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Acta Cryst. (2010). E66, m1401-m1402    [ doi:10.1107/S160053681003895X ]

Bis(tetraphenylarsonium) di-[mu]-hydroxido-bis[(nitrilotriacetato)cobalt(III)] octahydrate

H. G. Visser and J. K. Clegg

Abstract top

In the title compound, (C24H20As)2[Co2(C6H6NO6)2(OH)2]·8H2O, the CoIII atom in the binuclear centrosymmetric anion is octahedrally surrounded by one N atom and three O atoms of the tetradentate nitrilotriacetate ligand and two [mu]-hydroxide ligands. The crystal packing is controlled by C-H...O and O-H...O hydrogen-bonding interactions. The crystal employed in this study proved to be a two-component twin around (0\overline 11).

Comment top

The title complex, (AsC24H20)2[Co(C6H6N)(µ-OH)]2.8(H2O), forms a part of an ongoing investigation of the structural and kinetic behaviour of CoIII-nitrilotriacetato compounds (Visser et al., (1997, 1999, 2001, 2002, 2003). The CoIII atom is octahedrally surrounded by one N atom and three O atoms of the tetradentate nitrilotriacetato ligand and two µ-hydroxo ligands (Fig. 1). The Co–O bond distances which vary between 1.8806 (11) and 1.9027 (11) Å and the Co–N1 distance of 1.9312 (13) Å fall well within the normal range (Table 1). The octahedron around the Co atom is only slighlty distorted. The crystal packing is controlled by C—H–O and O—H–O hydrogen bonding interactions (Table 2), creating a three dimensional network.

Related literature top

For synthetic background, related structures and kinetics, see: Mori et al. (1958); Visser et al. (1997, 1999, 2001, 2002, 2003). Twinning which was resolved using the programs ROTAX, see: Cooper et al. (2002).

Experimental top

The title compound was prepared similar to the method described by Mori et al. (1958). CoCl2.6H2O (5 g, 21 mmol) and nitrilotriacetic acid (4 g, 21 mmol) was added to a KHCO3 solution (25 cm3, 2.5 M). H2O2 (1 ml, 30%) was added to this solution and the mixture was placed on an ice bath. After 5 h a purple precipitate separated out. The precipitate was filtered and washed several times with cold water. The product was then redissolved in hot water after which an excess of tetraphenylarsonium was added. Purple crystals of the title compound were obtained after several days.

Refinement top

The methyl and aromatic H atoms were placed in geometrically idealized positions (C—H = 0.93–0.96 Å) and constrained to ride on their parent atoms, with Uiso(H) = 1.5Ueq(C) and 1.2Ueq(C), respectively. The hydrogen atoms of the aqua solvent molecules were obtained from the difference Fourier map. Despite appearing (at least visually) to be single, the crystal employed in this study proved to be a two-component twin around (0 -1 1). Twinning which was resolved using the programs ROTAX (Cooper et al., 2002) and Make HKLF5 (Farrugia, 1999) with a final minor component of 0.0712 (4).

Computing details top

Data collection: APEX2 (Bruker, 2005); cell refinement: SAINT-Plus (Bruker, 2004); data reduction: SAINT-Plus and XPREP (Bruker, 2004); program(s) used to solve structure: SHELXL97 (Sheldrick, 2008); program(s) used to refine structure: SIR97 (Altomare et al., 1999); molecular graphics: DIAMOND (Brandenburg & Putz, 2005); software used to prepare material for publication: WinGX (Farrugia, 1999).

