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The azide-bridged mixed-valent cobalt(II,III) compound [(CH3)3NH]2[CoIICo2III(N3)10]

aPharmacy College, Henan University of Traditional Chinese Medicine, Zhengzhou 450008, People's Republic of China
*Correspondence e-mail: liuyanju886@163.com

(Received 14 November 2010; accepted 26 November 2010; online 4 December 2010)

The crystal structure of the title compound, poly[bis­(tri­methyl­ammonium) hexa-μ1,1-azido-tetra­azido­tricobalt­ate(II,III)], [(CH3)3NH]2[CoIICoIII2(N3)10], consists of anionic chains [CoIICoIII2(N3)10]2− extending parallel to the c axis and [(CH3)3NH]+ counter-cations situated between the chains. In the anionic chain, one tetra­hedrally coordinated CoII atom (site symmetry 2) and two octa­hedrally coordinated CoIII atoms are arranged alternately and are linked by μ1,1-azide bridges. The anionic chains and cations are connected via N—H⋯N hydrogen bonding into a three-dimensional structure.

Related literature

For background to transition-metal azido-complexes templated by counter-cations of various sizes, see: Liu et al. (2006[Liu, T., Zhang, Y.-J., Wang, Z.-M. & Gao, S. (2006). Inorg. Chem. 45, 2782-2784.], 2008[Liu, T., Yang, Y.-F., Wang, Z.-M. & Gao, S. (2008). Chem. Asian. J. 3, 950-957.]). For related cobalt complexes, see: Zhang et al. (2010[Zhang, Y.-J., Liu, T., Kanegawa, S. & Sato, O. (2010). J. Am. Chem. Soc. 132, 912-913.]).

[Scheme 1]

Experimental

Crystal data
  • (C3H10N)2[Co3(N3)10]

  • Mr = 717.33

  • Monoclinic, C 2/c

  • a = 21.7200 (6) Å

  • b = 11.3812 (4) Å

  • c = 12.1628 (4) Å

  • β = 115.524 (2)°

  • V = 2713.21 (15) Å3

  • Z = 4

  • Mo Kα radiation

  • μ = 1.88 mm−1

  • T = 293 K

  • 0.10 × 0.06 × 0.05 mm

Data collection
  • Rigaku Saturn diffractometer

  • Absorption correction: multi-scan (REQAB; Jacobson, 1998[Jacobson, R. (1998). REQAB. Private communication to the Rigaku Corporation, Tokyo, Japan.]) Tmin = 0.708, Tmax = 0.823

  • 22049 measured reflections

  • 2389 independent reflections

  • 1481 reflections with I > 2σ(I)

  • Rint = 0.103

Refinement
  • R[F2 > 2σ(F2)] = 0.032

  • wR(F2) = 0.061

  • S = 0.98

  • 2389 reflections

  • 190 parameters

  • 24 restraints

  • H-atom parameters constrained

  • Δρmax = 0.31 e Å−3

  • Δρmin = −0.35 e Å−3

Table 1
Selected bond lengths (Å)

Co1—N7 1.944 (3)
Co1—N4 1.948 (3)
Co1—N10 1.964 (3)
Co1—N1 1.979 (3)
Co1—N13i 2.008 (3)
Co1—N13 2.008 (3)
Co2—N1ii 1.968 (3)
Co2—N1 1.968 (3)
Co2—N10i 2.014 (3)
Co2—N10iii 2.014 (3)
Symmetry codes: (i) -x, -y, -z; (ii) [-x, y, -z+{\script{1\over 2}}]; (iii) [x, -y, z+{\script{1\over 2}}].

Table 2
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A DA D—H⋯A
N16—H16⋯N7 0.91 2.02 2.890 159

Data collection: CrystalClear (Rigaku/MSC, 2006[Rigaku/MSC (2006). CrystalClear. Rigaku/MSC, The Woodlands, Texas, USA.]); 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: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); software used to prepare material for publication: publCIF (Westrip, 2010[Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.]).

