supplementary materials


HTML versionpdf versioncif file3d viewstructure factorssupplementary materialsCIF check reportcited insimilar papers buy article online

Acta Cryst. (2007). E63, m1732-m1733    [ doi:10.1107/S1600536807024166 ]

Redetermination of trans-diaquatetramethanolcobalt(II) bis(rac-1,1'-binaphthalene-2,2'-diylphosphate) methanol disolvate monohydrate: a two-dimensional supramolecular hydrogen-bonded network

B. Wisser and C. Janiak

Abstract top

In the title compound, trans-[Co(CH3OH)4(H2O)2](C20H12PO4)2·2CH3OH·H2O, the crystal packing shows a separation of the hydrophobic naphthyl ring systems from the hydrophilic part of the structure, viz. the (RO)2PO2- phosphate anion, the cobalt complex cation and the solvent molecules. The binaphthyl tail-to-tail packing in the hydrophobic layer is governed by weak C-H...[pi] interactions. The present study performed at 203 K confirms the previous room-temperature study [McCann, Murphy, Cardin & Convery (1991), Polyhedron, 10, 2771-2777], but with improved precision. The centrosymmetric cobalt complex has very similar Co-O bond lengths and is isostructural with the trans-[Cu(H2O)2(CH3OH)4]2+ cation (which features a tetragonally compressed instead of the typical Jahn-Teller distorted elongated copper octahedron) in the isotypic copper(II) compound. The high degree of similarity in the Co and Cu structures shows the dominating effect of the hydrogen-bonding network on the metal coordination polyhedra. All H atoms of the Co and Cu aqua and methanol ligands are engaged in typical strong hydrogen-bonding interactions.

Comment top

In the structure of the title compound (I) one inversion-symmetrical trans-[Co(H2O)2(CH3OH)4]2+ cation is combined with two binaphthyl phosphate counterions, and one water and two methanol solvate molecules (McCann et al. 1991; Dorn et al., 2006). The packing of the title compound can be rationalized by a separation of the hydrophobic binaphthyl backbone from the hydrophilic (RO)2PO2- phosphate groups, the cobalt complex cation and the solvent molecules into an inverse bilayer structure, as seen before (Wisser & Janiak, 2007; Dorn et al., 2006). The structure of (I) is isotypic to that of the copper(II) analogue where the expected normal Jahn-Teller distortion of an elongated octahedron is absent. Instead, a tetragonal compressed octahedron, indicative of a dynamic Jahn-Teller effect, is observed (Dorn et al., 2006). The M—O (M = Co and Cu) bonds lengths and their variations in the analogous structures are highly similar with M–O(H2O) = 2.038 (3) and 1.937 (4) Å, and M–O(CH3OH) = 2.089 (3)/2.104 (3) and 2.112 (4)/2.167 (4) Å for M = Co and Cu. The close similarity between the Co and Cu structures and the metal coordination polyhedra indicates a structure directing effect of the hydrogen-bonding interactions. For the Cu structure the two elongated Jahn-Teller-distorted states along the two trans-CH3OH–Cu–CH3OH bonds are of identical low energy and both occupied. There is no differentiation from any intermolecular interactions between these two states. The average of two tetragonally elongated octahedra then looks like a compressed octahedron for Cu (Deeth & Hearnshaw, 2006).

Fig. 1 shows a projection of the unit cell crystal packing to illustrate the layer-like arrangement of the hydrophobic and hydrophilic regions. The latter are also highlighted by the hydrogen-bonding network as red dashes (see Table for bond distances and angles). The interaction between the binaphthyl phosphate and the octahedrally coordinated cobalt(II) cation is visualized in Fig. 2. The binaphthyl tail-to-tail packing in the hydrophobic layer is governed by C–H···π interactions (Dorn et al., 2006; Janiak, 2000; Nishio, 2004).

Related literature top

For isotypic compounds and closely related structures, see: Deeth & Hearnshaw (2006); Dorn et al. (2006); Janiak (2000); McCann et al. (1991); Nishio (2004); Wisser & Janiak (2007).

