metal-organic compounds
Aqua(3-hydroxybenzoato-κO)bis(1,10-phenanthroline-κ2N,N′)cobalt(II) 3-hydroxybenzoate pentahydrate
aDepartment of Chemistry, Zhejiang University, People's Republic of China
*Correspondence e-mail: xudj@mail.hz.zj.cn
The 7H5O3)(C12H8N2)2(H2O)](C7H5O3)·5H2O, consists of CoII complex cations, uncoordinated hydroxybenzoate anions and uncoordinated water molecules. The CoII ion is coordinated by two phenanthroline ligands, a water molecule and a 3-hydroxybenzoate anion, and displays a distorted octahedral geometry. π–π stacking is observed between parallel phenanthroline ligands, the face-to-face separations being 3.454 (19) and 3.435 (7) Å. An extensive hydrogen-bonding network helps to stabilize the The hydroxybenzoate ligand is disordered over two positions, with site occupancy factors 0.6 and 0.4. One solvent water molecule is also disordered over two positions, with site occupancy factors 0.6 and 0.4.
of the title compound, [Co(CRelated literature
For general background, see: Hu et al. (2002); Li et al. (2005). For related structures, see: Su et al. (2005); Pan et al. (2006).
Experimental
Crystal data
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Refinement
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Data collection: PROCESS-AUTO (Rigaku, 1998); cell PROCESS-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2002); program(s) used to solve structure: SIR92 (Altomare et al., 1993); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).
Supporting information
10.1107/S1600536808001815/ng2420sup1.cif
contains datablocks I, global. DOI:Structure factors: contains datablock I. DOI: 10.1107/S1600536808001815/ng2420Isup2.hkl
Co(CH3COO)2.4H2O (0.24 g, 1 mmol), sodium 3-hydroxybenzoate (0.16 g, 1 mmol) and phen (0.20 g, 1 mmol) was dissolved in water (15 ml). The solution was refluxed for 5 h, and filtered after cooling to room temperature. Single crystals of the title compound were obtained after 5 d.
The coordinated HBA anion is disordered over two sites, with the hydroxyl group located on the opposite position; occupancies were initially refined and converged to 0.588:0.412, and were fixed as 0.6 and 0.4, respectively, in final cycles of
Accordingly, lattice water molecule O5W is disordered over two sites. One disordered component O5WA is hydrogen bonded to the O3A while the other component O5WB is hydrogen bonded to the other lattice water molecules. Occupancies for O5WA and O5WB were set as 0.6 and 0.4, respectively. The C—Ocarboxyl distances in the disordered HBA components were restrained as 1.25±0.01 Å. The thermal parameters for C1A, C1B, C7A and C7B were constrained to be the same. H atoms of water molecules were placed in chemically sensible positions on the basis of hydrogen bonding interactions, Uiso(H) = 1.5Ueq(O). Aromatic H atoms were placed in calculated positions with C—H = 0.93 Å and refined in riding mode with Uiso(H) = 1.2Ueq(C).Data collection: PROCESS-AUTO (Rigaku, 1998); cell
PROCESS-AUTO (Rigaku, 1998); data reduction: CrystalStructure (Rigaku/MSC, 2002); program(s) used to solve structure: SIR92 (Altomare et al., 1993); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).Fig. 1. The molecular structure of the title compound with 30% probability displacement (arbitrary spheres for H atoms). One of disordered components has been omitted for clarity. | |
Fig. 2. A diagram showing π-π stacking between N1-containing phen rings [symmetry code: (A) 1 - x,-y,-z]. | |
Fig. 3. A diagram showing π-π stacking between N3-containing phen rings [symmetry code: (B) 2 - x,1 - y,1 - z]. |
[Co(C7H5O3)(C12H8N2)2(H2O)](C7H5O3)·5H2O | Z = 2 |
Mr = 801.65 | F(000) = 834 |