Supporting information


Comment top

Azido-bridged complexes have attracted a lot of attention in recent times because of their importance in diverse fields, encompassing condensed matter physics, materials chemistry, biological chemistry, etc. Having diverse coordination modes and being an efficient magnetic coupler, the azide anion is a versatile ligand in bridging different transition metals, generating rich and fascinating architectures ranging from discrete polynuclears to extended three-dimensional networks with interesting magnetic properties (antiferromagnetic, ferromagnetic, ferrimagnetic, canted and alternating systems). In fact, remarkable structural variations of azido-bridged complexes have been reported by using various ancillary ligands, with different number of coordination sites and steric hindrance, to control over the dimensions of complexes and bridging modes of the azide anions, thus leading to the control over their magnetic properties. However, only a few metal-azido systems devoid of ancillary ligands have been obtained by varying the size of the coutercations (Liu et al., 2006, 2008). A small coutercation such as (CH3)4N+ produced the one-dimensional ferromagnetic complex [(CH3)4N][Cu(N3)3], in which the Cu(II) ions are connected by a triple azido-bridge, including two µ1,3-N3 and one µ1,1-N3 anions. When more bulky coutercations were employed, the mononuclear paramagnetic complex [(CH3CH2)4N]2[Cu(N3)4], the dinuclear antiferromagnetic complex [(CH3CH2CH2CH2)4N]2[Cu2(N3)6] and the one-dimensional ferromagnetic complex [(CH3CH2CH2)4N]2[Cu3(N3)8] were obtained separately. For magnese(II)-azido complexes, use of small coutercations like (CH3)4N+ and Cs+ produced compounds with interesting three-dimensional structures [(CH3)4N][Mn(N3)3] and Cs[Mn(N3)3], where the cations are situated in the voids the anionic MnII-azido network. When using the more bulky cation (CH3CH2)4N+, the one-dimensional ferromagnetic complex [(CH3CH2)4N][Mn(N3)3] was obtained. Despite the results obtained above, azido-bridged complexes with mixed-valent metal ions have not been reported. In this work, we report on a mixed-valence cobalt(II,III) complex, [(CH3)3NH]2[CoIICoIII2(N3)10], (I).

The structure of (I) consists of anionic chains [CoIICoIII2(N3)10]2- extending parallel to the c-axis. The [(CH3)3NH]+ countercations are situated between the chains (Fig. 1). In the [CoIICoIII2(N3)10]2- anionic chain, the CoII atom (Co2, site symmetry 2) is tetrahedrally coordinated by N atoms, whereas the CoIII atom (Co1) is octahedrally coordinated. CoII and CoIII atoms are linked by µ1,1-azido ligands and are alternatively arranged along the chain direction. The Co1—N distances range between 1.944 (3)–2.008 (3) Å, slightly longer than those expected for CoIII. The Co2—N distances range between 1.968 (3)–2.014 (3) Å, slightly shorter than those expected for CoII (Zhang et al., 2010). The anionic chain and the cations are connected via N—H···N hydrogen bonding between the donating N—H function of the cation and non-bridging azido groups of the anion (Fig 2).

Related literature top

For background to transition-metal azido-complexes templated by counter-cations with various sizes, see: Liu et al. (2006, 2008). For related cobalt complexes, see: Zhang et al. (2010).

Experimental top

In a test tube a 5 ml methanol solution of 0.10M Co(ClO4)2.6H2O was layered carefully with 3 ml methanol and then with 10 ml methanol solution of 0.20M HCl, 0.20M NaN3, and 0.10M trimethylamine. The tube was sealed and kept undisturbed. Tiny red columnar crystals appeared overnight. Crystallization time of one week produced crystals in a yield of 25% based on the metal salt.

Refinement top

Hydrogen atoms were added geometrically and were refined using a riding model, with C—H = 0.98 Å (CH3) and N—H = 0.89 Å.

