Poly[[[diisothio­cyanato­cobalt(II)]-bis­[μ-4-tert-butyl-2,6-bis­(1,2,4-triazol-1-ylmeth­yl)phenol]] dimethyl­formamide disolvate dihydrate]

Chu, Z.

doi:10.1107/S1600536809005121

metal-organic compounds

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ISSN: 2056-9890

Volume 65| Part 3| March 2009| Page m288

doi:10.1107/S1600536809005121

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Poly[[[diisothiocyanatocobalt(II)]-bis[μ-4-tert-butyl-2,6-bis(1,2,4-triazol-1-ylmethyl)phenol]] dimethylformamide disolvate dihydrate]

Zhao-lian Chu ^a ^*

^aInstitute of Molecular Engineering & Applied Chemistry, School of Chemistry and Chemical Engineering, Anhui University of Technology, Maanshan 243002, People's Republic of China
^*Correspondence e-mail: zlchu@ahut.edu.cn

(Received 11 February 2009; accepted 12 February 2009; online 18 February 2009)

In the title compound, {[Co(NCS)₂(C₁₆H₂₀N₆O)₂]·2C₃H₇NO·2H₂O}_n, each Co^II ion located on an inversion center is six-coordinated by four equatorial N atoms from four different 4-tert-butyl-2,6-bis(1,2,4-triazol-1-ylmethyl)phenol (L) ligands, and by two N atoms from two axial thiocyanate anions [Co—N = 2.104 (3)–2.144 (3) Å]. The metal centres are connected via the bidentate L ligands into two-dimensional polymeric layers parallel to bc plane. The dimethylformamide and solvent water molecules participate in intermolecular O—H⋯O and O—H⋯S hydrogen bonds, which consolidate the crystal packing.

Related literature

For related structures, see: Chu et al. (2007 , 2008 ); Ma et al. (2003 ); Zhu et al. (2004 , 2007 ). For details of the synthesis, see Yan et al. (1994 ).

Experimental

Crystal data

[Co(NCS)₂(C₁₆H₂₀N₆O)₂]·2C₃H₇NO·2H₂O
M_r = 982.07
Monoclinic, P 2₁ /c
a = 12.561 (4) Å
b = 20.660 (6) Å
c = 10.571 (3) Å
β = 112.992 (5)°
V = 2525.2 (12) Å³
Z = 2
Mo Kα radiation
μ = 0.48 mm⁻¹
T = 291 K
0.30 × 0.30 × 0.20 mm

Data collection

Bruker SMART CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2000 ) T_min = 0.869, T_max = 0.910
13505 measured reflections
4950 independent reflections
2902 reflections with I > 2σ(I)
R_int = 0.057

Refinement

R[F² > 2σ(F²)] = 0.055
wR(F²) = 0.123
S = 0.90
4950 reflections
301 parameters
H-atom parameters constrained
Δρ_max = 0.45 e Å⁻³
Δρ_min = −0.28 e Å⁻³

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1—H1⋯O2	0.82	1.94	2.689 (4)	152
O2—H2A⋯O3	0.85	1.81	2.655 (5)	179
O2—H2B⋯S1ⁱ	0.85	2.51	3.321 (3)	161
Symmetry code: (i) $[x, -y+{\script{3\over 2}}, z+{\script{1\over 2}}]$ .

Data collection: SMART (Bruker, 2000); cell refinement: SAINT (Bruker, 2000); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 1998 ); software used to prepare material for publication: SHELXTL.

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536809005121/cv2519sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536809005121/cv2519Isup2.hkl

checkCIF report

Comment top

Ligand 2,6-bis(1,2,4-triazol-1-ylmethyl)-4-tert-butyl-phenol (bttp) has been used to generate various metal-organic architectures with different transitional metal ions due to its polydentate character and bridging ability (Chu et al., 2007, 2008; Ma et al., 2003; Zhu et al., 2004, 2007). As a further study of such complexes, the title Co^II complex is reported in this paper.