Triclinic, P1 | Dx = 1.448 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 12.3404 (12) Å | Cell parameters from 6882 reflections |
b = 12.6844 (16) Å | θ = 2.5–25.0° |
c = 13.561 (2) Å | µ = 0.54 mm−1 |
α = 101.507 (5)° | T = 295 K |
β = 101.781 (4)° | Prism, pink |
γ = 111.823 (7)° | 0.32 × 0.28 × 0.20 mm |
V = 1838.4 (4) Å3 |
Rigaku R-AXIS RAPID IP diffractometer | 6450 independent reflections |
Radiation source: fine-focus sealed tube | 4935 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.050 |
Detector resolution: 10.00 pixels mm-1 | θmax = 25.2°, θmin = 1.6° |
ω scans | h = −14→14 |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | k = −15→15 |
Tmin = 0.850, Tmax = 0.905 | l = −16→16 |
11865 measured reflections |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.070 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.247 | H-atom parameters constrained |
S = 1.02 | w = 1/[σ2(Fo2) + (0.196P)2] where P = (Fo2 + 2Fc2)/3 |
6450 reflections | (Δ/σ)max = 0.001 |
577 parameters | Δρmax = 0.42 e Å−3 |
4 restraints | Δρmin = −0.69 e Å−3 |
[Co(C7H5O3)(C12H8N2)2(H2O)](C7H5O3)·5H2O | γ = 111.823 (7)° |
Mr = 801.65 | V = 1838.4 (4) Å3 |
Triclinic, P1 | Z = 2 |
a = 12.3404 (12) Å | Mo Kα radiation |
b = 12.6844 (16) Å | µ = 0.54 mm−1 |
c = 13.561 (2) Å | T = 295 K |
α = 101.507 (5)° | 0.32 × 0.28 × 0.20 mm |
β = 101.781 (4)° |
Rigaku R-AXIS RAPID IP diffractometer | 6450 independent reflections |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | 4935 reflections with I > 2σ(I) |
Tmin = 0.850, Tmax = 0.905 | Rint = 0.050 |
11865 measured reflections |
R[F2 > 2σ(F2)] = 0.070 | 4 restraints |
wR(F2) = 0.247 | H-atom parameters constrained |
S = 1.02 | Δρmax = 0.42 e Å−3 |
6450 reflections | Δρmin = −0.69 e Å−3 |
577 parameters |
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. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Co | 0.60509 (5) | 0.22032 (5) | 0.34437 (4) | 0.0424 (2) | |
N1 | 0.6556 (3) | 0.4006 (3) | 0.4352 (3) | 0.0471 (8) | |
N2 | 0.7823 (3) | 0.2680 (3) | 0.4520 (3) | 0.0483 (8) | |
N3 | 0.6048 (3) | 0.0665 (3) | 0.2420 (3) | 0.0465 (8) | |
N4 | 0.6569 (3) | 0.2830 (3) | 0.2146 (3) | 0.0456 (8) | |
O1 | 0.5335 (3) | 0.1227 (3) | 0.4432 (2) | 0.0551 (8) | |
H1A | 0.5394 | 0.1655 | 0.5102 | 0.083* | |
H1B | 0.4574 | 0.0855 | 0.4018 | 0.083* | |
O11 | 0.5066 (4) | 0.2421 (4) | 0.6154 (3) | 0.0735 (10) | |
O12 | 0.5309 (4) | 0.4010 (4) | 0.7405 (3) | 0.0783 (11) | |
O13 | 0.8806 (3) | 0.1749 (4) | 0.7731 (3) | 0.0789 (11) | |
H13 | 0.8129 | 0.0979 | 0.7327 | 0.118* | |
C1A | 0.2218 (10) | 0.1511 (11) | 0.1942 (9) | 0.0508 (15) | 0.60 |
C2A | 0.2545 (14) | 0.2317 (14) | 0.1350 (17) | 0.059 (4) | 0.60 |
H2A | 0.3368 | 0.2788 | 0.1455 | 0.071* | 0.60 |
C3A | 0.1661 (14) | 0.2409 (12) | 0.0626 (12) | 0.075 (4) | 0.60 |
C4A | 0.0412 (15) | 0.1750 (12) | 0.0547 (10) | 0.078 (3) | 0.60 |
H4A | −0.0191 | 0.1842 | 0.0084 | 0.094* | 0.60 |
C5A | 0.0067 (13) | 0.0990 (14) | 0.1122 (14) | 0.071 (4) | 0.60 |
H5A | −0.0756 | 0.0550 | 0.1044 | 0.085* | 0.60 |
C6A | 0.0984 (13) | 0.0895 (12) | 0.1828 (10) | 0.067 (3) | 0.60 |
H6A | 0.0763 | 0.0399 | 0.2243 | 0.081* | 0.60 |
C7A | 0.3203 (11) | 0.1353 (11) | 0.2694 (14) | 0.0508 (15) | 0.60 |
O1A | 0.4263 (12) | 0.1942 (12) | 0.2653 (15) | 0.053 (4) | 0.60 |
O2A | 0.2963 (17) | 0.0622 (16) | 0.3208 (15) | 0.071 (4) | 0.60 |
O3A | 0.1860 (7) | 0.3081 (6) | −0.0005 (5) | 0.0820 (19) | 0.60 |
H1 | 0.2626 | 0.3600 | 0.0150 | 0.123* | 0.60 |
C1B | 0.2094 (15) | 0.1263 (15) | 0.2168 (11) | 0.0508 (15) | 0.40 |
C2B | 0.0995 (14) | 0.0641 (15) | 0.2263 (16) | 0.060 (4) | 0.40 |
H2B | 0.0939 | 0.0132 | 0.2678 | 0.072* | 0.40 |
C3B | −0.0032 (12) | 0.0716 (15) | 0.1789 (19) | 0.084 (5) | 0.40 |
C4B | 0.006 (2) | 0.147 (2) | 0.112 (3) | 0.083 (9) | 0.40 |