Experimental top

A solution of racemic 1,1'-binaphthalene-2,2'-diyl phosphoric acid (139.2 mg, 0.20 mmol) (Dorn et al., 2006) in 12 ml of methanol was added to a solution of CoCl2.6H2O (47.6 mg, 0.2 mmol) in 4 ml of distilled water. The solvent was slowly allowed to evaporate. After two days pink plates had formed which were separated by filtration. Crystal yield 96 mg, 48%. Analysis calculated for C46H54CoO17P2 (999.76): C 55.26, H 5.44; found: C 55.30, H 4.98. IR (KBr, ν cm-1): 3209, 1653, 1617, 1587, 1506, 1464, 1430, 1328, 1236, 1208, 1093, 1068, 1022, 991, 960, 944, 868, 852, 816, 747, 719, 657, 580, 565, 532, 479, 415.

Refinement top

The previous room-temperature study (McCann et al. 1991; Refcode:KUPYID) converged with R(F) = 0.13 for 1577 unique reflections with I>2σ(I) that were collected up to 20°/θ. Cell parameters were a = 41.93 (3), b = 8.683 (2), c = 13.21 (1) Å, β = 105.41 (4)°. The low precision of the previous data was attributed to the smallness of the largest available crystals. No bond lengths or angles were given, neither in the original publication nor in the entry of the Cambridge Crystallographic Data base (message: No three-dimensional coordinates available). Our low-temperature structure redetermination gave improved cell parameters by a factor of 3–10. Data was collected to over θ = 26°, so that 2576 unique reflections with I>2σ(I) were available and the R factors improved considerably. H atoms bonded to C were refined with riding models and Ueq(H) = 1.2 Ueq(C_aromatic) or 1.5 Ueq(C_methyl), respectively. H atoms bonded to O atoms (H2O, CH3OH) were found from difference Fourier maps and their positions were freely refined with Ueq(H) = 1.2 Ueq(O_CH3OH) and 1.5 Ueq(O_H2O), respectively.

Computing details top

Data collection: SMART (Bruker, 1997); cell refinement: SAINT (Bruker, 1997); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: Diamond (Crystal Impact, 2006); software used to prepare material for publication: publCIF (Westrip, 2007).

