Aqua­(hexa­methyl­enetetra­mine-κN)bis­(methanol-κO)bis­(thio­cyanato-κN)cobalt(II)

Shang, W.-L.; Bai, Y.; Ma, C.-Z.; Li, Z.-M.

doi:10.1107/S160053680802357X

metal-organic compounds

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ISSN: 2056-9890

Volume 64| Part 9| September 2008| Pages m1184-m1185

doi:10.1107/S160053680802357X

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Aqua(hexamethylenetetramine-κN)bis(methanol-κO)bis(thiocyanato-κN)cobalt(II)

Wei-Li Shang,^a Yan Bai,^a ^* Chao-Zhong Ma ^a and Zhi-Min Li ^a

^aInstitute of Molecular and Crystal Engineering, School of Chemistry and Chemical Engineering, Henan University, Kaifeng, Henan 475004, People's Republic of China
^*Correspondence e-mail: baiyan@henu.edu.cn

(Received 16 May 2008; accepted 25 July 2008; online 20 August 2008)

In the title complex, [Co(NCS)₂(C₆H₁₂N₄)(CH₄O)₂(H₂O)], the six-coordinated Co atom has a slightly distorted octahedral geometry. The molecules are linked by intermolecular O—H⋯S and O—H⋯N hydrogen bonds, forming a three- dimensional crystal structure. Intramolecular C—H⋯N and C—H⋯O hydrogen bonds are also present.

Related literature

For information on the self-assembly of transition-metal complexes, see: Guo et al. (2002 ); Kumar et al. (2007 ); Venkateswaran et al. (2007 ); Chi et al. (2008 ). For complexes including hexamethylenetetramine (hmt) as ligand, see: Liu et al. (2006 ); Zhang et al. (1999 ); Meng et al. (2001 ); Li et al. (2002 , 2007 ); Banerjee et al. (2007 ).

Experimental

Crystal data

[Co(NCS)₂(C₆H₁₂N₄)(CH₄O)₂(H₂O)]
M_r = 397.39
Orthorhombic, P b c a
a = 14.1128 (8) Å
b = 15.3684 (9) Å
c = 15.9839 (9) Å
V = 3466.8 (3) Å³
Z = 8
Mo Kα radiation
μ = 1.25 mm⁻¹
T = 296 (2) K
0.30 × 0.30 × 0.25 mm

Data collection

Bruker APEXII diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2000 ) T_min = 0.691, T_max = 0.730
20785 measured reflections
4287 independent reflections
3528 reflections with I > 2σ(I)
R_int = 0.022

Refinement

R[F² > 2σ(F²)] = 0.029
wR(F²) = 0.075
S = 1.04
4287 reflections
217 parameters
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 0.64 e Å⁻³
Δρ_min = −0.61 e Å⁻³

Table 1
Selected geometric parameters (Å, °)

Co1—N2	2.0400 (15)
Co1—N1	2.0585 (15)
Co1—O2	2.1024 (13)
Co1—O1W	2.1268 (14)
Co1—O1	2.1760 (13)
Co1—N3	2.2785 (13)

N2—Co1—N1	176.69 (6)
N2—Co1—O2	90.94 (6)
N1—Co1—O2	90.31 (6)
N2—Co1—O1W	89.59 (6)
N1—Co1—O1W	87.34 (6)
O2—Co1—O1W	90.09 (6)
N2—Co1—O1	89.30 (6)
N1—Co1—O1	89.35 (6)
O2—Co1—O1	178.06 (6)
O1W—Co1—O1	87.99 (6)
N2—Co1—N3	92.06 (6)
N1—Co1—N3	90.98 (5)
O2—Co1—N3	91.53 (5)
O1W—Co1—N3	177.67 (6)
O1—Co1—N3	90.39 (5)

