (3)C24—C25—H25A119.6
C4—O4—H0D110 (4)C25—C26—C27122.2 (4)
Co4—O4—H0D105 (4)C25—C26—H26A118.9
C5—O5—Co2120.88 (19)C27—C26—H26A118.9
C5—O5—Co3117.8 (2)O22—C27—C26120.0 (3)
Co2—O5—Co3100.48 (9)O22—C27—C22123.4 (3)
C5—O5—Co1122.4 (2)C26—C27—C22116.6 (3)
Co2—O5—Co195.47 (9)O31—C31—C32128.6 (3)
Co3—O5—Co194.26 (8)O31—C31—H31A115.7
C6—O6—Co4120.6 (2)C32—C31—H31A115.7
C6—O6—Co2121.51 (19)C37—C32—C33119.5 (3)
Co4—O6—Co296.72 (8)C37—C32—C31123.5 (3)
C6—O6—Co1118.77 (19)C33—C32—C31117.0 (3)
Co4—O6—Co198.87 (8)C34—C33—C32121.6 (4)
Co2—O6—Co194.77 (9)C34—C33—H33A119.2
C7—O7—Co1121.26 (19)C32—C33—H33A119.2
C7—O7—Co4119.3 (2)C33—C34—C35119.1 (4)
Co1—O7—Co499.12 (8)C33—C34—H34A120.4
C7—O7—Co3120.00 (19)C35—C34—H34A120.4
Co1—O7—Co396.22 (8)C36—C35—C34120.7 (4)
Co4—O7—Co395.37 (8)C36—C35—H35A119.7
C8—O8—Co3119.87 (19)C34—C35—H35A119.7
C8—O8—Co2118.07 (18)C35—C36—C37121.9 (4)
Co3—O8—Co299.73 (9)C35—C36—H36A119.1
C8—O8—Co4124.1 (2)C37—C36—H36A119.1
Co3—O8—Co495.48 (8)O32—C37—C36119.9 (3)
Co2—O8—Co493.69 (8)O32—C37—C32122.9 (3)
C11—O11—Co1125.8 (2)C36—C37—C32117.2 (3)
C17—O12—Co1129.4 (2)O41—C41—C42128.6 (3)
C21—O21—Co2125.5 (2)O41—C41—H41A115.7
C27—O22—Co2130.2 (2)C42—C41—H41A115.7
C31—O31—Co3123.3 (2)C43—C42—C47119.2 (4)
C37—O32—Co3126.3 (2)C43—C42—C41117.1 (4)
C41—O41—Co4125.9 (2)C47—C42—C41123.7 (3)
C47—O42—Co4128.8 (2)C44—C43—C42121.9 (5)
O1—C1—H1A109.5C44—C43—H43A119.1
O1—C1—H1B109.5C42—C43—H43A119.1
H1A—C1—H1B109.5C43—C44—C45119.3 (4)
O1—C1—H1C109.5C43—C44—H44A120.4
H1A—C1—H1C109.5C45—C44—H44A120.4
H1B—C1—H1C109.5C44—C45—C46121.6 (4)
O2—C2—H2A109.5C44—C45—H45A119.2
O2—C2—H2B109.5C46—C45—H45A119.2
H2A—C2—H2B109.5C45—C46—C47121.0 (4)
O2—C2—H2C109.5C45—C46—H46A119.5
H2A—C2—H2C109.5C47—C46—H46A119.5
H2B—C2—H2C109.5O42—C47—C46119.2 (4)
O3—C3—H3A109.5O42—C47—C42123.8 (3)
O3—C3—H3B109.5C46—C47—C42117.0 (3)

