metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890
Volume 67| Part 11| November 2011| Pages m1574-m1575

Poly[[tetra­aqua­tetra­kis­[μ3-5-(pyridine-4-carboxamido)­isophthalato]­cobalt(II)­diholmium(III)] tetra­hydrate]

aKey Laboratory of Functional Organometallic Materials, Hengyang Normal University, Department of Chemistry and Materials Science, Hengyang, Hunan 421008, People's Republic of China
*Correspondence e-mail: cmsniu@163.com

(Received 5 October 2011; accepted 15 October 2011; online 22 October 2011)

In the centrosymmetric polymeric title compound, {[CoHo2(C14H8N2O5)4(H2O)4]·4H2O}n, the HoIII ion is coordinated by one water mol­ecule and four 5-(pyridine-4-carboxamido)­isophthalate (L) ligands in a distorted square-anti­prismatic arrangement. The CoII ion, located on an inversion center, is coordinated by two pyridine N atoms, two carboxyl­ate O atoms and two water mol­ecules in a distorted octa­hedral geometry. One L ligand bridges two Ho ions and one Co ion through two carboxyl­ate groups and one pyridine N atom. The other L ligand bridges two Ho ions and one Co ion through two carboxyl­ate groups, while the uncoordinated pyridine N atom accepts a hydrogen bond from an adjacent coordinated water mol­ecule. Extensive O—H⋯O, N—H⋯O and O—H⋯N hydrogen bonding is present in the crystal.

Related literature

For related hetero-metallic complexes, see: Chen et al. (2011[Chen, M.-S., Zhao, Y., Okamura, T.-A., Su, Z., Sun, W.-Y. & Ueyama, N. (2011). Supramol. Chem. 23, 117-124.]); Deng et al. (2011[Deng, Y.-F., Chen, M.-S., Zhang, C.-H. & Kuang, D.-Z. (2011). Acta Cryst. E67, m1431-m1432.]); Gu & Xue (2006[Gu, X.-J. & Xue, D.-F. (2006). Inorg. Chem. 45, 9257-9261.]); Liang et al. (2000[Liang, Y.-C., Cao, R., Su, W.-P., Hong, M.-C. & Zhang, W.-J. (2000). Angew. Chem. Int. Ed. 39, 3304-3307.]); Prasad et al. (2007[Prasad, T. K., Rajasekharan, M. V. & Costes, J. P. (2007). Angew. Chem. Int. Ed. 46, 2851-2854.]); Zhao et al. (2003[Zhao, B., Cheng, P., Dai, Y., Cheng, C., Liao, D.-Z., Yan, S.-P., Jiang, Z.-H. & Wang, G.-L. (2003). Angew. Chem. Int. Ed. 42, 934-936.], 2004[Zhao, B., Cheng, P., Chen, X.-Y., Cheng, C., Shi, W., Liao, D.-Z., Yan, S.-P. & Jiang, Z.-H. (2004). J. Am. Chem. Soc. 126, 3012-3013.]).

[Scheme 1]

Experimental

Crystal data
  • [CoHo2(C14H8N2O5)4(H2O)4]·4H2O

  • Mr = 1669.81

  • Triclinic, [P \overline 1]

  • a = 10.0597 (9) Å

  • b = 10.7824 (10) Å

  • c = 13.7261 (13) Å

  • α = 79.141 (3)°

  • β = 78.801 (1)°

  • γ = 86.578 (3)°

  • V = 1433.9 (2) Å3

  • Z = 1

  • Mo Kα radiation

  • μ = 3.12 mm−1

  • T = 291 K

  • 0.20 × 0.14 × 0.10 mm

Data collection
  • Bruker APEX CCD diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2001[Bruker (2001). SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.574, Tmax = 0.746

  • 7154 measured reflections

  • 4968 independent reflections

  • 4756 reflections with I > 2σ(I)

  • Rint = 0.070

Refinement
  • R[F2 > 2σ(F2)] = 0.046

  • wR(F2) = 0.123

  • S = 1.06

  • 4968 reflections

  • 430 parameters

  • H-atom parameters constrained

  • Δρmax = 2.89 e Å−3

  • Δρmin = −1.93 e Å−3

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A DA D—H⋯A
O1W—H1WA⋯O4Wi 0.85 2.00 2.761 (8) 149
O1W—H1WB⋯O7ii 0.85 2.26 2.988 (7) 144
O2W—H2WB⋯N2iii 0.85 1.96 2.699 (8) 145
O3W—H3WA⋯O6iv 0.85 2.20 3.048 (8) 177
O3W—H3WB⋯O9v 0.85 2.20 3.054 (8) 177
O4W—H4WA⋯O4i 0.85 1.90 2.732 (8) 164
O4W—H4WB⋯O8vi 0.85 1.94 2.752 (8) 160
N1—H1⋯O3W 0.86 2.16 2.996 (7) 165
N3—H3⋯O3vii 0.86 2.16 2.933 (7) 150
Symmetry codes: (i) -x+1, -y+1, -z; (ii) -x+2, -y+2, -z; (iii) x, y+1, z-1; (iv) x, y-1, z; (v) -x+2, -y+1, -z+1; (vi) x-1, y-1, z; (vii) -x+2, -y+2, -z+1.

