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Acta Crystallogr Sect E Struct Rep Online. 2008 January 1; 64(Pt 1): m262–m263.
Published online 2007 December 21. doi:  10.1107/S1600536807067141
PMCID: PMC2915174

Tetra-μ-aqua-octaaqua­bis(μ-4-chloro­pyridine-2,6-dicarboxyl­ato)bis­(4-chloro­pyridine-2,6-dicarboxyl­ato)tri­cobalt(II)disodium(I) bis­[triaqua­bis(4-chloro­pyridine-2,6-dicarboxyl­ato)cobalt(II)] hexa­hydrate

Abstract

The title compound, [Co3Na2(C7H2ClNO4)4(H2O)12][Co(C7H2ClNO4)(H2O)3]2·6H2O, consists of a centrosymmetric dimer of [CoII(dipicCl)2]2− complex dianions [dipicCl is 4-chloro­pyridine-2,6-dicarboxyl­ate] bridged by an [Na2CoII(H2O)12]4+ tetra­cationic cluster, two independent [Co(dipicCl)(H2O)3] complexes, and six water mol­ecules of crystallization. The metals are all six-coordinate with distorted octahedral geometries. The [CoII(dipicCl)(H2O)3] complexes are neutral, with one tridentate ligand and three water molecules. The [CoII(dipicCl)2]2− complexes each have two tridentate ligands. The [Na2CoII(H2O)12]4+ cluster has a central CoII ion which is coordinated to six water molecules and lies on a crystallographic inversion center. Four of the water molecules bridge to two sodium ions, each of which have three other water molecules coordinated along with an O atom from the [CoII(dipicCl)2]2− complex. In the crystal structure, the various units are linked by O—H(...)O hydrogen bonds, forming a three-dimensional network. Two water molecules are disordered equally over two positions.

Related literature

For related literature, see: Anagnostopoulos (1975 [triangle]); Cassellato & Vigato (1978 [triangle]); Chatterjee, Ghosh, Wu & Mak (1998 [triangle]); Chatterjee, Maji, Ghosh & Mak (1998 [triangle]); Hartkamp (1962 [triangle]); Lukes & Jurecek (1948 [triangle]); Chatterjee et al. (1997 [triangle]); Crans et al. (2000 [triangle], 2003 [triangle], 2006 [triangle]); D’Ascenzo, Marino, Sabbatini & Bica (1978 [triangle]); Du et al. (2006 [triangle]); Furst et al. (1978 [triangle]); Ghosh et al. (1978 [triangle]); Lamture et al. (1995 [triangle]); Liu et al. (2006 [triangle]); Su et al. (2005 [triangle]); Yang et al. (2002 [triangle]); Zhou et al. (2004 [triangle]).

An external file that holds a picture, illustration, etc.
Object name is e-64-0m262-scheme1.jpg

Experimental

Crystal data

  • [Co3Na2(C7H2ClNO4)4(H2O)12][Co(C7H2ClNO4)(H2O)3]2·6H2O
  • M r = 1970.29
  • Triclinic, An external file that holds a picture, illustration, etc.
Object name is e-64-0m262-efi1.jpg
  • a = 9.1539 (18) Å
  • b = 14.475 (3) Å
  • c = 15.476 (3) Å
  • α = 62.54 (3)°
  • β = 83.32 (3)°
  • γ = 80.19 (3)°
  • V = 1791.4 (6) Å3
  • Z = 1
  • Mo Kα radiation
  • μ = 1.48 mm−1
  • T = 153 (2) K
  • 0.34 × 0.19 × 0.11 mm

Data collection

  • Rigaku Mercury CCD diffractometer
  • Absorption correction: multi-scan (REQAB; Rigaku/MSC 2006 [triangle]) T min = 0.633, T max = 0.854
  • 12735 measured reflections
  • 6520 independent reflections
  • 5060 reflections with I > 2σ(I)
  • R int = 0.024

Refinement

  • R[F 2 > 2σ(F 2)] = 0.034
  • wR(F 2) = 0.086
  • S = 1.04
  • 6520 reflections
  • 583 parameters
  • 24 restraints
  • H atoms treated by a mixture of independent and constrained refinement
  • Δρmax = 0.58 e Å−3
  • Δρmin = −0.38 e Å−3

Data collection: CrystalClear (Rigaku/MSC, 2006 [triangle]); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: SHELXTL (Bruker, 2000 [triangle]); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Table 1
Hydrogen-bond geometry (Å, °)

Supplementary Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536807067141/su2035sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536807067141/su2035Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Acknowledgments

AAH thanks the University of Southern Mississippi for its start-up grant, (project grant DE00977), which was very valuable in making this structural elucidation possible. SS thanks Alliance for Graduate Education in Mississippi (AGEM) for supporting her summer research based on this work in 2007.