H4B | −0.0614 | 0.1600 | 0.0832 | 0.100* | 0.40 |
C5B | 0.120 (2) | 0.204 (2) | 0.0892 (18) | 0.088 (8) | 0.40 |
H5B | 0.1265 | 0.2467 | 0.0403 | 0.106* | 0.40 |
C6B | 0.218 (2) | 0.192 (2) | 0.144 (2) | 0.058 (6) | 0.40 |
H6B | 0.2929 | 0.2276 | 0.1330 | 0.070* | 0.40 |
C7B | 0.3307 (16) | 0.1191 (18) | 0.268 (2) | 0.0508 (15) | 0.40 |
O1B | 0.4321 (19) | 0.202 (2) | 0.278 (2) | 0.070 (8) | 0.40 |
O2B | 0.311 (2) | 0.037 (2) | 0.310 (2) | 0.059 (5) | 0.40 |
O3B | −0.1123 (10) | 0.0191 (15) | 0.2019 (15) | 0.142 (6) | 0.40 |
H2 | −0.1000 | 0.0015 | 0.2657 | 0.213* | 0.40 |
C11 | 0.5705 (5) | 0.3309 (5) | 0.6973 (4) | 0.0636 (13) | |
C12 | 0.6997 (5) | 0.3480 (4) | 0.7466 (3) | 0.0565 (11) | |
C13 | 0.7313 (4) | 0.2527 (5) | 0.7315 (4) | 0.0576 (12) | |
H14 | 0.6737 | 0.1784 | 0.6861 | 0.069* | |
C14 | 0.8459 (5) | 0.2668 (5) | 0.7826 (4) | 0.0609 (12) | |
C15 | 0.9346 (5) | 0.3798 (5) | 0.8489 (4) | 0.0678 (14) | |
H15 | 1.0126 | 0.3905 | 0.8844 | 0.081* | |
C16 | 0.9037 (5) | 0.4740 (6) | 0.8601 (4) | 0.0753 (16) | |
H16 | 0.9632 | 0.5494 | 0.9014 | 0.090* | |
C17 | 0.7878 (5) | 0.4609 (5) | 0.8125 (4) | 0.0655 (13) | |
H17 | 0.7683 | 0.5255 | 0.8239 | 0.079* | |
C21 | 0.5936 (4) | 0.4671 (5) | 0.4228 (4) | 0.0560 (11) | |
H21 | 0.5167 | 0.4318 | 0.3724 | 0.067* | |
C22 | 0.6393 (5) | 0.5870 (5) | 0.4822 (5) | 0.0688 (14) | |
H22 | 0.5941 | 0.6304 | 0.4708 | 0.083* | |
C23 | 0.7511 (5) | 0.6384 (5) | 0.5569 (4) | 0.0669 (13) | |
H23 | 0.7827 | 0.7176 | 0.5976 | 0.080* | |
C24 | 0.8187 (4) | 0.5724 (4) | 0.5726 (3) | 0.0540 (11) | |
C25 | 0.9376 (5) | 0.6207 (4) | 0.6496 (4) | 0.0633 (13) | |
H25 | 0.9728 | 0.6994 | 0.6923 | 0.076* | |
C26 | 0.9991 (5) | 0.5519 (5) | 0.6602 (4) | 0.0623 (13) | |
H26 | 1.0754 | 0.5846 | 0.7111 | 0.075* | |
C27 | 0.9495 (4) | 0.4305 (5) | 0.5953 (3) | 0.0553 (11) | |
C28 | 1.0094 (5) | 0.3559 (5) | 0.6036 (4) | 0.0659 (14) | |
H28 | 1.0854 | 0.3847 | 0.6540 | 0.079* | |
C29 | 0.9566 (5) | 0.2421 (5) | 0.5383 (4) | 0.0681 (14) | |
H29 | 0.9958 | 0.1926 | 0.5442 | 0.082* | |
C30 | 0.8434 (4) | 0.2004 (5) | 0.4624 (4) | 0.0589 (12) | |
H30 | 0.8087 | 0.1229 | 0.4172 | 0.071* | |
C31 | 0.8347 (4) | 0.3812 (4) | 0.5182 (3) | 0.0471 (10) | |
C32 | 0.7674 (4) | 0.4524 (4) | 0.5088 (3) | 0.0462 (10) | |
C33 | 0.5792 (4) | −0.0416 (4) | 0.2556 (4) | 0.0555 (11) | |
H33 | 0.5602 | −0.0538 | 0.3166 | 0.067* | |
C34 | 0.5797 (5) | −0.1353 (5) | 0.1835 (5) | 0.0694 (14) | |
H34 | 0.5600 | −0.2085 | 0.1963 | 0.083* | |
C35 | 0.6090 (5) | −0.1212 (5) | 0.0941 (4) | 0.0690 (14) | |
H35 | 0.6101 | −0.1838 | 0.0459 | 0.083* | |
C36 | 0.6376 (4) | −0.0094 (5) | 0.0760 (4) | 0.0595 (12) | |
C37 | 0.6691 (5) | 0.0159 (6) | −0.0152 (4) | 0.0748 (16) | |
H37 | 0.6707 | −0.0438 | −0.0665 | 0.090* | |
C38 | 0.6962 (5) | 0.1239 (6) | −0.0284 (4) | 0.0705 (15) | |
H38 | 0.7169 | 0.1372 | −0.0885 | 0.085* | |
C39 | 0.6943 (4) | 0.2189 (5) | 0.0470 (4) | 0.0567 (12) | |
C40 | 0.7194 (5) | 0.3336 (5) | 0.0369 (4) | 0.0646 (13) | |
H40 | 0.7421 | 0.3523 | −0.0209 | 0.077* | |
C41 | 0.7105 (5) | 0.4165 (5) | 0.1111 (4) | 0.0696 (15) | |
H41 | 0.7251 | 0.4913 | 0.1032 | 0.084* | |
C42 | 0.6791 (4) | 0.3893 (4) | 0.2002 (4) | 0.0584 (12) | |
H42 | 0.6736 | 0.4472 | 0.2505 | 0.070* | |
C43 | 0.6633 (3) | 0.1978 (4) | 0.1388 (3) | 0.0461 (10) | |
C44 | 0.6349 (4) | 0.0821 (4) | 0.1533 (3) | 0.0455 (9) | |
O1W | 0.5758 (4) | 0.5521 (5) | 0.9411 (4) | 0.1013 (15) | |
H1AW | 0.5657 | 0.5095 | 0.8695 | 0.152* | |
H1BW | 0.5728 | 0.4970 | 0.9730 | 0.152* | |
O2W | 0.2485 (9) | 0.1055 (6) | 0.5219 (5) | 0.172 (3) | |
H2AW | 0.3251 | 0.1504 | 0.5602 | 0.258* | |
H2BW | 0.2501 | 0.0760 | 0.4575 | 0.258* | |