Structure description top

Azido-bridged complexes have attracted a lot of attention in recent times because of their importance in diverse fields, encompassing condensed matter physics, materials chemistry, biological chemistry, etc. Having diverse coordination modes and being an efficient magnetic coupler, the azide anion is a versatile ligand in bridging different transition metals, generating rich and fascinating architectures ranging from discrete polynuclears to extended three-dimensional networks with interesting magnetic properties (antiferromagnetic, ferromagnetic, ferrimagnetic, canted and alternating systems). In fact, remarkable structural variations of azido-bridged complexes have been reported by using various ancillary ligands, with different number of coordination sites and steric hindrance, to control over the dimensions of complexes and bridging modes of the azide anions, thus leading to the control over their magnetic properties. However, only a few metal-azido systems devoid of ancillary ligands have been obtained by varying the size of the coutercations (Liu et al., 2006, 2008). A small coutercation such as (CH3)4N+ produced the one-dimensional ferromagnetic complex [(CH3)4N][Cu(N3)3], in which the Cu(II) ions are connected by a triple azido-bridge, including two µ1,3-N3 and one µ1,1-N3 anions. When more bulky coutercations were employed, the mononuclear paramagnetic complex [(CH3CH2)4N]2[Cu(N3)4], the dinuclear antiferromagnetic complex [(CH3CH2CH2CH2)4N]2[Cu2(N3)6] and the one-dimensional ferromagnetic complex [(CH3CH2CH2)4N]2[Cu3(N3)8] were obtained separately. For magnese(II)-azido complexes, use of small coutercations like (CH3)4N+ and Cs+ produced compounds with interesting three-dimensional structures [(CH3)4N][Mn(N3)3] and Cs[Mn(N3)3], where the cations are situated in the voids the anionic MnII-azido network. When using the more bulky cation (CH3CH2)4N+, the one-dimensional ferromagnetic complex [(CH3CH2)4N][Mn(N3)3] was obtained. Despite the results obtained above, azido-bridged complexes with mixed-valent metal ions have not been reported. In this work, we report on a mixed-valence cobalt(II,III) complex, [(CH3)3NH]2[CoIICoIII2(N3)10], (I).

The structure of (I) consists of anionic chains [CoIICoIII2(N3)10]2- extending parallel to the c-axis. The [(CH3)3NH]+ countercations are situated between the chains (Fig. 1). In the [CoIICoIII2(N3)10]2- anionic chain, the CoII atom (Co2, site symmetry 2) is tetrahedrally coordinated by N atoms, whereas the CoIII atom (Co1) is octahedrally coordinated. CoII and CoIII atoms are linked by µ1,1-azido ligands and are alternatively arranged along the chain direction. The Co1—N distances range between 1.944 (3)–2.008 (3) Å, slightly longer than those expected for CoIII. The Co2—N distances range between 1.968 (3)–2.014 (3) Å, slightly shorter than those expected for CoII (Zhang et al., 2010). The anionic chain and the cations are connected via N—H···N hydrogen bonding between the donating N—H function of the cation and non-bridging azido groups of the anion (Fig 2).

For background to transition-metal azido-complexes templated by counter-cations with various sizes, see: Liu et al. (2006, 2008). For related cobalt complexes, see: Zhang et al. (2010).

Computing details top

Data collection: CrystalClear (Rigaku/MSC, 2006); cell refinement: CrystalClear (Rigaku/MSC, 2006); data reduction: CrystalClear (Rigaku/MSC, 2006); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: publCIF (Westrip, 2010).