supplementary crystallographic information

Comment

Many transition metal complexes involving dipicolinic acid and different cations have been reported (Anagnostopoulos, 1975, Cassellato & Vigato, 1978, D'Ascenzo et al., 1978, Ghosh et al., 1978, Furst et al., 1978). Other examples include metal ions such as chromium (Hartkamp, 1962), copper,(Lukes & Jurecek, 1948), and vanadium (Chatterjee et al., 1997; Chatterjee, Ghosh et al., 1998; Chatterjee, Maji et al., 1998; Crans et al., 2003; Crans et al., 2006, Crans et al., 2000). Examples of cobalt complexes with dipicolinic acid have been reported (Du et al., 2006; Liu et al., 2006; Su et al., 2005; Yanget al., 2002), but none with analogues of dipicolinic acid, except the structure of Co(dipicOH)3H2O.H2O.0.25MeCN reported by (Zhou et al., 2004). As part of our interest in the coordination chemistry of analogues of dipicolinic acid, we now extend this chemistry to include the structural elucidation of the title compound, (I), that was produced in conjunction with an unidentified violet complex.

In compound (I), the cobalt atoms appear in three different coordination environments. These include independent [CoII(dipicCl)(H2O)3] complexes (Fig. 1), and two [CoII(dipicCl)2]2- complex dianions bridged by a [Na2CoII(H2O)12]4+ tetra-cationic cluster (Fig. 2). In the latter the central cobalt atom, Co2, occupies a crystallographic inversion center.

In the crystal structure of compound (I) the different complexes and the water molecules of crystallization are linked by O—H···O hydrogen bonds to form a three dimensional network (Fig. 3).

Experimental

H2dipic Cl was synthesized according to the literature procedure (Lamture et al., 1995). [H2dipic Cl (4.03 g, 20.0 mmol) was added in small portions to a 100 cm3 beaker, which contained a mixture of Na2CO3 (2.12 g, 20.0 mmol) and warm H2O (50 cm3). The resulting solution was added dropwise to a stirred solution of CoCl2.6H2O (4.76 g, 20.0 mmol) in H2O (15 cm3) over a 30 minute period in a 250 cm3 round-bottom flask. The resulting mixture was refluxed for 5 h with stirring. It was then left to stand for 12 h, whereby a violet product formed. The product was filtered off, then washed with water, followed by acetone, and air dried. The filtrate was kept and the mass of the product was recorded. Yield = 3.0 g. This unidentified violet compound is very insoluble in water. The filtrate was allowed to evaporate over six weeks, after which the title complex appeared as brown crystals. For the unidentified violet complex, FT IR (cm-1): 3445 (br, ν(OH)), 1668 (s, νas(CO2-)), 1615 (very strong, νas(CO2-)),and1388 (s, ν(CO2-)). For [Co(dipic Cl)2].Na2[Co(dipic Cl)2] [Co(dipic Cl)(H2O)3], FT IR (cm-1): 3362 (br, ν(OH)), 1614 (very strong, νas(CO2-)),and1373 (s, ν(CO2-)).

Refinement

Two water molecules (O23 and O24) are each disordered over two positions (O23/O23' and O24/O24') with occupancies of 0.5/0.5. The positions of the water H atoms were located from difference Fourier maps. The O—H distances were restrained to 0.88 (2) Å, with Uiso(H) = 1.5Ueq(O). The remaining H atoms were geometrically placed and treated as riding atoms, with C—H = 0.96Å and Uiso(H) = 1.2Ueq(C).

Figures

Fig. 1.
The molecular structure of [Co(dipicCl)(H2O)3], with the thermal ellipsoids drawn at the 50% probability level.
Fig. 2.
The molecular structure of [Co(dipicCl)2]2. Na2Co(H2O)12, with the thermal ellipsoids drawn at the 50% probability level.
Fig. 3.
Crystal packing diagram of the title complex viewed along the c axis.

Crystal data

[Co3Na2(C7H2ClNO4)4(H2O)12][Co(C7H2ClNO4)(H2O)3]2·6H2OZ = 1
Mr = 1970.29F000 = 997
Triclinic, P1Dx = 1.826 Mg m3
Hall symbol: -P 1Mo Kα radiation λ = 0.71073 Å
a = 9.1539 (18) ÅCell parameters from 5409 reflections
b = 14.475 (3) Åθ = 3.7–26.4º
c = 15.476 (3) ŵ = 1.48 mm1
α = 62.54 (3)ºT = 153 (2) K
β = 83.32 (3)ºRod, purple
γ = 80.19 (3)º0.34 × 0.19 × 0.11 mm
V = 1791.4 (6) Å3

Data collection

Rigaku Mercury CCD diffractometer6520 independent reflections
Radiation source: Sealed Tube5060 reflections with I > 2σ(I)
Monochromator: Graphite MonochromatorRint = 0.024
Detector resolution: 14.6306 pixels mm-1θmax = 25.5º
T = 153(2) Kθmin = 3.2º
ω scansh = −11→11
Absorption correction: multi-scan(REQAB; Rigaku/MSC 2006)k = −15→17
Tmin = 0.633, Tmax = 0.854l = −16→18
12735 measured reflections