Figures top
[Figure 1] Fig. 1. : Projection of the crystal packing in compound (I) onto the (010) plane. Hydrogen bonds are indicated with red dashed lines. Displacement ellipsoids are drawn at the 50% probability level and H atoms are given as spheres of arbitrary radius.
[Figure 2] Fig. 2. : Interaction between the 1,1'-binaphthalene-2,2'-diyl phosphate anion and the trans-diaqua-tetramethanol-cobalt(II) cation in compound (I). The cobalt cation is located on an inversion center. Hydrogen bonds are indicated with red dashed lines. Displacement ellipsoids are drawn at the 50% probability level and H atoms are given as spheres of arbitrary radius. Symmetry code: i =– x, 1 – y, – z.
trans-Diaquatetramethanolcobalt(II) bis(rac-1,1'-binaphthalene-2,2'-diylphosphate) methanol disolvate monohydrate top
Crystal data top
[Co(CH4O)4(H2O)2](C20H12PO4)2·2CH4O·H2OF(000) = 2092
Mr = 999.76Dx = 1.446 Mg m−3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
a = 41.795 (9) ÅCell parameters from 1024 reflections
b = 8.6674 (19) Åθ = 2.4–20.0°
c = 13.161 (3) ŵ = 0.52 mm−1
β = 105.548 (4)°T = 203 K
V = 4593.2 (18) Å3Plate, pink
Z = 40.49 × 0.26 × 0.02 mm
Data collection top
Bruker APEX II CCD area-detector
diffractometer		4506 independent reflections
Radiation source: fine-focus sealed tube2576 reflections with I > 2σ(I)
graphiteRint = 0.085
\w scansθmax = 26.0°, θmin = 2.0°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)		h = −51→51
Tmin = 0.786, Tmax = 0.988k = −10→10
17662 measured reflectionsl = −16→16
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)] = 0.052Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.147H atoms treated by a mixture of independent and constrained refinement
S = 0.99 w = 1/[σ2(Fo2) + (0.0631P)2 + 8.4598P]
where P = (Fo2 + 2Fc2)/3
4506 reflections(Δ/σ)max < 0.001
317 parametersΔρmax = 0.53 e Å−3
1 restraintΔρmin = −0.57 e Å−3
Crystal data top
[Co(CH4O)4(H2O)2](C20H12PO4)2·2CH4O·H2OV = 4593.2 (18) Å3
Mr = 999.76Z = 4
Monoclinic, C2/cMo Kα radiation
a = 41.795 (9) ŵ = 0.52 mm−1
b = 8.6674 (19) ÅT = 203 K
c = 13.161 (3) Å0.49 × 0.26 × 0.02 mm
β = 105.548 (4)°
Data collection top
Bruker APEX II CCD area-detector
diffractometer		4506 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)		2576 reflections with I > 2σ(I)
Tmin = 0.786, Tmax = 0.988Rint = 0.085
17662 measured reflectionsθmax = 26.0°
Refinement top
R[F2 > 2σ(F2)] = 0.052H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.147Δρmax = 0.53 e Å−3
S = 0.99Δρmin = −0.57 e Å−3
4506 reflectionsAbsolute structure: ?
317 parametersFlack parameter: ?
1 restraintRogers parameter: ?
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 F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > σ(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ 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
Co0.00000.50000.50000.0259 (2)
O1−0.02130 (8)0.3144 (3)0.5593 (2)0.0382 (7)
H1D−0.0282 (11)0.320 (5)0.618 (3)0.046*
O20.02480 (8)0.3480 (4)0.4222 (3)0.0421 (8)
H2D0.0147 (12)0.313 (6)0.366 (4)0.050*
O30.03873 (8)0.5095 (4)0.6325 (2)0.0400 (8)