O3W | 0.2752 (6) | 0.3142 (7) | 0.7040 (6) | 0.154 (3) | |
H3AW | 0.3587 | 0.3523 | 0.7218 | 0.231* | |
H3BW | 0.2548 | 0.3157 | 0.7643 | 0.231* | |
O4W | 0.0758 (10) | 0.0332 (12) | 0.6051 (12) | 0.280 (6) | |
H4AW | 0.1166 | 0.1149 | 0.6377 | 0.419* | |
H4BW | 0.1266 | 0.0219 | 0.5707 | 0.419* | |
O5WA | 0.1205 (9) | 0.1918 (12) | −0.2128 (10) | 0.148 (4) | 0.60 |
H5A1 | 0.0408 | 0.1483 | −0.2283 | 0.222* | 0.60 |
H5A2 | 0.1433 | 0.2299 | −0.1480 | 0.222* | 0.60 |
O5WB | 0.198 (2) | 0.2812 (15) | 0.8858 (16) | 0.170 (8) | 0.40 |
H5B1 | 0.1772 | 0.3385 | 0.9099 | 0.255* | 0.40 |
H5B2 | 0.2755 | 0.3110 | 0.9254 | 0.255* | 0.40 |
U11 | U22 | U33 | U12 | U13 | U23 | |
Co | 0.0402 (4) | 0.0439 (4) | 0.0377 (3) | 0.0111 (3) | 0.0110 (2) | 0.0161 (2) |
N1 | 0.0447 (19) | 0.053 (2) | 0.0433 (18) | 0.0178 (17) | 0.0141 (15) | 0.0188 (16) |
N2 | 0.0487 (19) | 0.048 (2) | 0.0475 (19) | 0.0182 (17) | 0.0114 (16) | 0.0201 (16) |
N3 | 0.0439 (18) | 0.049 (2) | 0.0393 (17) | 0.0112 (16) | 0.0127 (15) | 0.0161 (15) |
N4 | 0.0440 (18) | 0.0445 (19) | 0.0447 (18) | 0.0128 (15) | 0.0128 (15) | 0.0192 (15) |
O1 | 0.0611 (18) | 0.0548 (18) | 0.0506 (16) | 0.0186 (15) | 0.0242 (14) | 0.0235 (14) |
O11 | 0.080 (2) | 0.088 (3) | 0.0471 (18) | 0.034 (2) | 0.0138 (17) | 0.0177 (18) |
O12 | 0.090 (3) | 0.083 (3) | 0.068 (2) | 0.047 (2) | 0.025 (2) | 0.016 (2) |
O13 | 0.059 (2) | 0.079 (3) | 0.093 (3) | 0.0218 (19) | 0.0203 (19) | 0.032 (2) |
C1A | 0.040 (2) | 0.059 (3) | 0.042 (2) | 0.016 (2) | 0.0118 (19) | 0.000 (2) |
C2A | 0.049 (8) | 0.057 (9) | 0.061 (6) | 0.019 (6) | 0.008 (6) | 0.012 (6) |
C3A | 0.075 (9) | 0.051 (6) | 0.075 (7) | 0.012 (6) | 0.009 (6) | 0.014 (5) |
C4A | 0.072 (8) | 0.077 (8) | 0.082 (8) | 0.037 (6) | 0.014 (7) | 0.018 (6) |
C5A | 0.050 (6) | 0.051 (9) | 0.092 (9) | 0.009 (6) | 0.008 (5) | 0.018 (8) |
C6A | 0.061 (7) | 0.053 (7) | 0.083 (8) | 0.019 (5) | 0.016 (6) | 0.025 (5) |
C7A | 0.040 (2) | 0.059 (3) | 0.042 (2) | 0.016 (2) | 0.0118 (19) | 0.000 (2) |
O1A | 0.040 (7) | 0.059 (7) | 0.055 (7) | 0.025 (6) | 0.005 (4) | 0.011 (4) |
O2A | 0.051 (7) | 0.086 (10) | 0.058 (6) | 0.002 (6) | 0.024 (4) | 0.031 (7) |
O3A | 0.089 (5) | 0.073 (4) | 0.065 (4) | 0.023 (4) | −0.003 (3) | 0.030 (3) |
C1B | 0.040 (2) | 0.059 (3) | 0.042 (2) | 0.016 (2) | 0.0118 (19) | 0.000 (2) |
C2B | 0.027 (6) | 0.039 (8) | 0.102 (14) | 0.012 (5) | 0.010 (8) | 0.012 (8) |
C3B | 0.033 (7) | 0.068 (10) | 0.141 (17) | 0.018 (6) | 0.011 (8) | 0.034 (11) |
C4B | 0.065 (11) | 0.047 (14) | 0.125 (19) | 0.036 (12) | 0.005 (11) | 0.003 (15) |
C5B | 0.055 (13) | 0.091 (17) | 0.084 (14) | 0.043 (12) | −0.035 (12) | −0.010 (11) |
C6B | 0.052 (13) | 0.068 (15) | 0.044 (9) | 0.031 (10) | 0.001 (9) | −0.002 (11) |
C7B | 0.040 (2) | 0.059 (3) | 0.042 (2) | 0.016 (2) | 0.0118 (19) | 0.000 (2) |
O1B | 0.042 (10) | 0.099 (16) | 0.046 (8) | −0.002 (8) | 0.010 (7) | 0.041 (10) |
O2B | 0.034 (6) | 0.067 (9) | 0.058 (8) | 0.016 (5) | 0.010 (5) | 0.000 (6) |
O3B | 0.053 (6) | 0.160 (13) | 0.241 (19) | 0.037 (7) | 0.063 (9) | 0.114 (13) |
C11 | 0.077 (3) | 0.066 (3) | 0.045 (2) | 0.022 (3) | 0.021 (2) | 0.027 (2) |
C12 | 0.068 (3) | 0.059 (3) | 0.043 (2) | 0.021 (2) | 0.021 (2) | 0.024 (2) |
C13 | 0.055 (3) | 0.065 (3) | 0.044 (2) | 0.014 (2) | 0.016 (2) | 0.023 (2) |
C14 | 0.062 (3) | 0.066 (3) | 0.057 (3) | 0.023 (3) | 0.022 (2) | 0.029 (2) |
C15 | 0.054 (3) | 0.071 (3) | 0.054 (3) | 0.004 (3) | 0.011 (2) | 0.020 (2) |
C16 | 0.077 (4) | 0.070 (4) | 0.056 (3) | 0.007 (3) | 0.020 (3) | 0.017 (3) |
C17 | 0.075 (3) | 0.063 (3) | 0.056 (3) | 0.020 (3) | 0.027 (3) | 0.024 (2) |
C21 | 0.059 (3) | 0.064 (3) | 0.053 (2) | 0.032 (2) | 0.021 (2) | 0.021 (2) |
C22 | 0.080 (4) | 0.069 (3) | 0.077 (3) | 0.044 (3) | 0.032 (3) | 0.031 (3) |
