Tris(2,2′-bipyridine-κ2N,N′)cobalt(III) octa­cyanido­tungstate(V)

Jun, Q.; Zhang, C.

doi:10.1107/S1600536809051654

metal-organic compounds

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Volume 66| Part 1| January 2010| Page m12

doi:10.1107/S1600536809051654

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Tris(2,2′-bipyridine-κ²N,N′)cobalt(III) octacyanidotungstate(V)

Qian Jun ^a and Chi Zhang ^a ^*

^aMolecular Materials Research Center, School of Chemical Engineering, Nanjing University of Science and Technology, 200 Xiaolingwei Road, Nanjing 210094, People's Republic of China
^*Correspondence e-mail: zhangchinjust@yahoo.com

(Received 13 November 2009; accepted 1 December 2009; online 4 December 2009)

In the title compound, [Co(C₁₀H₈N₂)₃][W(CN)₈], the Co atom (..2 site symmetry) is coordinated by six N atoms from three 2,2′-bipyridine ligands in an octahedral geometry; the Co—N bond distances range from 1.926 (2) to 1.939 (2) Å. The W (..2 site symmetry) metal center is coordinated by eight cyanide ligands, resulting in a dodecahedral conformation with W—C distances in the range 1.165 (3)–2.176 (3) Å. The cations and anions are linked into a three-demensional structure by weak C—H⋯N hydrogen bonds.

Related literature

For compounds with similar architectures, see: Przychodzeń et al. (2006 ); Withers et al. (2005 ); Mathonière et al. (2005 ). For related structures, see: Liu et al. (2008 ); Chang et al. (2002 ).

Experimental

Crystal data

[Co(C₁₀H₈N₂)₃][W(CN)₈]
M_r = 919.48
Orthorhombic, P c c n
a = 11.465 (2) Å
b = 15.141 (3) Å
c = 20.007 (4) Å
V = 3473.0 (12) Å³
Z = 4
Mo Kα radiation
μ = 3.84 mm⁻¹
T = 250 K
0.20 × 0.20 × 0.20 mm

Data collection

Rigaku Mercury CCD diffractometer
Absorption correction: multi-scan (ABSCOR; Higashi, 1995 ) T_min = 0.841, T_max = 1.000
12594 measured reflections
3554 independent reflections
3023 reflections with I > 2σ(I)
R_int = 0.018

Refinement

R[F² > 2σ(F²)] = 0.026
wR(F²) = 0.059
S = 1.10
3554 reflections
245 parameters
H-atom parameters constrained
Δρ_max = 1.33 e Å⁻³
Δρ_min = −0.41 e Å⁻³

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
C4—H4A⋯N4ⁱ	0.93	2.53	3.371 (4)	151
C10—H10A⋯N1ⁱⁱ	0.93	2.54	3.032 (4)	114
C12—H12A⋯N2ⁱⁱ	0.93	2.51	3.008 (4)	114
C1—H1A⋯N3	0.93	2.50	2.993 (4)	113
Symmetry codes: (i) $[-x+1, y-{\script{1\over 2}}, -z+{\script{1\over 2}}]$ ; (ii) $[-x+{\script{1\over 2}}, -y+{\script{1\over 2}}, z]$ .

Data collection: CrystalClear (Rigaku, 2008 ); 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/S1600536809051654/pv2237sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536809051654/pv2237Isup2.hkl

checkCIF report

Comment top

As the direct addition of transition metal salts and [W(CN)₈] ions (Przychodzeń et al., 2006; Withers et al., 2005; Mathonière et al., 2005) leads to the immediate precipitation, the title compound was obtained through the interdiffusion method (Liu et al., 2008; Chang et al., 2002). Based on the crystal structure determination, the cations, [Co(C₁₀H₈N₂)₃]²⁺, and the anions, [W(CN)₈]^3-, have a molar ratio of 1:1. It means that the Co²⁺ of Co(ClO₄)₂ has been oxided into Co³⁺ during the reaction process.

