Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807046648/sj2363sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807046648/sj2363Isup2.hkl |
CCDC reference: 663662
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (N-C) = 0.003 Å
- R factor = 0.031
- wR factor = 0.077
- Data-to-parameter ratio = 19.7
checkCIF/PLATON results
No syntax errors found
Alert level C PLAT153_ALERT_1_C The su's on the Cell Axes are Equal (x 100000) 300 Ang. PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.64 Ratio PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.32 Ratio PLAT230_ALERT_2_C Hirshfeld Test Diff for S1 - C1 .. 6.31 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Ni1 - O1W .. 5.99 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Ni1 - N1 .. 6.68 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Ni1 - N2 .. 5.45 su PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C1 PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 2
Alert level G PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 9 ALERT level C = Check and explain 2 ALERT level G = General alerts; check 3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 6 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
For information on the self-assembly of transition-metal complexes see Guo et al. (2002); Kumar et al. (2007); Venkateswaran et al. (2007). For complexes of the hexamethylenetetramine (hmt) ligand see Liu et al. (2006); Zhang et al. (1999); Meng et al. (2001); Li et al. (2002).
All chemicals were of reagent grade quality obtained from commercial sources and used without further purification. The hexamethylenetetramine (0.50 mmol, 0.07 g), KSCN (2 mmol, 0.19 g) and NiCl2.6H2O (0.50 mmol, 0.12 g) were mixed in methanol (25 ml). The green solution was left for several weeks at room temperature to afford green crystals (yield 68%).
All H-atoms were positioned geometrically and refined using a riding model with d(C—H) = 0.97 Å, Uiso = 1.2Ueq (C) for CH2, 0.96 Å, Uiso = 1.5Ueq (C) for CH3 atoms and 0.85 Å, Uiso = 1.2Ueq (O) for the OH groups.
During the past decade, the self-assembly of transition metal ions and organic molecules has become a powerful methodology for the construction of different supramolecular architectures with unusual and 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, Das et al., 2007; Venkateswaran et al., 2007). Among the ligands, hexamethylenetetramine (hmt) as a potential tetradentate ligand or hydrogen bond acceptor seems quite suitable in self-assembly systems. Several groups have reported that Co(II), Mn(II) or Ni(II) complexes with hmt and SCN- as ligands form two- or three-dimensional networks (Liu et al., 2006; Zhang et al., 1999; Meng et al., 2001; Li et al., 2002). Herein, we present a new hmt complex, (I), of nickel(II) with SCN-, Fig 1. The title complex, which contains one nickel center, one hmt, two NCS-, two coordinated methanol molecules and one coordinated water molecule, forms a mononuclear complex (Fig.1). The Ni2+ atom has a distorted octahedral coordination geometry. The N atom of hmt and the O atom of the water molecule, the N atoms of the two isothiocyanates and 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 1). The O1, O2 and O1w atoms form three O—H···N hydrogen bonds with the N6, N4 and N5 atoms of the adjacent hmt ligand, respectively. In addition, an O1w—H···S2 hydrogen bond is also found in the solid state.
For information on the self-assembly of transition-metal complexes see Guo et al. (2002); Kumar et al. (2007); Venkateswaran et al. (2007). For complexes of the hexamethylenetetramine (hmt) ligand see Liu et al. (2006); Zhang et al. (1999); Meng et al. (2001); Li et al. (2002).
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 (Bruker, 2000); molecular graphics: SHELXTL (Bruker, 2000); software used to prepare material for publication: SHELXTL (Bruker, 2000).