Data collection: SMART (Bruker, 2007[Bruker (2007). SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2007[Bruker (2007). SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXTL; molecular graphics: XP in SHELXTL, and DIAMOND (Brandenburg, 1999[Brandenburg, K. (1999). DIAMOND. Crystal Impact GbR, Bonn, Germany.]); software used to prepare material for publication: SHELXTL.

Supporting information


Comment top

The rational synthesis and investigation of 3d-4f or 4d-4f heterometallic complexes are challenge for chemists and have attracted increasing attention in last few years since the competitive reaction containing 3d-4f metal ions in conjunction with ligands often results in the formation of a mixture of homometallic assemblies rather than heterometallic analogous (Gu & Xue, 2006; Liang et al., 2000; Prasad et al., 2007; Zhao et al., 2003, 2004). We have recently prepared a new lanthanide(III)–transition metal(II) coordination polymer, the title compound, under hydrothermal conditions.

In the title compound, the HoIII ion is eight-coordinated by seven O atoms from four pyridine-4-carboxamidoisophthalate (L) ligands and one water molecule, forming a distorted square-antiprismatic geometry (Fig. 1). It is interesting that the carboxylate groups of two unique L ligands exhibit different coordination modes: one coordinates to two HoIII ions and one CoII ion using its two carboxylate groups with µ1-η1:η1-chelate and µ2-η1:η1-bis-monodentate coordination modes while the pyridyl group is free of coordination, the other one coordinates to two HoIII ions through the carboxylate groups with µ1-η1:η1-chelate coordination mode and to one CoII ion through the pyridyl group. Based on the coordination modes of the carboxylate and pyridyl groups, a complicated three-dimensional network is formed (Fig. 2), which is similar to the complex {[LnCo0.5(INAIP)2(H2O)2].2H2O}n (Chen et al. 2011) and a Gd analogue (Deng et al., 2011).

Related literature top

For related hetero-metallic complexes, see: Chen et al. (2011); Deng et al. (2011); Gu & Xue (2006); Liang et al. (2000); Prasad et al. (2007); Zhao et al. (2003, 2004). Supplementary Figure 2 is missing; please supply.

Experimental top

A mixture of Ho(NO3)3.6H2O (22.5 mg, 0.05 mmol), H2L (28.6 mg, 0.1 mmol), Co(OAc)2.4H2O (13.1 mg, 0.05 mmol), NaOH (6.0 mg, 0.15 mmol), MeOH (4 ml) and H2O (6 ml) was heated in a 16 ml capacity Teflon-lined reaction vessel at 433 K for 4 days. The reaction mixture was cooled to room temperature over a period of 40 h. The product was collected by filtration, washed with H2O and air-dried.

Refinement top

H atoms bonded to C and N atoms were placed geometrically and refiined as riding atoms, with C—H = 0.93 and N—H = 0.86 Å and with Uiso(H) = 1.2Ueq(C, N). The water H atoms were found from difference Fourier maps and refined with restraints of O—H = 0.85 Å and with Uiso(H) = 1.2Ueq(O). The highest residual electron density was found at 0.92 Å from Ho1 atom and the deepest hole at 1.06 Å from Ho1 atom.