Each Co^II atom exhibits a slightly distorted octahedral environment with four nitrogen atoms from the triazole groups of four bttp ligands in the equatorial plane, and two nitrogen atoms from two thiocyanate ligands at the axial positions (Fig. 1). Each ligand adopts a cis conformation in which two triazole groups are on the same direction of the central phenyl ring. The dihedral angles between the phenyl ring and the two triazole rings are 97.8 (3) ° and 88.8 (3) °, respectively. The two triazole rings are inclined to one another, with a dihedral angle of 65.3 (3) °. Each bttp serves as a bidentate bridging ligand via two exodentate nitrogen atoms at the 4-position of the triazole rings while the nitrogen atoms at 1,2-positions remain uncoordinated. In this way four metal atoms and four bttp ligands form a 48-membered [M₄L₄] metallocyclic ring, which is further assembled into a two-dimensional network via Co–N coordination bonds (Fig. 2). The Co···Co distance linked by the bridged bttp ligand is 11.604 (1) Å. The water oxygen atom is uncoordinated, and contributes to the formation of O–H···O and O–H···S hydrogen-bonding interactions with phenol group and DMF molecule (Table 1).

Related literature top

For related structures, see: Chu et al. (2007, 2008); Ma et al. (2003); Zhu et al. (2004, 2007). For details of the synthesis, see Yan et al. (1994).

Experimental top

All solvents and chemicals were of analytical grade and were used without further purification. Ligand bttp was prepared via a one-step Mannich reaction as a white powder in 57% yield (Yan et al., 1994). For the synthesis of title compoud, a solution of bttp (0.1 mmol), Co(NO₃)₂.6H₂O (0.1 mmol) and NH₄SCN (0.25 mmol) in 30 ml e thanol was refluxed for 2 h, and then cooled to room temperature and filtered. The collected solid was dissolved in 1 ml DMF, and 20 ml e thanol was added to this solution. The mixture was left to stand at room temperature for two weeks and pink crystalline products were obtained (30.5 mg, 62%). Anal. Calcd. for C₄₀H₅₈CoN₁₆O₆S₂: C, 48.92; H, 5.95; N, 22.82. Found: C, 48.88; H, 5.98; N, 22.72.

Computing details top

Data collection: SMART (Bruker, 2000); cell refinement: SAINT (Bruker, 2000); data reduction: SAINT (Bruker, 2000); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 1998); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Figures top

Fig. 1. A portion of the crystal structure of the title compound, showing 30% probability displacement ellipsoids and the atom-numbering [symmetry codes: (A) -x + 1, -y + 1, -z + 1; (B) -x + 1, y - 1/2, -z + 3/2; (C) x, -y + 3/2, z - 1/2].

Poly[[[diisothiocyanatocobalt(II)]-bis[µ-4-tert-butyl- 2,6-bis(1,2,4-triazol-1-ylmethyl)phenol]] dimethylformamide disolvate dihydrate] top

Crystal data top

[Co(NCS)₂(C₁₆H₂₀N₆O)₂]·2C₃H₇NO·2H₂O	F(000) = 1034
M_r = 982.07	D_x = 1.292 Mg m⁻³
Monoclinic, P2₁/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 2950 reflections
a = 12.561 (4) Å	θ = 2.2–26.3°
b = 20.660 (6) Å	µ = 0.48 mm⁻¹
c = 10.571 (3) Å	T = 291 K
β = 112.992 (5)°	Block, pink
V = 2525.2 (12) Å³	0.30 × 0.30 × 0.20 mm
Z = 2

Data collection top

Bruker SMART CCD area-detector diffractometer	4950 independent reflections
Radiation source: fine-focus sealed tube	2902 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.057
ϕ and ω scans	θ_max = 26.0°, θ_min = 2.0°
Absorption correction: multi-scan (SADABS; Bruker, 2000)	h = −15→9
T_min = 0.869, T_max = 0.910	k = −22→25
13505 measured reflections	l = −12→13

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)] = 0.055	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.123	H-atom parameters constrained
S = 0.90	w = 1/[σ²(F_o²) + (0.0486P)²] where P = (F_o² + 2F_c²)/3
4950 reflections	(Δ/σ)_max = 0.001
301 parameters	Δρ_max = 0.45 e Å⁻³
0 restraints	Δρ_min = −0.28 e Å⁻³

Crystal data top

[Co(NCS)₂(C₁₆H₂₀N₆O)₂]·2C₃H₇NO·2H₂O	V = 2525.2 (12) Å³
M_r = 982.07	Z = 2
Monoclinic, P2₁/c	Mo Kα radiation
a = 12.561 (4) Å	µ = 0.48 mm⁻¹
b = 20.660 (6) Å	T = 291 K
c = 10.571 (3) Å	0.30 × 0.30 × 0.20 mm
β = 112.992 (5)°

