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

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Tetra­aqua­bis­[1,1′-(4-meth­oxy­naph­thalene-1,3-diyldi­methyl­ene)pyridinium-3-carboxyl­ate-κO]cobalt(II) bis­­(perchlorate) hexa­hydrate

aState key laboratory of Elomento-Organic Chemistry, Nankai University, Tianjin 30071, People's Republic of China
*Correspondence e-mail: fengboxu23@eyou.com

(Received 30 November 2007; accepted 4 May 2008; online 14 May 2008)

In the molecule of the centrosymmetric title compound, [Co(C25H20N2O5)2(H2O)4](ClO4)2·6H2O, the Co atom is octa­hedrally coordinated by four water mol­ecules lying in the equatorial plane and two monodentate carboxyl­ate groups from two dicarboxylate ligands. The crystal structure involves O—H⋯O and O—H⋯Cl hydrogen bonds..

Related literature

For related literature, see: Li et al. (2006[Li, H.-S., Li, S.-L. & Hou, J.-F. (2006). Acta Cryst. E62, m2143-m2144.]).

[Scheme 1]

Experimental

Crystal data
  • [Co(C25H20N2O5)2(H2O)4](ClO4)2·6H2O

  • Mr = 1294.86

  • Triclinic, [P \overline 1]

  • a = 7.9162 (19) Å

  • b = 12.703 (3) Å

  • c = 14.757 (3) Å

  • α = 71.159 (6)°

  • β = 89.759 (8)°

  • γ = 77.175 (7)°

  • V = 1365.7 (5) Å3

  • Z = 1

  • Mo Kα radiation

  • μ = 0.51 mm−1

  • T = 113 (2) K

  • 0.18 × 0.16 × 0.14 mm

Data collection
  • Rigaku Saturn diffractometer

  • Absorption correction: multi-scan (Jacobson, 1998[Jacobson, R. (1998). Private communication to the Rigaku Corporation, Tokyo, Japan.]) Tmin = 0.914, Tmax = 0.932

  • 12559 measured reflections

  • 4738 independent reflections

  • 4261 reflections with I > 2σ(I)

  • Rint = 0.024

Refinement
  • R[F2 > 2σ(F2)] = 0.057

  • wR(F2) = 0.128

  • S = 1.08

  • 4738 reflections

  • 417 parameters

  • 17 restraints

  • H atoms treated by a mixture of independent and constrained refinement

  • Δρmax = 1.27 e Å−3

  • Δρmin = −0.45 e Å−3

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A DA D—H⋯A
O10—H10A⋯O13i 0.84 (4) 1.83 (4) 2.665 (5) 171 (6)
O10—H10B⋯O1ii 0.85 (4) 1.84 (4) 2.668 (6) 166 (6)
O11—H11A⋯O12i 0.87 (4) 1.83 (4) 2.690 (6) 174 (7)
O11—H11B⋯O14iii 0.86 (4) 1.85 (4) 2.701 (5) 173 (6)
O12—H12A⋯O1 0.83 (4) 1.84 (5) 2.654 (6) 164 (8)
O12—H12B⋯O4 0.87 (4) 1.91 (4) 2.772 (6) 173 (8)
O13—H13A⋯O5iv 0.86 (4) 1.94 (4) 2.787 (6) 172 (7)
O13—H13B⋯O9v 0.86 (4) 1.95 (4) 2.815 (6) 175 (7)
O13—H13B⋯Cl1v 0.86 (4) 2.69 (6) 3.451 (4) 147 (6)
O14—H14A⋯O4i 0.86 (4) 1.88 (4) 2.724 (6) 165 (7)
O14—H14B⋯O5vi 0.86 (4) 1.98 (4) 2.811 (6) 160 (7)
Symmetry codes: (i) -x+2, -y+1, -z+1; (ii) -x+3, -y+1, -z+1; (iii) x+1, y, z; (iv) -x+2, -y, -z+1; (v) -x+1, -y, -z+1; (vi) x-1, y+1, z.