H3A0.0530 (12)0.587 (6)0.645 (4)0.060*
H3B0.0410 (12)0.444 (6)0.682 (4)0.060*
C1−0.01939 (13)0.1553 (5)0.5351 (4)0.0532 (14)
H1A−0.01850.14450.46250.080*
H1B−0.03880.10210.54460.080*
H1C0.00050.11090.58170.080*
C20.05817 (12)0.3240 (7)0.4397 (4)0.0681 (17)
H2A0.06620.38150.38830.102*
H2B0.06230.21490.43300.102*
H2C0.06960.35850.51020.102*
P10.07186 (3)0.84064 (12)0.27597 (8)0.0261 (3)
O40.09320 (6)0.7848 (3)0.1977 (2)0.0278 (6)
O50.10030 (6)0.8622 (3)0.3853 (2)0.0279 (6)
O60.04962 (7)0.7097 (3)0.2814 (2)0.0308 (7)
O70.05750 (6)0.9960 (3)0.2485 (2)0.0333 (7)
C30.15083 (9)0.8126 (4)0.2862 (3)0.0229 (8)
C40.12404 (9)0.8498 (4)0.2035 (3)0.0264 (9)
C50.12665 (10)0.9437 (5)0.1196 (3)0.0311 (9)
H50.10790.96450.06330.037*
C60.15689 (10)1.0049 (5)0.1208 (3)0.0347 (10)
H60.15901.06570.06380.042*
C70.18505 (10)0.9783 (4)0.2061 (3)0.0308 (9)
C80.21623 (11)1.0472 (5)0.2093 (4)0.0381 (11)
H8A0.21841.10810.15250.046*
C90.24276 (11)1.0259 (5)0.2937 (4)0.0432 (12)
H9A0.26331.07150.29490.052*
C100.23970 (11)0.9358 (5)0.3792 (4)0.0401 (11)
H10A0.25810.92230.43790.048*
C110.21021 (10)0.8677 (5)0.3778 (3)0.0322 (10)
H110.20860.80860.43610.039*
C120.18207 (9)0.8835 (4)0.2913 (3)0.0256 (9)
C130.14619 (9)0.7076 (4)0.3716 (3)0.0233 (8)
C140.12153 (10)0.7362 (4)0.4189 (3)0.0258 (9)
C150.11689 (10)0.6481 (5)0.5036 (3)0.0325 (10)
H150.09990.67330.53520.039*
C160.13723 (11)0.5265 (5)0.5390 (3)0.0362 (10)
H160.13510.47100.59820.043*
C170.16142 (10)0.4822 (4)0.4885 (3)0.0312 (9)
C180.18039 (11)0.3463 (5)0.5177 (4)0.0397 (11)
H180.17810.28890.57600.048*
C190.20178 (12)0.2974 (5)0.4635 (4)0.0465 (13)
H190.21380.20570.48360.056*
C200.20605 (11)0.3825 (5)0.3777 (4)0.0409 (11)
H200.22090.34790.34010.049*
C210.18852 (10)0.5168 (4)0.3486 (3)0.0320 (9)
H210.19160.57340.29110.038*
C220.16599 (9)0.5716 (4)0.4030 (3)0.0255 (9)
O80.08231 (7)0.7421 (3)0.6938 (3)0.0385 (8)
H8B0.0747 (11)0.826 (5)0.702 (4)0.046*
C230.11277 (12)0.7125 (6)0.7674 (4)0.0559 (14)
H23A0.13070.73260.73540.084*
H23B0.11360.60540.78940.084*
H23C0.11510.77890.82820.084*
O90.0000 (2)0.1564 (4)0.2500 (8)0.0335 (9)
H9B0.01930.09540.24350.050*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co0.0305 (4)0.0208 (4)0.0277 (4)−0.0006 (3)0.0104 (3)−0.0001 (3)
O10.058 (2)0.0227 (15)0.0414 (18)−0.0052 (14)0.0267 (16)0.0016 (14)
O20.0330 (18)0.049 (2)0.045 (2)−0.0008 (15)0.0105 (15)−0.0194 (16)
O30.050 (2)0.0264 (17)0.0384 (18)−0.0094 (15)0.0023 (15)0.0069 (14)
C10.077 (4)0.030 (3)0.062 (3)−0.001 (2)0.035 (3)−0.002 (2)
C20.043 (3)0.096 (5)0.063 (4)0.017 (3)0.010 (3)−0.030 (3)
P10.0264 (6)0.0216 (5)0.0317 (6)−0.0004 (4)0.0102 (5)−0.0011 (4)
O40.0237 (14)0.0331 (15)0.0264 (15)−0.0022 (12)0.0065 (12)−0.0028 (12)
O50.0322 (15)0.0231 (14)0.0281 (15)0.0023 (12)0.0075 (12)−0.0038 (12)
O60.0321 (16)0.0269 (15)0.0356 (16)−0.0092 (12)0.0131 (13)−0.0031 (12)
O70.0267 (15)0.0246 (15)0.0483 (18)0.0058 (12)0.0095 (13)0.0076 (14)
C30.026 (2)0.0181 (19)0.025 (2)0.0021 (16)0.0088 (17)−0.0019 (16)
C40.026 (2)0.025 (2)0.031 (2)0.0027 (17)0.0129 (18)−0.0021 (17)
C50.031 (2)0.030 (2)0.033 (2)0.0070 (18)0.0102 (19)0.0022 (18)