Table 2
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
C4—H4A⋯N1	0.97	2.52	3.119 (2)	120
C4—H4B⋯O1	0.97	2.56	3.167 (2)	121
C9—H9D⋯N2	0.96	2.56	3.181 (3)	123
O1—H1⋯N5ⁱ	0.80 (2)	2.08 (3)	2.824 (2)	156 (2)
O1W—H1WA⋯N6ⁱⁱ	0.76 (2)	2.07 (2)	2.821 (2)	168 (3)
O2—H2⋯N4ⁱⁱⁱ	0.78 (2)	1.97 (2)	2.7417 (18)	172 (2)
O1W—H1WB⋯S2ⁱⁱⁱ	0.88 (3)	2.55 (3)	3.4146 (16)	168 (2)
Symmetry codes: (i) -x+1, -y+2, -z+1; (ii) $[-x+1, y+{\script{1\over 2}}, -z+{\script{1\over 2}}]$ ; (iii) $[x+{\script{1\over 2}}, y, -z+{\script{1\over 2}}]$ .

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

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S160053680802357X/bh2177sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S160053680802357X/bh2177Isup2.hkl

checkCIF report

Comment top

Much interest at present is focused on the deliberate construction of transition metal ions and organic molecules by self-assembly of the component metal complexes. These solid materials are attractive to chemists not only for the variety of topologies and intriguing frameworks, but also for their interesting properties either by strong metal-ligand bonding or by weaker bonding forces such as hydrogen bonding and π—π interactions (Guo et al., 2002; Kumar et al., 2007; Venkateswaran et al., 2007; Chi et al., 2008). Among the ligands, hexamethylenetetramine (hmt), as a potential tetradentate ligand or hydrogen bonds acceptor, seems quite suitable in self-assembly systems. Several groups have reported that Co(II), Cd(II), Mn(II) or Ni(II) complexes with hmt and SCN ^- as ligands form two-dimensional or three-dimensional networks (Liu et al., 2006; Zhang et al., 1999; Meng et al., 2001; Li et al., 2002; Banerjee et al., 2007; Li et al., 2007).

Herein, we present a new hmt complex, (I), based on Co^II, with SCN ^- as ligand (Fig. 1). The title complex, which contains one cobalt center, one hmt, two NCS^-, two coordinated methanol molecules and one coordinated water molecule, forms a mononuclear complex. The Co^II ion is surrounded by three N atoms and three O atoms (two N atoms from two isothiocyanates, one N atom from hmt, one O atom from coordinated water molecule and two O atoms from two methanol molecules) to attain a distorted octahedral coordination geometry. Moreover, the O atoms of both methanol molecules are each mutually trans to each other. Intramolecular C—H···N and C—H···O hydrogen bonds (Table 2) are important factors in the stabilization of the molecule.

In the crystal structure, molecules interact with each other, forming a three-dimensional supramolecular network through multiform intermolecular hydrogen bonds (Fig. 2 and Table 2). The O2 and O1w atoms form two O—H···N hydrogen bonds with N4 and N6 atoms of the adjacent hmt ligand, respectively. In addition, O1w—H···S2 hydrogen bond is also found in the solid state.

Related literature top

For information on the self-assembly of transition-metal complexes, see: Guo et al. (2002); Kumar et al. (2007); Venkateswaran et al. (2007); Chi et al. (2008). For complexes including hexamethylenetetramine (hmt) as ligand, see: Liu et al. (2006); Zhang et al. (1999); Meng et al. (2001); Li et al. (2002, 2007); Banerjee et al. (2007).

Experimental top

All chemicals were of reagent grade quality obtained from commercial sources and used without further purification. Hexamethylenetetramine (0.50 mmol, 0.07 g), KSCN (1 mmol, 0.10 g) and Co(NO₃)₂.6H₂O (0.50 mmol, 0.15 g) were mixed in methanol (25 ml).The resulting purple solution was left for few weeks at room temperature to afford purple crystals (yield 65%). Anal. Calcd. for [Co(hmt)(SCN)₂(CH₃OH)₂(H₂O)]: C 30.23, H 5.58, N 21.15%. Found: C 30.21, H 5.59, N 21.16%. IR (KBr pellet, cm ^-1): 3398 (m), 2951 (m), 2877 (m), 2079 (vs), 1666 (m), 1462 (s), 1379 (s), 1241 (s), 1010 (s), 814 (m), 687 (s), 516 (m), 480 (m).