Data collection top

Bruker SMART CCD area-detector diffractometer	4950 independent reflections
Absorption correction: multi-scan (SADABS; Bruker, 2000)	2902 reflections with I > 2σ(I)
T_min = 0.869, T_max = 0.910	R_int = 0.057
13505 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.055	0 restraints
wR(F²) = 0.123	H-atom parameters constrained
S = 0.90	Δρ_max = 0.45 e Å⁻³
4950 reflections	Δρ_min = −0.28 e Å⁻³
301 parameters

Special details top

Experimental. The structure was solved by direct methods (Bruker, 2000) and successive difference Fourier syntheses.

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	0.5000	0.5000	0.5000	0.03695 (19)
C1	0.5771 (3)	0.86800 (14)	0.5064 (3)	0.0393 (8)
C2	0.6792 (3)	0.90337 (13)	0.5400 (3)	0.0404 (8)
C3	0.7690 (3)	0.87839 (14)	0.5126 (3)	0.0433 (8)
H3	0.8360	0.9029	0.5346	0.052*
C4	0.7636 (3)	0.81724 (14)	0.4528 (3)	0.0420 (8)
C5	0.6623 (3)	0.78350 (14)	0.4230 (3)	0.0404 (8)
H5	0.6563	0.7426	0.3841	0.048*
C6	0.5691 (3)	0.80680 (13)	0.4473 (3)	0.0371 (8)
C7	0.8633 (3)	0.79381 (16)	0.4164 (4)	0.0550 (10)
C8	0.9756 (3)	0.7951 (2)	0.5444 (5)	0.0955 (15)
H8A	1.0379	0.7796	0.5216	0.143*
H8B	0.9678	0.7678	0.6138	0.143*
H8C	0.9916	0.8386	0.5783	0.143*
C9	0.8743 (5)	0.8385 (2)	0.3075 (5)	0.1115 (19)
H9A	0.8033	0.8381	0.2275	0.167*
H9B	0.9363	0.8239	0.2832	0.167*
H9C	0.8902	0.8818	0.3432	0.167*
C10	0.8440 (4)	0.72489 (18)	0.3605 (5)	0.0915 (15)
H10A	0.7729	0.7229	0.2806	0.137*
H10B	0.8397	0.6960	0.4295	0.137*
H10C	0.9070	0.7123	0.3360	0.137*
C11	0.6889 (3)	0.97044 (14)	0.6015 (3)	0.0478 (9)
H11A	0.7630	0.9889	0.6125	0.057*
H11B	0.6290	0.9977	0.5379	0.057*
C12	0.5946 (3)	0.99424 (14)	0.7654 (3)	0.0455 (8)
H12	0.5296	1.0151	0.7034	0.055*
C13	0.7154 (3)	0.95306 (17)	0.9391 (4)	0.0597 (10)
H13	0.7526	0.9391	1.0294	0.072*
C14	0.4596 (3)	0.76755 (13)	0.4002 (3)	0.0447 (9)
H14A	0.4007	0.7913	0.4189	0.054*
H14B	0.4318	0.7607	0.3018	0.054*
C15	0.4614 (3)	0.64600 (13)	0.4173 (3)	0.0421 (8)
H15	0.4319	0.6366	0.3239	0.050*
C16	0.5281 (3)	0.63924 (14)	0.6298 (3)	0.0507 (9)
H16	0.5557	0.6217	0.7178	0.061*
C17	0.2724 (3)	0.51848 (14)	0.2245 (4)	0.0446 (9)
C18	0.1450 (9)	0.6297 (5)	0.6463 (9)	0.298 (8)
H18A	0.2127	0.6063	0.7034	0.448*
H18B	0.0774	0.6090	0.6486	0.448*
H18C	0.1493	0.6733	0.6795	0.448*
C19	0.0711 (6)	0.5834 (3)	0.4258 (8)	0.178 (3)
H19A	−0.0069	0.5866	0.4200	0.267*
H19B	0.1015	0.5414	0.4597	0.267*
H19C	0.0720	0.5897	0.3362	0.267*
C20	0.1849 (6)	0.6730 (4)	0.4695 (12)	0.223 (6)
H20	0.1732	0.6685	0.3775	0.267*
N1	0.6785 (2)	0.97134 (11)	0.7339 (3)	0.0424 (7)
N2	0.7593 (3)	0.94366 (14)	0.8470 (3)	0.0633 (9)
N3	0.6134 (2)	0.98416 (11)	0.8952 (3)	0.0421 (7)
N4	0.4785 (2)	0.70493 (10)	0.4699 (2)	0.0381 (7)
N5	0.5213 (3)	0.70182 (11)	0.6081 (3)	0.0537 (8)
N6	0.4925 (2)	0.60231 (11)	0.5167 (3)	0.0419 (7)
