Di-μ-chlorido-bis­[aqua­(2,2′-bipyridine-κ2N,N′)chloridocobalt(II)]

Zhu, L.-L.; Sun, Y.; Zhang, H.-H.; Wang, Y.; Sun, B.-W.

doi:10.1107/S1600536809027846

metal-organic compounds

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ISSN: 2056-9890

Volume 65| Part 8| August 2009| Page m991

doi:10.1107/S1600536809027846

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Di-μ-chlorido-bis[aqua(2,2′-bipyridine-κ²N,N′)chloridocobalt(II)]

Li-Li Zhu,^a Yu Sun,^b ^* Huai-Hong Zhang,^c Yun Wang ^a and Bai-Wang Sun ^c

^aDepartment of Chemistry, Key Laboratory of Medicinal Chemistry for Natural Resources, Ministry of Education, Yunnan University, Kunming 650091, People's Republic of China, ^bCollege of Pharmacy, Jiangsu University, Zhenjiang 212013, People's Republic of China, and ^cOrdered Matter Science Research Center, College of Chemistry and Chemical Engineering, Southeast University, Nanjing 210096, People's Republic of China
^*Correspondence e-mail: chmsunbw@seu.edu.cn

(Received 10 July 2009; accepted 15 July 2009; online 25 July 2009)

The title complex, [Co₂Cl₄(C₁₀H₈N₂)₂(H₂O)₂], is composed of two Co^II atoms, each hexacoordinated by three Cl atoms, one 2,2′-bipyridine (bpy) ligand and one water molecule in a distorted octahedral geometry. Neighboring Co^II atoms are linked together by two Cl bridges, forming a dinuclear Co^II complex with inversion symmetry. There are intermolecular O—H⋯Cl hydrogen bonds and intermolecular π–π stacking interactions between adjacent bpy ligands [centroid–centroid distance = 3.617 (2) Å] in the structure.

Related literature

For Cl atoms acting as the bridging anions in transition metal complexes in multi-dimensional molecule-based magnetic materials, see: Jian et al. (2005 ). For related structures, see: Leznoff et al. (2003 ); Liu et al.(2004 ); Puschmann et al. (2001 ).

Experimental

Crystal data

[Co₂Cl₄(C₁₀H₈N₂)₂(H₂O)₂]
M_r = 608.06
Monoclinic, P 2₁ /n
a = 11.2939 (10) Å
b = 6.8969 (6) Å
c = 15.1339 (13) Å
β = 91.958 (3)°
V = 1178.14 (18) Å³
Z = 2
Mo Kα radiation
μ = 1.89 mm⁻¹
T = 293 K
0.26 × 0.20 × 0.20 mm

Data collection

Rigaku SCXmini diffractometer
Absorption correction: multi-scan (CrystalClear; Rigaku, 2005 ) T_min = 0.641, T_max = 0.688
11707 measured reflections
2693 independent reflections
2149 reflections with I > 2σ(I)
R_int = 0.054

Refinement

R[F² > 2σ(F²)] = 0.037
wR(F²) = 0.085
S = 1.03
2693 reflections
145 parameters
H-atom parameters constrained
Δρ_max = 0.41 e Å⁻³
Δρ_min = −0.49 e Å⁻³

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1—H1B⋯Cl1ⁱ	0.82	2.81	3.407 (2)	132
O1—H1C⋯Cl1ⁱⁱ	0.85	2.39	3.213 (2)	162
Symmetry codes: (i) -x+2, -y, -z+1; (ii) x, y+1, z.

Data collection: CrystalClear (Rigaku, 2005); cell refinement: CrystalClear; data reduction: CrystalClear; 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: SHELXTL.

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536809027846/at2843sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536809027846/at2843Isup2.hkl

checkCIF report

Comment top

In the study of multidimensional molecule-based magnetic materials and other areas, the Cl atoms acting as the bridging anions has frequently been used to bridge transition metal complexes (Jian et al., 2005). Many such compounds have been reported (Leznoff et al., 2003; Liu et al., 2004; Puschmann et al., 2001). Herein, we reported the structure of the title Co^II compound (I).