C23 | 0.078 (3) | 0.055 (3) | 0.068 (3) | 0.026 (3) | 0.029 (3) | 0.015 (2) |
C24 | 0.055 (3) | 0.053 (3) | 0.046 (2) | 0.013 (2) | 0.020 (2) | 0.014 (2) |
C25 | 0.068 (3) | 0.045 (3) | 0.048 (2) | 0.006 (2) | 0.008 (2) | 0.002 (2) |
C26 | 0.056 (3) | 0.057 (3) | 0.047 (2) | 0.004 (2) | 0.004 (2) | 0.014 (2) |
C27 | 0.047 (2) | 0.066 (3) | 0.045 (2) | 0.011 (2) | 0.0112 (19) | 0.029 (2) |
C28 | 0.052 (3) | 0.078 (4) | 0.057 (3) | 0.017 (3) | 0.006 (2) | 0.029 (3) |
C29 | 0.062 (3) | 0.075 (4) | 0.071 (3) | 0.033 (3) | 0.010 (3) | 0.034 (3) |
C30 | 0.055 (3) | 0.053 (3) | 0.066 (3) | 0.022 (2) | 0.012 (2) | 0.023 (2) |
C31 | 0.044 (2) | 0.051 (2) | 0.041 (2) | 0.0097 (19) | 0.0135 (17) | 0.0233 (19) |
C32 | 0.051 (2) | 0.051 (2) | 0.0370 (19) | 0.016 (2) | 0.0169 (18) | 0.0204 (18) |
C33 | 0.059 (3) | 0.058 (3) | 0.055 (2) | 0.022 (2) | 0.023 (2) | 0.026 (2) |
C34 | 0.077 (3) | 0.053 (3) | 0.079 (3) | 0.024 (3) | 0.028 (3) | 0.024 (3) |
C35 | 0.080 (4) | 0.061 (3) | 0.070 (3) | 0.034 (3) | 0.029 (3) | 0.014 (3) |
C36 | 0.055 (3) | 0.068 (3) | 0.055 (3) | 0.026 (2) | 0.020 (2) | 0.015 (2) |
C37 | 0.088 (4) | 0.090 (4) | 0.056 (3) | 0.043 (3) | 0.038 (3) | 0.019 (3) |
C38 | 0.071 (3) | 0.091 (4) | 0.051 (3) | 0.028 (3) | 0.030 (2) | 0.023 (3) |
C39 | 0.051 (2) | 0.074 (3) | 0.047 (2) | 0.021 (2) | 0.021 (2) | 0.028 (2) |
C40 | 0.061 (3) | 0.081 (4) | 0.057 (3) | 0.024 (3) | 0.024 (2) | 0.040 (3) |
C41 | 0.057 (3) | 0.068 (3) | 0.078 (4) | 0.012 (3) | 0.013 (3) | 0.047 (3) |
C42 | 0.051 (3) | 0.056 (3) | 0.060 (3) | 0.010 (2) | 0.012 (2) | 0.030 (2) |
C43 | 0.0334 (19) | 0.058 (3) | 0.041 (2) | 0.0113 (18) | 0.0091 (16) | 0.0220 (19) |
C44 | 0.038 (2) | 0.053 (2) | 0.043 (2) | 0.0153 (19) | 0.0111 (17) | 0.0191 (19) |
O1W | 0.104 (3) | 0.128 (4) | 0.080 (3) | 0.045 (3) | 0.037 (2) | 0.047 (3) |
O2W | 0.281 (10) | 0.121 (5) | 0.108 (4) | 0.075 (6) | 0.063 (5) | 0.039 (4) |
O3W | 0.123 (5) | 0.190 (7) | 0.217 (7) | 0.092 (5) | 0.082 (5) | 0.122 (6) |
O4W | 0.204 (10) | 0.316 (15) | 0.370 (16) | 0.166 (11) | 0.087 (10) | 0.102 (13) |
O5WA | 0.097 (7) | 0.185 (11) | 0.149 (9) | 0.044 (7) | 0.049 (6) | 0.044 (9) |
O5WB | 0.23 (2) | 0.096 (11) | 0.167 (16) | 0.043 (13) | 0.094 (16) | 0.019 (11) |
Co—O1 | 2.107 (3) | C15—C16 | 1.374 (9) |
Co—O1A | 2.116 (14) | C15—H15 | 0.9300 |
Co—O1B | 2.05 (2) | C16—C17 | 1.375 (8) |
Co—N1 | 2.154 (4) | C16—H16 | 0.9300 |
Co—N2 | 2.153 (3) | C17—H17 | 0.9300 |
Co—N3 | 2.155 (4) | C21—C22 | 1.404 (7) |
Co—N4 | 2.185 (3) | C21—H21 | 0.9300 |
N1—C21 | 1.345 (6) | C22—C23 | 1.361 (8) |
N1—C32 | 1.353 (5) | C22—H22 | 0.9300 |
N2—C30 | 1.345 (6) | C23—C24 | 1.400 (7) |
N2—C31 | 1.359 (6) | C23—H23 | 0.9300 |
N3—C33 | 1.348 (6) | C24—C32 | 1.415 (6) |
N3—C44 | 1.359 (5) | C24—C25 | 1.439 (7) |
N4—C42 | 1.336 (6) | C25—C26 | 1.361 (8) |
N4—C43 | 1.373 (6) | C25—H25 | 0.9300 |
O1—H1A | 0.9347 | C26—C27 | 1.435 (7) |
O1—H1B | 0.8775 | C26—H26 | 0.9300 |
O11—C11 | 1.268 (6) | C27—C31 | 1.402 (6) |
O12—C11 | 1.266 (7) | C27—C28 | 1.408 (8) |
O13—C14 | 1.377 (7) | C28—C29 | 1.359 (8) |
O13—H13 | 0.9714 | C28—H28 | 0.9300 |
C1A—C6A | 1.388 (18) | C29—C30 | 1.392 (7) |
C1A—C2A | 1.415 (18) | C29—H29 | 0.9300 |
C1A—C7A | 1.522 (17) | C30—H30 | 0.9300 |
C2A—C3A | 1.37 (3) | C31—C32 | 1.443 (6) |
C2A—H2A | 0.9300 | C33—C34 | 1.384 (7) |
C3A—O3A | 1.319 (14) | C33—H33 | 0.9300 |
C3A—C4A | 1.422 (19) | C34—C35 | 1.360 (8) |
C4A—C5A | 1.36 (2) | C34—H34 | 0.9300 |
C4A—H4A | 0.9300 | C35—C36 | 1.414 (7) |
C5A—C6A | 1.38 (2) | C35—H35 | 0.9300 |
C5A—H5A | 0.9300 | C36—C44 | 1.415 (7) |
C6A—H6A | 0.9300 | C36—C37 | 1.431 (7) |
C7A—O2A | 1.253 (8) | C37—C38 | 1.343 (8) |
C7A—O1A | 1.261 (8) | C37—H37 | 0.9300 |
O3A—H1 | 0.8786 | C38—C39 | 1.428 (8) |