Data collection: CrystalClear (Rigaku, 2002[Rigaku (2002). CrystalClear and CrystalStructure. Rigaku Corporation, Tokyo, Japan.]); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: CrystalStructure (Rigaku, 2002[Rigaku (2002). CrystalClear and CrystalStructure. Rigaku Corporation, Tokyo, Japan.]); software used to prepare material for publication: CrystalStructure.

Supporting information


Comment top

Recently, corrdination chemistry becomes more and more important in the structural design of supramolecular chemistry. The deprotonated carboxyl group, which easily coordinated to metal atoms and can be used to prepare soluble metal complexes. During the synthesis of polymeric complexes using 3-methoxyl-1,3-pyridinium-3-carboxylate (L) as bridging ligand, to our surprise, the title monomeric Co complex was obtained.

As shown in Fig. 1, the stucture of the title compound, (I), four water molecules and two monodentate carboxylate groups from L ligands corrdinate to Co. the other three water molecules and carboxylate group of the ligand L and the perchlorate anion are free from corrdination.

For related literature, see: Li et al. (2006).

Related literature top

For related literature, see: Li et al. (2006).

Experimental top

An aqueous and water (V/V=1:1) solution of L (0.042 g, 0.1 mmol)and Co(ClO4)6H2O (0.11 g, 0.3 mmol) was stirred at 333 K for 10 min and then left to stand at room temperature. Single crystals of (I) were obtained after 3 d.

Refinement top

(type here to add refinement details)

Computing details top

Data collection: CrystalClear (Rigaku, 2002); cell refinement: CrystalClear (Rigaku, 2002); data reduction: CrystalClear (Rigaku, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: [PLEASE PROVIDE SOFTWARE/REFERENCE]; software used to prepare material for publication: CrystalStructure (Rigaku, 2002).