The two Co atoms are bridged by two Cl anions into a four-membered Co₂Cl₂ ring. The Co atom is six-coordinated by three Cl atoms, one water molecules and one 2,2'-bipy ligand in an octahedral geometry. The molecule has an inversion symmetry (Fig. 1). In the crystal structure, the intermolecular O—H···Cl hydrogen bonds connect the molecules of (I) into a one-dimensional chain structure. There are π-π stacking interactions between adjacent bpy (2,2'-bipyridine) ligands, where the centroid–centroid separations are 3.617 (2) Å. π-π stacking interaction existing in every two O—H···Cl hydrogen bonds chains, and forming pairs of complex molecules into a two-dimensional structure (Fig. 2). A supramolecular network structure is consolidated by π-π stacking and hydrogen bonds.

Related literature top

For Cl atoms acting as the bridging anions in transition metal complexes in multi-dimensional molecule-based magnetic materials, see: Jian et al. (2005). For related structures, see: Leznoff et al. (2003); Liu et al.(2004) ; Puschmann et al. (2001).

Experimental top

All chemicals used (reagent grade) were commercially available. To a 10 ml MeCN solution of cobalt dichloride hexahydrate (0.0238 g, 0.1 mmol), a 4 ml CH₂Cl₂ solution of 2,2'-bipyridine (0.0156 g, 0.1 mmol) was added dropwise with stirring. The resulting solution was continuously stirred for about 30 min, and then filtered. The filtrate was slowly evaporated at room temperature over several days, and colourless prism crystals suitable for X-ray analysis were obtained.

Computing details top

Data collection: CrystalClear (Rigaku, 2005); cell refinement: CrystalClear (Rigaku, 2005); data reduction: CrystalClear (Rigaku, 2005); 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: SHELXTL (Sheldrick, 2008).

Figures top

	Fig. 1. The molecular structure of the title compound with the atom-numbering scheme and all hydrogen atoms. Displacement ellipsoids are drawn at the 30% probability level. [Symmetry code A: 2 - x, -y, 1 - z]
	Fig. 2. Crystal packing of the compound (I). Hydrogen bonds are shown as dashed lines.

Di-µ-chlorido-bis[aqua(2,2'-bipyridine- κ²N,N')chloridocobalt(II)] top

Crystal data top

[Co₂Cl₄(C₁₀H₈N₂)₂(H₂O)₂]	F(000) = 612
M_r = 608.06	D_x = 1.714 Mg m⁻³
Monoclinic, P2₁/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 10382 reflections
a = 11.2939 (10) Å	θ = 3.2–27.7°
b = 6.8969 (6) Å	µ = 1.89 mm⁻¹
c = 15.1339 (13) Å	T = 293 K
β = 91.958 (3)°	Prism, colourless
V = 1178.14 (18) Å³	0.26 × 0.20 × 0.20 mm
Z = 2

Data collection top

Rigaku SCXmini diffractometer	2693 independent reflections
Radiation source: fine-focus sealed tube	2149 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.054
Detector resolution: 8.192 pixels mm^-1	θ_max = 27.5°, θ_min = 3.3°
ω scans	h = −14→14
Absorption correction: multi-scan (CrystalClear; Rigaku, 2005)	k = −8→8
T_min = 0.641, T_max = 0.688	l = −19→19
11707 measured reflections

Refinement top

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)] = 0.037	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.085	H-atom parameters constrained
S = 1.03	w = 1/[σ²(F_o²) + (0.0346P)² + 0.3472P] where P = (F_o² + 2F_c²)/3
2693 reflections	(Δ/σ)_max = 0.001
145 parameters	Δρ_max = 0.41 e Å⁻³
0 restraints	Δρ_min = −0.49 e Å⁻³

Crystal data top

[Co₂Cl₄(C₁₀H₈N₂)₂(H₂O)₂]	V = 1178.14 (18) Å³
M_r = 608.06	Z = 2
Monoclinic, P2₁/n	Mo Kα radiation
a = 11.2939 (10) Å	µ = 1.89 mm⁻¹
b = 6.8969 (6) Å	T = 293 K
c = 15.1339 (13) Å	0.26 × 0.20 × 0.20 mm
β = 91.958 (3)°