Figures top
[Figure 1] Fig. 1. The asymmetric unit of the title structure. All non-H atoms are labelled and are shown with displacement ellipsoids at the 30% probability level. H atoms have been omitted.
[Figure 2] Fig. 2. A view of the crystal packing along the c axis.
poly[bis(trimethylammonium) [hexa-µ1,1-azido-tetraazidotricobaltate(II,III)]] top
Crystal data top
(C3H10N)2[Co3(N3)10]F(000) = 1444
Mr = 717.33Dx = 1.756 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 14377 reflections
a = 21.7200 (6) Åθ = 3.4–25.0°
b = 11.3812 (4) ŵ = 1.88 mm1
c = 12.1628 (4) ÅT = 293 K
β = 115.524 (2)°Pillar, red
V = 2713.21 (15) Å30.10 × 0.06 × 0.05 mm
Z = 4
Data collection top
Rigaku Saturn
diffractometer
2389 independent reflections
Radiation source: fine-focus sealed tube1481 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.103
Detector resolution: 0.76 pixels mm-1θmax = 25.0°, θmin = 3.6°
dtprofit.ref scansh = 2525
Absorption correction: multi-scan
(REQAB; Jacobson, 1998)
k = 1313
Tmin = 0.708, Tmax = 0.823l = 1414
22049 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)] = 0.032H-atom parameters constrained
wR(F2) = 0.061 w = 1/[σ2(Fo2) + (0.0204P)2]
where P = (Fo2 + 2Fc2)/3
S = 0.98(Δ/σ)max = 0.001
2389 reflectionsΔρmax = 0.31 e Å3
190 parametersΔρmin = 0.35 e Å3
24 restraintsExtinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.00084 (18)
Crystal data top
(C3H10N)2[Co3(N3)10]V = 2713.21 (15) Å3
Mr = 717.33Z = 4
Monoclinic, C2/cMo Kα radiation
a = 21.7200 (6) ŵ = 1.88 mm1
b = 11.3812 (4) ÅT = 293 K
c = 12.1628 (4) Å0.10 × 0.06 × 0.05 mm
β = 115.524 (2)°
Data collection top
Rigaku Saturn
diffractometer
2389 independent reflections
Absorption correction: multi-scan
(REQAB; Jacobson, 1998)
1481 reflections with I > 2σ(I)
Tmin = 0.708, Tmax = 0.823Rint = 0.103
22049 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.03224 restraints
wR(F2) = 0.061H-atom parameters constrained
S = 0.98Δρmax = 0.31 e Å3
2389 reflectionsΔρmin = 0.35 e Å3
190 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
Co10.04965 (2)0.10300 (4)0.05706 (4)0.03529 (17)
Co20.00000.04737 (5)0.25000.0402 (2)
N10.06948 (14)0.0409 (2)0.2209 (3)0.0428 (6)
N20.12002 (17)0.0827 (3)0.3042 (3)0.0448 (6)
N30.16669 (18)0.1210 (3)0.3810 (3)0.0740 (10)
N40.14720 (14)0.1256 (2)0.1097 (3)0.0523 (7)
N50.16894 (15)0.1348 (3)0.0363 (3)0.0540 (7)
N60.1925 (2)0.1442 (4)0.0308 (4)0.1069 (15)
N70.04578 (16)0.2621 (2)0.1120 (3)0.0489 (8)
N80.00656 (18)0.3009 (3)0.1097 (3)0.0504 (8)
N90.05415 (18)0.3426 (3)0.1100 (3)0.0806 (12)
N100.02748 (13)0.1593 (3)0.1084 (2)0.0434 (6)
N110.04393 (15)0.2609 (3)0.1156 (2)0.0492 (6)
N120.0599 (2)0.3555 (3)0.1195 (3)0.0930 (13)
N130.04827 (13)0.0595 (2)0.0083 (2)0.0384 (6)
N140.09288 (16)0.1253 (3)0.0627 (3)0.0425 (6)
N150.13450 (17)0.1858 (3)0.1255 (3)0.0715 (10)
N160.16193 (14)0.4179 (3)0.2144 (3)0.0539 (8)
H160.13360.35540.18280.065*
C10.2022 (2)0.3949 (5)0.3459 (4)0.1044 (17)
H1A0.22920.46280.38400.157*
H1B0.23160.32870.35650.157*
H1C0.17190.37830.38260.157*
C20.1190 (3)0.5217 (4)0.1950 (5)0.1125 (19)
H2A0.08520.50670.22420.169*
H2B0.09700.53960.10960.169*
H2C0.14680.58710.23840.169*
C30.2062 (2)0.4251 (5)0.1509 (4)0.1121 (19)
H3A0.17870.43790.06550.168*
H3B0.23110.35290.16210.168*