Computing details top

Data collection: SMART (Bruker, 2007); cell refinement: SAINT (Bruker, 2007); data reduction: SAINT (Bruker, 2007); program(s) used to solve structure: SHELXTL (Sheldrick, 2008); program(s) used to refine structure: SHELXTL (Sheldrick, 2008); molecular graphics: XP in SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 1999); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. The asymmetric unit of the title compound. Displacement ellipsoids are drawn at the 30% probability level. [Symmetry codes: (i) 2-x, 2-y, 1-z; (ii) x, -1+y, -1+z; (iii) 2-x, 1-y, -z; (iv) x, 1+y, z; (v) -1+x, y, z.]
[Figure 2] Fig. 2. A view of the three-dimensional network of the title compound.
Poly[[tetraaquatetrakis[µ3-5-(pyridine-4- carboxamido)isophthalato]cobalt(II)diholmium(III)] tetrahydrate] top
Crystal data top
[CoHo2(C14H8N2O5)4(H2O)4]·4H2OZ = 1
Mr = 1669.81F(000) = 825
Triclinic, P1Dx = 1.934 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 10.0597 (9) ÅCell parameters from 5442 reflections
b = 10.7824 (10) Åθ = 2.7–28.1°
c = 13.7261 (13) ŵ = 3.12 mm1
α = 79.141 (3)°T = 291 K
β = 78.801 (1)°Block, pink
γ = 86.578 (3)°0.20 × 0.14 × 0.10 mm
V = 1433.9 (2) Å3
Data collection top
Bruker APEX CCD
diffractometer
4968 independent reflections
Radiation source: fine-focus sealed tube4756 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.070
ϕ and ω scansθmax = 25.0°, θmin = 1.9°
Absorption correction: multi-scan
(SADABS; Bruker, 2001)
h = 1111
Tmin = 0.574, Tmax = 0.746k = 1210
7154 measured reflectionsl = 1516
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) = 0.123H-atom parameters constrained
S = 1.06 w = 1/[σ2(Fo2) + (0.0881P)2]
where P = (Fo2 + 2Fc2)/3
4968 reflections(Δ/σ)max = 0.002
430 parametersΔρmax = 2.89 e Å3
0 restraintsΔρmin = 1.93 e Å3
Crystal data top
[CoHo2(C14H8N2O5)4(H2O)4]·4H2Oγ = 86.578 (3)°
Mr = 1669.81V = 1433.9 (2) Å3
Triclinic, P1Z = 1
a = 10.0597 (9) ÅMo Kα radiation
b = 10.7824 (10) ŵ = 3.12 mm1
c = 13.7261 (13) ÅT = 291 K
α = 79.141 (3)°0.20 × 0.14 × 0.10 mm
β = 78.801 (1)°
Data collection top
Bruker APEX CCD
diffractometer
4968 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2001)
4756 reflections with I > 2σ(I)
Tmin = 0.574, Tmax = 0.746Rint = 0.070
7154 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0460 restraints
wR(F2) = 0.123H-atom parameters constrained
S = 1.06Δρmax = 2.89 e Å3
4968 reflectionsΔρmin = 1.93 e Å3
430 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Co11.00000.50000.00000.0253 (3)
Ho10.68057 (2)1.07784 (2)0.204341 (17)0.01470 (13)
C10.6994 (6)0.4719 (5)0.2279 (4)0.0217 (12)
C20.7035 (6)0.6032 (6)0.1993 (5)0.0236 (13)
H20.71930.64070.13150.028*
C30.6834 (6)0.6770 (5)0.2746 (4)0.0221 (12)
C40.6647 (6)0.6223 (6)0.3756 (5)0.0229 (12)
H40.65290.67300.42460.027*
C50.6636 (6)0.4913 (6)0.4041 (5)0.0233 (12)
C60.6770 (6)0.4169 (6)0.3298 (5)0.0240 (13)
H60.67090.32960.34850.029*
C70.6875 (6)0.8177 (6)0.2476 (5)0.0236 (13)
C80.7308 (6)0.3913 (6)0.1481 (5)0.0228 (13)
C90.6680 (7)0.4839 (6)0.5835 (5)0.0289 (14)
C100.6509 (6)0.4012 (6)0.6856 (5)0.0264 (13)
C110.6448 (8)0.4618 (7)0.7689 (5)0.0363 (16)
H110.64520.54940.76000.044*
C120.6382 (8)0.3898 (8)0.8632 (6)0.0425 (18)