Figures top
[Figure 1] Fig. 1. View of the title compund (50% probability displacement ellipsoids). Hydrogen atoms and solvent water molecules omitted for clarity.
Bis(tetraphenylarsonium) di-µ-hydroxido-bis[(nitrilotriacetato)cobalt(III)] octahydrate top
Crystal data top
(C24H20As)2[Co2(C6H6NO6)2(OH)2]·8H2OZ = 1
Mr = 1438.88F(000) = 740
Triclinic, P1Dx = 1.549 Mg m−3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 7.328 (5) ÅCell parameters from 9875 reflections
b = 14.491 (5) Åθ = 2.5–28.3°
c = 16.564 (5) ŵ = 1.68 mm−1
α = 113.555 (5)°T = 100 K
β = 97.040 (5)°Plate, purple
γ = 101.152 (5)°0.44 × 0.19 × 0.03 mm
V = 1542.4 (13) Å3
Data collection top
Bruker X8 APEXII 4K KappaCCD
diffractometer		23223 independent reflections
Radiation source: sealed tube20726 reflections with I > 2σ(I)
graphiteRint = 0.030
Detector resolution: 0 pixels mm-1θmax = 25.0°, θmin = 1.6°
phi and ω scansh = −8→8
Absorption correction: multi-scan
(SADABS; Bruker, 2004)		k = −17→17
Tmin = 0.687, Tmax = 0.950l = −19→19
23209 measured reflections
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)] = 0.030Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.098H atoms treated by a mixture of independent and constrained refinement
S = 0.93 w = 1/[σ2(Fo2) + (0.0699P)2 + 0.5465P]
where P = (Fo2 + 2Fc2)/3
23223 reflections(Δ/σ)max = 0.001
430 parametersΔρmax = 0.41 e Å−3
10 restraintsΔρmin = −0.35 e Å−3
Crystal data top
(C24H20As)2[Co2(C6H6NO6)2(OH)2]·8H2Oγ = 101.152 (5)°
Mr = 1438.88V = 1542.4 (13) Å3
Triclinic, P1Z = 1
a = 7.328 (5) ÅMo Kα radiation
b = 14.491 (5) ŵ = 1.68 mm−1
c = 16.564 (5) ÅT = 100 K
α = 113.555 (5)°0.44 × 0.19 × 0.03 mm
β = 97.040 (5)°
Data collection top
Bruker X8 APEXII 4K KappaCCD
diffractometer		23223 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2004)		20726 reflections with I > 2σ(I)
Tmin = 0.687, Tmax = 0.950Rint = 0.030
23209 measured reflectionsθmax = 25.0°
Refinement top
R[F2 > 2σ(F2)] = 0.030H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.098Δρmax = 0.41 e Å−3
S = 0.93Δρmin = −0.35 e Å−3
23223 reflectionsAbsolute structure: ?
430 parametersFlack parameter: ?
10 restraintsRogers parameter: ?
Special details top

Experimental. The crystal was coated in Exxon Paratone N hydrocarbon oil and mounted on a thin mohair fibre attached to a copper pin. Upon mounting on the diffractometer, the crystal was quenched to 100(K) under a cold nitrogen gas stream supplied by an Oxford Cryosystems Cryostream and data were collected at this temperature.