Computing details top

Data collection: SMART (Bruker, 2000); cell refinement: SAINT (Bruker, 2000); data reduction: SAINT (Bruker, 2000); program(s) used to solve structure: SHELXTL (Bruker, 2000); program(s) used to refine structure: SHELXTL (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 complex, with displacement ellipsoids drawn at the 50% probability level. The hydrogen atoms are omitted for clarity.
	Fig. 2. Perspective view of the three-dimensional network, showing the intermolecular hydrogen bonds (dashed solid lines) interactions.

Aqua(hexamethylenetetramine-κN)bis(methanol-κO)bis(thiocyanato-κN)cobalt(II) top

Crystal data top

[Co(NCS)₂(C₆H₁₂N₄)(CH₄O)₂(H₂O)]	F(000) = 1656
M_r = 397.39	D_x = 1.523 Mg m⁻³
Orthorhombic, Pbca	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2ab	Cell parameters from 7990 reflections
a = 14.1128 (8) Å	θ = 2.3–28.3°
b = 15.3684 (9) Å	µ = 1.25 mm⁻¹
c = 15.9839 (9) Å	T = 296 K
V = 3466.8 (3) Å³	Block, purple
Z = 8	0.30 × 0.30 × 0.25 mm

Data collection top

Bruker APEXII diffractometer	4287 independent reflections
Radiation source: sealed tube	3528 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.022
ϕ and ω scans	θ_max = 28.3°, θ_min = 2.3°
Absorption correction: multi-scan (SADABS; Bruker, 2000)	h = −14→18
T_min = 0.691, T_max = 0.730	k = −19→20
20785 measured reflections	l = −18→21

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)] = 0.029	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.075	H atoms treated by a mixture of independent and constrained refinement
S = 1.05	w = 1/[σ²(F_o²) + (0.0359P)² + 1.3724P] where P = (F_o² + 2F_c²)/3
4287 reflections	(Δ/σ)_max = 0.001
217 parameters	Δρ_max = 0.64 e Å⁻³
0 restraints	Δρ_min = −0.62 e Å⁻³

Crystal data top

[Co(NCS)₂(C₆H₁₂N₄)(CH₄O)₂(H₂O)]	V = 3466.8 (3) Å³
M_r = 397.39	Z = 8
Orthorhombic, Pbca	Mo Kα radiation
a = 14.1128 (8) Å	µ = 1.25 mm⁻¹
b = 15.3684 (9) Å	T = 296 K
c = 15.9839 (9) Å	0.30 × 0.30 × 0.25 mm

Data collection top

Bruker APEXII diffractometer	4287 independent reflections
Absorption correction: multi-scan (SADABS; Bruker, 2000)	3528 reflections with I > 2σ(I)
T_min = 0.691, T_max = 0.730	R_int = 0.022
20785 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.029	0 restraints
wR(F²) = 0.075	H atoms treated by a mixture of independent and constrained refinement
S = 1.05	Δρ_max = 0.64 e Å⁻³
4287 reflections	Δρ_min = −0.62 e Å⁻³
217 parameters