H120.63340.43100.91760.051*
C130.6446 (7)0.2083 (7)0.8032 (5)0.0366 (16)
H130.64530.12050.81500.044*
C140.6503 (7)0.2708 (7)0.7046 (5)0.0325 (15)
H140.65360.22600.65250.039*
C150.9066 (6)1.1082 (6)0.2811 (5)0.0229 (13)
C161.0260 (6)1.1190 (6)0.3296 (5)0.0238 (13)
C171.1593 (6)1.1035 (6)0.2809 (5)0.0248 (13)
H171.17741.08700.21540.030*
C181.2633 (6)1.1125 (6)0.3300 (5)0.0228 (13)
C191.2362 (6)1.1400 (6)0.4285 (5)0.0252 (13)
H191.30701.14400.46230.030*
C201.1051 (6)1.1606 (6)0.4744 (4)0.0231 (12)
C210.9979 (6)1.1474 (6)0.4250 (5)0.0234 (13)
H210.90861.15790.45680.028*
C221.4092 (6)1.0971 (5)0.2832 (5)0.0229 (13)
C230.9939 (6)1.2942 (6)0.5906 (5)0.0257 (13)
C240.9915 (6)1.3357 (6)0.6897 (5)0.0264 (13)
C250.9898 (7)1.4651 (7)0.6893 (5)0.0302 (15)
H250.99201.52280.62940.036*
C260.9847 (7)1.5063 (6)0.7794 (5)0.0294 (14)
H260.98521.59290.77800.035*
C270.9748 (7)1.3039 (6)0.8680 (5)0.0313 (15)
H270.96581.24850.92950.038*
C280.9831 (7)1.2549 (6)0.7813 (5)0.0306 (14)
H280.98311.16790.78440.037*
N10.6462 (5)0.4309 (5)0.5055 (4)0.0259 (11)
H10.61960.35410.51960.031*
N20.6383 (6)0.2642 (6)0.8813 (5)0.0399 (14)
N31.0799 (5)1.1948 (5)0.5708 (4)0.0260 (11)
H31.11901.15290.61760.031*
N40.9792 (5)1.4296 (5)0.8675 (4)0.0269 (12)
O10.8061 (5)0.4321 (4)0.0666 (3)0.0333 (11)
O20.6754 (5)0.2834 (4)0.1695 (4)0.0331 (11)
O30.7064 (6)0.8823 (4)0.3105 (4)0.0398 (13)
O40.6712 (6)0.8746 (4)0.1615 (4)0.0411 (13)
O50.6942 (7)0.5942 (5)0.5749 (4)0.0603 (18)
O60.7902 (4)1.1165 (4)0.3309 (3)0.0270 (9)
O70.9238 (5)1.0921 (5)0.1893 (3)0.0320 (11)
O81.4436 (5)1.0967 (5)0.1889 (4)0.0333 (11)
O91.4993 (5)1.0839 (5)0.3355 (3)0.0405 (12)
O100.9226 (5)1.3484 (5)0.5328 (4)0.0421 (13)
O1W0.9246 (5)0.6839 (4)0.0658 (3)0.0366 (11)
H1WA0.84260.70360.04400.044*
H1WB0.98280.74140.07640.044*
O2W0.7208 (5)1.0991 (5)0.0330 (3)0.0399 (12)
H2WA0.80391.08880.00780.048*
H2WB0.68561.16780.00620.048*
O3W0.5839 (8)0.1598 (5)0.5164 (4)0.0640 (19)
H3WA0.64150.14440.46570.077*
H3WB0.56330.09010.55620.077*
O4W0.3038 (7)0.1634 (8)0.0325 (5)0.084 (3)
H4WA0.32550.14400.02600.101*
H4WB0.36040.13400.07010.101*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co10.0279 (7)0.0260 (6)0.0239 (6)0.0029 (5)0.0040 (5)0.0097 (5)
Ho10.01438 (18)0.01247 (18)0.01903 (18)0.00036 (11)0.00550 (11)0.00507 (11)
C10.021 (3)0.019 (3)0.027 (3)0.002 (2)0.008 (2)0.008 (2)
C20.019 (3)0.022 (3)0.028 (3)0.001 (2)0.001 (2)0.002 (2)
C30.025 (3)0.018 (3)0.026 (3)0.001 (2)0.008 (2)0.007 (2)
C40.020 (3)0.021 (3)0.029 (3)0.002 (2)0.006 (2)0.006 (2)
C50.015 (3)0.024 (3)0.029 (3)0.003 (2)0.002 (2)0.005 (2)
C60.027 (3)0.018 (3)0.026 (3)0.000 (2)0.003 (3)0.006 (2)
C70.024 (3)0.023 (3)0.024 (3)0.006 (2)0.007 (2)0.002 (3)
C80.017 (3)0.024 (3)0.029 (3)0.000 (2)0.008 (2)0.005 (3)
C90.036 (4)0.026 (3)0.029 (3)0.005 (3)0.013 (3)0.005 (3)
C100.022 (3)0.028 (3)0.030 (3)0.004 (2)0.010 (3)0.003 (3)
C110.044 (4)0.036 (4)0.032 (4)0.003 (3)0.008 (3)0.011 (3)
C120.046 (5)0.055 (5)0.030 (4)0.000 (4)0.008 (3)0.016 (4)
C130.037 (4)0.037 (4)0.037 (4)0.007 (3)0.017 (3)0.000 (3)
C140.032 (4)0.039 (4)0.029 (3)0.007 (3)0.011 (3)0.005 (3)
C150.018 (3)0.022 (3)0.031 (3)0.003 (2)0.005 (3)0.010 (3)
C160.020 (3)0.023 (3)0.031 (3)0.000 (2)0.008 (3)0.008 (3)
