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In the title compound, {[Co(C14H8N2O5)(C10H8N2)]·3H2O}n, the CoII cation is five-coordinated with a slightly distorted trigonal–bipyramidal geometry, and the 5-isonicotinamido­isophthalate ligands link CoII atoms into a layered structure. These two-dimensional arrays are further pillared by rod-like 4,4′-bipyridine ligands to give a three-dimensional framework with pcu (primitive cubic) topology. The magnetic and adsorption properties of the title compound are also discussed.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270112030582/bg3154sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270112030582/bg3154Isup2.hkl
Contains datablock I

CCDC reference: 871316

Comment top

In recent years, metal–organic frameworks (MOFs) with carboxylate-containing ligands have been extensively studied because the carboxylate groups can have varied coordination modes resulting in the formation of different structures. MOFs show intriguing architectures and topologies, and have potential applications in catalysis, luminescence, ion exchange, magnetic materials and gas absorption (Férey et al., 2005; Banerjee et al., 2008; Chen et al., 2007). Furthermore, mixed ligands with N-donor groups acting as ancillary connectors are another group of effective building units to construct novel coordination polymers, because they have strong coordination affinity and can satisfy the geometric need of metal centres. Therefore, many reports show a boom in the exploratory synthesis and construction of porous frameworks to establish systems for selective gas sorption by long spacer ligands (Li et al., 2010; Zang et al., 2011). In the present case, in order to further investigate the influence of organic ligands on the coordination architectures and related properties, reactions with 5-(isonicotinamido)isophthalic acid (H2INAIP) and 4,4'-bipyridine [bpy?] N-donor bridging ligands were carried out. We report on the synthesis, crystal structure and properties of a new coordination polymer obtained through solvothermal reaction, namely {[Co(INAIP)(4,4'-bipy)].3H2O}n, (I).

The results of the structure analysis revealed that (I) exhibits a novel three-dimensional non-interpenetrated pillared framework. It is entirely different from the two-dimensional bilayer complex [Co(INAIP)(4,4'-bipy)0.5]n, (II) (Chen et al., 2010), which was obtained by hydrothermal synthesis with a similar source; therefore, the different structures of (I) and (II) showed that the reaction conditions play a crucial role in their formation. The asymmetric unit of (I) contains one unique CoII atom, one INAIP2- ligand, one 4,4'-bipy ligand and three free water molecules (Fig. 1); however, there is only half a 4,4'-bipy molecule in complex (I). In (I), the Co1 atom has an N2O3 coordination environment and a distorted square-pyramidal coordination geometry. The Co—N bond lengths are 2.010 (2) and 2.027 (2) Å, and the Co—O distances are in the range 1.9450 (18)–2.2546 (19) Å. Each INAIP2- ligand connects three CoII atoms via its two carboxylate groups (a weak Co1···O2 interaction of 2.571 Å has been omitted) and the pyridine ring of the ligand is free of coordination; however, in (II), the pyridine is connected to the central CoII atom.

It is noteworthy that the two carboxylate groups of the INAIP2- ligand have different coordination modes in (I), one is µ1-η1:η0-monodentate and the other is µ2-η1:η1-bridging. The bridging carboxylate group links two metal atoms to give a {Co(OCO)}2 unit, and the dimeric {Co(OCO)}2 units are linked together by the monodentate carboxylate groups to form a two-dimensional layered structure (see Fig. S1 in the Supplementary materials). The two-dimensional networks are further pillared by rod-like 4,4'-bipy ligands to form a three-dimensional architecture (Fig. 2a). The resultant three-dimensional framework contains channels along the a axis (Fig. 2b). The cavities of the framework are occupied by water molecules. After omitting the solvent molecules, a PLATON (Spek, 2009) analysis revealed that the three-dimensional porous structure has large voids of 453.0 Å in diameter which represent 18.5% of the unit-cell volume. To further understand this three-dimensional structure of (I), the dimeric {Co(OCO)}2 units are considered as the nodes, and the topology of (I), calculated by TOPOS (Blatov, 2006), is a uniform 6-connected three-dimensional pcu net.