C1B—C2B | 1.34 (2) | C38—H38 | 0.9300 |
C1B—C6B | 1.40 (3) | C39—C40 | 1.411 (8) |
C1B—C7B | 1.56 (2) | C39—C43 | 1.421 (6) |
C2B—C3B | 1.35 (2) | C40—C41 | 1.356 (8) |
C2B—H2B | 0.9300 | C40—H40 | 0.9300 |
C3B—O3B | 1.39 (2) | C41—C42 | 1.410 (7) |
C3B—C4B | 1.44 (4) | C41—H41 | 0.9300 |
C4B—C5B | 1.45 (4) | C42—H42 | 0.9300 |
C4B—H4B | 0.9300 | C43—C44 | 1.441 (6) |
C5B—C6B | 1.36 (3) | O1W—H1AW | 0.9705 |
C5B—H5B | 0.9300 | O1W—H1BW | 0.8857 |
C6B—H6B | 0.9300 | O2W—H2AW | 0.8762 |
C7B—O2B | 1.253 (10) | O2W—H2BW | 0.8867 |
C7B—O1B | 1.259 (10) | O3W—H3AW | 0.9143 |
O3B—H2 | 0.9326 | O3W—H3BW | 0.9019 |
C11—C12 | 1.512 (7) | O4W—H4AW | 0.9284 |
C12—C13 | 1.393 (7) | O4W—H4BW | 0.8901 |
C12—C17 | 1.402 (7) | O5WA—H5A1 | 0.8846 |
C13—C14 | 1.369 (7) | O5WA—H5A2 | 0.8442 |
C13—H14 | 0.9300 | O5WB—H5B1 | 0.8813 |
C14—C15 | 1.407 (7) | O5WB—H5B2 | 0.8883 |
O1B—Co—O1 | 87.8 (6) | C12—C13—H14 | 119.5 |
O1B—Co—O1A | 4.0 (12) | C13—C14—O13 | 123.4 (5) |
O1—Co—O1A | 89.6 (4) | C13—C14—C15 | 119.8 (5) |
O1B—Co—N2 | 164.3 (8) | O13—C14—C15 | 116.9 (5) |
O1—Co—N2 | 85.65 (13) | C16—C15—C14 | 118.6 (5) |
O1A—Co—N2 | 168.3 (5) | C16—C15—H15 | 120.7 |
O1B—Co—N1 | 89.9 (8) | C14—C15—H15 | 120.7 |
O1—Co—N1 | 102.07 (13) | C15—C16—C17 | 122.4 (5) |
O1A—Co—N1 | 93.0 (4) | C15—C16—H16 | 118.8 |
N2—Co—N1 | 77.61 (13) | C17—C16—H16 | 118.8 |
O1B—Co—N3 | 101.1 (8) | C16—C17—C12 | 118.6 (5) |
O1—Co—N3 | 91.94 (13) | C16—C17—H17 | 120.7 |
O1A—Co—N3 | 97.5 (4) | C12—C17—H17 | 120.7 |
N2—Co—N3 | 93.34 (14) | N1—C21—C22 | 123.1 (4) |
N1—Co—N3 | 162.56 (13) | N1—C21—H21 | 118.4 |
O1B—Co—N4 | 88.3 (7) | C22—C21—H21 | 118.4 |
O1—Co—N4 | 167.18 (13) | C23—C22—C21 | 118.5 (5) |
O1A—Co—N4 | 85.8 (5) | C23—C22—H22 | 120.7 |
N2—Co—N4 | 101.06 (13) | C21—C22—H22 | 120.7 |
N1—Co—N4 | 90.11 (13) | C22—C23—C24 | 120.2 (5) |
N3—Co—N4 | 76.88 (13) | C22—C23—H23 | 119.9 |
C21—N1—C32 | 118.2 (4) | C24—C23—H23 | 119.9 |
C21—N1—Co | 127.9 (3) | C23—C24—C32 | 118.1 (4) |
C32—N1—Co | 113.8 (3) | C23—C24—C25 | 123.3 (5) |
C30—N2—C31 | 117.9 (4) | C32—C24—C25 | 118.6 (5) |
C30—N2—Co | 128.6 (3) | C26—C25—C24 | 120.4 (4) |
C31—N2—Co | 113.4 (3) | C26—C25—H25 | 119.8 |
C33—N3—C44 | 116.8 (4) | C24—C25—H25 | 119.8 |
C33—N3—Co | 128.1 (3) | C25—C26—C27 | 121.9 (4) |
C44—N3—Co | 115.1 (3) | C25—C26—H26 | 119.0 |
C42—N4—C43 | 118.3 (4) | C27—C26—H26 | 119.0 |
C42—N4—Co | 128.5 (3) | C31—C27—C28 | 116.9 (5) |
C43—N4—Co | 113.2 (3) | C31—C27—C26 | 119.2 (5) |
Co—O1—H1A | 117.8 | C28—C27—C26 | 124.0 (4) |
Co—O1—H1B | 96.8 | C29—C28—C27 | 120.3 (5) |
H1A—O1—H1B | 111.6 | C29—C28—H28 | 119.8 |
C14—O13—H13 | 112.7 | C27—C28—H28 | 119.8 |
C6A—C1A—C2A | 118.0 (12) | C28—C29—C30 | 119.4 (5) |
C6A—C1A—C7A | 121.5 (11) | C28—C29—H29 | 120.3 |
C2A—C1A—C7A | 120.4 (12) | C30—C29—H29 | 120.3 |
C3A—C2A—C1A | 120.6 (12) | N2—C30—C29 | 122.5 (5) |
C3A—C2A—H2A | 119.7 | N2—C30—H30 | 118.8 |
C1A—C2A—H2A | 119.7 | C29—C30—H30 | 118.8 |
O3A—C3A—C2A | 125.6 (13) | N2—C31—C27 | 123.0 (4) |
O3A—C3A—C4A | 116.0 (13) | N2—C31—C32 | 117.8 (4) |
C2A—C3A—C4A | 118.3 (12) | C27—C31—C32 | 119.2 (4) |
C5A—C4A—C3A | 122.5 (13) | N1—C32—C24 | 121.9 (4) |
C5A—C4A—H4A | 118.8 | N1—C32—C31 | 117.4 (4) |
C3A—C4A—H4A | 118.8 | C24—C32—C31 | 120.7 (4) |
C4A—C5A—C6A | 117.6 (13) | N3—C33—C34 | 123.4 (4) |
C4A—C5A—H5A | 121.2 | N3—C33—H33 | 118.3 |
C6A—C5A—H5A | 121.2 | C34—C33—H33 | 118.3 |
C5A—C6A—C1A | 122.7 (13) | C35—C34—C33 | 120.5 (5) |
C5A—C6A—H6A | 118.7 | C35—C34—H34 | 119.8 |
C1A—C6A—H6A | 118.7 | C33—C34—H34 | 119.8 |
O2A—C7A—O1A | 124.2 (15) | C34—C35—C36 | 118.7 (5) |
O2A—C7A—C1A | 123.1 (13) | C34—C35—H35 | 120.6 |
O1A—C7A—C1A | 112.4 (15) | C36—C35—H35 | 120.6 |
C7A—O1A—Co | 134.9 (13) | C35—C36—C44 | 117.5 (4) |