C170.023 (3)0.027 (3)0.025 (3)0.002 (2)0.005 (2)0.005 (2)
C180.020 (3)0.022 (3)0.028 (3)0.001 (2)0.005 (2)0.007 (2)
C190.019 (3)0.030 (3)0.030 (3)0.002 (2)0.013 (3)0.007 (3)
C200.023 (3)0.024 (3)0.026 (3)0.005 (2)0.010 (2)0.011 (2)
C210.016 (3)0.029 (3)0.028 (3)0.001 (2)0.006 (2)0.010 (3)
C220.021 (3)0.019 (3)0.028 (3)0.000 (2)0.003 (3)0.003 (2)
C230.019 (3)0.034 (3)0.026 (3)0.001 (3)0.006 (3)0.011 (3)
C240.018 (3)0.039 (4)0.026 (3)0.003 (3)0.007 (2)0.015 (3)
C250.029 (4)0.038 (4)0.025 (3)0.000 (3)0.008 (3)0.008 (3)
C260.030 (4)0.029 (3)0.031 (3)0.001 (3)0.004 (3)0.013 (3)
C270.033 (4)0.030 (4)0.032 (4)0.005 (3)0.008 (3)0.004 (3)
C280.032 (4)0.030 (3)0.032 (3)0.006 (3)0.005 (3)0.014 (3)
N10.034 (3)0.018 (3)0.025 (3)0.001 (2)0.006 (2)0.001 (2)
N20.041 (4)0.046 (4)0.033 (3)0.002 (3)0.011 (3)0.002 (3)
N30.023 (3)0.030 (3)0.026 (3)0.000 (2)0.004 (2)0.010 (2)
N40.024 (3)0.032 (3)0.028 (3)0.004 (2)0.005 (2)0.014 (2)
O10.033 (3)0.039 (3)0.029 (2)0.011 (2)0.001 (2)0.011 (2)
O20.044 (3)0.021 (2)0.038 (3)0.004 (2)0.010 (2)0.009 (2)
O30.073 (4)0.019 (2)0.036 (3)0.003 (2)0.031 (3)0.008 (2)
O40.074 (4)0.021 (2)0.032 (3)0.001 (2)0.021 (3)0.003 (2)
O50.113 (6)0.034 (3)0.040 (3)0.025 (3)0.026 (3)0.001 (2)
O60.018 (2)0.035 (2)0.033 (2)0.0004 (18)0.0057 (18)0.0164 (19)
O70.026 (2)0.048 (3)0.027 (2)0.002 (2)0.0062 (19)0.020 (2)
O80.022 (2)0.049 (3)0.033 (3)0.003 (2)0.007 (2)0.019 (2)
O90.018 (2)0.074 (4)0.032 (3)0.006 (2)0.009 (2)0.013 (2)
O100.040 (3)0.054 (3)0.043 (3)0.019 (2)0.022 (2)0.027 (2)
O1W0.038 (3)0.034 (3)0.036 (3)0.005 (2)0.005 (2)0.004 (2)
O2W0.053 (3)0.034 (3)0.031 (3)0.002 (2)0.008 (2)0.001 (2)
O3W0.120 (6)0.037 (3)0.035 (3)0.023 (3)0.009 (3)0.008 (2)
O4W0.059 (4)0.155 (8)0.039 (3)0.029 (4)0.018 (3)0.022 (4)
Geometric parameters (Å, º) top
Co1—O12.098 (4)C13—H130.9300
Co1—O1i2.098 (4)C14—H140.9300
Co1—N4ii2.148 (5)C15—O61.243 (7)
Co1—N4iii2.148 (5)C15—O71.282 (7)
Co1—O1Wi2.176 (5)C15—C161.502 (8)
Co1—O1W2.176 (5)C16—C211.373 (8)
Ho1—O2iv2.177 (4)C16—C171.393 (9)
Ho1—O2W2.278 (5)C17—C181.367 (9)
Ho1—O9v2.307 (5)C17—H170.9300
Ho1—O62.341 (4)C18—C191.411 (8)
Ho1—O32.358 (4)C18—C221.496 (8)
Ho1—O42.385 (4)C19—C201.371 (9)
Ho1—O8v2.427 (5)C19—H190.9300
Ho1—O72.426 (5)C20—C211.408 (8)
Ho1—C22v2.745 (6)C20—N31.412 (7)
C1—C61.393 (8)C21—H210.9300
C1—C21.397 (8)C22—O91.248 (7)
C1—C81.499 (8)C22—O81.274 (8)
C2—C31.397 (8)C23—O101.217 (8)
C2—H20.9300C23—N31.370 (8)
C3—C41.381 (9)C23—C241.506 (8)
C3—C71.494 (8)C24—C281.379 (9)
C4—C51.393 (8)C24—C251.394 (10)
C4—H40.9300C25—C261.382 (9)
C5—C61.394 (8)C25—H250.9300
C5—N11.403 (8)C26—N41.324 (9)
C6—H60.9300C26—H260.9300
C7—O31.254 (8)C27—N41.358 (9)
C7—O41.261 (8)C27—C281.377 (9)
C8—O11.242 (7)C27—H270.9300
C8—O21.279 (7)C28—H280.9300
C9—O51.212 (8)N1—H10.8600
C9—N11.363 (8)N3—H30.8600
C9—C101.498 (9)O1W—H1WA0.8500
C10—C141.382 (10)O1W—H1WB0.8510
C10—C111.409 (9)O2W—H2WA0.8500
C11—C121.370 (10)O2W—H2WB0.8520
C11—H110.9300O3W—H3WA0.8503
C12—N21.331 (10)O3W—H3WB0.8522
C12—H120.9300O4W—H4WA0.8514
C13—N21.315 (9)O4W—H4WB0.8504
C13—C141.385 (10)
O1—Co1—O1i180.0 (2)C12—C11—H11120.4
O1—Co1—N4ii92.16 (19)C10—C11—H11120.4
O1i—Co1—N4ii87.84 (19)N2—C12—C11123.6 (7)
O1—Co1—N4iii87.84 (19)N2—C12—H12118.2
O1i—Co1—N4iii92.16 (19)C11—C12—H12118.2