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
As0.39743 (2)0.447716 (10)0.212481 (9)0.01293 (5)
Co10.52032 (3)0.909913 (13)0.511641 (11)0.00933 (6)
O50.37750 (13)0.76948 (7)0.46088 (6)0.0136 (2)
O60.37392 (15)0.61846 (7)0.46771 (7)0.0226 (2)
O30.67319 (13)0.87442 (7)0.42572 (6)0.0118 (2)
O70.35509 (14)0.94527 (7)0.43838 (6)0.0103 (2)
C25−0.0013 (2)0.57427 (12)0.12621 (10)0.0239 (4)
H25−0.11440.54860.08270.029*
C220.3389 (2)0.65222 (11)0.25432 (9)0.0183 (3)
H220.45370.67830.29690.022*
C240.0660 (2)0.68072 (12)0.18135 (10)0.0249 (4)
H24−0.00290.72610.17540.030*
N10.69776 (16)0.87921 (8)0.58731 (7)0.0111 (2)
C440.6324 (2)0.27716 (12)−0.04076 (10)0.0270 (4)
H440.67760.2413−0.09120.032*
C54−0.0652 (2)0.19678 (11)0.24101 (10)0.0223 (4)
H4−0.15890.14720.24590.027*
C130.7874 (2)0.53345 (10)0.45190 (9)0.0159 (3)
H130.79720.51650.50050.019*
C110.6130 (2)0.51328 (10)0.31153 (9)0.0141 (3)
C160.7629 (2)0.58563 (10)0.30779 (9)0.0171 (3)
H360.75380.60280.25930.021*
C120.6230 (2)0.48623 (10)0.38328 (9)0.0145 (3)
H120.52220.43780.38540.017*
C30.8420 (2)0.87705 (10)0.45975 (9)0.0114 (3)
C55−0.0350 (2)0.30323 (11)0.29762 (9)0.0189 (3)
H5−0.10830.32440.34030.023*
C60.6159 (2)0.76932 (10)0.57216 (9)0.0168 (3)
H6B0.57950.76980.62670.020*
H6A0.71290.73170.56030.020*
C230.2356 (2)0.71896 (12)0.24507 (10)0.0241 (4)
H230.28050.79030.28200.029*
C50.4429 (2)0.71259 (11)0.49372 (9)0.0150 (3)
C40.8820 (2)0.89285 (11)0.55782 (9)0.0136 (3)
H4B0.94680.84250.56310.016*
H4A0.96410.96240.59620.016*
C510.2135 (2)0.34422 (10)0.22566 (9)0.0141 (3)
C210.2698 (2)0.54575 (11)0.19945 (9)0.0155 (3)
C460.6374 (2)0.33354 (11)0.11640 (10)0.0209 (3)
H460.68680.33650.17210.025*
C140.9360 (2)0.60521 (11)0.44813 (9)0.0169 (3)
H141.04510.63620.49450.020*
C530.0440 (2)0.16579 (11)0.17818 (10)0.0229 (4)
H30.02340.09510.14100.028*
C450.7061 (2)0.28103 (11)0.04135 (10)0.0258 (4)
H450.80170.24850.04650.031*
C150.9256 (2)0.63202 (10)0.37639 (9)0.0170 (3)
H151.02660.68050.37450.020*
C520.1852 (2)0.23883 (11)0.16938 (9)0.0190 (3)
H20.25870.21750.12690.023*
C560.1045 (2)0.37675 (11)0.28960 (9)0.0163 (3)
H210.12520.44750.32680.020*
C410.4944 (2)0.38168 (10)0.10790 (9)0.0165 (3)
C420.4214 (2)0.37872 (12)0.02556 (10)0.0243 (4)
H420.32650.41150.02010.029*
C260.0983 (2)0.50630 (11)0.13542 (10)0.0195 (3)
H270.05160.43480.09930.023*
C430.4924 (3)0.32580 (12)−0.04900 (10)0.0322 (4)
H430.44480.3233−0.10470.039*
O10.38813 (13)0.94103 (7)0.60717 (6)0.0128 (2)
O40.97100 (13)0.86981 (7)0.41750 (6)0.0142 (2)
O20.45349 (15)1.00672 (8)0.75721 (6)0.0219 (2)
C10.4993 (2)0.96884 (10)0.68350 (9)0.0144 (3)
C20.7004 (2)0.95505 (11)0.68087 (9)0.0143 (3)
H2A0.79021.02160.69670.017*
H2B0.73950.92880.72380.017*