The magnetic susceptibilities were measured on a crystalline sample of (I) in the temperature range 1.8–300 K under 2 kOe using a SQUID magnetometer. At room temperature, the observed χMT value is 4.81 emu K mol-1, which is larger than the expected value of 3.75 emu K mol-1 corresponding to the binuclear CoII (S = 3/2) ion (Fig. 3). Upon cooling from 300 to 100 K, the values of χMT decrease slowly and then rapidly reach a value of 3.37 emu K mol-1 at 1.8 K. The χM versus T plot follows the Curie–Weiss law with C = 5.01 emu K mol-1 and Θ = -5.12 K. The negative Θ value suggests that there is a weak antiferromagnetic interaction among the CoII atoms transferred through the INAIP2- ligands.

To verify whether the framework of (I) can be sustained after removal of the solvent molecules, powder X-ray diffraction (PXRD) patterns were measured. The framework of (I) still has good crystallinity without solvent molecules (Fig. 4a). The results show that (I) has permanent porosity in the absence of free water molecules, and thus gas sorption was investigated. The N2 and CO2 adsorption isotherms for (I) are shown in Fig. 4(b). The results indicate that no N2 uptake was observed at 273 K, and the hysteresis behaviour is characteristic for type H3 (Liu et al., 2008; Cheon & Suh, 2008). In contrast, it was found that significant amounts of CO2 (273 K) were adsorbed and the isotherms present typical type-I curves, which is the characteristic of a microporous material. The CO2 uptake increases abruptly at the beginning and reaches 46.8 cm3 (STP)/g approximately 0.45 CO2 molecules per formula unit were adsorbed, indicating a uniform microporous structure. The gas sorption isotherms show a small hysteresis between the adsorption–desorption curves. Therefore, the selective sorption of CO2 rather than N2 gas can also be attributed to the significant quadrupole moment of CO2 (-1.4 × 10 -39 C m2). Also the small difference of the kinetic diameters (3.64 Å of N2 and 3.3 Å of CO2) may induce specific interactions with the host framework to open up the channels, because of the favourable interactions between adsorbed CO2 molecules and the Lewis basic amide functionalities decorating the pores (Chen et al., 2011; Vogiatzis, et al., 2009).

Related literature top

For related literature, see: Banerjee et al. (2008); Blatov (2006); Chen et al. (2007, 2010, 2011); Cheon & Suh (2008); Férey et al. (2005); Li et al. (2010); Liu et al. (2008); Spek (2009); Vogiatzis et al. (2009); Zang et al. (2011).

Experimental top

All reagents and solvents were used as obtained commercially without further purification. A mixture of H2INAIP (0.029 g, 0.1 mmol), CoCl2.6H2O (0.024 g, 0.1 mmol), 4,4'-bipy (0.008 g, 0.05 mmol), N,N'-dimethylformamide (DMF, 6 ml) and EtOH (6 ml) was placed in a Teflon-lined stainless steel vessel, heated to 403 K for 3 d, and then cooled to room temperature over a period of 24 h. Red block-shaped crystals of (I) were obtained (yield of 31%). IR (KBr pellet, cm-1): 3422 (s), 2841 (w), 1627 (w), 1607 (s), 1518 (m), 1417 (m), 1386 (s), 1364 (m), 1288 (w), 789 (w), 742 (w), 721 (m), 585 (w).

Refinement top

H atoms bonded to C or N atoms were placed geometrically and treated as riding, with C—H = 0.93 Å or N—H = 0.86 Å, and with Uiso(H) = 1.2Ueq(C,N). The H atoms of the water molecules were placed so as to form a reasonable hydrogen-bond network, with O—H distances of 0.85 Å, and were refined as riding, with Uiso(H) = 1.2Ueq(O).