Data collection top

Rigaku SCXmini diffractometer	2693 independent reflections
Absorption correction: multi-scan (CrystalClear; Rigaku, 2005)	2149 reflections with I > 2σ(I)
T_min = 0.641, T_max = 0.688	R_int = 0.054
11707 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.037	0 restraints
wR(F²) = 0.085	H-atom parameters constrained
S = 1.03	Δρ_max = 0.41 e Å⁻³
2693 reflections	Δρ_min = −0.49 e Å⁻³
145 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

	x	y	z	U_iso*/U_eq
Co1	0.84715 (3)	0.03942 (5)	0.50354 (2)	0.02938 (12)
O1	0.90322 (17)	0.3279 (3)	0.55130 (12)	0.0420 (5)
H1B	0.9629	0.3171	0.5833	0.050*
H1C	0.8639	0.4280	0.5357	0.050*
N1	0.71222 (19)	0.0653 (3)	0.59523 (14)	0.0328 (5)
N2	0.70852 (19)	0.1700 (3)	0.42759 (14)	0.0340 (5)
C1	0.7206 (3)	0.0099 (4)	0.67984 (19)	0.0418 (7)
H1A	0.7894	−0.0524	0.6999	0.050*
C2	0.6322 (3)	0.0407 (5)	0.7389 (2)	0.0504 (8)
H2A	0.6418	0.0035	0.7977	0.060*
C3	0.5291 (3)	0.1284 (4)	0.7079 (2)	0.0500 (8)
H3A	0.4673	0.1493	0.7459	0.060*
C4	0.5178 (3)	0.1848 (4)	0.6209 (2)	0.0441 (7)
H4A	0.4485	0.2437	0.5995	0.053*
C5	0.6114 (2)	0.1524 (4)	0.56541 (18)	0.0325 (6)
C6	0.6095 (2)	0.2104 (4)	0.47093 (19)	0.0345 (6)
C7	0.5126 (3)	0.2985 (4)	0.4275 (2)	0.0430 (7)
H7A	0.4448	0.3272	0.4581	0.052*
C8	0.5184 (3)	0.3423 (4)	0.3396 (2)	0.0513 (9)
H8A	0.4543	0.4011	0.3102	0.062*
C9	0.6192 (3)	0.2994 (4)	0.2947 (2)	0.0493 (8)
H9A	0.6242	0.3275	0.2348	0.059*
C10	0.7123 (3)	0.2134 (4)	0.34111 (19)	0.0430 (7)
H10A	0.7807	0.1842	0.3113	0.052*
Cl1	0.79648 (6)	−0.29082 (10)	0.45617 (5)	0.0445 (2)
Cl2	0.99818 (6)	0.07599 (10)	0.39243 (4)	0.03617 (17)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Co1	0.0223 (2)	0.0359 (2)	0.0300 (2)	0.00151 (15)	0.00089 (14)	0.00302 (16)
O1	0.0374 (11)	0.0386 (11)	0.0496 (12)	−0.0004 (9)	−0.0023 (9)	−0.0006 (10)
N1	0.0269 (12)	0.0365 (12)	0.0349 (12)	−0.0016 (10)	0.0014 (9)	−0.0011 (10)
N2	0.0264 (12)	0.0348 (12)	0.0405 (13)	−0.0018 (9)	−0.0020 (10)	0.0042 (10)
C1	0.0373 (17)	0.0510 (17)	0.0373 (15)	−0.0046 (13)	0.0049 (13)	0.0032 (13)
C2	0.052 (2)	0.063 (2)	0.0364 (16)	−0.0128 (17)	0.0123 (15)	−0.0067 (15)
C3	0.0406 (18)	0.0510 (19)	0.060 (2)	−0.0077 (15)	0.0227 (15)	−0.0188 (16)
C4	0.0323 (16)	0.0383 (16)	0.062 (2)	−0.0014 (13)	0.0101 (14)	−0.0134 (15)
C5	0.0263 (14)	0.0254 (13)	0.0459 (15)	−0.0025 (11)	0.0025 (12)	−0.0061 (12)
C6	0.0268 (14)	0.0259 (13)	0.0503 (16)	−0.0012 (11)	−0.0052 (12)	−0.0037 (12)
C7	0.0308 (15)	0.0313 (15)	0.066 (2)	0.0051 (12)	−0.0099 (14)	−0.0088 (14)
C8	0.051 (2)	0.0340 (16)	0.066 (2)	0.0049 (14)	−0.0279 (17)	0.0019 (15)
C9	0.051 (2)	0.0462 (18)	0.0489 (18)	−0.0039 (15)	−0.0170 (15)	0.0133 (15)
C10	0.0374 (16)	0.0493 (18)	0.0420 (16)	−0.0032 (13)	−0.0043 (13)	0.0103 (14)
Cl1	0.0343 (4)	0.0364 (4)	0.0624 (5)	−0.0001 (3)	−0.0050 (3)	−0.0031 (3)
Cl2	0.0264 (3)	0.0535 (4)	0.0286 (3)	0.0013 (3)	0.0003 (3)	0.0078 (3)