[Ni(SCN)2(C6H14N4)(CH4O)2(H2O)] | F(000) = 1664 |
Mr = 397.17 | Dx = 1.527 Mg m−3 |
Orthorhombic, Pbca | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ac 2ab | Cell parameters from 5794 reflections |
a = 14.069 (3) Å | θ = 2.3–27.0° |
b = 15.312 (3) Å | µ = 1.38 mm−1 |
c = 16.036 (3) Å | T = 293 K |
V = 3454.6 (12) Å3 | Block, green |
Z = 8 | 0.25 × 0.20 × 0.20 mm |
Bruker SMART CCD area-detector diffractometer | 3102 reflections with I > 2σ(I) |
Radiation source: sealed tube | Rint = 0.037 |
Graphite monochromator | θmax = 27.5°, θmin = 2.3° |
φ and ω scans | h = −17→18 |
20196 measured reflections | k = −19→19 |
3954 independent reflections | l = −15→20 |
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)] = 0.031 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.077 | H-atom parameters constrained |
S = 1.02 | w = 1/[σ2(Fo2) + (0.0346P)2 + 1.4403P] where P = (Fo2 + 2Fc2)/3 |
3954 reflections | (Δ/σ)max = 0.002 |
201 parameters | Δρmax = 0.63 e Å−3 |
0 restraints | Δρmin = −0.53 e Å−3 |
[Ni(SCN)2(C6H14N4)(CH4O)2(H2O)] | V = 3454.6 (12) Å3 |
Mr = 397.17 | Z = 8 |
Orthorhombic, Pbca | Mo Kα radiation |
a = 14.069 (3) Å | µ = 1.38 mm−1 |
b = 15.312 (3) Å | T = 293 K |
c = 16.036 (3) Å | 0.25 × 0.20 × 0.20 mm |
Bruker SMART CCD area-detector diffractometer | 3102 reflections with I > 2σ(I) |
20196 measured reflections | Rint = 0.037 |
3954 independent reflections |
R[F2 > 2σ(F2)] = 0.031 | 0 restraints |
wR(F2) = 0.077 | H-atom parameters constrained |
S = 1.02 | Δρmax = 0.63 e Å−3 |
3954 reflections | Δρmin = −0.53 e Å−3 |
201 parameters |
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. |
x | y | z | Uiso*/Ueq | ||
Ni1 | 1.051115 (17) | 1.037270 (16) | 0.284126 (16) | 0.02737 (9) | |
N1 | 1.15174 (12) | 0.97450 (11) | 0.35135 (12) | 0.0348 (4) | |
C1 | 1.21094 (14) | 0.94091 (13) | 0.38983 (13) | 0.0298 (4) | |
S1 | 1.29502 (5) | 0.89385 (4) | 0.44312 (5) | 0.0560 (2) | |
N2 | 0.95730 (13) | 1.10636 (13) | 0.21696 (12) | 0.0379 (4) | |
C2 | 0.90475 (15) | 1.14612 (13) | 0.17719 (13) | 0.0308 (4) | |
S2 | 0.83037 (4) | 1.20509 (4) | 0.12261 (4) | 0.04665 (16) | |
N3 | 0.94070 (11) | 0.94372 (10) | 0.32743 (10) | 0.0248 (3) | |
N4 | 0.88319 (12) | 0.86786 (11) | 0.45339 (11) | 0.0319 (4) | |
N5 | 0.88039 (12) | 0.79295 (11) | 0.31899 (10) | 0.0307 (4) | |
N6 | 0.77062 (11) | 0.91318 (11) | 0.34617 (11) | 0.0294 (4) | |
C3 | 0.95225 (14) | 0.93031 (14) | 0.41893 (12) | 0.0301 (4) | |
H3A | 1.0160 | 0.9092 | 0.4299 | 0.036* | |
H3B | 0.9450 | 0.9860 | 0.4471 | 0.036* | |
C4 | 0.89509 (16) | 0.78346 (14) | 0.40984 (13) | 0.0353 (5) | |
H4A | 0.9585 | 0.7611 | 0.4202 | 0.042* | |
H4B | 0.8498 | 0.7416 | 0.4318 | 0.042* | |
C5 | 0.78700 (15) | 0.90098 (15) | 0.43675 (13) | 0.0346 (5) | |
H5A | 0.7784 | 0.9563 | 0.4652 | 0.042* | |
H5B | 0.7406 | 0.8601 | 0.4586 | 0.042* | |