Computing details top

Data collection: SMART (Bruker, 2001); cell refinement: SAINT (Bruker, 2003); data reduction: SAINT (Bruker, 2003); program(s) used to solve structure: SHELXTL (Sheldrick, 2008); program(s) used to refine structure: SHELXTL (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. The structure of (I), with displacement ellipsoids drawn at the 30% probability level. [Symmetry codes: (i) -x+1, y-1/2, -z+3/2; (ii) x+1, y, z; (iii) x, -y+3/2, z+1/2.]
[Figure 2] Fig. 2. View of the the porous framework of (I) along the (a) b and (b) a axes. [check added text]
[Figure 3] Fig. 3. The temperature dependence of the magnetic susceptibility of (I).
[Figure 4] Fig. 4. (a) The powder X-ray diffraction patterns of complex (I) and (b) the N2 and CO2 adsorption isotherm (273 K) of (I). Key: square and triangle curves represent N2 and CO2 adsorption, filled shapes represent adsorption and open shapes represent desorption.
Poly[[(µ2-4,4'-bipyridine)(µ3-5-isonicotinamidoisophthalato)cobalt(II)] trihydrate] top
Crystal data top
[Co(C14H8N2O5)(C10H8N2)]·3H2OF(000) = 1140
Mr = 553.39Dx = 1.501 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 3735 reflections
a = 11.1247 (11) Åθ = 2.1–24.7°
b = 13.8704 (14) ŵ = 0.76 mm1
c = 16.0515 (19) ÅT = 293 K
β = 98.621 (2)°Block, red
V = 2448.8 (5) Å30.18 × 0.14 × 0.10 mm
Z = 4
Data collection top
Bruker SMART APEX CCD
diffractometer
4790 independent reflections
Radiation source: fine-focus sealed tube3743 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.068
ϕ and ω scansθmax = 26.0°, θmin = 2.0°
Absorption correction: multi-scan
(SADABS; Bruker, 2003)
h = 1313
Tmin = 0.876, Tmax = 0.928k = 1716
12940 measured reflectionsl = 919
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)] = 0.046Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.111H-atom parameters constrained
S = 1.01 w = 1/[σ2(Fo2) + (0.0489P)2]
where P = (Fo2 + 2Fc2)/3
4790 reflections(Δ/σ)max < 0.001
334 parametersΔρmax = 0.54 e Å3
0 restraintsΔρmin = 0.48 e Å3
Crystal data top
[Co(C14H8N2O5)(C10H8N2)]·3H2OV = 2448.8 (5) Å3
Mr = 553.39Z = 4
Monoclinic, P21/cMo Kα radiation
a = 11.1247 (11) ŵ = 0.76 mm1
b = 13.8704 (14) ÅT = 293 K
c = 16.0515 (19) Å0.18 × 0.14 × 0.10 mm
β = 98.621 (2)°
Data collection top
Bruker SMART APEX CCD
diffractometer
4790 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2003)
3743 reflections with I > 2σ(I)
Tmin = 0.876, Tmax = 0.928Rint = 0.068
12940 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0460 restraints
wR(F2) = 0.111H-atom parameters constrained
S = 1.01Δρmax = 0.54 e Å3
4790 reflectionsΔρmin = 0.48 e Å3
334 parameters
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
C180.0439 (3)0.4998 (2)0.8764 (2)0.0320 (7)
C10.6545 (3)0.57619 (19)0.51747 (18)0.0270 (6)
C20.6187 (3)0.5353 (2)0.58839 (18)0.0301 (7)
H20.63500.47060.60040.036*
C30.5589 (2)0.59009 (19)0.64180 (17)0.0256 (6)
C40.5326 (2)0.68525 (19)0.62320 (17)0.0262 (6)
H40.49430.72260.65950.031*
C50.5635 (2)0.72545 (18)0.55029 (17)0.0238 (6)