H3C0.23770.48910.18370.168*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co10.0382 (3)0.0364 (3)0.0331 (3)0.0041 (2)0.0171 (2)0.0013 (2)
Co20.0487 (4)0.0370 (4)0.0412 (5)0.0000.0253 (4)0.000
N10.0456 (15)0.0502 (15)0.0338 (16)0.0052 (12)0.0181 (13)0.0022 (12)
N20.0475 (15)0.0518 (15)0.0353 (16)0.0042 (13)0.0180 (13)0.0033 (13)
N30.065 (2)0.095 (3)0.052 (2)0.019 (2)0.015 (2)0.006 (2)
N40.0449 (15)0.0647 (16)0.0528 (17)0.0104 (12)0.0264 (12)0.0027 (13)
N50.0453 (15)0.0637 (16)0.0561 (18)0.0079 (12)0.0249 (13)0.0055 (13)
N60.097 (3)0.148 (4)0.112 (4)0.027 (3)0.079 (3)0.026 (3)
N70.061 (2)0.0407 (19)0.051 (2)0.0085 (16)0.0293 (18)0.0088 (15)
N80.062 (2)0.040 (2)0.050 (2)0.0019 (17)0.025 (2)0.0050 (15)
N90.071 (3)0.068 (3)0.103 (3)0.009 (2)0.037 (3)0.020 (2)
N100.0570 (15)0.0435 (16)0.0329 (14)0.0095 (13)0.0222 (12)0.0004 (13)
N110.0626 (15)0.0478 (16)0.0348 (15)0.0086 (14)0.0186 (12)0.0007 (13)
N120.150 (4)0.054 (2)0.064 (3)0.036 (2)0.036 (3)0.004 (2)
N130.0378 (15)0.0388 (15)0.0414 (17)0.0002 (10)0.0197 (13)0.0025 (11)
N140.0408 (15)0.0412 (16)0.0447 (17)0.0017 (11)0.0176 (13)0.0036 (11)
N150.058 (2)0.058 (2)0.081 (3)0.0085 (19)0.014 (2)0.005 (2)
N160.0501 (19)0.050 (2)0.061 (2)0.0163 (15)0.0234 (19)0.0118 (16)
C10.083 (3)0.143 (5)0.067 (4)0.039 (3)0.013 (3)0.007 (3)
C20.115 (4)0.052 (3)0.165 (6)0.015 (3)0.055 (4)0.001 (3)
C30.093 (4)0.173 (5)0.099 (4)0.055 (4)0.069 (3)0.045 (4)
Geometric parameters (Å, º) top
Co1—N71.944 (3)N11—N121.139 (4)
Co1—N41.948 (3)N13—N141.234 (4)
Co1—N101.964 (3)N13—Co1i2.008 (3)
Co1—N11.979 (3)N14—N151.131 (4)
Co1—N13i2.008 (3)N16—C21.460 (5)
Co1—N132.008 (3)N16—C31.473 (4)
Co2—N1ii1.968 (3)N16—C11.478 (5)
Co2—N11.968 (3)N16—H160.9100
Co2—N10i2.014 (3)C1—H1A0.9600
Co2—N10iii2.014 (3)C1—H1B0.9600
N1—N21.224 (4)C1—H1C0.9600
N2—N31.129 (4)C2—H2A0.9600
N4—N51.181 (4)C2—H2B0.9600
N5—N61.140 (4)C2—H2C0.9600
N7—N81.209 (4)C3—H3A0.9600
N8—N91.139 (4)C3—H3B0.9600
N10—N111.225 (4)C3—H3C0.9600
N10—Co2i2.014 (3)
N7—Co1—N488.05 (12)Co1—N10—Co2i121.43 (14)
N7—Co1—N1091.18 (12)N12—N11—N10178.5 (4)
N4—Co1—N1092.62 (12)N14—N13—Co1i114.1 (2)
N7—Co1—N190.55 (12)N14—N13—Co1118.0 (2)
N4—Co1—N188.97 (12)Co1i—N13—Co1100.22 (11)
N10—Co1—N1177.69 (12)N15—N14—N13178.2 (4)
N7—Co1—N13i176.56 (13)C2—N16—C3112.7 (4)
N4—Co1—N13i94.61 (11)C2—N16—C1110.9 (4)
N10—Co1—N13i86.53 (11)C3—N16—C1111.2 (3)
N1—Co1—N13i91.67 (11)C2—N16—H16107.3
N7—Co1—N1397.71 (11)C3—N16—H16107.3
N4—Co1—N13173.16 (12)C1—N16—H16107.3
N10—Co1—N1390.96 (11)N16—C1—H1A109.5
N1—Co1—N1387.29 (11)N16—C1—H1B109.5
N13i—Co1—N1379.78 (11)H1A—C1—H1B109.5
N1ii—Co2—N1118.61 (16)N16—C1—H1C109.5
N1ii—Co2—N10i120.58 (11)H1A—C1—H1C109.5
N1—Co2—N10i97.86 (11)H1B—C1—H1C109.5
N1ii—Co2—N10iii97.86 (11)N16—C2—H2A109.5
N1—Co2—N10iii120.58 (11)N16—C2—H2B109.5
N10i—Co2—N10iii101.58 (16)H2A—C2—H2B109.5
N2—N1—Co2122.3 (2)N16—C2—H2C109.5
N2—N1—Co1115.0 (2)H2A—C2—H2C109.5
Co2—N1—Co1120.82 (15)H2B—C2—H2C109.5
N3—N2—N1179.9 (5)N16—C3—H3A109.5
N5—N4—Co1119.7 (3)N16—C3—H3B109.5
N6—N5—N4177.2 (4)H3A—C3—H3B109.5
N8—N7—Co1120.8 (2)N16—C3—H3C109.5
N9—N8—N7176.5 (4)H3A—C3—H3C109.5
N11—N10—Co1115.5 (2)H3B—C3—H3C109.5
N11—N10—Co2i121.6 (2)
Symmetry codes: (i) x, y, z; (ii) x, y, z+1/2; (iii) x, y, z+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N16—H16···N70.912.022.890159