C60.041 (3)0.029 (2)0.039 (2)0.007 (2)0.020 (2)0.007 (2)
C70.034 (2)0.026 (2)0.037 (2)0.0030 (18)0.0168 (19)−0.0012 (18)
C80.038 (3)0.035 (2)0.048 (3)−0.007 (2)0.023 (2)−0.003 (2)
C90.031 (2)0.043 (3)0.058 (3)−0.011 (2)0.017 (2)−0.013 (2)
C100.030 (2)0.037 (3)0.052 (3)−0.002 (2)0.008 (2)−0.009 (2)
C110.034 (2)0.026 (2)0.035 (2)−0.0004 (18)0.0076 (19)−0.0025 (18)
C120.025 (2)0.0181 (19)0.034 (2)0.0017 (16)0.0088 (18)−0.0029 (17)
C130.027 (2)0.0177 (19)0.023 (2)−0.0013 (16)0.0031 (17)−0.0012 (15)
C140.030 (2)0.021 (2)0.026 (2)0.0000 (17)0.0053 (18)0.0007 (16)
C150.036 (2)0.038 (2)0.026 (2)−0.004 (2)0.0128 (19)0.0024 (19)
C160.045 (3)0.035 (3)0.028 (2)−0.009 (2)0.010 (2)0.0058 (19)
C170.031 (2)0.024 (2)0.033 (2)−0.0059 (18)−0.0002 (18)0.0045 (18)
C180.040 (3)0.026 (2)0.047 (3)−0.004 (2)0.000 (2)0.013 (2)
C190.043 (3)0.022 (2)0.066 (3)0.005 (2)0.000 (3)0.005 (2)
C200.037 (3)0.025 (2)0.058 (3)0.0079 (19)0.006 (2)−0.005 (2)
C210.030 (2)0.023 (2)0.041 (2)−0.0015 (18)0.0060 (19)0.0003 (19)
C220.022 (2)0.0192 (19)0.032 (2)−0.0039 (16)0.0027 (18)−0.0001 (17)
O80.0364 (18)0.0285 (17)0.0480 (19)0.0082 (13)0.0069 (15)0.0007 (15)
C230.044 (3)0.071 (4)0.051 (3)0.017 (3)0.008 (3)0.012 (3)
O90.028 (2)0.027 (2)0.047 (3)0.0000.0125 (19)0.000
Geometric parameters (Å, °) top
Co—O32.038 (3)C7—C81.424 (6)
Co—O3i2.038 (3)C8—C91.355 (6)
Co—O12.089 (3)C8—H8A0.9400
Co—O1i2.089 (3)C9—C101.404 (6)
Co—O22.104 (3)C9—H9A0.9400
Co—O2i2.104 (3)C10—C111.362 (6)
O1—C11.422 (5)C10—H10A0.9400
O1—H1D0.90 (3)C11—C121.407 (5)
O2—C21.367 (5)C11—H110.9400
O2—H2D0.80 (5)C13—C141.362 (5)
O3—H3A0.88 (5)C13—C221.435 (5)
O3—H3B0.85 (5)C14—C151.407 (5)
C1—H1A0.9700C15—C161.356 (6)
C1—H1B0.9700C15—H150.9400
C1—H1C0.9700C16—C171.404 (6)
C2—H2A0.9700C16—H160.9400
C2—H2B0.9700C17—C181.414 (6)
C2—H2C0.9700C17—C221.420 (5)
P1—O71.479 (3)C18—C191.353 (7)
P1—O61.481 (3)C18—H180.9400
P1—O41.607 (3)C19—C201.400 (6)
P1—O51.613 (3)C19—H190.9400
O4—C41.389 (4)C20—C211.374 (5)
O5—C141.402 (4)C20—H200.9400
C3—C41.375 (5)C21—C221.410 (5)
C3—C121.429 (5)C21—H210.9400
C3—C131.498 (5)O8—C231.401 (5)
C4—C51.400 (5)O8—H8B0.81 (5)
C5—C61.367 (6)C23—H23A0.9700
C5—H50.9400C23—H23B0.9700
C6—C71.411 (6)C23—H23C0.9700
C6—H60.9400O9—H9B0.9881
C7—C121.422 (5)
O3—Co—O3i180.00 (16)C6—C7—C12119.4 (4)
O3—Co—O191.81 (13)C6—C7—C8121.1 (4)
O3i—Co—O188.19 (13)C12—C7—C8119.5 (4)
O3—Co—O1i88.19 (13)C9—C8—C7120.5 (4)
O3i—Co—O1i91.81 (13)C9—C8—H8A119.7
O1—Co—O1i180.00 (17)C7—C8—H8A119.7
O3—Co—O293.42 (13)C8—C9—C10120.2 (4)
O3i—Co—O286.58 (13)C8—C9—H9A119.9
O1—Co—O290.83 (12)C10—C9—H9A119.9
O1i—Co—O289.17 (12)C11—C10—C9120.4 (4)
O3—Co—O2i86.58 (13)C11—C10—H10A119.8
O3i—Co—O2i93.42 (13)C9—C10—H10A119.8
O1—Co—O2i89.17 (12)C10—C11—C12121.8 (4)
O1i—Co—O2i90.83 (12)C10—C11—H11119.1
O2—Co—O2i180.00 (16)C12—C11—H11119.1
C1—O1—Co127.4 (3)C11—C12—C7117.6 (4)
C1—O1—H1D107 (3)C11—C12—C3123.5 (4)
Co—O1—H1D123 (3)C7—C12—C3118.9 (4)
C2—O2—Co128.8 (3)C14—C13—C22117.8 (3)
C2—O2—H2D111 (4)C14—C13—C3119.8 (3)
Co—O2—H2D118 (4)C22—C13—C3122.3 (3)
Co—O3—H3A122 (3)C13—C14—O5119.4 (3)