C3A—O3A—H1 | 114.8 | C35—C36—C37 | 123.7 (5) |
O5WBi—O3A—H1 | 82.4 | C44—C36—C37 | 118.8 (5) |
C2B—C1B—C6B | 119.4 (18) | C38—C37—C36 | 121.4 (5) |
C2B—C1B—C7B | 125.2 (14) | C38—C37—H37 | 119.3 |
C6B—C1B—C7B | 114.7 (18) | C36—C37—H37 | 119.3 |
C1B—C2B—C3B | 123.2 (18) | C37—C38—C39 | 122.0 (5) |
C1B—C2B—H2B | 118.4 | C37—C38—H38 | 119.0 |
C3B—C2B—H2B | 118.4 | C39—C38—H38 | 119.0 |
C2B—C3B—O3B | 121.8 (19) | C40—C39—C43 | 116.6 (5) |
C2B—C3B—C4B | 117.7 (17) | C40—C39—C38 | 124.9 (5) |
O3B—C3B—C4B | 120.1 (17) | C43—C39—C38 | 118.5 (5) |
C3B—C4B—C5B | 120.5 (19) | C41—C40—C39 | 120.4 (4) |
C3B—C4B—H4B | 119.7 | C41—C40—H40 | 119.8 |
C5B—C4B—H4B | 119.7 | C39—C40—H40 | 119.8 |
C6B—C5B—C4B | 115 (2) | C40—C41—C42 | 119.9 (5) |
C6B—C5B—H5B | 122.3 | C40—C41—H41 | 120.0 |
C4B—C5B—H5B | 122.3 | C42—C41—H41 | 120.0 |
C5B—C6B—C1B | 123 (2) | N4—C42—C41 | 122.1 (5) |
C5B—C6B—H6B | 118.5 | N4—C42—H42 | 119.0 |
C1B—C6B—H6B | 118.5 | C41—C42—H42 | 119.0 |
O2B—C7B—O1B | 128 (3) | N4—C43—C39 | 122.7 (4) |
O2B—C7B—C1B | 111.4 (18) | N4—C43—C44 | 117.8 (4) |
O1B—C7B—C1B | 119 (2) | C39—C43—C44 | 119.5 (4) |
C7B—O1B—Co | 129 (2) | N3—C44—C36 | 123.2 (4) |
C3B—O3B—H2 | 112.5 | N3—C44—C43 | 117.0 (4) |
O12—C11—O11 | 124.0 (5) | C36—C44—C43 | 119.8 (4) |
O12—C11—C12 | 119.7 (5) | H1AW—O1W—H1BW | 100.9 |
O11—C11—C12 | 116.2 (5) | H2AW—O2W—H2BW | 106.1 |
C13—C12—C17 | 119.4 (5) | H3AW—O3W—H3BW | 107.9 |
C13—C12—C11 | 121.2 (4) | H4AW—O4W—H4BW | 100.6 |
C17—C12—C11 | 119.3 (5) | H5A1—O5WA—H5A2 | 104.6 |
C14—C13—C12 | 121.0 (5) | H5B1—O5WB—H5B2 | 101.6 |
C14—C13—H14 | 119.5 |
Symmetry code: (i) x, y, z−1. |
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1A···O11 | 0.93 | 1.77 | 2.671 (5) | 162 |
O1—H1B···O2A | 0.88 | 1.95 | 2.78 (2) | 159 |
O3A—H1···O1Wii | 0.88 | 1.78 | 2.650 (10) | 170 |
O13—H13···O2Aiii | 0.97 | 1.86 | 2.81 (2) | 166 |
O1W—H1AW···O12 | 0.97 | 1.85 | 2.810 (7) | 168 |
O1W—H1BW···O1Wiv | 0.89 | 2.33 | 2.833 (8) | 116 |
O2W—H2AW···O11 | 0.88 | 1.99 | 2.851 (11) | 167 |
O2W—H2BW···O2A | 0.89 | 2.04 | 2.90 (2) | 162 |
O3W—H3AW···O12 | 0.91 | 1.92 | 2.824 (10) | 168 |
O3W—H3BW···O5WAv | 0.90 | 1.94 | 2.589 (16) | 127 |
O3W—H3BW···O5WB | 0.90 | 1.98 | 2.87 (3) | 168 |
O4W—H4AW···O5WAv | 0.93 | 2.05 | 2.66 (2) | 122 |
O4W—H4AW···O3W | 0.93 | 2.39 | 3.284 (17) | 161 |
O4W—H4BW···O2W | 0.89 | 1.82 | 2.569 (18) | 140 |
O5WA—H5A1···O13vi | 0.88 | 2.13 | 2.851 (13) | 138 |
O5WA—H5A2···O3A | 0.84 | 1.91 | 2.754 (14) | 176 |
O5WB—H5B2···O1Wiv | 0.89 | 2.16 | 2.955 (17) | 148 |
Symmetry codes: (ii) −x+1, −y+1, −z+1; (iii) −x+1, −y, −z+1; (iv) −x+1, −y+1, −z+2; (v) x, y, z+1; (vi) x−1, y, z−1. |
Experimental details
Crystal data | |
Chemical formula | [Co(C7H5O3)(C12H8N2)2(H2O)](C7H5O3)·5H2O |
Mr | 801.65 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 295 |
a, b, c (Å) | 12.3404 (12), 12.6844 (16), 13.561 (2) |
α, β, γ (°) | 101.507 (5), 101.781 (4), 111.823 (7) |
V (Å3) | 1838.4 (4) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 0.54 |
Crystal size (mm) | 0.32 × 0.28 × 0.20 |
Data collection | |
Diffractometer | Rigaku R-AXIS RAPID IP diffractometer |
Absorption correction | Multi-scan (ABSCOR; Higashi, 1995) |
Tmin, Tmax | 0.850, 0.905 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 11865, 6450, 4935 |
Rint | 0.050 |
(sin θ/λ)max (Å−1) | 0.599 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.070, 0.247, 1.02 |
No. of reflections | 6450 |
No. of parameters | 577 |
No. of restraints | 4 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.42, −0.69 |
Computer programs: PROCESS-AUTO (Rigaku, 1998), CrystalStructure (Rigaku/MSC, 2002), SIR92 (Altomare et al., 1993), SHELXL97 (Sheldrick, 2008), ORTEP-3 for Windows (Farrugia, 1997), WinGX (Farrugia, 1999).