N7	0.3582 (3)	0.50307 (12)	0.3096 (3)	0.0498 (7)
N8	0.1387 (4)	0.6307 (2)	0.5147 (7)	0.1162 (19)
O1	0.4893 (2)	0.89753 (10)	0.5304 (3)	0.0546 (6)
H1	0.4390	0.8709	0.5237	0.082*
O2	0.3105 (2)	0.83963 (13)	0.5642 (3)	0.1002 (11)
H2A	0.2885	0.8004	0.5513	0.120*
H2B	0.2559	0.8631	0.5668	0.150*
O3	0.2404 (4)	0.7173 (2)	0.5249 (8)	0.239 (4)
S1	0.14960 (9)	0.54051 (5)	0.10273 (12)	0.0765 (4)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Co1	0.0484 (4)	0.0262 (3)	0.0367 (4)	−0.0040 (3)	0.0171 (3)	0.0003 (3)
C1	0.051 (2)	0.0312 (17)	0.0407 (19)	0.0049 (16)	0.0238 (17)	0.0051 (14)
C2	0.055 (2)	0.0296 (16)	0.043 (2)	−0.0029 (16)	0.0258 (18)	−0.0028 (14)
C3	0.049 (2)	0.0362 (17)	0.049 (2)	−0.0073 (16)	0.0249 (18)	−0.0029 (15)
C4	0.056 (2)	0.0307 (17)	0.044 (2)	0.0001 (16)	0.0247 (18)	0.0025 (14)
C5	0.055 (2)	0.0258 (16)	0.041 (2)	0.0040 (16)	0.0191 (17)	−0.0010 (14)
C6	0.049 (2)	0.0241 (15)	0.0377 (18)	0.0004 (15)	0.0166 (16)	0.0046 (13)
C7	0.064 (3)	0.042 (2)	0.073 (3)	0.0009 (18)	0.041 (2)	−0.0084 (18)
C8	0.066 (3)	0.093 (3)	0.134 (4)	0.004 (3)	0.046 (3)	−0.024 (3)
C9	0.165 (5)	0.082 (3)	0.156 (5)	0.028 (3)	0.137 (4)	0.023 (3)
C10	0.092 (3)	0.060 (3)	0.146 (4)	0.000 (2)	0.072 (3)	−0.033 (3)
C11	0.062 (2)	0.0335 (17)	0.060 (2)	−0.0091 (17)	0.037 (2)	−0.0046 (16)
C12	0.054 (2)	0.0373 (18)	0.048 (2)	0.0070 (17)	0.0233 (18)	−0.0025 (16)
C13	0.061 (3)	0.071 (3)	0.045 (2)	0.012 (2)	0.019 (2)	0.0028 (19)
C14	0.053 (2)	0.0302 (17)	0.047 (2)	0.0053 (15)	0.0148 (18)	0.0054 (14)
C15	0.054 (2)	0.0330 (17)	0.0365 (19)	−0.0066 (16)	0.0143 (17)	−0.0067 (14)
C16	0.081 (3)	0.0337 (18)	0.039 (2)	−0.0038 (18)	0.0247 (19)	0.0002 (15)
C17	0.057 (2)	0.0317 (18)	0.050 (2)	−0.0062 (16)	0.027 (2)	−0.0054 (15)
C18	0.396 (17)	0.376 (16)	0.121 (7)	0.258 (14)	0.099 (9)	0.043 (8)
C19	0.159 (7)	0.117 (5)	0.234 (9)	0.029 (5)	0.051 (7)	0.011 (6)
C20	0.093 (6)	0.113 (6)	0.475 (19)	0.010 (5)	0.125 (9)	0.039 (9)
N1	0.0509 (19)	0.0322 (14)	0.0500 (18)	−0.0032 (13)	0.0263 (16)	−0.0068 (13)
N2	0.058 (2)	0.075 (2)	0.059 (2)	0.0159 (17)	0.0251 (18)	−0.0012 (17)
N3	0.0483 (18)	0.0381 (15)	0.0432 (18)	0.0033 (13)	0.0215 (14)	−0.0014 (12)
N4	0.0478 (18)	0.0279 (13)	0.0381 (17)	−0.0048 (12)	0.0163 (14)	−0.0010 (11)
N5	0.089 (2)	0.0319 (15)	0.0385 (17)	−0.0037 (15)	0.0229 (16)	−0.0047 (12)
N6	0.0578 (18)	0.0286 (13)	0.0404 (16)	−0.0038 (13)	0.0202 (14)	0.0003 (12)
N7	0.056 (2)	0.0466 (16)	0.0410 (17)	−0.0040 (16)	0.0127 (15)	0.0024 (14)
N8	0.065 (3)	0.065 (3)	0.192 (6)	0.003 (2)	0.022 (3)	−0.008 (3)
O1	0.0581 (16)	0.0363 (12)	0.0824 (18)	−0.0020 (12)	0.0416 (15)	−0.0086 (12)
O2	0.087 (2)	0.082 (2)	0.157 (3)	−0.0222 (17)	0.075 (2)	−0.0334 (19)
O3	0.106 (4)	0.096 (3)	0.512 (10)	−0.033 (3)	0.118 (5)	−0.063 (5)
S1	0.0555 (7)	0.0812 (7)	0.0776 (8)	0.0190 (6)	0.0094 (6)	−0.0002 (6)