Co—O3—H3B122 (3)C13—C14—C15123.0 (4)
H3A—O3—H3B116 (5)O5—C14—C15117.5 (3)
O1—C1—H1A109.5C16—C15—C14119.2 (4)
O1—C1—H1B109.5C16—C15—H15120.4
H1A—C1—H1B109.5C14—C15—H15120.4
O1—C1—H1C109.5C15—C16—C17121.0 (4)
H1A—C1—H1C109.5C15—C16—H16119.5
H1B—C1—H1C109.5C17—C16—H16119.5
O2—C2—H2A109.5C16—C17—C18121.4 (4)
O2—C2—H2B109.5C16—C17—C22119.5 (4)
H2A—C2—H2B109.5C18—C17—C22119.0 (4)
O2—C2—H2C109.5C19—C18—C17121.3 (4)
H2A—C2—H2C109.5C19—C18—H18119.4
H2B—C2—H2C109.5C17—C18—H18119.4
O7—P1—O6119.39 (16)C18—C19—C20120.3 (4)
O7—P1—O4112.08 (16)C18—C19—H19119.8
O6—P1—O4105.30 (15)C20—C19—H19119.8
O7—P1—O5105.46 (15)C21—C20—C19119.8 (4)
O6—P1—O5111.56 (15)C21—C20—H20120.1
O4—P1—O5101.75 (14)C19—C20—H20120.1
C4—O4—P1120.6 (2)C20—C21—C22121.5 (4)
C14—O5—P1116.4 (2)C20—C21—H21119.2
C4—C3—C12118.5 (3)C22—C21—H21119.2
C4—C3—C13119.6 (3)C21—C22—C17117.9 (4)
C12—C3—C13121.8 (3)C21—C22—C13122.8 (4)
C3—C4—O4119.7 (3)C17—C22—C13119.1 (4)
C3—C4—C5122.8 (4)C23—O8—H8B113 (3)
O4—C4—C5117.4 (4)O8—C23—H23A109.5
C6—C5—C4118.9 (4)O8—C23—H23B109.5
C6—C5—H5120.5H23A—C23—H23B109.5
C4—C5—H5120.5O8—C23—H23C109.5
C5—C6—C7121.1 (4)H23A—C23—H23C109.5
C5—C6—H6119.4H23B—C23—H23C109.5
C7—C6—H6119.4
Symmetry codes: (i) −x, −y+1, −z+1.
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
O1—H1D···O6i0.90 (3)1.80 (4)2.677 (4)164 (4)
O2—H2D···O90.80 (5)2.02 (5)2.777 (7)158 (5)
O3—H3A···O80.88 (5)1.82 (5)2.692 (4)170 (5)
O3—H3B···O6ii0.85 (5)1.83 (5)2.679 (4)172 (5)
O8—H8B···O7iii0.81 (5)1.87 (5)2.673 (4)168 (5)
O9—H9B···O7iv0.991.802.781 (9)172.1
Symmetry codes: (i) −x, −y+1, −z+1; (ii) x, −y+1, z+1/2; (iii) x, −y+2, z+1/2; (iv) x, y−1, z.
Table 1
Selected geometric parameters (Å) top
Co—O32.038 (3)P1—O61.481 (3)
Co—O12.089 (3)P1—O41.607 (3)
Co—O22.104 (3)P1—O51.613 (3)
P1—O71.479 (3)
Table 2
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
O1—H1D···O6i0.90 (3)1.80 (4)2.677 (4)164 (4)
O2—H2D···O90.80 (5)2.02 (5)2.777 (7)158 (5)
O3—H3A···O80.88 (5)1.82 (5)2.692 (4)170 (5)
O3—H3B···O6ii0.85 (5)1.83 (5)2.679 (4)172 (5)
O8—H8B···O7iii0.81 (5)1.87 (5)2.673 (4)168 (5)
O9—H9B···O7iv0.991.802.781 (9)172.1
Symmetry codes: (i) −x, −y+1, −z+1; (ii) x, −y+1, z+1/2; (iii) x, −y+2, z+1/2; (iv) x, y−1, z.
Acknowledgements top

Support through grant Ja466/14–1 [where is this grant from?] is acknowledged.

references
References top

Bruker (1997). SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.

Crystal Impact (2006). DIAMOND. Version 3.1d. Crystal Impact GbR, Bonn, Germany.

Deeth, R. J. & Hearnshaw, L. J. A. (2006). Dalton Trans. pp. 1092–1100.

Dorn, T., Chamayou, A.-C. & Janiak, C. (2006). New J. Chem. 30, 156–167.

Janiak, C. (2000). J. Chem. Soc. Dalton Trans. pp. 3885–3896.

McCann, M., Murphy, E., Cardin, C. & Convery, M. (1991). Polyhedron, 10, 2771–2777.

Nishio, M. (2004). CrystEngComm, 6, 130–158.

Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.

Sheldrick, G. M. (1997). SHELXS97 and SHELXL97. University of Göttingen, Germany.

Westrip, S. P. (2007). PublCIF. In preparation.

Wisser, B. & Janiak, C. (2007). Acta Cryst. E63, o2871–o2872.