Geometric parameters (Å, º) top

Co1—N1	2.103 (2)	C2—H2A	0.9300
Co1—N2	2.112 (2)	C3—C4	1.375 (4)
Co1—O1	2.2021 (18)	C3—H3A	0.9300
Co1—Cl2ⁱ	2.4445 (7)	C4—C5	1.391 (4)
Co1—Cl2	2.4488 (7)	C4—H4A	0.9300
Co1—Cl1	2.4497 (8)	C5—C6	1.484 (4)
O1—H1B	0.8200	C6—C7	1.396 (4)
O1—H1C	0.8500	C7—C8	1.368 (4)
N1—C1	1.336 (3)	C7—H7A	0.9300
N1—C5	1.351 (3)	C8—C9	1.377 (5)
N2—C10	1.345 (3)	C8—H8A	0.9300
N2—C6	1.345 (3)	C9—C10	1.379 (4)
C1—C2	1.378 (4)	C9—H9A	0.9300
C1—H1A	0.9300	C10—H10A	0.9300
C2—C3	1.380 (5)	Cl2—Co1ⁱ	2.4445 (7)

N1—Co1—N2	77.44 (8)	C1—C2—H2A	121.0
N1—Co1—O1	85.04 (8)	C3—C2—H2A	121.0
N2—Co1—O1	89.59 (8)	C4—C3—C2	119.9 (3)
N1—Co1—Cl2ⁱ	96.93 (6)	C4—C3—H3A	120.1
N2—Co1—Cl2ⁱ	171.68 (7)	C2—C3—H3A	120.1
O1—Co1—Cl2ⁱ	83.78 (5)	C3—C4—C5	119.0 (3)
N1—Co1—Cl2	169.00 (6)	C3—C4—H4A	120.5
N2—Co1—Cl2	95.92 (6)	C5—C4—H4A	120.5
O1—Co1—Cl2	86.16 (5)	N1—C5—C4	121.3 (3)
Cl2ⁱ—Co1—Cl2	88.66 (2)	N1—C5—C6	115.2 (2)
N1—Co1—Cl1	96.01 (6)	C4—C5—C6	123.5 (3)
N2—Co1—Cl1	94.35 (6)	N2—C6—C7	120.8 (3)
O1—Co1—Cl1	176.05 (5)	N2—C6—C5	115.4 (2)
Cl2ⁱ—Co1—Cl1	92.31 (3)	C7—C6—C5	123.8 (3)
Cl2—Co1—Cl1	93.21 (3)	C8—C7—C6	119.4 (3)
Co1—O1—H1B	109.5	C8—C7—H7A	120.3
Co1—O1—H1C	120.1	C6—C7—H7A	120.3
H1B—O1—H1C	130.4	C7—C8—C9	120.0 (3)
C1—N1—C5	118.6 (2)	C7—C8—H8A	120.0
C1—N1—Co1	125.36 (19)	C9—C8—H8A	120.0
C5—N1—Co1	116.00 (17)	C8—C9—C10	118.0 (3)
C10—N2—C6	118.9 (2)	C8—C9—H9A	121.0
C10—N2—Co1	125.24 (19)	C10—C9—H9A	121.0
C6—N2—Co1	115.86 (18)	N2—C10—C9	122.9 (3)
N1—C1—C2	123.2 (3)	N2—C10—H10A	118.6
N1—C1—H1A	118.4	C9—C10—H10A	118.6
C2—C1—H1A	118.4	Co1ⁱ—Cl2—Co1	91.34 (2)
C1—C2—C3	118.0 (3)