N4ii—Co1—N4iii180.0 (3)N2—C13—C14124.7 (7)
O1—Co1—O1Wi85.97 (19)N2—C13—H13117.6
O1i—Co1—O1Wi94.03 (19)C14—C13—H13117.6
N4ii—Co1—O1Wi89.3 (2)C10—C14—C13118.4 (6)
N4iii—Co1—O1Wi90.7 (2)C10—C14—H14120.8
O1—Co1—O1W94.03 (19)C13—C14—H14120.8
O1i—Co1—O1W85.97 (19)O6—C15—O7120.1 (5)
N4ii—Co1—O1W90.7 (2)O6—C15—C16119.1 (5)
N4iii—Co1—O1W89.3 (2)O7—C15—C16120.8 (5)
O1Wi—Co1—O1W180.0 (2)C21—C16—C17120.8 (6)
O2iv—Ho1—O2W82.48 (17)C21—C16—C15116.6 (5)
O2iv—Ho1—O9v89.62 (19)C17—C16—C15122.6 (5)
O2W—Ho1—O9v138.85 (17)C18—C17—C16119.6 (6)
O2iv—Ho1—O681.57 (16)C18—C17—H17120.2
O2W—Ho1—O6138.55 (17)C16—C17—H17120.2
O9v—Ho1—O678.95 (15)C17—C18—C19120.3 (6)
O2iv—Ho1—O3153.22 (17)C17—C18—C22123.0 (6)
O2W—Ho1—O3122.18 (16)C19—C18—C22116.7 (5)
O9v—Ho1—O378.12 (19)C20—C19—C18119.9 (6)
O6—Ho1—O372.81 (15)C20—C19—H19120.1
O2iv—Ho1—O4152.59 (18)C18—C19—H19120.1
O2W—Ho1—O471.43 (17)C19—C20—C21119.7 (5)
O9v—Ho1—O4104.37 (19)C19—C20—N3119.3 (5)
O6—Ho1—O4123.81 (16)C21—C20—N3121.0 (5)
O3—Ho1—O454.16 (15)C16—C21—C20119.6 (6)
O2iv—Ho1—O8v84.81 (18)C16—C21—H21120.2
O2W—Ho1—O8v84.52 (17)C20—C21—H21120.2
O9v—Ho1—O8v54.48 (15)O9—C22—O8118.7 (6)
O6—Ho1—O8v131.43 (15)O9—C22—C18120.9 (5)
O3—Ho1—O8v106.24 (18)O8—C22—C18120.4 (5)
O4—Ho1—O8v84.49 (17)O9—C22—Ho1vi56.6 (3)
O2iv—Ho1—O786.64 (18)O8—C22—Ho1vi62.1 (3)
O2W—Ho1—O786.51 (17)C18—C22—Ho1vi176.7 (4)
O9v—Ho1—O7133.46 (15)O10—C23—N3123.5 (6)
O6—Ho1—O754.60 (14)O10—C23—C24120.2 (6)
O3—Ho1—O784.87 (18)N3—C23—C24116.3 (5)
O4—Ho1—O799.70 (18)C28—C24—C25118.0 (6)
O8v—Ho1—O7168.33 (16)C28—C24—C23124.5 (6)
O2iv—Ho1—C22v86.17 (18)C25—C24—C23117.5 (6)
O2W—Ho1—C22v112.05 (19)C26—C25—C24118.8 (6)
O9v—Ho1—C22v26.84 (16)C26—C25—H25120.6
O6—Ho1—C22v104.75 (16)C24—C25—H25120.6
O3—Ho1—C22v92.79 (19)N4—C26—C25123.8 (6)
O4—Ho1—C22v95.75 (18)N4—C26—H26118.1
O8v—Ho1—C22v27.66 (17)C25—C26—H26118.1
O7—Ho1—C22v158.98 (17)N4—C27—C28122.8 (6)
C6—C1—C2120.0 (5)N4—C27—H27118.6
C6—C1—C8120.6 (5)C28—C27—H27118.6
C2—C1—C8119.2 (5)C27—C28—C24119.5 (6)
C3—C2—C1118.7 (6)C27—C28—H28120.3
C3—C2—H2120.6C24—C28—H28120.3
C1—C2—H2120.6C9—N1—C5125.3 (5)
C4—C3—C2121.3 (6)C9—N1—H1117.4
C4—C3—C7118.1 (5)C5—N1—H1117.4
C2—C3—C7120.6 (5)C13—N2—C12116.9 (6)
C3—C4—C5120.0 (6)C23—N3—C20120.8 (5)
C3—C4—H4120.0C23—N3—H3119.6
C5—C4—H4120.0C20—N3—H3119.6
C4—C5—C6119.2 (6)C26—N4—C27117.0 (6)
C4—C5—N1122.4 (5)C26—N4—Co1vii121.1 (4)
C6—C5—N1118.4 (5)C27—N4—Co1vii121.5 (4)
C1—C6—C5120.7 (6)C8—O1—Co1144.4 (4)
C1—C6—H6119.6C8—O2—Ho1viii153.1 (4)
C5—C6—H6119.6C7—O3—Ho194.4 (4)
O3—C7—O4118.3 (6)C7—O4—Ho193.0 (4)
O3—C7—C3120.6 (5)C15—O6—Ho195.1 (3)
O4—C7—C3121.0 (6)C15—O7—Ho190.1 (4)
O1—C8—O2124.3 (6)C22—O8—Ho1vi90.2 (4)
O1—C8—C1119.4 (5)C22—O9—Ho1vi96.5 (4)
O2—C8—C1116.3 (5)Co1—O1W—H1WA117.2
O5—C9—N1123.5 (6)Co1—O1W—H1WB112.7
O5—C9—C10119.3 (6)H1WA—O1W—H1WB117.3
N1—C9—C10117.1 (5)Ho1—O2W—H2WA113.0
C14—C10—C11117.2 (6)Ho1—O2W—H2WB110.9
C14—C10—C9125.8 (6)H2WA—O2W—H2WB113.5
C11—C10—C9116.9 (6)H3WA—O3W—H3WB108.4
C12—C11—C10119.1 (7)H4WA—O4W—H4WB112.3
C6—C1—C2—C30.6 (9)C6—C5—N1—C9161.2 (6)
C8—C1—C2—C3175.6 (5)C14—C13—N2—C120.4 (11)
C1—C2—C3—C42.4 (9)C11—C12—N2—C130.3 (12)
C1—C2—C3—C7179.7 (6)O10—C23—N3—C209.1 (10)
C2—C3—C4—C51.0 (9)C24—C23—N3—C20170.5 (5)
C7—C3—C4—C5178.4 (5)C19—C20—N3—C23132.3 (6)