As illustrated in Fig. 1, Co³⁺ has an octahedral geometry, coordinated by six nitrogen atoms from three 2,2'-bipyridine ligands. The W metal center is coordinated by eight cyanide ligands, forming a dodecahedron. The Co—N bond distances range from 1.926 (2) Å to 1.939 (2) Å, while the W—C distances in the [W(CN)₈] unit range from 1.165 (3) to 2.176 (3) Å and C—N distances lie between 1.137 (4) Å to 1.144 (4) Å. The cations and the anions are linked with each other by weak C—H···N hydrogen bond into a three-demensional structure. (Fig. 2).

Related literature top

For compounds with similar architectures, see: Przychodzeń et al. (2006); Withers et al. (2005); Mathonière et al. (2005). For related structures, see: Liu et al. (2008); Chang et al. (2002).

Experimental top

Co(ClO₄)₂ . 6H₂O (146.4 mg, 0.4 mmol) and (Bu₃N)₃[W(CN)₈] (44.72 mg, 0.1 mmol) were added into 2 ml dimethylformamide with thorough stirring for 5 minutes. After filtration, 2 ml dimethylformamide solvent and a solution of 2,2'-bipyridine (124.96 mg, 0.8 mmol) in 2 ml CH₃OH were successively laid on the surface of the above filtrate. Red block crystals were obtained after five days.

Computing details top

Data collection: CrystalClear (Rigaku, 2008); cell refinement: CrystalClear (Rigaku, 2008); data reduction: CrystalClear (Rigaku, 2008); 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 a portion of the title compound, with atom labels and 30% probability displacement ellipsoids. [Symmerty codes: (i) -x + 1/2,-y + 1/2,z; (ii) -x + 3/2,-y + 1/2,z.]
	Fig. 2. The unit cell packing diagram.

Tris(2,2'-bipyridine-κ²N,N')cobalt(III) octacyanidotungstate(V) top

Crystal data top

[Co(C₁₀H₈N₂)₃][W(CN)₈]	F(000) = 1803
M_r = 919.48	D_x = 1.758 Mg m⁻³
Orthorhombic, Pccn	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ab 2ac	Cell parameters from 10230 reflections
a = 11.465 (2) Å	θ = 2.5–31.3°
b = 15.141 (3) Å	µ = 3.84 mm⁻¹
c = 20.007 (4) Å	T = 250 K
V = 3473.0 (12) Å³	Prism, red
Z = 4	0.20 × 0.20 × 0.20 mm

Data collection top

Rigaku Mercury CCD diffractometer	3554 independent reflections
Radiation source: fine-focus sealed tube	3023 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.018
Detector resolution: 28.5714 pixels mm^-1	θ_max = 26.4°, θ_min = 2.5°
dtprofit.ref scans	h = −14→11
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	k = −15→18
T_min = 0.841, T_max = 1.000	l = −25→15
12594 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)] = 0.026	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.059	H-atom parameters constrained
S = 1.10	w = 1/[σ²(F_o²) + (0.0237P)² + 2.7418P] where P = (F_o² + 2F_c²)/3
3554 reflections	(Δ/σ)_max = 0.001
245 parameters	Δρ_max = 1.33 e Å⁻³
0 restraints	Δρ_min = −0.41 e Å⁻³

Crystal data top

[Co(C₁₀H₈N₂)₃][W(CN)₈]	V = 3473.0 (12) Å³
M_r = 919.48	Z = 4
Orthorhombic, Pccn	Mo Kα radiation
a = 11.465 (2) Å	µ = 3.84 mm⁻¹
b = 15.141 (3) Å	T = 250 K
c = 20.007 (4) Å	0.20 × 0.20 × 0.20 mm

Data collection top

Rigaku Mercury CCD diffractometer	3554 independent reflections
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	3023 reflections with I > 2σ(I)
T_min = 0.841, T_max = 1.000	R_int = 0.018
12594 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.026	0 restraints
wR(F²) = 0.059	H-atom parameters constrained
S = 1.10	Δρ_max = 1.33 e Å⁻³
3554 reflections	Δρ_min = −0.41 e Å⁻³
245 parameters

Special details top

Experimental. Yield: 62.1 mg in pure form, 42.1% based on Co. Analysis calculated for C₃₈H₂₄CoN₁₄W: C 49.59, H 2.61, N 21.32%; found: C 50.31, H 2.88, N 21.44%. IR: ν, cm^-1,2132 s.