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Co1	0.553065 (15)	1.038335 (14)	0.283547 (14)	0.02795 (7)
N1	0.65439 (11)	0.97495 (10)	0.35331 (10)	0.0373 (3)
C1	0.71280 (12)	0.94096 (11)	0.39145 (11)	0.0309 (3)
S1	0.79561 (4)	0.89311 (4)	0.44512 (4)	0.05772 (17)
N2	0.45742 (11)	1.10745 (11)	0.21469 (10)	0.0412 (4)
C2	0.40515 (12)	1.14790 (11)	0.17538 (10)	0.0318 (3)
S2	0.33147 (4)	1.20788 (3)	0.12175 (3)	0.04690 (13)
N3	0.43978 (9)	0.94296 (9)	0.32720 (8)	0.0262 (3)
N4	0.27067 (9)	0.91344 (9)	0.34713 (9)	0.0310 (3)
N5	0.38399 (10)	0.86701 (9)	0.45350 (9)	0.0329 (3)
N6	0.37919 (10)	0.79376 (9)	0.31828 (9)	0.0320 (3)
C3	0.34122 (11)	0.97472 (10)	0.31390 (11)	0.0295 (3)
H3A	0.3336	1.0306	0.3412	0.035*
H3B	0.3304	0.9829	0.2545	0.035*
C4	0.45227 (12)	0.92901 (11)	0.41871 (10)	0.0311 (3)
H4A	0.5159	0.9078	0.4291	0.037*
H4B	0.4455	0.9843	0.4473	0.037*
C5	0.44845 (11)	0.85686 (11)	0.28545 (10)	0.0301 (3)
H5A	0.4387	0.8639	0.2258	0.036*
H5B	0.5120	0.8344	0.2939	0.036*
C6	0.28784 (12)	0.90063 (12)	0.43761 (10)	0.0359 (4)
H6A	0.2798	0.9556	0.4665	0.043*
H6B	0.2416	0.8600	0.4597	0.043*
C7	0.28332 (12)	0.82913 (11)	0.30472 (11)	0.0341 (4)
H7A	0.2726	0.8364	0.2452	0.041*
H7B	0.2368	0.7881	0.3257	0.041*
C8	0.39459 (13)	0.78357 (11)	0.40908 (11)	0.0355 (4)
H8A	0.3493	0.7420	0.4312	0.043*
H8B	0.4577	0.7607	0.4188	0.043*
O1	0.52358 (11)	1.12213 (8)	0.39015 (8)	0.0416 (3)
H1	0.5632 (16)	1.1230 (15)	0.4256 (16)	0.054 (7)*
C9	0.4697 (2)	1.19973 (17)	0.39250 (16)	0.0775 (9)
H9A	0.4301	1.1996	0.4413	0.116*
H9D	0.4308	1.2033	0.3433	0.116*
H9B	0.5116	1.2489	0.3945	0.116*
O2	0.58559 (9)	0.95999 (9)	0.17962 (8)	0.0368 (3)
H2	0.6396 (16)	0.9493 (13)	0.1762 (13)	0.039 (6)*
C10	0.54971 (15)	0.97087 (17)	0.09672 (13)	0.0556 (6)
H10D	0.5700	0.9230	0.0625	0.083*
H10A	0.5733	1.0243	0.0737	0.083*
H10B	0.4817	0.9726	0.0983	0.083*
O1W	0.66088 (11)	1.12763 (9)	0.24788 (10)	0.0439 (3)
H1WA	0.6425 (17)	1.1713 (16)	0.2319 (16)	0.054 (7)*
H1WB	0.7014 (18)	1.1426 (16)	0.2873 (16)	0.063 (8)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Co1	0.02528 (12)	0.02913 (12)	0.02945 (12)	0.00166 (8)	−0.00442 (8)	0.00671 (8)
N1	0.0328 (8)	0.0382 (8)	0.0408 (8)	0.0019 (6)	−0.0058 (6)	0.0072 (6)
C1	0.0299 (8)	0.0296 (8)	0.0333 (8)	−0.0020 (6)	−0.0040 (7)	−0.0008 (6)
S1	0.0564 (3)	0.0461 (3)	0.0707 (4)	0.0114 (2)	−0.0366 (3)	−0.0015 (3)
N2	0.0362 (8)	0.0436 (9)	0.0437 (9)	0.0042 (7)	−0.0059 (7)	0.0111 (7)
C2	0.0306 (8)	0.0336 (8)	0.0314 (8)	−0.0002 (7)	−0.0020 (7)	0.0022 (7)
S2	0.0437 (3)	0.0503 (3)	0.0468 (3)	0.0126 (2)	−0.0123 (2)	0.0089 (2)
N3	0.0253 (6)	0.0283 (7)	0.0251 (6)	−0.0001 (5)	−0.0025 (5)	0.0014 (5)
N4	0.0265 (7)	0.0330 (7)	0.0336 (7)	0.0002 (5)	0.0006 (6)	−0.0010 (6)
N5	0.0338 (7)	0.0373 (8)	0.0277 (7)	−0.0022 (6)	0.0008 (6)	0.0043 (6)
N6	0.0356 (7)	0.0268 (7)	0.0336 (7)	−0.0008 (6)	0.0021 (6)	−0.0015 (6)
C3	0.0284 (8)	0.0286 (8)	0.0314 (8)	0.0024 (6)	−0.0020 (6)	0.0011 (6)
C4	0.0327 (9)	0.0363 (9)	0.0243 (7)	−0.0034 (7)	−0.0044 (6)	0.0020 (6)
C5	0.0307 (8)	0.0299 (8)	0.0297 (8)	0.0017 (6)	0.0031 (6)	−0.0018 (6)
C6	0.0335 (9)	0.0435 (10)	0.0308 (8)	0.0009 (7)	0.0065 (7)	−0.0010 (7)
C7	0.0314 (9)	0.0346 (9)	0.0364 (9)	−0.0058 (7)	−0.0025 (7)	−0.0032 (7)
C8	0.0379 (9)	0.0310 (8)	0.0377 (9)	−0.0003 (7)	0.0013 (7)	0.0075 (7)
O1	0.0519 (8)	0.0371 (7)	0.0358 (7)	0.0080 (6)	−0.0109 (6)	−0.0021 (5)
C9	0.116 (2)	0.0597 (15)	0.0565 (15)	0.0428 (15)	−0.0207 (15)	−0.0112 (12)
O2	0.0253 (6)	0.0531 (8)	0.0319 (6)	0.0018 (5)	−0.0003 (5)	0.0017 (5)
C10	0.0418 (12)	0.0907 (18)	0.0343 (10)	0.0045 (11)	−0.0045 (8)	0.0006 (10)
O1W	0.0411 (8)	0.0344 (7)	0.0562 (9)	−0.0044 (6)	−0.0076 (7)	0.0132 (7)