C60.6251 (2)0.67154 (19)0.49713 (18)0.0269 (6)
H60.64630.69900.44850.032*
C70.5268 (3)0.5436 (2)0.72019 (19)0.0288 (7)
C80.5301 (2)0.82925 (19)0.52935 (18)0.0239 (6)
C90.7999 (3)0.5436 (2)0.4188 (2)0.0356 (7)
C100.8589 (3)0.4634 (2)0.37781 (19)0.0316 (7)
C110.9835 (3)0.4634 (2)0.3780 (2)0.0416 (8)
H111.03230.51140.40580.050*
C121.0333 (3)0.3899 (3)0.3358 (2)0.0496 (9)
H121.11720.38920.33720.060*
C130.8486 (3)0.3218 (2)0.2930 (2)0.0413 (8)
H130.80140.27450.26290.050*
C140.7906 (3)0.3908 (2)0.3353 (2)0.0377 (8)
H140.70700.38810.33500.045*
C150.2714 (3)0.4336 (2)0.8364 (2)0.0370 (8)
H150.30890.38470.81000.044*
C160.1477 (3)0.4281 (2)0.8363 (2)0.0373 (8)
H160.10370.37600.81110.045*
C170.0888 (3)0.5013 (2)0.8741 (2)0.0308 (7)
C190.1115 (3)0.4156 (2)0.8683 (2)0.0442 (9)
H190.07390.35710.86040.053*
C200.2351 (3)0.4184 (2)0.8719 (2)0.0405 (8)
H200.27840.36080.86710.049*
C210.2299 (3)0.5814 (2)0.8892 (2)0.0430 (9)
H210.26990.63910.89600.052*
C220.1066 (3)0.5839 (2)0.8871 (2)0.0445 (9)
H220.06530.64230.89300.053*
C230.1603 (2)0.5768 (2)0.90939 (19)0.0324 (7)
H230.12490.62780.93440.039*
C240.2838 (2)0.5764 (2)0.90759 (19)0.0318 (7)
H240.32960.62800.93200.038*
Co10.52257 (3)0.50479 (2)0.87893 (2)0.01609 (12)
N10.9683 (3)0.31979 (19)0.29307 (18)0.0452 (7)
N20.7194 (2)0.51615 (16)0.46842 (16)0.0336 (6)
H2A0.70550.45530.47070.040*
N30.3408 (2)0.50620 (16)0.87285 (15)0.0280 (6)
N40.2948 (2)0.49992 (16)0.88181 (16)0.0294 (6)
O10.51457 (17)0.59900 (13)0.78187 (12)0.0279 (5)
O20.5158 (2)0.45483 (15)0.72408 (13)0.0440 (6)
O30.47330 (16)0.87209 (13)0.58160 (12)0.0276 (5)
O40.55740 (18)0.86566 (14)0.46395 (12)0.0325 (5)
O50.8257 (2)0.62762 (16)0.40703 (17)0.0615 (8)
O1W0.7424 (2)0.32033 (16)0.54060 (17)0.0674 (8)
H1X0.81440.31590.56680.081*
H1Y0.69340.30950.57540.081*
O2W0.0317 (2)0.69965 (18)0.35282 (18)0.0727 (8)
H2X0.03720.68150.36370.087*
H2Y0.02090.73450.30880.087*
O3W0.6047 (2)0.28045 (16)0.67452 (16)0.0585 (7)
H3X0.56670.23170.68920.070*
H3Y0.57310.33110.69180.070*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C180.0225 (16)0.0339 (17)0.0411 (19)0.0001 (13)0.0091 (13)0.0013 (14)
C10.0279 (16)0.0249 (15)0.0304 (17)0.0026 (12)0.0115 (13)0.0007 (13)
C20.0377 (18)0.0226 (14)0.0319 (17)0.0023 (13)0.0115 (14)0.0048 (13)
C30.0275 (15)0.0252 (15)0.0255 (16)0.0005 (12)0.0079 (13)0.0017 (12)
C40.0279 (16)0.0270 (15)0.0255 (16)0.0026 (12)0.0096 (13)0.0025 (12)
C50.0229 (15)0.0233 (14)0.0258 (16)0.0013 (11)0.0059 (12)0.0004 (12)
C60.0305 (16)0.0271 (15)0.0248 (16)0.0044 (12)0.0097 (13)0.0023 (12)
C70.0264 (16)0.0309 (16)0.0305 (18)0.0023 (13)0.0088 (13)0.0033 (14)
C80.0207 (14)0.0261 (15)0.0259 (15)0.0009 (11)0.0062 (12)0.0014 (13)
C90.0400 (19)0.0315 (17)0.039 (2)0.0022 (14)0.0192 (16)0.0014 (15)
C100.0343 (17)0.0312 (16)0.0321 (18)0.0048 (13)0.0145 (14)0.0019 (14)
C110.0341 (18)0.0429 (18)0.049 (2)0.0012 (15)0.0107 (16)0.0062 (17)
C120.0309 (19)0.056 (2)0.064 (2)0.0089 (16)0.0160 (17)0.011 (2)
C130.040 (2)0.0381 (18)0.046 (2)0.0045 (15)0.0082 (16)0.0044 (16)
C140.0303 (17)0.0410 (18)0.044 (2)0.0059 (14)0.0132 (15)0.0015 (16)