Figures top
[Figure 1] Fig. 1. The molecular structure of (I), shown with 30% probability displacement ellipsoids.
Tetraaquabis[1,1'-(4-methoxynaphthalene-1,3-diyldimethylene)pyridinium-3- carboxylate-κO]cobalt(II) bis(perchlorate) hexahydrate top
Crystal data top
[Co(C25H20N2O5)2(H2O)4](ClO4)2·6H2OZ = 1
Mr = 1294.86F(000) = 673
Triclinic, P1Dx = 1.574 Mg m3
a = 7.9162 (19) ÅMo Kα radiation, λ = 0.71070 Å
b = 12.703 (3) ÅCell parameters from 4046 reflections
c = 14.757 (3) Åθ = 2.6–27.8°
α = 71.159 (6)°µ = 0.51 mm1
β = 89.759 (8)°T = 113 K
γ = 77.175 (7)°Prism, colorless
V = 1365.7 (5) Å30.18 × 0.16 × 0.14 mm
Data collection top
Rigaku Saturn
diffractometer
4738 independent reflections
Radiation source: fine-focus sealed tube4261 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.024
Detector resolution: 7.31 pixels mm-1θmax = 25.0°, θmin = 2.7°
ω scansh = 99
Absorption correction: multi-scan
(Jacobson, 1998)
k = 1315
Tmin = 0.914, Tmax = 0.932l = 1717
12559 measured reflections
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.057H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.128 w = 1/[σ2(Fo2) + (0.0385P)2 + 4.0784P]
where P = (Fo2 + 2Fc2)/3
S = 1.08(Δ/σ)max = 0.004
4738 reflectionsΔρmax = 1.27 e Å3
417 parametersΔρmin = 0.45 e Å3
17 restraintsExtinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.013 (3)
Crystal data top
[Co(C25H20N2O5)2(H2O)4](ClO4)2·6H2Oγ = 77.175 (7)°
Mr = 1294.86V = 1365.7 (5) Å3
Triclinic, P1Z = 1
a = 7.9162 (19) ÅMo Kα radiation
b = 12.703 (3) ŵ = 0.51 mm1
c = 14.757 (3) ÅT = 113 K
α = 71.159 (6)°0.18 × 0.16 × 0.14 mm
β = 89.759 (8)°
Data collection top
Rigaku Saturn
diffractometer
4738 independent reflections
Absorption correction: multi-scan
(Jacobson, 1998)
4261 reflections with I > 2σ(I)
Tmin = 0.914, Tmax = 0.932Rint = 0.024
12559 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.05717 restraints
wR(F2) = 0.128H atoms treated by a mixture of independent and constrained refinement
S = 1.08Δρmax = 1.27 e Å3
4738 reflectionsΔρmin = 0.45 e Å3
417 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
Co11.50000.50000.50000.0166 (3)
N10.7742 (5)0.6740 (4)0.2020 (3)0.0175 (9)
N20.7187 (6)0.1380 (4)0.2728 (3)0.0228 (10)
O11.1365 (7)0.4585 (4)0.4208 (5)0.073 (2)
O21.2985 (5)0.5855 (3)0.3906 (3)0.0245 (9)
O30.6931 (6)0.2768 (4)0.0159 (4)0.0443 (12)
O41.1873 (5)0.1697 (3)0.3646 (3)0.0325 (10)
O51.2889 (5)0.0172 (3)0.4167 (3)0.0321 (10)
C11.1687 (7)0.5520 (5)0.3763 (4)0.0277 (13)
C21.0353 (7)0.6348 (5)0.2975 (4)0.0220 (12)
C31.0486 (7)0.7466 (5)0.2532 (4)0.0268 (13)
H31.14460.77170.27010.032*
C40.9214 (7)0.8213 (5)0.1842 (4)0.0266 (13)
H40.92920.89820.15380.032*