Geometric parameters (Å, º) top

Co1—N2	2.0400 (15)	C3—H3B	0.9700
Co1—N1	2.0585 (15)	C4—H4A	0.9700
Co1—O2	2.1024 (13)	C4—H4B	0.9700
Co1—O1W	2.1268 (14)	C5—H5A	0.9700
Co1—O1	2.1760 (13)	C5—H5B	0.9700
Co1—N3	2.2785 (13)	C6—H6A	0.9700
N1—C1	1.151 (2)	C6—H6B	0.9700
C1—S1	1.6256 (17)	C7—H7A	0.9700
N2—C2	1.151 (2)	C7—H7B	0.9700
C2—S2	1.6327 (17)	C8—H8A	0.9700
N3—C5	1.487 (2)	C8—H8B	0.9700
N3—C4	1.489 (2)	O1—C9	1.415 (2)
N3—C3	1.489 (2)	O1—H1	0.80 (2)
N4—C3	1.470 (2)	C9—H9A	0.9600
N4—C7	1.473 (2)	C9—H9D	0.9600
N4—C6	1.480 (2)	C9—H9B	0.9600
N5—C4	1.465 (2)	O2—C10	1.428 (2)
N5—C8	1.473 (2)	O2—H2	0.78 (2)
N5—C6	1.474 (2)	C10—H10D	0.9600
N6—C5	1.473 (2)	C10—H10A	0.9600
N6—C7	1.474 (2)	C10—H10B	0.9600
N6—C8	1.476 (2)	O1W—H1WA	0.76 (3)
C3—H3A	0.9700	O1W—H1WB	0.88 (3)