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	0.2500	0.2500	0.44279 (2)	0.02694 (12)
N1	0.0967 (2)	0.19603 (17)	0.44129 (11)	0.0332 (5)
N2	0.2836 (2)	0.16505 (16)	0.37377 (12)	0.0329 (5)
N3	0.2091 (2)	0.32944 (16)	0.51483 (12)	0.0328 (5)
C1	0.0030 (3)	0.2192 (2)	0.47655 (17)	0.0474 (8)
H1A	0.0068	0.2693	0.5033	0.057*
C2	−0.0986 (3)	0.1720 (3)	0.47478 (18)	0.0574 (10)
H2A	−0.1631	0.1906	0.4992	0.069*
C3	−0.1042 (3)	0.0979 (3)	0.43700 (18)	0.0606 (11)
H3A	−0.1725	0.0647	0.4358	0.073*
C4	−0.0087 (3)	0.0716 (2)	0.40038 (18)	0.0521 (9)
H4A	−0.0114	0.0204	0.3747	0.063*
C5	0.0911 (3)	0.1222 (2)	0.40228 (14)	0.0352 (7)
C6	0.1962 (2)	0.10663 (18)	0.36179 (14)	0.0321 (6)
C7	0.2071 (3)	0.0426 (2)	0.31379 (16)	0.0434 (8)
H7A	0.1467	0.0027	0.3064	0.052*
C8	0.3073 (3)	0.0376 (2)	0.27679 (17)	0.0479 (8)
H8A	0.3156	−0.0056	0.2440	0.058*
C9	0.3944 (3)	0.0961 (2)	0.28839 (17)	0.0499 (9)
H9A	0.4628	0.0935	0.2635	0.060*
C10	0.3813 (3)	0.1595 (2)	0.33709 (16)	0.0442 (8)
H10A	0.4415	0.1995	0.3448	0.053*
C12	0.1644 (3)	0.4112 (2)	0.50934 (16)	0.0399 (7)
H12A	0.1572	0.4364	0.4671	0.048*
C13	0.1381 (3)	0.4211 (2)	0.62628 (17)	0.0530 (9)
H13A	0.1120	0.4514	0.6639	0.064*
C14	0.1288 (3)	0.4588 (2)	0.56437 (16)	0.0455 (8)
H14A	0.0989	0.5155	0.5595	0.055*
C11	0.1858 (3)	0.3387 (2)	0.63277 (17)	0.0522 (9)
H11A	0.1927	0.3130	0.6748	0.063*
C15	0.2235 (3)	0.2939 (2)	0.57651 (15)	0.0369 (7)
W1	0.7500	0.2500	0.194217 (8)	0.02995 (7)
N4	0.9827 (3)	0.3555 (2)	0.13727 (15)	0.0565 (8)
N5	0.8322 (3)	0.3742 (2)	0.32171 (16)	0.0571 (8)
N6	0.5146 (3)	0.3489 (2)	0.25333 (15)	0.0590 (8)
N7	0.6578 (3)	0.3788 (2)	0.07078 (15)	0.0569 (8)
C16	0.9012 (3)	0.3203 (2)	0.15643 (15)	0.0398 (7)
C17	0.8039 (3)	0.3325 (2)	0.27706 (16)	0.0401 (7)
C18	0.5961 (3)	0.3157 (2)	0.23298 (15)	0.0397 (7)
C19	0.6896 (3)	0.3344 (2)	0.11329 (16)	0.0396 (7)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Co1	0.0231 (3)	0.0306 (3)	0.0271 (3)	−0.0031 (2)	0.000	0.000
N1	0.0237 (12)	0.0422 (15)	0.0337 (13)	−0.0050 (11)	0.0019 (10)	0.0019 (11)