C6 | 0.78424 (15) | 0.82792 (14) | 0.30448 (14) | 0.0338 (5) | |
H6A | 0.7376 | 0.7867 | 0.3253 | 0.041* | |
H6B | 0.7740 | 0.8347 | 0.2450 | 0.041* | |
C7 | 0.94994 (14) | 0.85635 (13) | 0.28606 (13) | 0.0290 (4) | |
H7A | 0.9404 | 0.8630 | 0.2265 | 0.035* | |
H7B | 1.0137 | 0.8341 | 0.2948 | 0.035* | |
C8 | 0.84141 (13) | 0.97490 (13) | 0.31293 (13) | 0.0284 (4) | |
H8A | 0.8330 | 1.0313 | 0.3395 | 0.034* | |
H8B | 0.8311 | 0.9824 | 0.2535 | 0.034* | |
O1 | 1.08313 (10) | 0.95834 (10) | 0.18127 (9) | 0.0344 (3) | |
H1A | 1.1430 | 0.9511 | 0.1796 | 0.041* | |
C9 | 1.05023 (17) | 0.9745 (2) | 0.09820 (15) | 0.0551 (7) | |
H9A | 1.0726 | 0.9291 | 0.0619 | 0.083* | |
H9B | 1.0740 | 1.0298 | 0.0793 | 0.083* | |
H9C | 0.9820 | 0.9754 | 0.0977 | 0.083* | |
O2 | 1.02424 (11) | 1.12126 (9) | 0.38967 (9) | 0.0396 (4) | |
H2A | 1.0708 | 1.1218 | 0.4234 | 0.048* | |
C10 | 0.9735 (3) | 1.20139 (19) | 0.39099 (19) | 0.0753 (10) | |
H10A | 0.9296 | 1.2013 | 0.4369 | 0.113* | |
H10B | 0.9390 | 1.2081 | 0.3397 | 0.113* | |
H10C | 1.0173 | 1.2489 | 0.3973 | 0.113* | |
O1W | 1.15882 (11) | 1.12462 (9) | 0.24620 (10) | 0.0408 (4) | |
H1WB | 1.1952 | 1.1361 | 0.2871 | 0.049* | |
H1WD | 1.1343 | 1.1721 | 0.2292 | 0.049* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ni1 | 0.02452 (14) | 0.02876 (15) | 0.02882 (15) | 0.00163 (10) | −0.00440 (10) | 0.00596 (10) |
N1 | 0.0296 (10) | 0.0369 (10) | 0.0378 (10) | 0.0010 (8) | −0.0052 (8) | 0.0060 (8) |
C1 | 0.0302 (11) | 0.0277 (10) | 0.0315 (11) | −0.0021 (8) | −0.0029 (9) | −0.0016 (8) |
S1 | 0.0549 (4) | 0.0463 (4) | 0.0668 (5) | 0.0131 (3) | −0.0356 (3) | −0.0032 (3) |
N2 | 0.0335 (10) | 0.0405 (10) | 0.0398 (11) | 0.0044 (8) | −0.0047 (8) | 0.0108 (8) |
C2 | 0.0303 (11) | 0.0308 (11) | 0.0313 (11) | 0.0006 (9) | −0.0006 (9) | 0.0019 (9) |
S2 | 0.0430 (3) | 0.0513 (4) | 0.0457 (4) | 0.0130 (3) | −0.0128 (3) | 0.0088 (3) |
N3 | 0.0241 (8) | 0.0275 (8) | 0.0228 (8) | 0.0004 (6) | −0.0025 (6) | 0.0015 (6) |
N4 | 0.0333 (10) | 0.0356 (10) | 0.0269 (9) | −0.0019 (7) | 0.0003 (7) | 0.0042 (7) |
N5 | 0.0342 (10) | 0.0263 (9) | 0.0318 (9) | −0.0009 (7) | 0.0025 (7) | −0.0004 (7) |
N6 | 0.0247 (9) | 0.0318 (9) | 0.0318 (9) | −0.0007 (7) | 0.0004 (7) | −0.0013 (7) |
C3 | 0.0296 (11) | 0.0368 (11) | 0.0239 (10) | −0.0031 (9) | −0.0032 (8) | 0.0019 (8) |
C4 | 0.0357 (12) | 0.0318 (11) | 0.0385 (12) | 0.0014 (9) | 0.0007 (9) | 0.0079 (9) |
C5 | 0.0303 (11) | 0.0443 (13) | 0.0294 (11) | 0.0001 (9) | 0.0062 (9) | −0.0017 (9) |
C6 | 0.0310 (11) | 0.0348 (11) | 0.0356 (12) | −0.0055 (9) | −0.0019 (9) | −0.0024 (9) |
C7 | 0.0296 (10) | 0.0289 (10) | 0.0285 (10) | 0.0022 (8) | 0.0041 (8) | −0.0016 (8) |
C8 | 0.0250 (10) | 0.0297 (10) | 0.0307 (10) | 0.0021 (8) | −0.0025 (8) | 0.0006 (8) |
O1 | 0.0246 (7) | 0.0492 (9) | 0.0292 (8) | −0.0004 (6) | −0.0002 (6) | 0.0020 (7) |