C50.7833 (7)0.7839 (4)0.1596 (4)0.0217 (11)
H50.69460.83520.11300.026*
C60.8963 (7)0.6001 (4)0.2702 (4)0.0203 (11)
H60.88620.52350.29970.024*
C70.6205 (7)0.6347 (5)0.1771 (4)0.0222 (12)
H7A0.54140.70000.12880.027*
H7B0.55670.61140.23540.027*
C80.6653 (7)0.5364 (4)0.1382 (4)0.0213 (12)
C90.7197 (7)0.5518 (5)0.0436 (4)0.0238 (12)
C100.7556 (11)0.6557 (5)0.0161 (4)0.0432 (19)
H100.73890.71900.00660.052*
C110.8159 (8)0.6675 (6)0.1092 (5)0.0381 (15)
H110.84910.73560.14540.046*
C120.8263 (8)0.5787 (6)0.1474 (5)0.0387 (15)
H120.86200.58710.21040.046*
C130.7823 (8)0.4757 (5)0.0902 (4)0.0307 (14)
H130.78520.41600.11610.037*
C140.7340 (7)0.4612 (5)0.0052 (4)0.0243 (12)
C150.6947 (7)0.3564 (5)0.0618 (5)0.0260 (13)
C160.6448 (7)0.3420 (4)0.1539 (5)0.0278 (14)
C170.6314 (7)0.4329 (5)0.1918 (4)0.0243 (12)
H170.59820.42230.25550.029*
C180.8347 (13)0.1867 (7)0.0329 (7)0.068 (3)
H18A0.93850.21570.01280.082*
H18B0.81660.13730.00350.082*
H18C0.85040.14270.10160.082*
C190.5813 (7)0.2382 (5)0.2098 (5)0.0327 (15)
H19A0.52530.21210.16380.039*
H19B0.49110.26100.25080.039*
C200.6727 (7)0.0366 (5)0.3076 (4)0.0261 (12)
H200.55970.03110.29140.031*
C210.7884 (8)0.0581 (5)0.3660 (4)0.0280 (13)
H210.75560.12900.39070.034*
C220.9537 (7)0.0498 (5)0.3889 (4)0.0249 (12)
H221.03630.11570.42720.030*
C230.9980 (7)0.0553 (4)0.3556 (4)0.0209 (11)
C240.8756 (7)0.1483 (4)0.2974 (4)0.0223 (12)
H240.90330.22100.27440.027*
C251.1779 (7)0.0706 (5)0.3813 (4)0.0241 (12)
Cl10.30440 (18)0.00621 (11)0.11433 (10)0.0254 (4)
O60.2137 (9)0.0363 (5)0.1891 (3)0.072 (2)
O70.4485 (8)0.0568 (5)0.0958 (6)0.075 (2)
O80.1939 (7)0.0440 (4)0.0298 (3)0.0463 (13)
O90.3657 (6)0.1168 (3)0.1445 (3)0.0324 (10)
O101.6526 (5)0.6076 (3)0.4204 (3)0.0222 (8)
H10A1.604 (7)0.678 (4)0.399 (4)0.033*
H10B1.724 (7)0.597 (5)0.467 (4)0.033*
O111.4046 (5)0.6184 (3)0.5691 (3)0.0241 (9)
H11A1.293 (5)0.645 (5)0.563 (5)0.036*
H11B1.447 (7)0.676 (5)0.566 (5)0.036*
O120.9425 (6)0.3085 (4)0.4369 (4)0.0470 (14)
H12A0.985 (10)0.365 (5)0.431 (6)0.070*
H12B1.017 (9)0.260 (5)0.418 (6)0.070*
O130.5220 (6)0.1760 (3)0.6610 (3)0.0319 (10)
H13A0.589 (8)0.128 (5)0.639 (4)0.048*
H13B0.562 (9)0.160 (6)0.720 (3)0.048*
O140.5114 (6)0.8080 (3)0.5631 (4)0.0372 (11)
H14A0.598 (7)0.828 (6)0.582 (5)0.056*
H14B0.444 (8)0.871 (5)0.528 (5)0.056*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co10.0134 (5)0.0155 (5)0.0214 (6)0.0038 (4)0.0016 (4)0.0065 (4)
N10.018 (2)0.018 (2)0.017 (2)0.0025 (17)0.0011 (17)0.0080 (18)
N20.017 (2)0.017 (2)0.034 (3)0.0035 (18)0.001 (2)0.008 (2)
O10.064 (4)0.032 (3)0.097 (5)0.031 (3)0.062 (3)0.027 (3)
O20.0179 (19)0.024 (2)0.031 (2)0.0065 (15)0.0067 (16)0.0058 (17)