Geometric parameters (Å, º) top

Co1—N7ⁱ	2.104 (3)	C12—N3	1.314 (4)
Co1—N7	2.104 (3)	C12—H12	0.9300
Co1—N6	2.126 (2)	C13—N2	1.306 (4)
Co1—N6ⁱ	2.126 (2)	C13—N3	1.344 (4)
Co1—N3ⁱⁱ	2.144 (3)	C13—H13	0.9300
Co1—N3ⁱⁱⁱ	2.144 (3)	C14—N4	1.461 (3)
C1—O1	1.368 (4)	C14—H14A	0.9700
C1—C2	1.396 (4)	C14—H14B	0.9700
C1—C6	1.397 (4)	C15—N4	1.321 (3)
C2—C3	1.370 (4)	C15—N6	1.323 (4)
C2—C11	1.515 (4)	C15—H15	0.9300
C3—C4	1.403 (4)	C16—N5	1.310 (3)
C3—H3	0.9300	C16—N6	1.339 (4)
C4—C5	1.375 (4)	C16—H16	0.9300
C4—C7	1.526 (5)	C17—N7	1.147 (4)
C5—C6	1.380 (4)	C17—S1	1.641 (4)
C5—H5	0.9300	C18—N8	1.361 (8)
C6—C14	1.504 (4)	C18—H18A	0.9600
C7—C9	1.523 (5)	C18—H18B	0.9600
C7—C10	1.525 (5)	C18—H18C	0.9600
C7—C8	1.526 (5)	C19—N8	1.391 (7)
C8—H8A	0.9600	C19—H19A	0.9600
C8—H8B	0.9600	C19—H19B	0.9600
C8—H8C	0.9600	C19—H19C	0.9600
C9—H9A	0.9600	C20—O3	1.161 (9)
C9—H9B	0.9600	C20—N8	1.243 (8)
C9—H9C	0.9600	C20—H20	0.9300
C10—H10A	0.9600	N1—N2	1.356 (4)
C10—H10B	0.9600	N3—Co1^iv	2.144 (3)
C10—H10C	0.9600	N4—N5	1.347 (3)
C11—N1	1.456 (4)	O1—H1	0.8200
C11—H11A	0.9700	O2—H2A	0.8500
C11—H11B	0.9700	O2—H2B	0.8501
C12—N1	1.311 (4)