C3—C4—C5—C62.1 (9)C21—C20—N3—C2347.7 (8)
C3—C4—C5—N1179.5 (6)C25—C26—N4—C271.8 (10)
C2—C1—C6—C52.5 (9)C25—C26—N4—Co1vii171.2 (5)
C8—C1—C6—C5172.4 (5)C28—C27—N4—C263.5 (10)
C4—C5—C6—C13.9 (9)C28—C27—N4—Co1vii169.4 (5)
N1—C5—C6—C1177.7 (5)O2—C8—O1—Co1122.1 (7)
C4—C3—C7—O316.9 (9)C1—C8—O1—Co158.6 (10)
C2—C3—C7—O3160.6 (6)N4ii—Co1—O1—C828.2 (8)
C4—C3—C7—O4162.6 (6)N4iii—Co1—O1—C8151.8 (8)
C2—C3—C7—O420.0 (9)O1Wi—Co1—O1—C860.9 (7)
C6—C1—C8—O1148.0 (6)O1W—Co1—O1—C8119.1 (7)
C2—C1—C8—O126.9 (8)O1—C8—O2—Ho1viii69.4 (12)
C6—C1—C8—O232.6 (8)C1—C8—O2—Ho1viii111.3 (9)
C2—C1—C8—O2152.5 (6)O4—C7—O3—Ho13.2 (7)
O5—C9—C10—C14165.1 (7)C3—C7—O3—Ho1176.3 (5)
N1—C9—C10—C1418.0 (10)O2iv—Ho1—O3—C7179.7 (4)
O5—C9—C10—C1110.0 (10)O2W—Ho1—O3—C725.1 (5)
N1—C9—C10—C11166.8 (6)O9v—Ho1—O3—C7115.9 (4)
C14—C10—C11—C120.2 (10)O6—Ho1—O3—C7162.2 (4)
C9—C10—C11—C12175.8 (7)O4—Ho1—O3—C71.8 (4)
C10—C11—C12—N20.6 (12)O8v—Ho1—O3—C768.7 (4)
C11—C10—C14—C130.4 (10)O7—Ho1—O3—C7107.7 (4)
C9—C10—C14—C13174.7 (6)C22v—Ho1—O3—C793.3 (4)
N2—C13—C14—C100.7 (11)O3—C7—O4—Ho13.1 (7)
O6—C15—C16—C214.9 (9)C3—C7—O4—Ho1176.3 (5)
O7—C15—C16—C21174.4 (6)O2iv—Ho1—O4—C7179.8 (4)
O6—C15—C16—C17176.2 (6)O2W—Ho1—O4—C7161.2 (5)
O7—C15—C16—C174.6 (9)O9v—Ho1—O4—C761.6 (4)
C21—C16—C17—C182.2 (9)O6—Ho1—O4—C724.6 (5)
C15—C16—C17—C18179.0 (6)O3—Ho1—O4—C71.8 (4)
C16—C17—C18—C191.3 (9)O8v—Ho1—O4—C7112.8 (4)
C16—C17—C18—C22180.0 (6)O7—Ho1—O4—C778.2 (4)
C17—C18—C19—C201.6 (9)C22v—Ho1—O4—C787.5 (4)
C22—C18—C19—C20177.2 (6)O7—C15—O6—Ho14.0 (6)
C18—C19—C20—C213.5 (9)C16—C15—O6—Ho1176.8 (5)
C18—C19—C20—N3176.5 (6)O2iv—Ho1—O6—C1594.1 (4)
C17—C16—C21—C200.2 (9)O2W—Ho1—O6—C1525.7 (5)
C15—C16—C21—C20179.2 (5)O9v—Ho1—O6—C15174.6 (4)
C19—C20—C21—C162.6 (9)O3—Ho1—O6—C1593.8 (4)
N3—C20—C21—C16177.4 (6)O4—Ho1—O6—C1574.6 (4)
C17—C18—C22—O9167.3 (6)O8v—Ho1—O6—C15169.5 (3)
C19—C18—C22—O913.9 (9)O7—Ho1—O6—C152.2 (3)
C17—C18—C22—O812.4 (9)C22v—Ho1—O6—C15177.9 (4)
C19—C18—C22—O8166.4 (6)O6—C15—O7—Ho13.8 (6)
O10—C23—C24—C28133.8 (7)C16—C15—O7—Ho1176.9 (5)
N3—C23—C24—C2846.7 (9)O2iv—Ho1—O7—C1584.2 (4)
O10—C23—C24—C2542.3 (9)O2W—Ho1—O7—C15166.9 (4)
N3—C23—C24—C25137.2 (6)O9v—Ho1—O7—C152.1 (5)
C28—C24—C25—C262.3 (9)O6—Ho1—O7—C152.2 (3)
C23—C24—C25—C26178.6 (6)O3—Ho1—O7—C1570.4 (4)
C24—C25—C26—N41.1 (10)O4—Ho1—O7—C15122.7 (4)
N4—C27—C28—C242.4 (10)O8v—Ho1—O7—C15127.1 (7)
C25—C24—C28—C270.6 (10)C22v—Ho1—O7—C1514.0 (7)
C23—C24—C28—C27176.7 (6)O9—C22—O8—Ho1vi2.7 (6)
O5—C9—N1—C56.6 (11)C18—C22—O8—Ho1vi177.6 (5)
C10—C9—N1—C5176.7 (6)O8—C22—O9—Ho1vi2.9 (6)
C4—C5—N1—C920.3 (9)C18—C22—O9—Ho1vi177.4 (5)
Symmetry codes: (i) x+2, y+1, z; (ii) x+2, y+2, z+1; (iii) x, y1, z1; (iv) x, y+1, z; (v) x1, y, z; (vi) x+1, y, z; (vii) x, y+1, z+1; (viii) x, y1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H1WA···O4Wix0.852.002.761 (8)149
O1W—H1WB···O7x0.852.262.988 (7)144
O2W—H2WB···N2xi0.851.962.699 (8)145
O3W—H3WA···O6viii0.852.203.048 (8)177
O3W—H3WB···O9xii0.852.203.054 (8)177
O4W—H4WA···O4ix0.851.902.732 (8)164
O4W—H4WB···O8xiii0.851.942.752 (8)160
N1—H1···O3W0.862.162.996 (7)165
N3—H3···O3ii0.862.162.933 (7)150
Symmetry codes: (ii) x+2, y+2, z+1; (viii) x, y1, z; (ix) x+1, y+1, z; (x) x+2, y+2, z; (xi) x, y+1, z1; (xii) x+2, y+1, z+1; (xiii) x1, y1, z.