O30.043 (3)0.034 (2)0.063 (3)0.006 (2)0.001 (2)0.028 (2)
O40.018 (2)0.027 (2)0.054 (3)0.0024 (16)0.0073 (19)0.017 (2)
O50.028 (2)0.028 (2)0.035 (2)0.0062 (18)0.0103 (18)0.0130 (19)
C10.027 (3)0.018 (3)0.036 (3)0.006 (2)0.013 (3)0.005 (2)
C20.020 (3)0.020 (3)0.026 (3)0.004 (2)0.006 (2)0.007 (2)
C30.024 (3)0.025 (3)0.032 (3)0.010 (2)0.006 (2)0.007 (2)
C40.029 (3)0.018 (3)0.031 (3)0.008 (2)0.004 (2)0.003 (2)
C50.023 (3)0.020 (3)0.020 (3)0.000 (2)0.001 (2)0.007 (2)
C60.020 (3)0.017 (3)0.023 (3)0.004 (2)0.003 (2)0.005 (2)
C70.018 (3)0.024 (3)0.026 (3)0.005 (2)0.005 (2)0.011 (2)
C80.018 (3)0.018 (3)0.026 (3)0.002 (2)0.012 (2)0.006 (2)
C90.022 (3)0.021 (3)0.025 (3)0.001 (2)0.015 (2)0.005 (2)
C100.089 (6)0.010 (3)0.022 (3)0.005 (3)0.034 (3)0.004 (2)
C110.032 (3)0.042 (4)0.036 (4)0.009 (3)0.001 (3)0.007 (3)
C120.033 (3)0.046 (4)0.032 (4)0.001 (3)0.000 (3)0.011 (3)
C130.029 (3)0.031 (3)0.032 (3)0.005 (2)0.012 (3)0.018 (3)
C140.014 (3)0.021 (3)0.035 (3)0.002 (2)0.010 (2)0.010 (2)
C150.016 (3)0.020 (3)0.044 (4)0.001 (2)0.005 (2)0.015 (3)
C160.014 (3)0.013 (3)0.051 (4)0.000 (2)0.013 (3)0.005 (3)
C170.017 (3)0.023 (3)0.029 (3)0.002 (2)0.011 (2)0.005 (2)
C180.081 (6)0.050 (5)0.069 (6)0.020 (4)0.024 (5)0.036 (5)
C190.018 (3)0.020 (3)0.054 (4)0.002 (2)0.007 (3)0.005 (3)
C200.025 (3)0.021 (3)0.036 (3)0.011 (2)0.003 (2)0.011 (2)
C210.034 (3)0.019 (3)0.032 (3)0.012 (2)0.003 (3)0.006 (2)
C220.029 (3)0.019 (3)0.022 (3)0.000 (2)0.002 (2)0.006 (2)
C230.024 (3)0.019 (3)0.020 (3)0.003 (2)0.001 (2)0.008 (2)
C240.017 (3)0.018 (3)0.033 (3)0.005 (2)0.001 (2)0.009 (2)
C250.023 (3)0.023 (3)0.025 (3)0.002 (2)0.003 (2)0.012 (2)
Cl10.0301 (7)0.0203 (7)0.0229 (7)0.0008 (5)0.0019 (6)0.0076 (5)
O60.110 (5)0.048 (3)0.025 (3)0.039 (3)0.012 (3)0.006 (2)
O70.058 (4)0.046 (3)0.133 (6)0.031 (3)0.002 (4)0.034 (4)
O80.053 (3)0.043 (3)0.032 (3)0.006 (2)0.018 (2)0.008 (2)
O90.041 (2)0.018 (2)0.034 (2)0.0019 (18)0.0040 (19)0.0081 (18)
O100.0179 (19)0.0174 (19)0.028 (2)0.0036 (15)0.0002 (16)0.0041 (16)
O110.0197 (19)0.024 (2)0.034 (2)0.0066 (16)0.0017 (17)0.0143 (18)
O120.025 (2)0.026 (2)0.098 (4)0.0120 (19)0.014 (2)0.027 (3)
O130.036 (2)0.022 (2)0.031 (2)0.0036 (18)0.0073 (19)0.0067 (18)
O140.032 (2)0.022 (2)0.055 (3)0.0050 (18)0.020 (2)0.010 (2)
Geometric parameters (Å, º) top
Co1—O112.086 (4)C12—C131.426 (9)
Co1—O11i2.086 (4)C12—H120.9500
Co1—O102.096 (4)C13—C141.422 (9)
Co1—O10i2.096 (4)C13—H130.9500
Co1—O2i2.110 (4)C14—C151.425 (8)
Co1—O22.110 (4)C15—C161.380 (9)
N1—C61.351 (7)C16—C171.422 (8)
N1—C51.350 (7)C16—C191.503 (8)
N1—C71.502 (6)C17—H170.9500
N2—C241.340 (7)C18—H18A0.9800
N2—C201.355 (7)C18—H18B0.9800
N2—C191.516 (7)C18—H18C0.9800