N2	0.0287 (12)	0.0375 (14)	0.0326 (13)	−0.0011 (10)	0.0032 (10)	−0.0005 (11)
N3	0.0290 (12)	0.0350 (13)	0.0343 (13)	−0.0030 (10)	0.0011 (10)	−0.0033 (11)
C1	0.0336 (16)	0.063 (2)	0.0456 (18)	−0.0053 (16)	0.0092 (15)	−0.0064 (17)
C2	0.0346 (18)	0.081 (3)	0.057 (2)	−0.0131 (18)	0.0170 (16)	−0.009 (2)
C3	0.0351 (19)	0.080 (3)	0.067 (2)	−0.0240 (19)	0.0093 (17)	−0.004 (2)
C4	0.0433 (19)	0.055 (2)	0.058 (2)	−0.0181 (17)	0.0029 (16)	−0.0068 (18)
C5	0.0304 (15)	0.0398 (17)	0.0356 (15)	−0.0044 (13)	−0.0006 (12)	0.0055 (14)
C6	0.0301 (15)	0.0328 (15)	0.0334 (15)	−0.0011 (12)	−0.0028 (12)	0.0044 (13)
C7	0.0379 (17)	0.0415 (19)	0.051 (2)	−0.0034 (15)	−0.0036 (14)	−0.0026 (15)
C8	0.052 (2)	0.0439 (19)	0.0476 (19)	0.0035 (16)	0.0046 (17)	−0.0108 (16)
C9	0.0405 (19)	0.061 (2)	0.0481 (19)	0.0016 (17)	0.0129 (16)	−0.0079 (17)
C10	0.0307 (16)	0.053 (2)	0.0486 (19)	−0.0076 (14)	0.0094 (14)	−0.0056 (16)
C12	0.0357 (16)	0.0383 (17)	0.0457 (18)	−0.0006 (14)	0.0011 (14)	0.0009 (15)
C13	0.065 (2)	0.048 (2)	0.047 (2)	−0.0058 (18)	0.0108 (17)	−0.0167 (17)
C14	0.0397 (18)	0.0386 (18)	0.058 (2)	−0.0019 (15)	0.0057 (15)	−0.0076 (16)
C11	0.070 (3)	0.050 (2)	0.0364 (18)	−0.0059 (19)	0.0034 (17)	−0.0029 (16)
C15	0.0372 (17)	0.0398 (17)	0.0336 (15)	−0.0084 (13)	0.0014 (13)	−0.0033 (14)
W1	0.02626 (9)	0.03213 (11)	0.03147 (10)	0.00157 (7)	0.000	0.000
N4	0.0450 (17)	0.065 (2)	0.0592 (19)	−0.0143 (15)	0.0015 (15)	0.0043 (16)
N5	0.0503 (19)	0.062 (2)	0.0592 (19)	−0.0056 (16)	−0.0012 (15)	−0.0185 (16)
N6	0.0415 (17)	0.082 (2)	0.0530 (18)	0.0177 (16)	0.0023 (14)	−0.0080 (16)
N7	0.0489 (18)	0.069 (2)	0.0526 (18)	0.0133 (16)	0.0029 (14)	0.0204 (16)
C16	0.0356 (17)	0.0418 (17)	0.0421 (18)	−0.0027 (14)	−0.0030 (14)	0.0017 (15)
C17	0.0314 (16)	0.0430 (18)	0.0459 (18)	−0.0010 (14)	0.0006 (14)	−0.0029 (16)
C18	0.0346 (17)	0.0471 (19)	0.0373 (16)	0.0043 (14)	−0.0005 (13)	−0.0007 (15)
C19	0.0312 (16)	0.0458 (18)	0.0419 (17)	0.0057 (14)	0.0043 (14)	0.0032 (15)