N7ⁱ—Co1—N7	180.0	C2—C11—H11A	108.8
N7ⁱ—Co1—N6	89.94 (10)	N1—C11—H11B	108.8
N7—Co1—N6	90.06 (10)	C2—C11—H11B	108.8
N7ⁱ—Co1—N6ⁱ	90.06 (10)	H11A—C11—H11B	107.7
N7—Co1—N6ⁱ	89.94 (10)	N1—C12—N3	111.9 (3)
N6—Co1—N6ⁱ	180.000 (1)	N1—C12—H12	124.0
N7ⁱ—Co1—N3ⁱⁱ	89.21 (11)	N3—C12—H12	124.0
N7—Co1—N3ⁱⁱ	90.79 (11)	N2—C13—N3	115.9 (3)
N6—Co1—N3ⁱⁱ	92.79 (9)	N2—C13—H13	122.0
N6ⁱ—Co1—N3ⁱⁱ	87.21 (9)	N3—C13—H13	122.0
N7ⁱ—Co1—N3ⁱⁱⁱ	90.79 (11)	N4—C14—C6	111.3 (2)
N7—Co1—N3ⁱⁱⁱ	89.21 (11)	N4—C14—H14A	109.4
N6—Co1—N3ⁱⁱⁱ	87.21 (9)	C6—C14—H14A	109.4
N6ⁱ—Co1—N3ⁱⁱⁱ	92.79 (9)	N4—C14—H14B	109.4
N3ⁱⁱ—Co1—N3ⁱⁱⁱ	180.0	C6—C14—H14B	109.4
O1—C1—C2	116.5 (3)	H14A—C14—H14B	108.0
O1—C1—C6	124.4 (3)	N4—C15—N6	110.2 (3)
C2—C1—C6	119.1 (3)	N4—C15—H15	124.9
C3—C2—C1	120.0 (3)	N6—C15—H15	124.9
C3—C2—C11	120.0 (3)	N5—C16—N6	115.4 (3)
C1—C2—C11	120.0 (3)	N5—C16—H16	122.3
C2—C3—C4	122.4 (3)	N6—C16—H16	122.3
C2—C3—H3	118.8	N7—C17—S1	180.0 (4)
C4—C3—H3	118.8	N8—C18—H18A	109.5
C5—C4—C3	116.0 (3)	N8—C18—H18B	109.5
C5—C4—C7	124.0 (3)	H18A—C18—H18B	109.5
C3—C4—C7	119.9 (3)	N8—C18—H18C	109.5
C4—C5—C6	123.8 (3)	H18A—C18—H18C	109.5
C4—C5—H5	118.1	H18B—C18—H18C	109.5
C6—C5—H5	118.1	N8—C19—H19A	109.5
C5—C6—C1	118.8 (3)	N8—C19—H19B	109.5
C5—C6—C14	118.9 (3)	H19A—C19—H19B	109.5
C1—C6—C14	122.2 (3)	N8—C19—H19C	109.5
C9—C7—C10	108.7 (3)	H19A—C19—H19C	109.5
C9—C7—C4	108.9 (3)	H19B—C19—H19C	109.5
C10—C7—C4	111.8 (3)	O3—C20—N8	129.7 (12)
C9—C7—C8	109.6 (4)	O3—C20—H20	115.1
C10—C7—C8	108.2 (3)	N8—C20—H20	115.1
C4—C7—C8	109.7 (3)	C12—N1—N2	109.1 (3)
C7—C8—H8A	109.5	C12—N1—C11	129.2 (3)
C7—C8—H8B	109.5	N2—N1—C11	121.7 (3)
H8A—C8—H8B	109.5	C13—N2—N1	101.9 (3)
C7—C8—H8C	109.5	C12—N3—C13	101.2 (3)
H8A—C8—H8C	109.5	C12—N3—Co1^iv	129.1 (2)
H8B—C8—H8C	109.5	C13—N3—Co1^iv	129.2 (2)
C7—C9—H9A	109.5	C15—N4—N5	110.1 (2)
C7—C9—H9B	109.5	C15—N4—C14	129.5 (3)
H9A—C9—H9B	109.5	N5—N4—C14	120.4 (2)
C7—C9—H9C	109.5	C16—N5—N4	102.0 (2)
H9A—C9—H9C	109.5	C15—N6—C16	102.3 (2)
H9B—C9—H9C	109.5	C15—N6—Co1	128.4 (2)
C7—C10—H10A	109.5	C16—N6—Co1	129.1 (2)
C7—C10—H10B	109.5	C17—N7—Co1	160.7 (3)
H10A—C10—H10B	109.5	C20—N8—C18	123.5 (8)
C7—C10—H10C	109.5	C20—N8—C19	119.1 (9)
H10A—C10—H10C	109.5	C18—N8—C19	117.2 (8)
H10B—C10—H10C	109.5	C1—O1—H1	109.5
N1—C11—C2	113.7 (3)	H2A—O2—H2B	109.5
N1—C11—H11A	108.8