Refinement

Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.034H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.086  w = 1/[σ2(Fo2) + (0.0467P)2 + 0.1717P] where P = (Fo2 + 2Fc2)/3
S = 1.04(Δ/σ)max = 0.001
6520 reflectionsΔρmax = 0.58 e Å3
583 parametersΔρmin = −0.38 e Å3
24 restraintsExtinction correction: none
Primary atom site location: structure-invariant direct methods

Special details

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)

xyzUiso*/UeqOcc. (<1)
Co10.27302 (4)0.83775 (3)0.19235 (3)0.01340 (10)
Cl10.34541 (10)0.46841 (7)0.63440 (6)0.0316 (2)
Cl20.21294 (9)1.22256 (6)−0.24098 (6)0.02708 (19)
N10.3011 (3)0.71984 (18)0.32895 (18)0.0138 (5)
N20.2483 (3)0.95501 (18)0.05598 (18)0.0138 (5)
O10.1696 (2)0.71166 (16)0.19327 (16)0.0188 (5)
O20.3910 (2)0.90072 (16)0.26077 (16)0.0186 (5)
O30.1353 (2)0.54304 (16)0.28689 (17)0.0220 (5)
O40.4945 (2)0.86338 (17)0.39863 (16)0.0230 (5)
O50.0749 (2)0.93466 (16)0.20562 (16)0.0194 (5)
O60.4625 (2)0.80119 (15)0.11290 (15)0.0169 (4)
O7−0.0654 (2)1.08848 (16)0.12304 (16)0.0203 (5)
O80.5652 (2)0.85418 (16)−0.03851 (16)0.0210 (5)
C10.1770 (3)0.6265 (2)0.2730 (2)0.0163 (6)
C20.2456 (3)0.6301 (2)0.3554 (2)0.0165 (6)
C30.2570 (4)0.5501 (2)0.4498 (2)0.0212 (7)
H30.21620.48610.46930.025*
C40.3296 (3)0.5654 (2)0.5155 (2)0.0203 (7)
C50.3905 (3)0.6572 (2)0.4871 (2)0.0185 (7)
H50.44340.66690.53170.022*
C60.3722 (3)0.7337 (2)0.3927 (2)0.0151 (6)
C70.4242 (3)0.8415 (2)0.3475 (2)0.0156 (6)
C80.0404 (3)1.0182 (2)0.1294 (2)0.0151 (6)
C90.1373 (3)1.0341 (2)0.0390 (2)0.0143 (6)
C100.1218 (3)1.1194 (2)−0.0532 (2)0.0159 (6)
H100.04351.1768−0.06580.019*
C110.2245 (3)1.1174 (2)−0.1258 (2)0.0165 (6)
C120.3385 (3)1.0352 (2)−0.1082 (2)0.0165 (6)
H120.40851.0340−0.15900.020*
C130.3468 (3)0.9550 (2)−0.0140 (2)0.0144 (6)
C140.4697 (3)0.8627 (2)0.0210 (2)0.0153 (6)
Co30.67155 (4)0.11941 (3)0.36043 (3)0.01259 (10)
Cl31.12718 (10)0.29703 (7)0.52031 (6)0.0343 (2)
N30.8057 (2)0.17914 (18)0.41349 (18)0.0125 (5)
O90.7150 (2)−0.00397 (15)0.50786 (15)0.0156 (4)
O100.6749 (2)0.27965 (16)0.24966 (15)0.0164 (4)
O110.8694 (2)−0.05463 (16)0.62997 (16)0.0185 (5)
O120.8157 (2)0.41056 (16)0.19307 (16)0.0195 (5)
O130.4629 (2)0.16346 (16)0.42191 (16)0.0165 (4)
H13A0.395 (3)0.124 (2)0.432 (3)0.025*
H13B0.477 (4)0.159 (3)0.4786 (17)0.025*
O140.8596 (2)0.06266 (18)0.30523 (17)0.0208 (5)
H14A0.950 (2)0.061 (3)0.320 (3)0.031*
H14B0.870 (4)0.074 (3)0.2449 (16)0.031*
O150.5546 (2)0.06640 (18)0.29292 (17)0.0225 (5)
H15A0.477 (3)0.103 (3)0.263 (3)0.034*
H15B0.538 (4)0.0025 (17)0.326 (3)0.034*
C150.8112 (3)0.0107 (2)0.5519 (2)0.0144 (6)
C160.8614 (3)0.1193 (2)0.5014 (2)0.0135 (6)
C170.9592 (3)0.1542 (2)0.5388 (2)0.0177 (6)
H170.99560.11270.60310.021*
C181.0013 (3)0.2528 (2)0.4775 (2)0.0177 (7)
C190.9472 (3)0.3142 (2)0.3847 (2)0.0181 (7)
H190.97780.38180.34300.022*
C200.8469 (3)0.2737 (2)0.3550 (2)0.0146 (6)
C210.7745 (3)0.3273 (2)0.2569 (2)0.0138 (6)
Co20.50000.50000.00000.01317 (13)
O160.7253 (2)0.51517 (17)0.00124 (16)0.0170 (4)
H16A0.758 (4)0.477 (2)0.0607 (16)0.025*
H16B0.778 (4)0.497 (3)−0.037 (2)0.025*
O170.4626 (2)0.66360 (16)−0.08005 (16)0.0156 (4)
H17A0.424 (4)0.674 (3)−0.1328 (18)0.023*
H17B0.394 (3)0.689 (3)−0.051 (2)0.023*
O180.4605 (2)0.51588 (17)0.12724 (16)0.0203 (5)
H18A0.528 (3)0.540 (3)0.142 (3)0.030*
H18B0.439 (4)0.464 (2)0.1846 (18)0.030*
Na10.69526 (12)0.70953 (9)−0.05481 (9)0.0185 (3)
O190.6582 (3)0.63560 (18)0.12553 (18)0.0242 (5)
H19A0.740 (3)0.621 (3)0.154 (3)0.036*
H19B0.614 (4)0.686 (2)0.137 (3)0.036*
O200.2393 (2)0.73840 (18)−0.99731 (17)0.0240 (5)
H20A0.183 (4)0.795 (2)−1.031 (3)0.036*
H20B0.225 (4)0.724 (3)−0.9359 (16)0.036*
O210.0629 (3)0.52400 (19)−0.87565 (18)0.0259 (5)
H21A0.083 (4)0.538 (3)−0.830 (2)0.039*
H21B0.001 (4)0.479 (3)−0.845 (3)0.039*
O220.9464 (3)0.6958 (2)−0.0502 (2)0.0404 (7)
H22A0.994 (5)0.749 (3)−0.084 (3)0.061*
H22B0.997 (5)0.650 (3)0.000 (2)0.061*
O230.3333 (6)0.3650 (4)−0.7100 (4)0.0199 (11)0.50
H23A0.376 (4)0.311 (2)−0.661 (2)0.030*
H23B0.278 (4)0.398 (3)−0.680 (3)0.030*
O23'0.3847 (7)0.3859 (5)−0.6866 (5)0.0347 (14)0.50
O240.7164 (5)0.7828 (4)−0.2286 (3)0.0232 (10)0.50
H24A0.766 (4)0.833 (2)−0.270 (3)0.035*
H24B0.685 (6)0.826 (4)−0.203 (4)0.035*
O24'0.7025 (6)0.8604 (4)−0.2068 (4)0.0271 (12)0.50