O1—C11.240 (7)C19—H19A0.9900
O2—C11.240 (7)C19—H19B0.9900
O3—C181.370 (9)C20—C211.370 (8)
O3—C151.389 (7)C20—H200.9500
O4—C251.222 (7)C21—C221.388 (8)
O5—C251.217 (7)C21—H210.9500
C1—C21.517 (8)C22—C231.389 (8)
C2—C61.379 (7)C22—H220.9500
C2—C31.386 (8)C23—C241.384 (8)
C3—C41.383 (8)C23—C251.544 (8)
C3—H30.9500C24—H240.9500
C4—C51.378 (8)Cl1—O81.410 (5)
C4—H40.9500Cl1—O71.413 (5)
C5—H50.9500Cl1—O61.423 (5)
C6—H60.9500Cl1—O91.446 (4)
C7—C81.509 (7)O10—H10A0.84 (4)
C7—H7A0.9900O10—H10B0.85 (4)
C7—H7B0.9900O11—H11A0.87 (4)
C8—C171.382 (8)O11—H11B0.86 (4)
C8—C91.424 (8)O12—H12A0.83 (4)
C9—C101.419 (9)O12—H12B0.87 (4)
C9—C141.421 (8)O13—H13A0.86 (4)
C10—C111.425 (10)O13—H13B0.86 (4)
C10—H100.9500O14—H14A0.86 (4)
C11—C121.402 (10)O14—H14B0.86 (4)
C11—H110.9500
O11—Co1—O11i180.0C13—C12—H12120.5
O11—Co1—O1089.89 (15)C14—C13—C12120.8 (5)
O11i—Co1—O1090.11 (15)C14—C13—H13119.6
O11—Co1—O10i90.11 (15)C12—C13—H13119.6
O11i—Co1—O10i89.89 (15)C9—C14—C13120.4 (5)
O10—Co1—O10i179.999 (1)C9—C14—C15119.7 (5)
O11—Co1—O2i90.63 (15)C13—C14—C15119.8 (5)
O11i—Co1—O2i89.37 (15)C16—C15—O3123.0 (5)
O10—Co1—O2i91.78 (15)C16—C15—C14120.4 (5)
O10i—Co1—O2i88.22 (15)O3—C15—C14116.3 (6)
O11—Co1—O289.37 (15)C15—C16—C17119.5 (5)
O11i—Co1—O290.63 (15)C15—C16—C19120.9 (5)
O10—Co1—O288.22 (15)C17—C16—C19119.1 (6)
O10i—Co1—O291.78 (15)C8—C17—C16121.6 (6)
O2i—Co1—O2179.998 (1)C8—C17—H17119.2
C6—N1—C5121.2 (4)C16—C17—H17119.2
C6—N1—C7119.1 (4)O3—C18—H18A109.5
C5—N1—C7119.6 (4)O3—C18—H18B109.5
C24—N2—C20120.7 (5)H18A—C18—H18B109.5
C24—N2—C19122.8 (4)O3—C18—H18C109.5
C20—N2—C19116.5 (4)H18A—C18—H18C109.5
C1—O2—Co1127.1 (4)H18B—C18—H18C109.5
C18—O3—C15117.9 (6)C16—C19—N2115.7 (4)
O2—C1—O1126.4 (5)C16—C19—H19A108.3
O2—C1—C2116.4 (5)N2—C19—H19A108.3
O1—C1—C2117.2 (5)C16—C19—H19B108.3
C6—C2—C3118.9 (5)N2—C19—H19B108.3
C6—C2—C1120.1 (5)H19A—C19—H19B107.4
C3—C2—C1121.0 (5)N2—C20—C21120.3 (5)
C4—C3—C2119.6 (5)N2—C20—H20119.8
C4—C3—H3120.2C21—C20—H20119.8
C2—C3—H3120.2C20—C21—C22119.6 (5)
C5—C4—C3119.8 (5)C20—C21—H21120.2
C5—C4—H4120.1C22—C21—H21120.2
C3—C4—H4120.1C21—C22—C23119.7 (5)
N1—C5—C4119.8 (5)C21—C22—H22120.1
N1—C5—H5120.1C23—C22—H22120.1
C4—C5—H5120.1C24—C23—C22118.2 (5)
N1—C6—C2120.6 (5)C24—C23—C25119.7 (5)
N1—C6—H6119.7C22—C23—C25122.1 (5)
C2—C6—H6119.7N2—C24—C23121.4 (5)
N1—C7—C8114.6 (4)N2—C24—H24119.3
N1—C7—H7A108.6C23—C24—H24119.3
C8—C7—H7A108.6O5—C25—O4129.2 (5)
N1—C7—H7B108.6O5—C25—C23115.8 (5)
C8—C7—H7B108.6O4—C25—C23115.0 (5)
H7A—C7—H7B107.6O8—Cl1—O7109.3 (4)
C17—C8—C9119.5 (5)O8—Cl1—O6110.4 (3)
C17—C8—C7118.3 (5)O7—Cl1—O6109.7 (4)
C9—C8—C7121.7 (5)O8—Cl1—O9109.5 (3)
C10—C9—C14117.9 (5)O7—Cl1—O9109.0 (3)
C10—C9—C8122.8 (5)O6—Cl1—O9108.9 (3)