N2—Co1—N1—C1	−179.5 (2)	C1—N1—C5—C6	179.7 (2)
O1—Co1—N1—C1	−88.8 (2)	Co1—N1—C5—C6	2.2 (3)
Cl2ⁱ—Co1—N1—C1	−5.7 (2)	C3—C4—C5—N1	0.6 (4)
Cl2—Co1—N1—C1	−125.8 (3)	C3—C4—C5—C6	−178.9 (3)
Cl1—Co1—N1—C1	87.3 (2)	C10—N2—C6—C7	−0.9 (4)
N2—Co1—N1—C5	−2.25 (17)	Co1—N2—C6—C7	179.38 (19)
O1—Co1—N1—C5	88.43 (18)	C10—N2—C6—C5	178.2 (2)
Cl2ⁱ—Co1—N1—C5	171.53 (17)	Co1—N2—C6—C5	−1.5 (3)
Cl2—Co1—N1—C5	51.4 (4)	N1—C5—C6—N2	−0.5 (3)
Cl1—Co1—N1—C5	−95.39 (17)	C4—C5—C6—N2	179.1 (2)
N1—Co1—N2—C10	−177.7 (2)	N1—C5—C6—C7	178.7 (2)
O1—Co1—N2—C10	97.3 (2)	C4—C5—C6—C7	−1.8 (4)
Cl2—Co1—N2—C10	11.2 (2)	N2—C6—C7—C8	0.7 (4)
Cl1—Co1—N2—C10	−82.5 (2)	C5—C6—C7—C8	−178.4 (3)
N1—Co1—N2—C6	1.99 (18)	C6—C7—C8—C9	0.0 (4)
O1—Co1—N2—C6	−83.02 (18)	C7—C8—C9—C10	−0.4 (4)
Cl2—Co1—N2—C6	−169.12 (17)	C6—N2—C10—C9	0.5 (4)
Cl1—Co1—N2—C6	97.19 (18)	Co1—N2—C10—C9	−179.8 (2)
C5—N1—C1—C2	−1.3 (4)	C8—C9—C10—N2	0.1 (4)
Co1—N1—C1—C2	175.9 (2)	N1—Co1—Cl2—Co1ⁱ	120.8 (3)
N1—C1—C2—C3	1.8 (5)	N2—Co1—Cl2—Co1ⁱ	173.04 (6)
C1—C2—C3—C4	−1.0 (5)	O1—Co1—Cl2—Co1ⁱ	83.85 (5)
C2—C3—C4—C5	−0.1 (4)	Cl2ⁱ—Co1—Cl2—Co1ⁱ	0.0
C1—N1—C5—C4	0.1 (4)	Cl1—Co1—Cl2—Co1ⁱ	−92.24 (3)
Co1—N1—C5—C4	−177.4 (2)

Symmetry code: (i) −x+2, −y, −z+1.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1B···Cl1ⁱ	0.82	2.81	3.407 (2)	132
O1—H1C···Cl1ⁱⁱ	0.85	2.39	3.213 (2)	162

Symmetry codes: (i) −x+2, −y, −z+1; (ii) x, y+1, z.

Experimental details

Crystal data
Chemical formula	[Co₂Cl₄(C₁₀H₈N₂)₂(H₂O)₂]
M_r	608.06
Crystal system, space group	Monoclinic, P2₁/n
Temperature (K)	293
a, b, c (Å)	11.2939 (10), 6.8969 (6), 15.1339 (13)
β (°)	91.958 (3)
V (Å³)	1178.14 (18)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	1.89
Crystal size (mm)	0.26 × 0.20 × 0.20

Data collection
Diffractometer	Rigaku SCXmini diffractometer
Absorption correction	Multi-scan (CrystalClear; Rigaku, 2005)
T_min, T_max	0.641, 0.688
No. of measured, independent and observed [I > 2σ(I)] reflections	11707, 2693, 2149
R_int	0.054
(sin θ/λ)_max (Å⁻¹)	0.649

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.037, 0.085, 1.03
No. of reflections	2693
No. of parameters	145
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.41, −0.49

Computer programs: CrystalClear (Rigaku, 2005), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1B···Cl1ⁱ	0.82	2.81	3.407 (2)	131.5
O1—H1C···Cl1ⁱⁱ	0.85	2.39	3.213 (2)	162.2

Symmetry codes: (i) −x+2, −y, −z+1; (ii) x, y+1, z.

References

Jian, F.-F., Wang, K.-F., Xiao, H.-L. & Qiao, Y.-B. (2005). Acta Cryst. E61, m1324–m1325. Web of Science CSD CrossRef IUCr Journals Google Scholar
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CRYSTALLOGRAPHIC
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ISSN: 2056-9890

Volume 65| Part 8| August 2009| Page m991

doi:10.1107/S1600536809027846

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