O80.68108 (17)1.03630 (9)0.91382 (8)0.0247 (3)
O110.17288 (17)0.12264 (9)0.75373 (7)0.0268 (3)
O90.33579 (19)1.08138 (10)0.99202 (9)0.0304 (3)
O100.04230 (18)0.13286 (10)0.91136 (8)0.0327 (3)
H9B0.315 (4)1.0439 (17)1.0176 (15)0.079 (9)*
H8B0.616 (3)1.0211 (15)0.8671 (13)0.056 (5)*
H8A0.789 (3)1.0632 (15)0.9127 (13)0.056 (5)*
H9A0.430 (3)1.0771 (13)0.9721 (12)0.035 (4)*
H10B0.069 (3)0.1294 (14)0.8674 (12)0.047 (4)*
H11A0.157 (3)0.1295 (14)0.7106 (12)0.044 (4)*
H11B0.265 (3)0.0912 (13)0.7531 (12)0.044 (4)*
H70.254 (3)0.9294 (13)0.4445 (11)0.035 (4)*
H10C0.126 (3)0.1179 (14)0.9378 (12)0.047 (4)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
As0.01200 (8)0.01345 (9)0.01245 (8)0.00238 (6)0.00164 (6)0.00552 (6)
Co10.00692 (10)0.01049 (10)0.01102 (10)0.00240 (8)0.00233 (8)0.00496 (8)
O50.0106 (5)0.0127 (5)0.0169 (5)0.0017 (4)0.0024 (4)0.0068 (4)
O60.0148 (6)0.0148 (5)0.0392 (6)0.0025 (5)0.0063 (5)0.0133 (5)
O30.0095 (5)0.0139 (5)0.0123 (5)0.0044 (4)0.0034 (4)0.0051 (4)
O70.0070 (5)0.0105 (5)0.0128 (5)0.0014 (4)0.0021 (4)0.0049 (4)
C250.0205 (9)0.0330 (9)0.0250 (8)0.0095 (8)0.0061 (7)0.0180 (7)
C220.0254 (9)0.0190 (8)0.0117 (7)0.0051 (7)0.0077 (7)0.0071 (6)
C240.0349 (10)0.0310 (9)0.0272 (9)0.0213 (8)0.0195 (8)0.0217 (8)
N10.0099 (6)0.0112 (6)0.0125 (6)0.0030 (5)0.0024 (5)0.0055 (5)
C440.0320 (10)0.0193 (8)0.0241 (9)0.0003 (7)0.0169 (8)0.0040 (7)
C540.0172 (8)0.0223 (8)0.0296 (9)−0.0005 (7)0.0019 (7)0.0170 (7)
C130.0173 (8)0.0187 (8)0.0146 (7)0.0092 (7)0.0038 (6)0.0081 (6)
C110.0154 (8)0.0130 (7)0.0114 (7)0.0048 (6)0.0026 (6)0.0025 (6)
C160.0192 (8)0.0176 (8)0.0157 (7)0.0060 (7)0.0055 (6)0.0073 (6)
C120.0121 (7)0.0133 (7)0.0180 (7)0.0038 (6)0.0040 (6)0.0061 (6)
C30.0112 (7)0.0058 (7)0.0145 (7)0.0004 (6)0.0017 (6)0.0029 (6)
C550.0159 (8)0.0254 (8)0.0187 (8)0.0059 (7)0.0042 (6)0.0126 (7)
C60.0175 (8)0.0154 (7)0.0226 (8)0.0044 (6)0.0054 (7)0.0130 (6)
C230.0397 (11)0.0175 (8)0.0191 (8)0.0104 (8)0.0139 (8)0.0087 (7)
C50.0123 (8)0.0153 (8)0.0208 (8)0.0049 (6)0.0104 (6)0.0086 (6)
C40.0095 (7)0.0154 (7)0.0174 (7)0.0045 (6)0.0034 (6)0.0079 (6)
C510.0119 (7)0.0157 (7)0.0143 (7)0.0012 (6)−0.0009 (6)0.0084 (6)
C210.0170 (8)0.0178 (7)0.0153 (7)0.0051 (6)0.0065 (6)0.0097 (6)
C460.0171 (8)0.0211 (8)0.0179 (8)0.0033 (7)0.0000 (7)0.0040 (6)
C140.0126 (8)0.0173 (8)0.0159 (7)0.0052 (6)0.0007 (6)0.0025 (6)
C530.0237 (9)0.0139 (8)0.0257 (8)0.0011 (7)0.0013 (7)0.0061 (7)
C450.0191 (9)0.0192 (8)0.0321 (9)0.0040 (7)0.0078 (7)0.0042 (7)
C150.0145 (8)0.0152 (7)0.0211 (8)0.0043 (6)0.0079 (6)0.0066 (6)
C520.0184 (8)0.0189 (8)0.0190 (8)0.0069 (7)0.0052 (7)0.0064 (6)
C560.0182 (8)0.0139 (7)0.0144 (7)0.0053 (6)0.0014 (6)0.0040 (6)