Experimental details

Crystal data
Chemical formula[CoHo2(C14H8N2O5)4(H2O)4]·4H2O
Mr1669.81
Crystal system, space groupTriclinic, P1
Temperature (K)291
a, b, c (Å)10.0597 (9), 10.7824 (10), 13.7261 (13)
α, β, γ (°)79.141 (3), 78.801 (1), 86.578 (3)
V3)1433.9 (2)
Z1
Radiation typeMo Kα
µ (mm1)3.12
Crystal size (mm)0.20 × 0.14 × 0.10
Data collection
DiffractometerBruker APEX CCD
diffractometer
Absorption correctionMulti-scan
(SADABS; Bruker, 2001)
Tmin, Tmax0.574, 0.746
No. of measured, independent and
observed [I > 2σ(I)] reflections
7154, 4968, 4756
Rint0.070
(sin θ/λ)max1)0.595
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.046, 0.123, 1.06
No. of reflections4968
No. of parameters430
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)2.89, 1.93

Computer programs: SMART (Bruker, 2007), SAINT (Bruker, 2007), XP in SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 1999).

Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H1WA···O4Wi0.852.002.761 (8)149
O1W—H1WB···O7ii0.852.262.988 (7)144
O2W—H2WB···N2iii0.851.962.699 (8)145
O3W—H3WA···O6iv0.852.203.048 (8)177
O3W—H3WB···O9v0.852.203.054 (8)177
O4W—H4WA···O4i0.851.902.732 (8)164
O4W—H4WB···O8vi0.851.942.752 (8)160
N1—H1···O3W0.862.162.996 (7)165
N3—H3···O3vii0.862.162.933 (7)150
Symmetry codes: (i) x+1, y+1, z; (ii) x+2, y+2, z; (iii) x, y+1, z1; (iv) x, y1, z; (v) x+2, y+1, z+1; (vi) x1, y1, z; (vii) x+2, y+2, z+1.
 

Acknowledgements

This work was supported by the Open Fund Project of Key Laboratories in Hunan Universities (grant No. 11 K009) and the Science Foundation of Hengyang Normal University of China (grant No. 10B67).

References

First citationBrandenburg, K. (1999). DIAMOND. Crystal Impact GbR, Bonn, Germany.  Google Scholar
First citationBruker (2001). SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.  Google Scholar
First citationBruker (2007). SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.  Google Scholar
First citationChen, M.-S., Zhao, Y., Okamura, T.-A., Su, Z., Sun, W.-Y. & Ueyama, N. (2011). Supramol. Chem. 23, 117–124.  Web of Science CSD CrossRef CAS Google Scholar
First citationDeng, Y.-F., Chen, M.-S., Zhang, C.-H. & Kuang, D.-Z. (2011). Acta Cryst. E67, m1431–m1432.  Web of Science CSD CrossRef CAS IUCr Journals Google Scholar
First citationGu, X.-J. & Xue, D.-F. (2006). Inorg. Chem. 45, 9257–9261.  Web of Science CSD CrossRef PubMed CAS Google Scholar
First citationLiang, Y.-C., Cao, R., Su, W.-P., Hong, M.-C. & Zhang, W.-J. (2000). Angew. Chem. Int. Ed. 39, 3304–3307.  Web of Science CrossRef CAS Google Scholar
First citationPrasad, T. K., Rajasekharan, M. V. & Costes, J. P. (2007). Angew. Chem. Int. Ed. 46, 2851–2854.  Web of Science CSD CrossRef CAS Google Scholar
First citationSheldrick, G. M. (2008). Acta Cryst. A64, 112–122.  Web of Science CrossRef CAS IUCr Journals Google Scholar
First citationZhao, B., Cheng, P., Chen, X.-Y., Cheng, C., Shi, W., Liao, D.-Z., Yan, S.-P. & Jiang, Z.-H. (2004). J. Am. Chem. Soc. 126, 3012–3013.  Web of Science CSD CrossRef PubMed CAS Google Scholar
First citationZhao, B., Cheng, P., Dai, Y., Cheng, C., Liao, D.-Z., Yan, S.-P., Jiang, Z.-H. & Wang, G.-L. (2003). Angew. Chem. Int. Ed. 42, 934–936.  Web of Science CSD CrossRef CAS Google Scholar

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Volume 67| Part 11| November 2011| Pages m1574-m1575
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