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
Co10.01611 (19)0.0112 (2)0.0106 (2)−0.00180 (15)−0.00031 (15)−0.00306 (16)
Cl10.0474 (5)0.0228 (4)0.0135 (4)−0.0051 (4)−0.0029 (4)0.0016 (3)
Cl20.0288 (4)0.0243 (4)0.0135 (4)−0.0013 (3)−0.0002 (3)0.0029 (3)
N10.0164 (12)0.0101 (12)0.0146 (14)−0.0010 (9)0.0002 (10)−0.0056 (10)
N20.0147 (11)0.0126 (13)0.0147 (14)−0.0022 (9)−0.0016 (10)−0.0063 (10)
O10.0228 (11)0.0158 (11)0.0169 (12)−0.0044 (8)−0.0016 (9)−0.0059 (9)
O20.0230 (10)0.0168 (11)0.0157 (12)−0.0073 (9)−0.0009 (9)−0.0056 (9)
O30.0290 (11)0.0156 (11)0.0225 (13)−0.0086 (9)−0.0014 (10)−0.0074 (9)
O40.0306 (12)0.0241 (12)0.0176 (12)−0.0115 (9)−0.0010 (10)−0.0096 (10)
O50.0193 (10)0.0170 (11)0.0159 (12)0.0027 (8)0.0021 (9)−0.0047 (9)
O60.0172 (10)0.0153 (11)0.0144 (12)−0.0004 (8)0.0011 (8)−0.0046 (9)
O70.0197 (10)0.0205 (12)0.0151 (12)0.0059 (9)−0.0005 (9)−0.0062 (9)
O80.0194 (10)0.0206 (12)0.0209 (13)−0.0007 (9)0.0062 (9)−0.0099 (10)
C10.0173 (14)0.0166 (16)0.0170 (17)−0.0027 (12)0.0009 (12)−0.0095 (13)
C20.0210 (14)0.0129 (15)0.0161 (17)−0.0028 (11)0.0012 (12)−0.0073 (12)
C30.0330 (17)0.0128 (16)0.0166 (17)−0.0070 (13)0.0004 (14)−0.0046 (13)
C40.0292 (16)0.0146 (16)0.0104 (16)−0.0008 (12)0.0014 (13)−0.0012 (13)
C50.0214 (15)0.0188 (16)0.0153 (17)−0.0029 (12)0.0000 (13)−0.0078 (13)
C60.0184 (14)0.0167 (16)0.0112 (15)−0.0025 (11)0.0007 (12)−0.0075 (12)
C70.0173 (14)0.0160 (16)0.0149 (17)−0.0039 (11)0.0032 (12)−0.0085 (13)
C80.0162 (14)0.0160 (15)0.0141 (16)−0.0026 (12)−0.0018 (12)−0.0071 (13)
C90.0157 (14)0.0146 (15)0.0134 (16)−0.0039 (11)−0.0012 (12)−0.0064 (12)
C100.0169 (14)0.0134 (15)0.0162 (16)−0.0020 (11)−0.0013 (12)−0.0057 (12)
C110.0189 (14)0.0152 (15)0.0110 (16)−0.0076 (12)−0.0027 (12)0.0001 (12)
C120.0153 (14)0.0197 (16)0.0144 (16)−0.0070 (12)0.0023 (12)−0.0066 (13)
C130.0140 (13)0.0168 (15)0.0161 (16)−0.0036 (11)0.0006 (12)−0.0104 (13)
C140.0141 (13)0.0162 (16)0.0167 (17)−0.0028 (11)−0.0008 (12)−0.0081 (13)
Co30.01322 (19)0.0124 (2)0.0116 (2)−0.00269 (14)−0.00176 (15)−0.00440 (16)