C410.0154 (8)0.0140 (7)0.0164 (7)−0.0001 (6)0.0046 (6)0.0046 (6)
C420.0298 (10)0.0277 (9)0.0204 (8)0.0116 (8)0.0080 (7)0.0131 (7)
C260.0191 (8)0.0184 (8)0.0212 (8)0.0043 (7)0.0049 (7)0.0091 (6)
C430.0478 (12)0.0314 (9)0.0189 (8)0.0078 (9)0.0119 (8)0.0125 (7)
O10.0102 (5)0.0159 (5)0.0142 (5)0.0039 (4)0.0042 (4)0.0078 (4)
O40.0097 (5)0.0163 (5)0.0160 (5)0.0031 (4)0.0051 (4)0.0058 (4)
O20.0205 (6)0.0339 (6)0.0144 (5)0.0131 (5)0.0085 (5)0.0096 (5)
C10.0147 (8)0.0144 (7)0.0164 (8)0.0031 (6)0.0041 (6)0.0092 (6)
C20.0142 (8)0.0177 (7)0.0119 (7)0.0054 (6)0.0034 (6)0.0065 (6)
O80.0244 (7)0.0317 (7)0.0205 (6)0.0069 (6)0.0048 (5)0.0142 (5)
O110.0276 (7)0.0400 (7)0.0196 (6)0.0191 (6)0.0096 (5)0.0141 (6)
O90.0297 (7)0.0379 (7)0.0403 (7)0.0168 (6)0.0195 (6)0.0267 (6)
O100.0264 (7)0.0510 (8)0.0320 (7)0.0129 (6)0.0107 (6)0.0267 (7)
Geometric parameters (Å, °) top
As—C111.9049 (15)C3—O31.2816 (18)
As—C211.9102 (15)C3—C41.5288 (19)
As—C511.9145 (15)C55—C561.387 (2)
As—C411.9134 (15)C55—H50.9300
Co1—O51.8806 (11)C6—C51.520 (2)
Co1—O11.9027 (11)C6—H6B0.9700
Co1—O31.8903 (11)C6—H6A0.9700
Co1—O51.8806 (11)C23—H230.9300
Co1—O31.8903 (11)C5—O61.2295 (16)
Co1—O71.8915 (11)C5—O51.2855 (17)
Co1—O71.8915 (11)C4—H4B0.9700
Co1—O7i1.8994 (11)C4—H4A0.9700
Co1—N11.9312 (13)C51—C561.391 (2)
Co1—Co1i2.8516 (10)C51—C521.3916 (19)
O5—C51.2855 (17)C21—C261.394 (2)
O6—C51.2295 (16)C46—C411.389 (2)
O3—C31.2816 (18)C46—C451.387 (2)
O7—Co1i1.8994 (11)C46—H460.9300
O7—H70.765 (18)C14—C151.3881 (19)
C25—C261.377 (2)C14—H140.9300
C25—C241.388 (2)C53—C521.396 (2)
C25—H250.9300C53—H30.9300
C22—C231.381 (2)C45—H450.9300
C22—C211.388 (2)C15—H150.9300
C22—H220.9300C52—H20.9300
C24—C231.382 (2)C56—H210.9300
C24—H240.9300C41—C421.383 (2)
N1—C41.4956 (19)C42—C431.392 (2)
N1—C61.4943 (17)C42—H420.9300
N1—C21.4941 (17)C26—H270.9300
C44—C431.375 (3)C43—H430.9300
C44—C451.375 (2)O1—C11.2799 (16)
C44—H440.9300O2—C11.2415 (17)
C54—C531.376 (2)C1—O21.2415 (17)
C54—C551.403 (2)C1—C21.528 (2)
C54—H40.9300C2—H2A0.9700
C13—C141.379 (2)C2—H2B0.9700
C13—C121.391 (2)O8—H8B0.780 (19)
C13—H130.9300O8—H8A0.82 (2)
C11—C121.3906 (19)O11—H11A0.758 (17)
C11—C161.390 (2)O11—H11B0.886 (19)
C16—C151.383 (2)O9—H9B0.82 (2)
C16—H360.9300O9—H9A0.800 (19)
C12—H120.9300O10—H10B0.762 (18)
C3—O41.2396 (18)O10—H10C0.822 (18)
C3—O41.2396 (18)
C11—As—C21112.01 (6)O4—C3—O3122.95 (13)
C11—As—C51111.91 (6)O4—C3—O3122.95 (13)
C21—As—C51107.22 (7)O4—C3—O3122.95 (13)
C11—As—C41105.75 (7)O4—C3—C4120.09 (12)
C21—As—C41110.79 (6)O4—C3—C4120.09 (12)
C51—As—C41109.18 (6)O3—C3—C4116.94 (12)
O5—Co1—O389.83 (5)O3—C3—C4116.94 (12)
O5—Co1—O389.83 (5)C56—C55—C54119.66 (15)
O5—Co1—O389.83 (5)C56—C55—H5120.2
O5—Co1—O389.83 (5)C54—C55—H5120.2