Geometric parameters (Å, º) top

Co1—N2	1.926 (2)	C8—H8A	0.9300
Co1—N2ⁱ	1.926 (2)	C9—C10	1.376 (4)
Co1—N3ⁱ	1.935 (2)	C9—H9A	0.9300
Co1—N3	1.935 (2)	C10—H10A	0.9300
Co1—N1ⁱ	1.939 (2)	C12—C14	1.377 (4)
Co1—N1	1.939 (2)	C12—H12A	0.9300
N1—C1	1.332 (4)	C13—C14	1.368 (5)
N1—C5	1.364 (4)	C13—C11	1.368 (5)
N2—C10	1.342 (4)	C13—H13A	0.9300
N2—C6	1.358 (4)	C14—H14A	0.9300
N3—C12	1.345 (4)	C11—C15	1.384 (4)
N3—C15	1.357 (4)	C11—H11A	0.9300
C1—C2	1.367 (5)	C15—C15ⁱ	1.460 (6)
C1—H1A	0.9300	W1—C17	2.165 (3)
C2—C3	1.355 (5)	W1—C17ⁱⁱ	2.165 (3)
C2—H2A	0.9300	W1—C18ⁱⁱ	2.169 (3)
C3—C4	1.376 (5)	W1—C18	2.169 (3)
C3—H3A	0.9300	W1—C16	2.170 (3)
C4—C5	1.378 (4)	W1—C16ⁱⁱ	2.170 (3)
C4—H4A	0.9300	W1—C19ⁱⁱ	2.176 (3)
C5—C6	1.471 (4)	W1—C19	2.176 (3)
C6—C7	1.370 (4)	N4—C16	1.142 (4)
C7—C8	1.369 (5)	N5—C17	1.141 (4)
C7—H7A	0.9300	N6—C18	1.137 (4)
C8—C9	1.355 (5)	N7—C19	1.144 (4)

N2—Co1—N2ⁱ	88.39 (15)	N2—C10—C9	121.5 (3)
N2—Co1—N3ⁱ	94.04 (11)	N2—C10—H10A	119.3
N2ⁱ—Co1—N3ⁱ	176.06 (10)	C9—C10—H10A	119.3
N2—Co1—N3	176.06 (10)	N3—C12—C14	121.9 (3)
N2ⁱ—Co1—N3	94.04 (11)	N3—C12—H12A	119.0
N3ⁱ—Co1—N3	83.70 (15)	C14—C12—H12A	119.0
N2—Co1—N1ⁱ	95.11 (10)	C14—C13—C11	119.8 (3)
N2ⁱ—Co1—N1ⁱ	83.60 (10)	C14—C13—H13A	120.1
N3ⁱ—Co1—N1ⁱ	93.09 (10)	C11—C13—H13A	120.1
N3—Co1—N1ⁱ	88.24 (10)	C13—C14—C12	118.9 (3)
N2—Co1—N1	83.60 (10)	C13—C14—H14A	120.6
N2ⁱ—Co1—N1	95.11 (10)	C12—C14—H14A	120.6
N3ⁱ—Co1—N1	88.24 (10)	C13—C11—C15	119.7 (3)
N3—Co1—N1	93.09 (10)	C13—C11—H11A	120.2
N1ⁱ—Co1—N1	178.22 (13)	C15—C11—H11A	120.2
C1—N1—C5	118.7 (3)	N3—C15—C11	120.5 (3)
C1—N1—Co1	127.7 (2)	N3—C15—C15ⁱ	114.32 (17)
C5—N1—Co1	113.36 (19)	C11—C15—C15ⁱ	125.2 (2)
C10—N2—C6	118.6 (3)	C17—W1—C17ⁱⁱ	80.10 (17)
C10—N2—Co1	126.9 (2)	C17—W1—C18ⁱⁱ	76.03 (12)
C6—N2—Co1	114.46 (19)	C17ⁱⁱ—W1—C18ⁱⁱ	72.18 (12)
C12—N3—C15	119.1 (3)	C17—W1—C18	72.18 (12)
C12—N3—Co1	127.2 (2)	C17ⁱⁱ—W1—C18	76.03 (12)
C15—N3—Co1	113.7 (2)	C18ⁱⁱ—W1—C18	138.10 (16)
N1—C1—C2	122.4 (3)	C17—W1—C16	75.86 (12)
N1—C1—H1A	118.8	C17ⁱⁱ—W1—C16	141.03 (12)
C2—C1—H1A	118.8	C18ⁱⁱ—W1—C16	72.52 (12)
C3—C2—C1	119.2 (3)	C18—W1—C16	123.33 (12)
C3—C2—H2A	120.4	C17—W1—C16ⁱⁱ	141.03 (12)
C1—C2—H2A	120.4	C17ⁱⁱ—W1—C16ⁱⁱ	75.86 (12)
C2—C3—C4	119.9 (3)	C18ⁱⁱ—W1—C16ⁱⁱ	123.33 (12)
C2—C3—H3A	120.0	C18—W1—C16ⁱⁱ	72.52 (12)
C4—C3—H3A	120.0	C16—W1—C16ⁱⁱ	139.23 (16)
C3—C4—C5	119.0 (3)	C17—W1—C19ⁱⁱ	144.84 (12)
C3—C4—H4A	120.5	C17ⁱⁱ—W1—C19ⁱⁱ	108.76 (12)
C5—C4—H4A	120.5	C18ⁱⁱ—W1—C19ⁱⁱ	74.80 (11)
N1—C5—C4	120.7 (3)	C18—W1—C19ⁱⁱ	142.59 (11)
N1—C5—C6	114.1 (2)	C16—W1—C19ⁱⁱ	76.99 (12)
C4—C5—C6	125.1 (3)	C16ⁱⁱ—W1—C19ⁱⁱ	72.95 (11)
N2—C6—C7	121.1 (3)	C17—W1—C19	108.76 (12)
N2—C6—C5	113.7 (3)	C17ⁱⁱ—W1—C19	144.84 (12)
C7—C6—C5	125.1 (3)	C18ⁱⁱ—W1—C19	142.59 (11)
C8—C7—C6	119.6 (3)	C18—W1—C19	74.80 (11)
C8—C7—H7A	120.2	C16—W1—C19	72.95 (11)
C6—C7—H7A	120.2	C16ⁱⁱ—W1—C19	76.99 (12)
C9—C8—C7	119.3 (3)	C19ⁱⁱ—W1—C19	83.84 (16)
C9—C8—H8A	120.3	N4—C16—W1	178.2 (3)
C7—C8—H8A	120.3	N5—C17—W1	178.3 (3)
C8—C9—C10	119.8 (3)	N6—C18—W1	178.9 (3)
C8—C9—H9A	120.1	N7—C19—W1	179.9 (4)
C10—C9—H9A	120.1