Cl30.0461 (5)0.0309 (5)0.0254 (5)−0.0225 (4)−0.0155 (4)−0.0033 (4)
N30.0096 (11)0.0129 (12)0.0136 (13)0.0003 (9)−0.0001 (9)−0.0055 (10)
O90.0152 (10)0.0157 (11)0.0147 (11)−0.0038 (8)−0.0029 (8)−0.0047 (9)
O100.0165 (10)0.0153 (11)0.0153 (11)−0.0036 (8)−0.0033 (8)−0.0040 (9)
O110.0189 (10)0.0166 (11)0.0148 (12)−0.0026 (8)−0.0051 (9)−0.0016 (9)
O120.0219 (10)0.0173 (11)0.0140 (12)−0.0070 (9)−0.0028 (9)−0.0007 (9)
O130.0151 (10)0.0163 (11)0.0160 (12)−0.0039 (8)−0.0001 (9)−0.0050 (9)
O140.0167 (10)0.0305 (13)0.0165 (12)0.0007 (9)−0.0026 (9)−0.0125 (10)
O150.0251 (11)0.0213 (13)0.0236 (13)−0.0082 (10)−0.0036 (10)−0.0098 (10)
C150.0167 (13)0.0134 (15)0.0121 (16)−0.0013 (11)0.0009 (12)−0.0055 (12)
C160.0109 (13)0.0156 (15)0.0132 (16)−0.0012 (11)−0.0008 (11)−0.0059 (12)
C170.0194 (14)0.0175 (16)0.0140 (16)−0.0033 (12)−0.0036 (12)−0.0044 (13)
C180.0194 (14)0.0188 (16)0.0172 (17)−0.0078 (12)−0.0032 (12)−0.0076 (13)
C190.0202 (15)0.0144 (15)0.0191 (17)−0.0058 (12)−0.0017 (13)−0.0056 (13)
C200.0141 (13)0.0139 (15)0.0125 (16)−0.0019 (11)−0.0001 (11)−0.0033 (12)
C210.0135 (13)0.0143 (15)0.0137 (16)−0.0014 (11)−0.0005 (12)−0.0065 (12)
Co20.0134 (3)0.0121 (3)0.0124 (3)−0.0013 (2)−0.0015 (2)−0.0041 (2)
O160.0163 (10)0.0193 (12)0.0137 (12)−0.0009 (8)−0.0021 (9)−0.0062 (9)
O170.0171 (10)0.0149 (11)0.0134 (12)0.0013 (8)−0.0037 (9)−0.0058 (9)
O180.0285 (12)0.0184 (12)0.0125 (12)−0.0052 (9)0.0003 (10)−0.0054 (9)
Na10.0182 (6)0.0175 (6)0.0186 (7)−0.0023 (5)−0.0006 (5)−0.0072 (5)
O190.0289 (12)0.0181 (12)0.0245 (14)0.0041 (10)−0.0058 (10)−0.0101 (10)
O200.0261 (12)0.0253 (13)0.0157 (12)0.0068 (9)−0.0024 (10)−0.0081 (10)
O210.0260 (12)0.0349 (14)0.0227 (14)−0.0129 (10)0.0017 (10)−0.0155 (11)
O220.0240 (13)0.0384 (17)0.0504 (19)−0.0080 (11)−0.0110 (12)−0.0095 (14)
O230.023 (3)0.016 (3)0.019 (3)0.003 (2)−0.001 (2)−0.008 (2)
O23'0.035 (3)0.022 (3)0.035 (4)−0.001 (2)0.011 (3)−0.006 (3)
O240.024 (2)0.028 (3)0.018 (3)−0.012 (2)0.0065 (19)−0.009 (2)
O24'0.027 (3)0.027 (3)0.020 (3)−0.005 (2)0.005 (2)−0.006 (2)