C150.0264 (17)0.0402 (18)0.045 (2)0.0013 (14)0.0064 (15)0.0109 (16)
C160.0219 (16)0.0363 (18)0.054 (2)0.0035 (13)0.0066 (15)0.0148 (16)
C170.0220 (15)0.0339 (17)0.0373 (18)0.0004 (13)0.0073 (13)0.0047 (14)
C190.0245 (17)0.0316 (17)0.080 (3)0.0007 (13)0.0176 (17)0.0140 (18)
C200.0269 (17)0.0283 (17)0.068 (2)0.0040 (13)0.0137 (16)0.0114 (16)
C210.0288 (17)0.0275 (17)0.075 (3)0.0011 (13)0.0166 (17)0.0009 (17)
C220.0239 (17)0.0296 (17)0.082 (3)0.0050 (13)0.0151 (17)0.0022 (18)
C230.0226 (15)0.0322 (16)0.0439 (19)0.0013 (12)0.0098 (14)0.0070 (15)
C240.0224 (15)0.0303 (16)0.0423 (19)0.0003 (12)0.0033 (14)0.0028 (15)
Co10.01091 (18)0.01686 (19)0.0217 (2)0.00063 (14)0.00622 (14)0.00475 (15)
N10.0419 (17)0.0437 (16)0.0524 (19)0.0075 (13)0.0155 (14)0.0113 (15)
N20.0407 (15)0.0241 (13)0.0401 (15)0.0019 (11)0.0197 (13)0.0038 (11)
N30.0166 (12)0.0339 (14)0.0345 (14)0.0001 (10)0.0076 (10)0.0046 (12)
N40.0166 (11)0.0302 (13)0.0430 (15)0.0003 (10)0.0099 (11)0.0026 (11)
O10.0335 (11)0.0290 (10)0.0237 (11)0.0031 (9)0.0120 (9)0.0068 (9)
O20.0687 (17)0.0254 (11)0.0424 (14)0.0013 (11)0.0232 (12)0.0062 (10)
O30.0267 (11)0.0235 (10)0.0352 (12)0.0013 (8)0.0132 (9)0.0023 (9)
O40.0389 (12)0.0289 (11)0.0328 (12)0.0079 (9)0.0151 (10)0.0088 (10)
O50.0731 (18)0.0319 (13)0.093 (2)0.0012 (12)0.0570 (16)0.0013 (14)
O1W0.0663 (18)0.0476 (15)0.092 (2)0.0089 (13)0.0239 (16)0.0166 (15)
O2W0.0582 (18)0.0686 (18)0.095 (2)0.0068 (14)0.0243 (16)0.0322 (17)
O3W0.0556 (16)0.0348 (13)0.089 (2)0.0014 (11)0.0226 (15)0.0042 (13)
Geometric parameters (Å, º) top
C18—C221.382 (4)C15—C161.378 (4)
C18—C191.385 (4)C15—H150.9300
C18—C171.483 (4)C16—C171.395 (4)
C1—C21.382 (4)C16—H160.9300
C1—C61.389 (4)C17—C231.383 (4)
C1—N21.416 (3)C19—C201.385 (4)
C2—C31.388 (4)C19—H190.9300
C2—H20.9300C20—N41.333 (3)
C3—C41.375 (4)C20—H200.9300
C3—C71.503 (4)C21—N41.337 (3)
C4—C51.385 (4)C21—C221.377 (4)
C4—H40.9300C21—H210.9300
C5—C61.390 (4)C22—H220.9300
C5—C81.512 (4)C23—C241.378 (4)
C6—H60.9300C23—H230.9300
C7—O21.241 (4)C24—N31.329 (3)
C7—O11.276 (3)C24—H240.9300
C8—O41.243 (3)Co1—O3i1.9450 (18)
C8—O31.271 (3)Co1—N32.010 (2)
C9—O51.221 (4)Co1—O12.0250 (18)
C9—N21.340 (4)Co1—N4ii2.027 (2)
C9—C101.495 (4)Co1—O4iii2.2546 (19)
C10—C141.379 (4)N2—H2A0.8600
C10—C111.385 (4)N4—Co1iv2.027 (2)
C11—C121.386 (4)O3—Co1v1.9450 (18)
C11—H110.9300O4—Co1vi2.2546 (19)
C12—N11.337 (4)O1W—H1X0.8501
C12—H120.9300O1W—H1Y0.8499
C13—N11.332 (4)O2W—H2X0.8500
C13—C141.387 (4)O2W—H2Y0.8501
C13—H130.9300O3W—H3X0.8500
C14—H140.9300O3W—H3Y0.8500
C15—N31.348 (3)
C22—C18—C19116.5 (3)C15—C16—H16120.2
C22—C18—C17121.0 (3)C17—C16—H16120.2
C19—C18—C17122.5 (3)C23—C17—C16116.8 (3)
C2—C1—C6119.8 (3)C23—C17—C18120.9 (3)
C2—C1—N2116.8 (2)C16—C17—C18122.3 (3)
C6—C1—N2123.4 (3)C18—C19—C20120.0 (3)
C1—C2—C3120.5 (3)C18—C19—H19120.0
C1—C2—H2119.7C20—C19—H19120.0
C3—C2—H2119.7N4—C20—C19123.0 (3)
C4—C3—C2119.8 (3)N4—C20—H20118.5
C4—C3—C7121.6 (3)C19—C20—H20118.5
C2—C3—C7118.6 (2)N4—C21—C22123.0 (3)
C3—C4—C5119.9 (3)N4—C21—H21118.5
C3—C4—H4120.0C22—C21—H21118.5
C5—C4—H4120.0C21—C22—C18120.4 (3)