C14—C9—C8119.3 (5)Co1—O10—H10A116 (5)
C9—C10—C11121.7 (5)Co1—O10—H10B96 (4)
C9—C10—H10119.1H10A—O10—H10B109 (4)
C11—C10—H10119.1Co1—O11—H11A116 (4)
C12—C11—C10120.0 (6)Co1—O11—H11B124 (4)
C12—C11—H11120.0H11A—O11—H11B105 (4)
C10—C11—H11120.0H12A—O12—H12B107 (5)
C11—C12—C13119.0 (6)H13A—O13—H13B105 (4)
C11—C12—H12120.5H14A—O14—H14B105 (4)
O11—Co1—O2—C1107.3 (5)C10—C9—C14—C15178.3 (5)
O11i—Co1—O2—C172.7 (5)C8—C9—C14—C150.2 (7)
O10—Co1—O2—C1162.8 (5)C12—C13—C14—C93.4 (8)
O10i—Co1—O2—C117.2 (5)C12—C13—C14—C15178.5 (5)
O2i—Co1—O2—C140 (29)C18—O3—C15—C1684.6 (8)
Co1—O2—C1—O14.0 (10)C18—O3—C15—C14101.7 (8)
Co1—O2—C1—C2174.9 (4)C9—C14—C15—C160.8 (8)
O2—C1—C2—C6173.3 (5)C13—C14—C15—C16178.9 (5)
O1—C1—C2—C67.7 (9)C9—C14—C15—O3173.1 (5)
O2—C1—C2—C38.1 (9)C13—C14—C15—O35.0 (7)
O1—C1—C2—C3171.0 (7)O3—C15—C16—C17172.9 (5)
C6—C2—C3—C41.2 (9)C14—C15—C16—C170.6 (8)
C1—C2—C3—C4177.5 (6)O3—C15—C16—C191.3 (8)
C2—C3—C4—C50.4 (9)C14—C15—C16—C19172.2 (5)
C6—N1—C5—C41.7 (8)C9—C8—C17—C161.7 (8)
C7—N1—C5—C4178.1 (5)C7—C8—C17—C16170.2 (5)
C3—C4—C5—N11.1 (9)C15—C16—C17—C80.7 (8)
C5—N1—C6—C21.0 (8)C19—C16—C17—C8171.1 (5)
C7—N1—C6—C2177.4 (5)C15—C16—C19—N292.2 (7)
C3—C2—C6—N10.5 (8)C17—C16—C19—N296.1 (6)
C1—C2—C6—N1178.2 (5)C24—N2—C19—C1616.4 (8)
C6—N1—C7—C861.4 (6)C20—N2—C19—C16166.5 (5)
C5—N1—C7—C8122.1 (5)C24—N2—C20—C212.2 (8)
N1—C7—C8—C17114.7 (5)C19—N2—C20—C21179.3 (5)
N1—C7—C8—C973.6 (6)N2—C20—C21—C220.5 (9)
C17—C8—C9—C10179.5 (5)C20—C21—C22—C232.6 (9)
C7—C8—C9—C107.8 (8)C21—C22—C23—C242.2 (8)
C17—C8—C9—C141.5 (7)C21—C22—C23—C25178.1 (5)
C7—C8—C9—C14170.2 (5)C20—N2—C24—C232.6 (8)
C14—C9—C10—C114.3 (9)C19—N2—C24—C23179.6 (5)
C8—C9—C10—C11177.6 (6)C22—C23—C24—N20.4 (8)
C9—C10—C11—C125.8 (10)C25—C23—C24—N2179.3 (5)
C10—C11—C12—C132.5 (9)C24—C23—C25—O5166.5 (5)
C11—C12—C13—C142.0 (9)C22—C23—C25—O513.3 (8)
C10—C9—C14—C130.2 (8)C24—C23—C25—O414.9 (8)
C8—C9—C14—C13177.9 (5)C22—C23—C25—O4165.4 (5)
Symmetry code: (i) x+3, y+1, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O10—H10A···O13ii0.84 (4)1.83 (4)2.665 (5)171 (6)
O10—H10B···O1i0.85 (4)1.84 (4)2.668 (6)166 (6)
O11—H11A···O12ii0.87 (4)1.83 (4)2.690 (6)174 (7)
O11—H11B···O14iii0.86 (4)1.85 (4)2.701 (5)173 (6)
O12—H12A···O10.83 (4)1.84 (5)2.654 (6)164 (8)
O12—H12B···O40.87 (4)1.91 (4)2.772 (6)173 (8)
O13—H13A···O5iv0.86 (4)1.94 (4)2.787 (6)172 (7)
O13—H13B···O9v0.86 (4)1.95 (4)2.815 (6)175 (7)
O13—H13B···Cl1v0.86 (4)2.69 (6)3.451 (4)147 (6)
O14—H14A···O4ii0.86 (4)1.88 (4)2.724 (6)165 (7)
O14—H14B···O5vi0.86 (4)1.98 (4)2.811 (6)160 (7)
Symmetry codes: (i) x+3, y+1, z+1; (ii) x+2, y+1, z+1; (iii) x+1, y, z; (iv) x+2, y, z+1; (v) x+1, y, z+1; (vi) x1, y+1, z.