Geometric parameters (Å, °)

Co1—N22.016 (3)O14—H14A0.879 (19)
Co1—N12.024 (3)O14—H14B0.866 (19)
Co1—O62.143 (2)O15—H15A0.854 (19)
Co1—O22.147 (2)O15—H15B0.858 (19)
Co1—O52.147 (2)C15—C161.524 (4)
Co1—O12.188 (2)C16—C171.391 (4)
Cl1—C41.729 (3)C17—C181.392 (4)
Cl2—C111.730 (3)C17—H170.9600
N1—C21.341 (4)C18—C191.391 (4)
N1—C61.347 (4)C19—C201.388 (4)
N2—C131.326 (4)C19—H190.9600
N2—C91.341 (4)C20—C211.523 (4)
O1—C11.279 (4)Co2—O18i2.070 (2)
O2—C71.255 (4)Co2—O182.070 (2)
O3—C11.244 (4)Co2—O172.092 (2)
O4—C71.248 (4)Co2—O17i2.092 (2)
O5—C81.263 (4)Co2—O16i2.114 (2)
O6—C141.285 (4)Co2—O162.114 (2)
O7—C81.256 (4)Co2—Na1i3.4979 (15)
O8—C141.228 (4)Co2—Na13.4979 (15)
O8—Na12.331 (3)O16—Na12.507 (3)
C1—C21.511 (4)O16—H16A0.884 (19)
C2—C31.386 (4)O16—H16B0.833 (19)
C3—C41.392 (5)O17—Na12.459 (2)
C3—H30.9600O17—H17A0.866 (19)
C4—C51.388 (4)O17—H17B0.855 (18)
C5—C61.375 (4)O18—H18A0.862 (19)
C5—H50.9600O18—H18B0.883 (19)
C6—C71.523 (4)Na1—O222.280 (3)
C8—C91.510 (4)Na1—O24'2.362 (6)
C9—C101.394 (4)Na1—O242.390 (5)
C10—C111.386 (4)Na1—O192.490 (3)
C10—H100.9600Na1—H24B2.13 (6)
C11—C121.387 (4)O19—H19A0.852 (19)
C12—C131.383 (4)O19—H19B0.861 (19)
C12—H120.9600O20—H20A0.857 (19)
C13—C141.519 (4)O20—H20B0.872 (19)
Co3—O152.026 (2)O21—H21A0.862 (19)
Co3—N32.045 (2)O21—H21B0.860 (19)
Co3—O142.047 (2)O22—H22A0.872 (19)
Co3—O102.160 (2)O22—H22B0.87 (2)
Co3—O132.164 (2)O23—O23'0.795 (7)
Co3—O92.183 (2)O23—H23A0.872 (19)
Cl3—C181.732 (3)O23—H23B0.877 (19)
N3—C161.337 (4)O23'—H23A0.98 (3)
N3—C201.337 (4)O23'—H23B0.97 (3)
O9—C151.273 (4)O24—O24'1.297 (7)
O10—C211.276 (3)O24—H24A0.874 (18)
O11—C151.250 (4)O24—H24B0.88 (2)
O12—C211.241 (3)O24'—H24A1.27 (4)
O13—H13A0.869 (18)O24'—H24B0.52 (4)
O13—H13B0.873 (19)
N2—Co1—N1179.17 (9)N3—C20—C19120.9 (3)
N2—Co1—O676.81 (9)N3—C20—C21113.2 (2)
N1—Co1—O6102.47 (9)C19—C20—C21125.9 (3)
N2—Co1—O2103.45 (9)O12—C21—O10126.6 (3)
N1—Co1—O276.18 (9)O12—C21—C20118.8 (2)
O6—Co1—O295.69 (8)O10—C21—C20114.6 (2)
N2—Co1—O576.44 (10)O18i—Co2—O18180.00 (12)
N1—Co1—O5104.26 (10)O18i—Co2—O1790.81 (9)
O6—Co1—O5153.20 (8)O18—Co2—O1789.19 (9)
O2—Co1—O588.90 (9)O18i—Co2—O17i89.19 (9)
N2—Co1—O1104.41 (9)O18—Co2—O17i90.81 (9)
N1—Co1—O175.95 (9)O17—Co2—O17i180.000 (1)
O6—Co1—O189.72 (8)O18i—Co2—O16i88.93 (9)
O2—Co1—O1152.13 (8)O18—Co2—O16i91.07 (9)
O5—Co1—O198.48 (8)O17—Co2—O16i92.68 (9)
C2—N1—C6121.0 (3)O17i—Co2—O16i87.32 (9)
C2—N1—Co1119.6 (2)O18i—Co2—O1691.07 (9)
C6—N1—Co1119.39 (19)O18—Co2—O1688.93 (9)
C13—N2—C9121.4 (3)O17—Co2—O1687.32 (9)
C13—N2—Co1119.1 (2)O17i—Co2—O1692.68 (9)
C9—N2—Co1119.4 (2)O16i—Co2—O16180.00 (14)
C1—O1—Co1115.42 (19)O18i—Co2—Na1i79.08 (7)
C7—O2—Co1116.71 (18)O18—Co2—Na1i100.92 (7)
C8—O5—Co1115.56 (18)O17—Co2—Na1i136.21 (6)
C14—O6—Co1115.74 (19)O17i—Co2—Na1i43.79 (6)
C14—O8—Na1132.80 (19)O16i—Co2—Na1i45.20 (7)
O3—C1—O1125.9 (3)O16—Co2—Na1i134.80 (7)
O3—C1—C2118.8 (3)O18i—Co2—Na1100.92 (7)
O1—C1—C2115.2 (2)O18—Co2—Na179.08 (7)
N1—C2—C3120.8 (3)O17—Co2—Na143.79 (6)
N1—C2—C1113.5 (3)O17i—Co2—Na1136.21 (6)
C3—C2—C1125.7 (3)O16i—Co2—Na1134.80 (7)
C2—C3—C4117.9 (3)O16—Co2—Na145.20 (7)
C2—C3—H3121.1Na1i—Co2—Na1180.0