Experimental details

Crystal data
Chemical formula[Co4(CH3O)4(C7H5O2)4(CH4O)4]
Mr972.46
Crystal system, space groupMonoclinic, P21/n
Temperature (K)293
a, b, c (Å)14.6546 (5), 14.7082 (5), 20.3235 (7)
β (°) 103.789 (1)
V3)4254.3 (3)
Z4
Radiation typeMo Kα
µ (mm1)1.60
Crystal size (mm)0.50 × 0.45 × 0.45
Data collection
DiffractometerSiemens SMART CCD
diffractometer
Absorption correctionEmpirical (using intensity measurements)
(SADABS; Sheldrick, 1996)
Tmin, Tmax0.454, 0.487
No. of measured, independent and
observed [I > 2σ(I)] reflections
15156, 7411, 5377
Rint0.039
(sin θ/λ)max1)0.592
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.037, 0.103, 1.01
No. of reflections7411
No. of parameters521
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.58, 0.37

Computer programs: SMART (Siemens, 1994), SMART, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXL97.

Selected geometric parameters (Å, º) top
Co1—O12.147 (3)Co3—O32.165 (3)
Co1—O52.131 (2)Co3—O52.103 (2)
Co1—O62.116 (2)Co3—O72.114 (2)
Co1—O72.054 (2)Co3—O82.076 (2)
Co1—O112.101 (2)Co3—O312.125 (2)
Co1—O122.030 (2)Co3—O322.022 (2)
Co2—O22.152 (3)Co4—O42.194 (3)
Co2—O52.064 (2)Co4—O62.052 (2)
Co2—O62.102 (2)Co4—O72.107 (2)
Co2—O82.114 (2)Co4—O82.141 (2)
Co2—O212.115 (2)Co4—O412.088 (2)
Co2—O222.035 (2)Co4—O422.024 (2)
O12—Co1—O591.51 (8)O5—Co3—O3166.01 (11)
O12—Co1—O693.66 (9)O5—Co3—O783.52 (8)
O12—Co1—O7173.41 (9)O5—Co3—O3199.04 (9)
O12—Co1—O1188.30 (9)O7—Co3—O388.13 (10)
O5—Co1—O191.44 (10)O7—Co3—O31175.72 (8)
O6—Co1—O1168.34 (9)O8—Co3—O388.19 (10)
O6—Co1—O583.07 (8)O8—Co3—O579.88 (8)
O7—Co1—O188.44 (10)O8—Co3—O784.54 (8)
O7—Co1—O584.30 (8)O8—Co3—O3199.25 (9)
O7—Co1—O680.81 (8)O31—Co3—O390.01 (11)
O7—Co1—O1195.88 (9)O32—Co3—O395.88 (11)
O11—Co1—O188.68 (10)O32—Co3—O595.24 (9)
O11—Co1—O5179.78 (9)O32—Co3—O789.46 (9)
O11—Co1—O696.84 (9)O32—Co3—O8172.64 (9)
O12—Co1—O196.77 (10)O32—Co3—O3186.90 (9)
O5—Co2—O287.72 (10)O6—Co4—O489.08 (10)
O5—Co2—O685.07 (8)O6—Co4—O781.07 (8)
O5—Co2—O879.89 (8)O6—Co4—O884.32 (8)
O5—Co2—O2198.71 (9)O6—Co4—O4193.95 (9)
O6—Co2—O290.07 (10)O7—Co4—O4168.73 (10)
O6—Co2—O883.79 (8)O7—Co4—O883.12 (8)
O6—Co2—O21176.18 (8)O8—Co4—O490.50 (9)
O8—Co2—O2166.58 (10)O41—Co4—O487.92 (10)
O8—Co2—O2197.34 (9)O41—Co4—O798.16 (9)
O21—Co2—O289.57 (10)O41—Co4—O8177.67 (9)
O22—Co2—O298.48 (11)O42—Co4—O496.68 (11)
O22—Co2—O5171.91 (9)O42—Co4—O6173.63 (10)
O22—Co2—O689.70 (9)O42—Co4—O792.92 (9)
O22—Co2—O893.42 (9)O42—Co4—O892.88 (8)
O22—Co2—O2186.59 (9)O42—Co4—O4189.00 (9)
 

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