Co—O1 | 2.107 (3) | Co—N2 | 2.153 (3) |
Co—O1A | 2.116 (14) | Co—N3 | 2.155 (4) |
Co—O1B | 2.05 (2) | Co—N4 | 2.185 (3) |
Co—N1 | 2.154 (4) |
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1A···O11 | 0.93 | 1.77 | 2.671 (5) | 162 |
O1—H1B···O2A | 0.88 | 1.95 | 2.78 (2) | 159 |
O3A—H1···O1Wi | 0.88 | 1.78 | 2.650 (10) | 170 |
O13—H13···O2Aii | 0.97 | 1.86 | 2.81 (2) | 166 |
O1W—H1AW···O12 | 0.97 | 1.85 | 2.810 (7) | 168 |
O1W—H1BW···O1Wiii | 0.89 | 2.33 | 2.833 (8) | 116 |
O2W—H2AW···O11 | 0.88 | 1.99 | 2.851 (11) | 167 |
O2W—H2BW···O2A | 0.89 | 2.04 | 2.90 (2) | 162 |
O3W—H3AW···O12 | 0.91 | 1.92 | 2.824 (10) | 168 |
O3W—H3BW···O5WAiv | 0.90 | 1.94 | 2.589 (16) | 127 |
O3W—H3BW···O5WB | 0.90 | 1.98 | 2.87 (3) | 168 |
O4W—H4AW···O5WAiv | 0.93 | 2.05 | 2.66 (2) | 122 |
O4W—H4AW···O3W | 0.93 | 2.39 | 3.284 (17) | 161 |
O4W—H4BW···O2W | 0.89 | 1.82 | 2.569 (18) | 140 |
O5WA—H5A1···O13v | 0.88 | 2.13 | 2.851 (13) | 138 |
O5WA—H5A2···O3A | 0.84 | 1.91 | 2.754 (14) | 176 |
O5WB—H5B2···O1Wiii | 0.89 | 2.16 | 2.955 (17) | 148 |
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) −x+1, −y, −z+1; (iii) −x+1, −y+1, −z+2; (iv) x, y, z+1; (v) x−1, y, z−1. |
Acknowledgements
This work was supported by the ZIJIN project of Zhejiang University, China.
References
Altomare, A., Cascarano, G., Giacovazzo, C. & Guagliardi, A. (1993). J. Appl. Cryst. 26, 343–350. CrossRef Web of Science IUCr Journals Google Scholar
Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565. CrossRef IUCr Journals Google Scholar
Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837–838. CrossRef CAS IUCr Journals Google Scholar
Higashi, T. (1995). ABSCOR. Rigaku Corporation, Tokyo, Japan. Google Scholar
Hu, M.-L., Xu, D.-J. & Cheng, D.-P. (2002). J. Coord. Chem. 55, 11–16. Web of Science CSD CrossRef CAS Google Scholar
Li, H., Yin, K.-L. & Xu, D.-J. (2005). Acta Cryst. C61, m19–m21. Web of Science CSD CrossRef CAS IUCr Journals Google Scholar
Pan, T.-T., Su, J.-R. & Xu, D.-J. (2006). Acta Cryst. E62, m1403–m1404. Web of Science CSD CrossRef IUCr Journals Google Scholar
Rigaku (1998). PROCESS-AUTO. Rigaku Corporation, Tokyo, Japan. Google Scholar
Rigaku/MSC (2002). CrystalStructure. Version 3.00. Rigaku/MSC, The Woodlands, Texas, USA. Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Su, J.-R., Zhang, L. & Xu, D.-J. (2005). Acta Cryst. E61, m939–m941. Web of Science CSD CrossRef IUCr Journals Google Scholar
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As part of our ongoing investigation on the nature of aromatic stacking in crystals of metal complexes (Hu et al., 2002; Li et al., 2005), the title compound has been prepared and its crystal structure is presented here.
The crystal consists of CoII complex cations, uncoordinated 3-hydroxybenzoate (HBA) anions and lattice water molecules. The CoII ion is coordinated by two 1,10-phenanthroline (phen), one water molecule and one HBA anion in a distorted octahedral geometry (Fig. 1 and Table 1). This is similar to that found in aqua(4-hydroxybenzoato)bis(phenanthroline)manganese(II) 4-hydroxybenzoate monohydrate (Su et al., 2005) and in aqua(3-hydroxybenzoato)bis(1,10-phenanthroline)manganese(II) 3-hydroxybenzoate (Pan et al., 2006). Within the molecule two phen ligands are nearly perpendicular to each other, the dihedral angle being 78.68 (18)°. The uncoordinated HBA anion links with the complex cation via O—H···O hydrogen bonding (Table 2).
π-π stacking is observed in the crystal structure (Fig. 2 and 3). The face-to-face separation between parallel N1-phen and N1A-phen rings is 3.454 (19) Å [symmetry code: (A) 1 - x,-y,-z]; face-to-face separation between parallel N3-phen and N3B-phen rings is 3.435 (7) Å [symmetry code: (B) 2 - x,1 - y,1 - z]. The extensive hydrogen bonding network (Table 2) helps to stabilize the crystal structure.