C4—C3—H3121.1Co2—O16—Na198.04 (9)
C5—C4—C3121.2 (3)Co2—O16—H16A110 (2)
C5—C4—Cl1119.2 (3)Na1—O16—H16A114 (2)
C3—C4—Cl1119.6 (2)Co2—O16—H16B111 (3)
C6—C5—C4117.5 (3)Na1—O16—H16B113 (2)
C6—C5—H5121.2H16A—O16—H16B110 (3)
C4—C5—H5121.2Co2—O17—Na1100.14 (9)
N1—C6—C5121.6 (3)Co2—O17—H17A104 (2)
N1—C6—C7112.0 (3)Na1—O17—H17A131 (2)
C5—C6—C7126.3 (3)Co2—O17—H17B110 (2)
O4—C7—O2126.0 (3)Na1—O17—H17B106 (2)
O4—C7—C6118.4 (3)H17A—O17—H17B105 (3)
O2—C7—C6115.7 (3)Co2—O18—H18A116 (3)
O7—C8—O5125.7 (3)Co2—O18—H18B124 (3)
O7—C8—C9118.1 (3)H18A—O18—H18B101 (3)
O5—C8—C9116.2 (3)O22—Na1—O8114.12 (11)
N2—C9—C10121.0 (3)O22—Na1—O24'89.33 (16)
N2—C9—C8112.2 (3)O8—Na1—O24'71.02 (15)
C10—C9—C8126.8 (3)O22—Na1—O2489.85 (14)
C11—C10—C9116.9 (3)O8—Na1—O2499.61 (14)
C11—C10—H10121.6O24'—Na1—O2431.68 (18)
C9—C10—H10121.6O22—Na1—O17155.17 (11)
C10—C11—C12122.0 (3)O8—Na1—O1790.42 (8)
C10—C11—Cl2118.9 (2)O24'—Na1—O1795.61 (15)
C12—C11—Cl2119.1 (2)O24—Na1—O1782.00 (12)
C13—C12—C11117.0 (3)O22—Na1—O1993.27 (11)
C13—C12—H12121.5O8—Na1—O1978.70 (9)
C11—C12—H12121.5O24'—Na1—O19147.79 (15)
N2—C13—C12121.7 (3)O24—Na1—O19176.85 (13)
N2—C13—C14113.6 (3)O17—Na1—O1995.32 (9)
C12—C13—C14124.6 (3)O22—Na1—O1687.95 (10)
O8—C14—O6126.6 (3)O8—Na1—O16147.57 (9)
O8—C14—C13118.8 (3)O24'—Na1—O16135.71 (16)
O6—C14—C13114.6 (3)O24—Na1—O16104.09 (14)
O15—Co3—N3173.05 (9)O17—Na1—O1671.57 (8)
O15—Co3—O1487.23 (9)O19—Na1—O1676.49 (9)
N3—Co3—O1487.62 (9)O22—Na1—Co2124.68 (9)
O15—Co3—O1099.86 (9)O8—Na1—Co2117.26 (6)
N3—Co3—O1075.88 (9)O24'—Na1—Co2125.49 (14)
O14—Co3—O1094.18 (9)O24—Na1—Co2100.42 (12)
O15—Co3—O1387.85 (9)O17—Na1—Co236.07 (5)
N3—Co3—O1397.62 (9)O19—Na1—Co278.16 (7)
O14—Co3—O13173.53 (8)O16—Na1—Co236.76 (5)
O10—Co3—O1390.79 (9)O22—Na1—H24B94.7 (14)
O15—Co3—O9109.07 (9)O8—Na1—H24B78.5 (7)
N3—Co3—O975.73 (9)O24'—Na1—H24B11.9 (10)
O14—Co3—O991.55 (9)O24—Na1—H24B21.5 (6)
O10—Co3—O9150.74 (8)O17—Na1—H24B86.3 (14)
O13—Co3—O986.10 (9)O19—Na1—H24B157.2 (6)
C16—N3—C20121.5 (3)O16—Na1—H24B125.2 (6)
C16—N3—Co3119.51 (19)Co2—Na1—H24B114.0 (12)
C20—N3—Co3118.6 (2)Na1—O19—H19A112 (3)
C15—O9—Co3115.55 (17)Na1—O19—H19B107 (3)
C21—O10—Co3115.63 (18)H19A—O19—H19B102 (4)
Co3—O13—H13A114 (2)H20A—O20—H20B109 (4)
Co3—O13—H13B110 (2)H21A—O21—H21B100 (4)
H13A—O13—H13B106 (3)Na1—O22—H22A122 (3)
Co3—O14—H14A124 (3)Na1—O22—H22B123 (3)
Co3—O14—H14B122 (3)H22A—O22—H22B110 (4)
H14A—O14—H14B104 (3)O23'—O23—H23A72 (3)
Co3—O15—H15A121 (3)O23'—O23—H23B70 (3)
Co3—O15—H15B115 (3)H23A—O23—H23B101 (4)
H15A—O15—H15B109 (4)O23—O23'—H23A57.8 (18)
O11—C15—O9126.9 (3)O23—O23'—H23B58.8 (18)
O11—C15—C16117.6 (3)H23A—O23'—H23B88 (3)
O9—C15—C16115.4 (3)O24'—O24—Na173.0 (3)
N3—C16—C17121.8 (3)O24'—O24—H24A68 (3)
N3—C16—C15113.0 (2)Na1—O24—H24A129 (3)
C17—C16—C15125.2 (3)O24'—O24—H24B17 (3)
C16—C17—C18116.2 (3)Na1—O24—H24B62 (4)
C16—C17—H17121.9H24A—O24—H24B85 (4)
C18—C17—H17121.9O24—O24'—Na175.3 (3)
C19—C18—C17122.3 (3)O24—O24'—H24A39.8 (10)
C19—C18—Cl3120.3 (2)Na1—O24'—H24A108.9 (13)
C17—C18—Cl3117.4 (2)O24—O24'—H24B29 (4)
C20—C19—C18117.2 (3)Na1—O24'—H24B58 (7)
C20—C19—H19121.4H24A—O24'—H24B69 (5)
C18—C19—H19121.4