N2—Co1—N1	176.69 (6)	N6—C5—N3	111.79 (12)
N2—Co1—O2	90.94 (6)	N6—C5—H5A	109.3
N1—Co1—O2	90.31 (6)	N3—C5—H5A	109.3
N2—Co1—O1W	89.59 (6)	N6—C5—H5B	109.3
N1—Co1—O1W	87.34 (6)	N3—C5—H5B	109.3
O2—Co1—O1W	90.09 (6)	H5A—C5—H5B	107.9
N2—Co1—O1	89.30 (6)	N5—C6—N4	111.46 (13)
N1—Co1—O1	89.35 (6)	N5—C6—H6A	109.3
O2—Co1—O1	178.06 (6)	N4—C6—H6A	109.3
O1W—Co1—O1	87.99 (6)	N5—C6—H6B	109.3
N2—Co1—N3	92.06 (6)	N4—C6—H6B	109.3
N1—Co1—N3	90.98 (5)	H6A—C6—H6B	108.0
O2—Co1—N3	91.53 (5)	N4—C7—N6	111.58 (13)
O1W—Co1—N3	177.67 (6)	N4—C7—H7A	109.3
O1—Co1—N3	90.39 (5)	N6—C7—H7A	109.3
C1—N1—Co1	178.20 (15)	N4—C7—H7B	109.3
N1—C1—S1	179.8 (2)	N6—C7—H7B	109.3
C2—N2—Co1	178.33 (16)	H7A—C7—H7B	108.0
N2—C2—S2	178.14 (17)	N5—C8—N6	111.51 (13)
C5—N3—C4	107.64 (13)	N5—C8—H8A	109.3
C5—N3—C3	107.72 (12)	N6—C8—H8A	109.3
C4—N3—C3	107.34 (12)	N5—C8—H8B	109.3
C5—N3—Co1	112.16 (9)	N6—C8—H8B	109.3
C4—N3—Co1	108.08 (9)	H8A—C8—H8B	108.0
C3—N3—Co1	113.63 (9)	C9—O1—Co1	128.49 (13)
C3—N4—C7	108.37 (13)	C9—O1—H1	110.2 (17)
C3—N4—C6	109.12 (13)	Co1—O1—H1	115.6 (17)
C7—N4—C6	108.23 (13)	O1—C9—H9A	109.5
C4—N5—C8	108.45 (13)	O1—C9—H9D	109.5
C4—N5—C6	108.18 (13)	H9A—C9—H9D	109.5
C8—N5—C6	108.39 (14)	O1—C9—H9B	109.5
C5—N6—C7	108.29 (13)	H9A—C9—H9B	109.5
C5—N6—C8	108.81 (13)	H9D—C9—H9B	109.5
C7—N6—C8	108.60 (13)	C10—O2—Co1	126.06 (13)
N4—C3—N3	111.79 (12)	C10—O2—H2	107.8 (16)
N4—C3—H3A	109.3	Co1—O2—H2	112.9 (16)
N3—C3—H3A	109.3	O2—C10—H10D	109.5
N4—C3—H3B	109.3	O2—C10—H10A	109.5
N3—C3—H3B	109.3	H10D—C10—H10A	109.5
H3A—C3—H3B	107.9	O2—C10—H10B	109.5
N5—C4—N3	112.87 (13)	H10D—C10—H10B	109.5
N5—C4—H4A	109.0	H10A—C10—H10B	109.5
N3—C4—H4A	109.0	Co1—O1W—H1WA	114.4 (19)
N5—C4—H4B	109.0	Co1—O1W—H1WB	116.1 (16)
N3—C4—H4B	109.0	H1WA—O1W—H1WB	103 (2)
H4A—C4—H4B	107.8

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
C4—H4A···N1	0.97	2.52	3.119 (2)	120
C4—H4B···O1	0.97	2.56	3.167 (2)	121
C9—H9D···N2	0.96	2.56	3.181 (3)	123
O1—H1···N5ⁱ	0.80 (2)	2.08 (3)	2.824 (2)	156 (2)
O1W—H1WA···N6ⁱⁱ	0.76 (2)	2.07 (2)	2.821 (2)	168 (3)
O2—H2···N4ⁱⁱⁱ	0.78 (2)	1.97 (2)	2.7417 (18)	172 (2)
O1W—H1WB···S2ⁱⁱⁱ	0.88 (3)	2.55 (3)	3.4146 (16)	168 (2)