O5—Co1—O793.60 (5)N1—C6—C5112.41 (11)
O5—Co1—O793.60 (5)N1—C6—H6B109.1
O3—Co1—O792.04 (5)C5—C6—H6B109.1
O3—Co1—O792.04 (5)N1—C6—H6A109.1
O5—Co1—O793.60 (5)C5—C6—H6A109.1
O5—Co1—O793.60 (5)H6B—C6—H6A107.9
O3—Co1—O792.04 (5)C24—C23—C22120.60 (14)
O3—Co1—O792.04 (5)C24—C23—H23119.7
O7—Co1—O70.00 (5)C22—C23—H23119.7
O5—Co1—O7i175.18 (4)O6—C5—O5125.03 (13)
O5—Co1—O7i175.18 (4)O6—C5—O5125.03 (13)
O3—Co1—O7i93.03 (5)O6—C5—O5125.03 (13)
O3—Co1—O7i93.03 (5)O6—C5—O5125.03 (13)
O7—Co1—O7i82.43 (5)O6—C5—C6119.13 (12)
O7—Co1—O7i82.43 (5)O6—C5—C6119.13 (12)
O5—Co1—O189.72 (5)O5—C5—C6115.82 (12)
O5—Co1—O189.72 (5)O5—C5—C6115.82 (12)
O3—Co1—O1172.72 (4)N1—C4—C3109.35 (11)
O3—Co1—O1172.72 (4)N1—C4—H4B109.8
O7—Co1—O195.25 (6)C3—C4—H4B109.8
O7—Co1—O195.25 (6)N1—C4—H4A109.8
O7i—Co1—O187.93 (4)C3—C4—H4A109.8
O5—Co1—N188.78 (5)H4B—C4—H4A108.3
O5—Co1—N188.78 (5)C56—C51—C52121.13 (13)
O3—Co1—N187.07 (6)C56—C51—As118.76 (10)
O3—Co1—N187.07 (6)C52—C51—As120.06 (11)
O7—Co1—N1177.45 (4)C22—C21—C26120.58 (14)
O7—Co1—N1177.45 (4)C22—C21—As121.78 (11)
O7i—Co1—N195.23 (5)C26—C21—As117.57 (11)
O1—Co1—N185.65 (6)C41—C46—C45119.64 (14)
O5—Co1—Co1i134.86 (4)C41—C46—H46120.2
O5—Co1—Co1i134.86 (4)C45—C46—H46120.2
O3—Co1—Co1i93.37 (3)C13—C14—C15121.14 (13)
O3—Co1—Co1i93.37 (3)C13—C14—H14119.4
O7—Co1—Co1i41.32 (3)C15—C14—H14119.4
O7—Co1—Co1i41.32 (3)C54—C53—C52121.04 (14)
O7i—Co1—Co1i41.11 (4)C54—C53—H3119.5
O1—Co1—Co1i92.10 (3)C52—C53—H3119.5
N1—Co1—Co1i136.33 (3)C44—C45—C46119.77 (16)
C5—O5—Co1115.09 (9)C44—C45—H45120.1
C3—O3—Co1113.20 (9)C46—C45—H45120.1
Co1—O7—Co1i97.57 (5)C16—C15—C14119.09 (14)
Co1—O7—H7108.2 (13)C16—C15—H15120.5
Co1i—O7—H7117.9 (13)C14—C15—H15120.5
C26—C25—C24120.49 (15)C53—C52—C51118.51 (15)
C26—C25—H25119.8C53—C52—H2120.7
C24—C25—H25119.8C51—C52—H2120.7
C23—C22—C21119.29 (14)C55—C56—C51119.68 (13)
C23—C22—H22120.4C55—C56—H21120.2
C21—C22—H22120.4C51—C56—H21120.2
C23—C24—C25119.74 (14)C46—C41—C42120.64 (14)
C23—C24—H24120.1C46—C41—As117.79 (11)
C25—C24—H24120.1C42—C41—As121.54 (12)
C4—N1—C6112.32 (10)C41—C42—C43118.91 (16)
C4—N1—C2115.56 (11)C41—C42—H42120.5
C6—N1—C2111.17 (10)C43—C42—H42120.5
C4—N1—Co1106.22 (8)C25—C26—C21119.29 (14)
C6—N1—Co1107.09 (8)C25—C26—H27120.4
C2—N1—Co1103.62 (9)C21—C26—H27120.4
C43—C44—C45120.61 (15)C44—C43—C42120.42 (15)
C43—C44—H44119.7C44—C43—H43119.8
C45—C44—H44119.7C42—C43—H43119.8
C53—C54—C55119.99 (14)C1—O1—Co1111.85 (10)
C53—C54—H4120.0O2—C1—O1123.92 (14)
C55—C54—H4120.0O2—C1—O1123.92 (14)
C14—C13—C12120.32 (13)O2—C1—C2119.79 (12)
C14—C13—H13119.8O2—C1—C2119.79 (12)
C12—C13—H13119.8O1—C1—C2116.28 (12)
C12—C11—C16121.26 (13)N1—C2—C1108.05 (11)
C12—C11—As120.89 (11)N1—C2—H2A110.1
C16—C11—As117.79 (10)C1—C2—H2A110.1