Symmetry codes: (i) −x+1, −y+1, −z.

Hydrogen-bond geometry (Å, °)

D—H···AD—HH···AD···AD—H···A
O13—H13A···O9ii0.869 (18)1.95 (2)2.778 (3)160 (3)
O13—H13B···O4iii0.873 (19)1.82 (2)2.687 (3)174 (3)
O14—H14A···O11iv0.879 (19)1.88 (2)2.747 (3)171 (4)
O14—H14B···O7v0.866 (19)1.84 (2)2.688 (3)167 (4)
O15—H15A···O24'i0.854 (19)1.83 (2)2.650 (6)161 (4)
O15—H15A···O24i0.854 (19)2.13 (2)2.939 (5)158 (4)
O15—H15B···O4vi0.858 (19)1.885 (19)2.743 (3)178 (4)
O16—H16A···O120.884 (19)1.91 (2)2.791 (3)172 (4)
O16—H16B···O21vii0.833 (19)1.95 (2)2.761 (3)165 (3)
O17—H17A···O10i0.866 (19)1.89 (2)2.752 (3)170 (3)
O17—H17B···O20viii0.855 (18)1.776 (19)2.628 (3)174 (4)
O18—H18A···O190.862 (19)1.89 (2)2.701 (3)157 (4)
O18—H18B···O23'viii0.883 (19)1.84 (2)2.703 (7)165 (4)
O18—H18B···O23viii0.883 (19)1.90 (2)2.753 (6)162 (3)
O19—H19B···O60.861 (19)1.89 (3)2.679 (3)151 (4)
O20—H20A···O7ix0.857 (19)1.89 (2)2.732 (3)170 (4)
O21—H21A···O3x0.862 (19)1.96 (2)2.816 (3)170 (4)
O20—H20B···O1x0.872 (19)1.94 (2)2.802 (3)171 (4)
O21—H21B···O12xi0.860 (19)2.01 (2)2.837 (3)161 (4)
O22—H22A···O7xii0.872 (19)2.33 (3)3.136 (4)154 (4)
O22—H22B···O21xiii0.87 (2)2.02 (2)2.862 (4)164 (4)
O22—H22A···O20xiii0.872 (19)2.69 (5)3.127 (3)112 (4)
O23—H23A···O13x0.872 (19)1.99 (2)2.825 (6)159 (4)
O23'—H23B···O3x0.97 (3)2.14 (3)2.854 (6)129 (3)
O24—H24A···O11xiv0.874 (18)1.95 (2)2.820 (5)176 (4)

Symmetry codes: (ii) −x+1, −y, −z+1; (iii) −x+1, −y+1, −z+1; (iv) −x+2, −y, −z+1; (v) x+1, y−1, z; (i) −x+1, −y+1, −z; (vi) x, y−1, z; (vii) −x+1, −y+1, −z−1; (viii) x, y, z+1; (ix) −x, −y+2, −z−1; (x) x, y, z−1; (xi) x−1, y, z−1; (xii) −x+1, −y+2, −z; (xiii) x+1, y, z+1; (xiv) x, y+1, z−1.

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: SU2035).

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