Experimental details

Crystal data
Chemical formula(C3H10N)2[Co3(N3)10]
Mr717.33
Crystal system, space groupMonoclinic, C2/c
Temperature (K)293
a, b, c (Å)21.7200 (6), 11.3812 (4), 12.1628 (4)
β (°) 115.524 (2)
V3)2713.21 (15)
Z4
Radiation typeMo Kα
µ (mm1)1.88
Crystal size (mm)0.10 × 0.06 × 0.05
Data collection
DiffractometerRigaku Saturn
Absorption correctionMulti-scan
(REQAB; Jacobson, 1998)
Tmin, Tmax0.708, 0.823
No. of measured, independent and
observed [I > 2σ(I)] reflections
22049, 2389, 1481
Rint0.103
(sin θ/λ)max1)0.595
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.032, 0.061, 0.98
No. of reflections2389
No. of parameters190
No. of restraints24
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.31, 0.35

Computer programs: CrystalClear (Rigaku/MSC, 2006), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008), publCIF (Westrip, 2010).

Selected bond lengths (Å) top
Co1—N71.944 (3)Co1—N132.008 (3)
Co1—N41.948 (3)Co2—N1ii1.968 (3)
Co1—N101.964 (3)Co2—N11.968 (3)
Co1—N11.979 (3)Co2—N10i2.014 (3)
Co1—N13i2.008 (3)Co2—N10iii2.014 (3)
Symmetry codes: (i) x, y, z; (ii) x, y, z+1/2; (iii) x, y, z+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N16—H16···N70.9102.0232.890158.68
 

Acknowledgements

This study was supported by the Doctoral Research Fund of Henan Chinese Medicine (BSJJ2009–38).

References

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