C15—C16—C11119.81 (13)N1—C2—H2B110.1
C15—C16—H36120.1C1—C2—H2B110.1
C11—C16—H36120.1H2A—C2—H2B108.4
C13—C12—C11118.38 (13)H8B—O8—H8A107 (2)
C13—C12—H12120.8H11A—O11—H11B108 (2)
C11—C12—H12120.8H9B—O9—H9A112 (2)
O4—C3—O3122.95 (13)H10B—O10—H10C107 (2)
O3—Co1—O5—C588.39 (10)N1—C6—C5—O5−9.19 (18)
O3—Co1—O5—C588.39 (10)N1—C6—C5—O5−9.19 (18)
O7—Co1—O5—C5−179.58 (10)C6—N1—C4—C391.91 (12)
O7—Co1—O5—C5−179.58 (10)C2—N1—C4—C3−139.11 (11)
O1—Co1—O5—C5−84.34 (10)Co1—N1—C4—C3−24.85 (12)
N1—Co1—O5—C51.32 (10)O4—C3—C4—N1−169.55 (11)
Co1i—Co1—O5—C5−177.02 (8)O4—C3—C4—N1−169.55 (11)
O5—Co1—O3—C3−107.97 (9)O3—C3—C4—N112.06 (16)
O5—Co1—O3—C3−107.97 (9)O3—C3—C4—N112.06 (16)
O7—Co1—O3—C3158.44 (9)C11—As—C51—C5672.54 (12)
O7—Co1—O3—C3158.44 (9)C21—As—C51—C56−50.66 (12)
O7i—Co1—O3—C375.91 (9)C41—As—C51—C56−170.74 (11)
N1—Co1—O3—C3−19.18 (9)C11—As—C51—C52−110.07 (12)
Co1i—Co1—O3—C3117.09 (8)C21—As—C51—C52126.73 (11)
O5—Co1—O7—Co1i177.26 (4)C41—As—C51—C526.65 (13)
O5—Co1—O7—Co1i177.26 (4)C23—C22—C21—C260.2 (2)
O3—Co1—O7—Co1i−92.78 (5)C23—C22—C21—As−176.62 (11)
O3—Co1—O7—Co1i−92.78 (5)C11—As—C21—C223.51 (14)
O1—Co1—O7—Co1i87.20 (5)C51—As—C21—C22126.65 (12)
O5—Co1—N1—C4114.14 (8)C41—As—C21—C22−114.30 (12)
O5—Co1—N1—C4114.14 (8)C11—As—C21—C26−173.39 (11)
O3—Co1—N1—C424.25 (8)C51—As—C21—C26−50.25 (13)
O3—Co1—N1—C424.25 (8)C41—As—C21—C2668.80 (13)
O7i—Co1—N1—C4−68.53 (8)C55—C54—C53—C52−0.2 (2)
O1—Co1—N1—C4−156.04 (8)C43—C44—C45—C460.7 (2)
Co1i—Co1—N1—C4−67.56 (9)C41—C46—C45—C440.1 (2)
O5—Co1—N1—C6−6.07 (8)C56—C51—C52—C530.2 (2)
O5—Co1—N1—C6−6.07 (8)As—C51—C52—C53−177.17 (11)
O3—Co1—N1—C6−95.97 (9)C54—C55—C56—C51−0.1 (2)
O3—Co1—N1—C6−95.97 (9)C52—C51—C56—C55−0.1 (2)
O7i—Co1—N1—C6171.26 (8)As—C51—C56—C55177.30 (10)
O1—Co1—N1—C683.74 (9)C45—C46—C41—C42−0.7 (2)
Co1i—Co1—N1—C6172.23 (7)C45—C46—C41—As177.33 (11)
O5—Co1—N1—C2−123.66 (9)C11—As—C41—C4639.24 (12)
O5—Co1—N1—C2−123.66 (9)C21—As—C41—C46160.81 (11)
O3—Co1—N1—C2146.44 (8)C51—As—C41—C46−81.33 (12)
O3—Co1—N1—C2146.44 (8)C11—As—C41—C42−142.74 (12)
O7i—Co1—N1—C253.67 (9)C21—As—C41—C42−21.17 (13)
O1—Co1—N1—C2−33.85 (8)C51—As—C41—C4296.69 (13)
Co1i—Co1—N1—C254.64 (10)C46—C41—C42—C430.6 (2)
C21—As—C11—C12119.23 (12)As—C41—C42—C43−177.37 (12)
C51—As—C11—C12−1.21 (14)C24—C25—C26—C21−1.4 (2)
C41—As—C11—C12−119.99 (12)C22—C21—C26—C250.8 (2)
C21—As—C11—C16−63.40 (13)As—C21—C26—C25177.78 (11)
C51—As—C11—C16176.16 (11)C45—C44—C43—C42−0.8 (2)
C41—As—C11—C1657.38 (13)C41—C42—C43—C440.1 (2)
As—C11—C16—C15−177.37 (11)O5—Co1—O1—C1114.55 (9)
As—C11—C12—C13177.29 (10)O5—Co1—O1—C1114.55 (9)
Co1—O3—C3—O4−170.26 (10)O7—Co1—O1—C1−151.86 (9)
Co1—O3—C3—O4−170.26 (10)O7—Co1—O1—C1−151.86 (9)
Co1—O3—C3—C48.08 (14)O7i—Co1—O1—C1−69.66 (9)