C4—C5—C6120.6 (2)C21—C22—H22119.8
C4—C5—C8119.2 (2)C18—C22—H22119.8
C6—C5—C8120.2 (2)C24—C23—C17120.1 (3)
C1—C6—C5119.2 (3)C24—C23—H23119.9
C1—C6—H6120.4C17—C23—H23119.9
C5—C6—H6120.4N3—C24—C23123.5 (3)
O2—C7—O1122.4 (3)N3—C24—H24118.3
O2—C7—C3120.3 (3)C23—C24—H24118.3
O1—C7—C3117.2 (2)O3i—Co1—N389.97 (8)
O4—C8—O3125.2 (3)O3i—Co1—O1149.03 (8)
O4—C8—C5119.4 (2)N3—Co1—O191.64 (8)
O3—C8—C5115.4 (2)O3i—Co1—N4ii89.22 (8)
O5—C9—N2123.8 (3)N3—Co1—N4ii178.01 (10)
O5—C9—C10120.9 (3)O1—Co1—N4ii88.13 (9)
N2—C9—C10115.3 (3)O3i—Co1—O4iii124.30 (8)
C14—C10—C11118.6 (3)N3—Co1—O4iii95.85 (8)
C14—C10—C9121.1 (3)O1—Co1—O4iii86.28 (8)
C11—C10—C9120.3 (3)N4ii—Co1—O4iii86.10 (9)
C10—C11—C12118.2 (3)C13—N1—C12116.7 (3)
C10—C11—H11120.9C9—N2—C1127.2 (2)
C12—C11—H11120.9C9—N2—H2A116.4
N1—C12—C11124.1 (3)C1—N2—H2A116.4
N1—C12—H12118.0C24—N3—C15116.8 (3)
C11—C12—H12118.0C24—N3—Co1121.77 (19)
N1—C13—C14123.5 (3)C15—N3—Co1121.3 (2)
N1—C13—H13118.2C20—N4—C21117.1 (3)
C14—C13—H13118.2C20—N4—Co1iv122.77 (19)
C10—C14—C13118.9 (3)C21—N4—Co1iv120.0 (2)
C10—C14—H14120.5C7—O1—Co1102.19 (17)
C13—C14—H14120.5C8—O3—Co1v131.90 (18)
N3—C15—C16123.2 (3)C8—O4—Co1vi142.51 (18)
N3—C15—H15118.4H1X—O1W—H1Y108.1
C16—C15—H15118.4H2X—O2W—H2Y108.7
C15—C16—C17119.5 (3)H3X—O3W—H3Y108.6
C6—C1—C2—C33.2 (4)C17—C18—C19—C20179.3 (3)
N2—C1—C2—C3177.5 (3)C18—C19—C20—N41.0 (6)
C1—C2—C3—C41.3 (4)N4—C21—C22—C180.5 (6)
C1—C2—C3—C7177.3 (3)C19—C18—C22—C210.1 (5)
C2—C3—C4—C51.5 (4)C17—C18—C22—C21180.0 (3)
C7—C3—C4—C5179.9 (2)C16—C17—C23—C241.2 (4)
C3—C4—C5—C62.5 (4)C18—C17—C23—C24179.2 (3)
C3—C4—C5—C8177.9 (2)C17—C23—C24—N30.2 (5)
C2—C1—C6—C52.2 (4)C14—C13—N1—C121.1 (5)
N2—C1—C6—C5178.5 (3)C11—C12—N1—C130.8 (5)
C4—C5—C6—C10.7 (4)O5—C9—N2—C12.6 (6)
C8—C5—C6—C1179.8 (2)C10—C9—N2—C1177.1 (3)
C4—C3—C7—O2157.8 (3)C2—C1—N2—C9153.1 (3)
C2—C3—C7—O223.6 (4)C6—C1—N2—C927.6 (5)
C4—C3—C7—O123.9 (4)C23—C24—N3—C151.4 (4)
C2—C3—C7—O1154.7 (3)C23—C24—N3—Co1175.8 (2)
C4—C5—C8—O4179.9 (3)C16—C15—N3—C242.1 (4)
C6—C5—C8—O40.5 (4)C16—C15—N3—Co1175.1 (2)
C4—C5—C8—O30.9 (4)O1—Co1—N3—C2481.0 (2)
C6—C5—C8—O3179.6 (3)O4iii—Co1—N3—C245.5 (2)
O5—C9—C10—C14130.7 (4)O3i—Co1—N3—C1547.1 (2)
N2—C9—C10—C1449.6 (4)O1—Co1—N3—C15102.0 (2)
O5—C9—C10—C1145.8 (5)O4iii—Co1—N3—C15171.6 (2)
N2—C9—C10—C11133.9 (3)C19—C20—N4—C210.6 (5)
C14—C10—C11—C120.4 (5)C19—C20—N4—Co1iv175.7 (3)
C9—C10—C11—C12177.0 (3)C22—C21—N4—C200.2 (5)
C10—C11—C12—N11.5 (5)C22—C21—N4—Co1iv176.5 (3)
C11—C10—C14—C131.3 (5)O2—C7—O1—Co114.4 (3)
C9—C10—C14—C13175.2 (3)C3—C7—O1—Co1163.9 (2)
N1—C13—C14—C102.2 (5)O3i—Co1—O1—C78.3 (3)
N3—C15—C16—C171.1 (5)N3—Co1—O1—C7100.93 (18)
C15—C16—C17—C230.6 (5)N4ii—Co1—O1—C777.09 (18)
C15—C16—C17—C18179.8 (3)O4iii—Co1—O1—C7163.31 (18)
C22—C18—C17—C2321.8 (5)O4—C8—O3—Co1v36.2 (4)
C19—C18—C17—C23158.1 (3)C5—C8—O3—Co1v144.80 (19)
C22—C18—C17—C16157.8 (3)O3—C8—O4—Co1vi11.4 (5)
C19—C18—C17—C1622.3 (5)C5—C8—O4—Co1vi167.6 (2)
C22—C18—C19—C200.6 (5)
Symmetry codes: (i) x+1, y1/2, z+3/2; (ii) x+1, y, z; (iii) x, y+3/2, z+1/2; (iv) x1, y, z; (v) x+1, y+1/2, z+3/2; (vi) x, y+3/2, z1/2.