Symmetry codes: (i) −x+1/2, −y+1/2, z; (ii) −x+3/2, −y+1/2, z.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
C4—H4A···N4ⁱⁱⁱ	0.93	2.53	3.371 (4)	151
C10—H10A···N1ⁱ	0.93	2.54	3.032 (4)	114
C12—H12A···N2ⁱ	0.93	2.51	3.008 (4)	114
C1—H1A···N3	0.93	2.50	2.993 (4)	113

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

Experimental details

Crystal data
Chemical formula	[Co(C₁₀H₈N₂)₃][W(CN)₈]
M_r	919.48
Crystal system, space group	Orthorhombic, Pccn
Temperature (K)	250
a, b, c (Å)	11.465 (2), 15.141 (3), 20.007 (4)
V (Å³)	3473.0 (12)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	3.84
Crystal size (mm)	0.20 × 0.20 × 0.20

Data collection
Diffractometer	Rigaku Mercury CCD diffractometer
Absorption correction	Multi-scan (ABSCOR; Higashi, 1995)
T_min, T_max	0.841, 1.000
No. of measured, independent and observed [I > 2σ(I)] reflections	12594, 3554, 3023
R_int	0.018
(sin θ/λ)_max (Å⁻¹)	0.625

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.026, 0.059, 1.10
No. of reflections	3554
No. of parameters	245
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	1.33, −0.41

Computer programs: CrystalClear (Rigaku, 2008), 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
C4—H4A···N4ⁱ	0.93	2.53	3.371 (4)	151
C10—H10A···N1ⁱⁱ	0.93	2.54	3.032 (4)	114
C12—H12A···N2ⁱⁱ	0.93	2.51	3.008 (4)	114
C1—H1A···N3	0.93	2.50	2.993 (4)	113

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

Acknowledgements

This work was supported by the Graduate Innovation Foundation of Nanjing University of Science and Technology.

References

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