C53—C54—C55—C560.3 (2)N1—Co1—O1—C125.75 (9)
C4—N1—C6—C5−106.93 (13)Co1i—Co1—O1—C1−110.57 (8)
C2—N1—C6—C5121.84 (13)Co1—O1—C1—O2169.64 (11)
Co1—N1—C6—C59.30 (13)Co1—O1—C1—O2169.64 (11)
C25—C24—C23—C220.1 (2)Co1—O1—C1—C2−9.27 (14)
C21—C22—C23—C24−0.6 (2)C4—N1—C2—C1151.43 (11)
Co1—O5—C5—O6−177.51 (11)C6—N1—C2—C1−79.03 (13)
Co1—O5—C5—O6−177.51 (11)Co1—N1—C2—C135.68 (12)
Co1—O5—C5—C64.07 (15)O2—C1—C2—N1162.19 (12)
N1—C6—C5—O6172.29 (12)O2—C1—C2—N1162.19 (12)
N1—C6—C5—O6172.29 (12)O1—C1—C2—N1−18.86 (16)
Symmetry codes: (i) −x+1, −y+2, −z+1.
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
C4—H4A···O4ii0.972.493.239 (2)134
C13—H13···O6iii0.932.393.1207 (19)135
C14—H14···O6iv0.932.553.146 (3)123
C15—H15···O5iv0.932.583.313 (3)136
C23—H23···O70.932.563.4034 (19)150
C52—H2···O9v0.932.533.386 (2)153
O7—H7···O4vi0.77 (2)2.00 (2)2.740 (2)162 (2)
O8—H8A···O10vii0.82 (2)1.94 (2)2.758 (2)178 (2)
O8—H8B···O20.78 (2)1.96 (2)2.7329 (17)171 (2)
O9—H9A···O80.80 (2)2.25 (2)3.045 (2)170 (2)
O9—H9B···O8viii0.82 (2)1.92 (2)2.7290 (19)169 (3)
O10—H10B···O110.76 (2)2.09 (2)2.8483 (18)174 (2)
O10—H10C···O9ix0.82 (2)1.95 (2)2.771 (2)175 (2)
O11—H11A···O4iii0.76 (2)2.22 (2)2.9542 (16)164 (2)
O11—H11B···O2ix0.89 (2)2.02 (2)2.905 (2)172 (2)
Symmetry codes: (ii) −x+2, −y+2, −z+1; (iii) −x+1, −y+1, −z+1; (iv) x+1, y, z; (v) x, y−1, z−1; (vi) x−1, y, z; (vii) x+1, y+1, z; (viii) −x+1, −y+2, −z+2; (ix) x, y−1, z.
Table 1
Selected geometric parameters (Å) top
Co1—O11.9027 (11)Co1—O71.8915 (11)
Co1—O31.8903 (11)Co1—O7i1.8994 (11)
Co1—O51.8806 (11)Co1—N11.9312 (13)
Symmetry codes: (i) −x+1, −y+2, −z+1.
Table 2
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
C4—H4A···O4ii0.972.493.239 (2)134
C13—H13···O6iii0.932.393.1207 (19)135
C14—H14···O6iv0.932.553.146 (3)123
C15—H15···O5iv0.932.583.313 (3)136
C23—H23···O70.932.563.4034 (19)150
C52—H2···O9v0.932.533.386 (2)153
O7—H7···O4vi0.77 (2)2.00 (2)2.740 (2)162 (2)
O8—H8A···O10vii0.82 (2)1.94 (2)2.758 (2)178 (2)
O8—H8B···O20.78 (2)1.96 (2)2.7329 (17)171 (2)
O9—H9A···O80.80 (2)2.25 (2)3.045 (2)170 (2)
O9—H9B···O8viii0.82 (2)1.92 (2)2.7290 (19)169 (3)
O10—H10B···O110.76 (2)2.09 (2)2.8483 (18)174 (2)
O10—H10C···O9ix0.82 (2)1.95 (2)2.771 (2)175 (2)
O11—H11A···O4iii0.76 (2)2.22 (2)2.9542 (16)164 (2)
O11—H11B···O2ix0.89 (2)2.02 (2)2.905 (2)172 (2)
Symmetry codes: (ii) −x+2, −y+2, −z+1; (iii) −x+1, −y+1, −z+1; (iv) x+1, y, z; (v) x, y−1, z−1; (vi) x−1, y, z; (vii) x+1, y+1, z; (viii) −x+1, −y+2, −z+2; (ix) x, y−1, z.
Acknowledgements top

The UFS is gratefully acknowledged for funding. JKC acknowledges the Marie Curie IIF scheme of the 7th EU Framework Program

references
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