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1···O2	0.82	1.94	2.689 (4)	152
O2—H2A···O3	0.85	1.81	2.655 (5)	179
O2—H2B···S1^v	0.85	2.51	3.321 (3)	161

Symmetry code: (v) x, −y+3/2, z+1/2.

Experimental details

Crystal data
Chemical formula	[Co(NCS)₂(C₁₆H₂₀N₆O)₂]·2C₃H₇NO·2H₂O
M_r	982.07
Crystal system, space group	Monoclinic, P2₁/c
Temperature (K)	291
a, b, c (Å)	12.561 (4), 20.660 (6), 10.571 (3)
β (°)	112.992 (5)
V (Å³)	2525.2 (12)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	0.48
Crystal size (mm)	0.30 × 0.30 × 0.20

Data collection
Diffractometer	Bruker SMART CCD area-detector diffractometer
Absorption correction	Multi-scan (SADABS; Bruker, 2000)
T_min, T_max	0.869, 0.910
No. of measured, independent and observed [I > 2σ(I)] reflections	13505, 4950, 2902
R_int	0.057
(sin θ/λ)_max (Å⁻¹)	0.617

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.055, 0.123, 0.90
No. of reflections	4950
No. of parameters	301
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.45, −0.28

Computer programs: SMART (Bruker, 2000), SAINT (Bruker, 2000), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 1998), SHELXTL (Sheldrick, 2008).

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1···O2	0.82	1.94	2.689 (4)	152.0
O2—H2A···O3	0.85	1.81	2.655 (5)	179.0
O2—H2B···S1ⁱ	0.85	2.51	3.321 (3)	161.0

Symmetry code: (i) x, −y+3/2, z+1/2.

Acknowledgements

The author acknowledges Anhui University of Technology for supporting this work.

References

Brandenburg, K. (1998). DIAMOND. Crystal Impact GbR, Bonn, Germany. Google Scholar
Bruker (2000). SADABS, SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Chu, Z.-L., Huang, W., Zhu, H.-B. & Gou, S.-H. (2008). J. Mol. Struct. 874, 1–13. Web of Science CSD CrossRef CAS Google Scholar
Chu, Z.-L., Xu, G., Huang, W. & Gou, S.-H. (2007). Acta Cryst. E63, m2155–m2156. Web of Science CSD CrossRef IUCr Journals Google Scholar
Ma, Y.-L., Huang, W., Yao, J.-C., Li, B., Gou, S.-H. & Fun, H.-K. (2003). J. Mol. Struct. 658, 51–58. Web of Science CSD CrossRef CAS Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Yan, J.-M., Zhang, Z.-J., Yuan, D.-Q., Xie, R.-G. & Zhao, H.-M. (1994). Synth. Commun. 24, 47–52. CrossRef CAS Web of Science Google Scholar
Zhu, H.-B., Chu, Z.-L., Hu, D.-H., Huang, W. & Gou, S.-H. (2007). Inorg. Chem. Commun. 10, 362–366. Web of Science CSD CrossRef CAS Google Scholar
Zhu, H.-B., Huang, C.-H., Huang, W. & Gou, S.-H. (2004). Inorg. Chem. Commun. 7, 1095–1099. Web of Science CSD CrossRef CAS Google Scholar

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Volume 65| Part 3| March 2009| Page m288

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

Poly[[[diiso­thio­cyanato­cobalt(II)]-bis­­[μ-4-tert-butyl-2,6-bis­­(1,2,4-triazol-1-ylmeth­yl)phenol]] di­methyl­formamide disolvate dihydrate]

Related literature

Experimental

Crystal data

Data collection

Refinement

Supporting information

Acknowledgements

References

metal-organic compounds

Poly[[[diisothiocyanatocobalt(II)]-bis[μ-4-tert-butyl-2,6-bis(1,2,4-triazol-1-ylmethyl)phenol]] dimethylformamide disolvate dihydrate]