Experimental details

Crystal data
Chemical formula[Co(C14H8N2O5)(C10H8N2)]·3H2O
Mr553.39
Crystal system, space groupMonoclinic, P21/c
Temperature (K)293
a, b, c (Å)11.1247 (11), 13.8704 (14), 16.0515 (19)
β (°) 98.621 (2)
V3)2448.8 (5)
Z4
Radiation typeMo Kα
µ (mm1)0.76
Crystal size (mm)0.18 × 0.14 × 0.10
Data collection
DiffractometerBruker SMART APEX CCD
diffractometer
Absorption correctionMulti-scan
(SADABS; Bruker, 2003)
Tmin, Tmax0.876, 0.928
No. of measured, independent and
observed [I > 2σ(I)] reflections
12940, 4790, 3743
Rint0.068
(sin θ/λ)max1)0.617
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.046, 0.111, 1.01
No. of reflections4790
No. of parameters334
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.54, 0.48

Computer programs: SMART (Bruker, 2001), SAINT (Bruker, 2003), SHELXTL (Sheldrick, 2008).

Selected bond lengths (Å) top
Co1—O3i1.9450 (18)Co1—N4ii2.027 (2)
Co1—N32.010 (2)Co1—O4iii2.2546 (19)
Co1—O12.0250 (18)
Symmetry codes: (i) x+1, y1/2, z+3/2; (ii) x+1, y, z; (iii) x, y+3/2, z+1/2.
 

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