Experimental details

Crystal data
Chemical formula[Co(C25H20N2O5)2(H2O)4](ClO4)2·6H2O
Mr1294.86
Crystal system, space groupTriclinic, P1
Temperature (K)113
a, b, c (Å)7.9162 (19), 12.703 (3), 14.757 (3)
α, β, γ (°)71.159 (6), 89.759 (8), 77.175 (7)
V3)1365.7 (5)
Z1
Radiation typeMo Kα
µ (mm1)0.51
Crystal size (mm)0.18 × 0.16 × 0.14
Data collection
DiffractometerRigaku Saturn
diffractometer
Absorption correctionMulti-scan
(Jacobson, 1998)
Tmin, Tmax0.914, 0.932
No. of measured, independent and
observed [I > 2σ(I)] reflections
12559, 4738, 4261
Rint0.024
(sin θ/λ)max1)0.595
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.057, 0.128, 1.08
No. of reflections4738
No. of parameters417
No. of restraints17
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)1.27, 0.45

Computer programs: CrystalClear (Rigaku, 2002), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), [PLEASE PROVIDE SOFTWARE/REFERENCE], CrystalStructure (Rigaku, 2002).

Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O10—H10A···O13i0.84 (4)1.83 (4)2.665 (5)171 (6)
O10—H10B···O1ii0.85 (4)1.84 (4)2.668 (6)166 (6)
O11—H11A···O12i0.87 (4)1.83 (4)2.690 (6)174 (7)
O11—H11B···O14iii0.86 (4)1.85 (4)2.701 (5)173 (6)
O12—H12A···O10.83 (4)1.84 (5)2.654 (6)164 (8)
O12—H12B···O40.87 (4)1.91 (4)2.772 (6)173 (8)
O13—H13A···O5iv0.86 (4)1.94 (4)2.787 (6)172 (7)
O13—H13B···O9v0.86 (4)1.95 (4)2.815 (6)175 (7)
O13—H13B···Cl1v0.86 (4)2.69 (6)3.451 (4)147 (6)
O14—H14A···O4i0.86 (4)1.88 (4)2.724 (6)165 (7)
O14—H14B···O5vi0.86 (4)1.98 (4)2.811 (6)160 (7)
Symmetry codes: (i) x+2, y+1, z+1; (ii) x+3, y+1, z+1; (iii) x+1, y, z; (iv) x+2, y, z+1; (v) x+1, y, z+1; (vi) x1, y+1, z.
 

References

First citationJacobson, R. (1998). Private communication to the Rigaku Corporation, Tokyo, Japan.  Google Scholar
First citationLi, H.-S., Li, S.-L. & Hou, J.-F. (2006). Acta Cryst. E62, m2143–m2144.  Web of Science CSD CrossRef IUCr Journals Google Scholar
First citationRigaku (2002). CrystalClear and CrystalStructure. Rigaku Corporation, Tokyo, Japan.  Google Scholar
First citationSheldrick, G. M. (2008). Acta Cryst. A64, 112–122.  Web of Science CrossRef CAS IUCr Journals Google Scholar

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