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

Experimental details

Crystal data
Chemical formula	[Co(NCS)₂(C₆H₁₂N₄)(CH₄O)₂(H₂O)]
M_r	397.39
Crystal system, space group	Orthorhombic, Pbca
Temperature (K)	296
a, b, c (Å)	14.1128 (8), 15.3684 (9), 15.9839 (9)
V (Å³)	3466.8 (3)
Z	8
Radiation type	Mo Kα
µ (mm⁻¹)	1.25
Crystal size (mm)	0.30 × 0.30 × 0.25

Data collection
Diffractometer	Bruker APEXII diffractometer
Absorption correction	Multi-scan (SADABS; Bruker, 2000)
T_min, T_max	0.691, 0.730
No. of measured, independent and observed [I > 2σ(I)] reflections	20785, 4287, 3528
R_int	0.022
(sin θ/λ)_max (Å⁻¹)	0.668

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.029, 0.075, 1.05
No. of reflections	4287
No. of parameters	217
H-atom treatment	H atoms treated by a mixture of independent and constrained refinement
Δρ_max, Δρ_min (e Å⁻³)	0.64, −0.62

Computer programs: SMART (Bruker, 2000), SAINT (Bruker, 2000), SHELXTL (Bruker, 2000), SHELXTL (Sheldrick, 2008).

Selected geometric parameters (Å, º) top

Co1—N2	2.0400 (15)	Co1—O1W	2.1268 (14)
Co1—N1	2.0585 (15)	Co1—O1	2.1760 (13)
Co1—O2	2.1024 (13)	Co1—N3	2.2785 (13)

N2—Co1—N1	176.69 (6)	O2—Co1—O1	178.06 (6)
N2—Co1—O2	90.94 (6)	O1W—Co1—O1	87.99 (6)
N1—Co1—O2	90.31 (6)	N2—Co1—N3	92.06 (6)
N2—Co1—O1W	89.59 (6)	N1—Co1—N3	90.98 (5)
N1—Co1—O1W	87.34 (6)	O2—Co1—N3	91.53 (5)
O2—Co1—O1W	90.09 (6)	O1W—Co1—N3	177.67 (6)
N2—Co1—O1	89.30 (6)	O1—Co1—N3	90.39 (5)
N1—Co1—O1	89.35 (6)

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
C4—H4A···N1	0.9700	2.5200	3.119 (2)	120.00
C4—H4B···O1	0.9700	2.5600	3.167 (2)	121.00
C9—H9D···N2	0.9600	2.5600	3.181 (3)	123.00
O1—H1···N5ⁱ	0.80 (2)	2.08 (3)	2.824 (2)	156 (2)
O1W—H1WA···N6ⁱⁱ	0.76 (2)	2.07 (2)	2.821 (2)	168 (3)
O2—H2···N4ⁱⁱⁱ	0.78 (2)	1.97 (2)	2.7417 (18)	172 (2)
O1W—H1WB···S2ⁱⁱⁱ	0.88 (3)	2.55 (3)	3.4146 (16)	168 (2)

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

Acknowledgements

We are grateful for financial support from the Natural Science Foundation of Henan Province and the Education Department of Henan Province.

References

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Volume 64| Part 9| September 2008| Pages m1184-m1185

doi:10.1107/S160053680802357X

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

Aqua­(hexa­methyl­ene­tetra­mine-κN)bis­­(methanol-κO)bis­­(thio­cyanato-κN)cobalt(II)

Related literature

Experimental

Crystal data

Data collection

Refinement

Supporting information

Acknowledgements

References

metal-organic compounds

Aqua(hexamethylenetetramine-κN)bis(methanol-κO)bis(thiocyanato-κN)cobalt(II)