C9 | 0.0417 (15) | 0.091 (2) | 0.0326 (13) | 0.0067 (14) | −0.0027 (10) | −0.0001 (13) |
O2 | 0.0487 (9) | 0.0349 (8) | 0.0352 (9) | 0.0078 (7) | −0.0121 (7) | −0.0017 (7) |
C10 | 0.115 (3) | 0.0549 (18) | 0.0561 (18) | 0.0408 (18) | −0.0207 (18) | −0.0111 (14) |
O1W | 0.0380 (9) | 0.0340 (8) | 0.0504 (10) | −0.0035 (7) | −0.0073 (7) | 0.0114 (7) |
Ni1—N2 | 2.005 (2) | C3—H3B | 0.9700 |
Ni1—N1 | 2.022 (2) | C4—H4A | 0.9700 |
Ni1—O1 | 2.094 (2) | C4—H4B | 0.9700 |
Ni1—O1W | 2.111 (2) | C5—H5A | 0.9700 |
Ni1—O2 | 2.159 (2) | C5—H5B | 0.9700 |
Ni1—N3 | 2.224 (2) | C6—H6A | 0.9700 |
N1—C1 | 1.157 (3) | C6—H6B | 0.9700 |
C1—S1 | 1.627 (2) | C7—H7A | 0.9700 |
N2—C2 | 1.151 (3) | C7—H7B | 0.9700 |
C2—S2 | 1.636 (2) | C8—H8A | 0.9700 |
N3—C3 | 1.490 (2) | C8—H8B | 0.9700 |
N3—C8 | 1.494 (2) | O1—C9 | 1.432 (3) |
N3—C7 | 1.499 (2) | O1—H1A | 0.8500 |
N4—C5 | 1.470 (3) | C9—H9A | 0.9600 |
N4—C3 | 1.471 (3) | C9—H9B | 0.9600 |
N4—C4 | 1.479 (3) | C9—H9C | 0.9600 |
N5—C6 | 1.473 (3) | O2—C10 | 1.420 (3) |
N5—C7 | 1.476 (3) | O2—H2A | 0.8500 |
N5—C4 | 1.479 (3) | C10—H10A | 0.9600 |
N6—C8 | 1.473 (2) | C10—H10B | 0.9600 |
N6—C6 | 1.479 (3) | C10—H10C | 0.9600 |
N6—C5 | 1.482 (3) | O1W—H1WB | 0.8500 |
C3—H3A | 0.9700 | O1W—H1WD | 0.8500 |
N2—Ni1—N1 | 176.16 (7) | N4—C5—N6 | 111.39 (16) |
N2—Ni1—O1 | 91.32 (7) | N4—C5—H5A | 109.4 |
N1—Ni1—O1 | 89.71 (7) | N6—C5—H5A | 109.4 |
N2—Ni1—O1W | 89.05 (7) | N4—C5—H5B | 109.4 |
N1—Ni1—O1W | 87.26 (7) | N6—C5—H5B | 109.4 |
O1—Ni1—O1W | 89.10 (6) | H5A—C5—H5B | 108.0 |
N2—Ni1—O2 | 89.51 (7) | N5—C6—N6 | 111.62 (16) |
N1—Ni1—O2 | 89.31 (7) | N5—C6—H6A | 109.3 |
O1—Ni1—O2 | 177.47 (6) | N6—C6—H6A | 109.3 |
O1W—Ni1—O2 | 88.52 (6) | N5—C6—H6B | 109.3 |
N2—Ni1—N3 | 92.74 (7) | N6—C6—H6B | 109.3 |
N1—Ni1—N3 | 90.94 (7) | H6A—C6—H6B | 108.0 |
O1—Ni1—N3 | 91.40 (6) | N5—C7—N3 | 111.79 (15) |
O1W—Ni1—N3 | 178.13 (6) | N5—C7—H7A | 109.3 |
O2—Ni1—N3 | 90.95 (6) | N3—C7—H7A | 109.3 |
C1—N1—Ni1 | 177.90 (17) | N5—C7—H7B | 109.3 |
N1—C1—S1 | 179.4 (2) | N3—C7—H7B | 109.3 |
C2—N2—Ni1 | 178.66 (19) | H7A—C7—H7B | 107.9 |
N2—C2—S2 | 178.3 (2) | N6—C8—N3 | 111.76 (15) |
C3—N3—C8 | 107.41 (15) | N6—C8—H8A | 109.3 |
C3—N3—C7 | 107.66 (15) | N3—C8—H8A | 109.3 |
C8—N3—C7 | 107.29 (15) | N6—C8—H8B | 109.3 |
C3—N3—Ni1 | 108.66 (11) | N3—C8—H8B | 109.3 |
C8—N3—Ni1 | 113.48 (11) | H8A—C8—H8B | 107.9 |
C7—N3—Ni1 | 112.09 (11) | C9—O1—Ni1 | 124.31 (15) |
C5—N4—C3 | 108.40 (16) | C9—O1—H1A | 108.3 |
C5—N4—C4 | 108.67 (17) | Ni1—O1—H1A | 108.3 |
C3—N4—C4 | 108.42 (16) | O1—C9—H9A | 109.5 |
C6—N5—C7 | 108.24 (16) | O1—C9—H9B | 109.5 |
C6—N5—C4 | 108.65 (16) | H9A—C9—H9B | 109.5 |
C7—N5—C4 | 108.93 (16) | O1—C9—H9C | 109.5 |
C8—N6—C6 | 108.37 (16) | H9A—C9—H9C | 109.5 |
C8—N6—C5 | 109.29 (16) | H9B—C9—H9C | 109.5 |
C6—N6—C5 | 108.14 (16) | C10—O2—Ni1 | 127.92 (15) |
N4—C3—N3 | 112.79 (16) | C10—O2—H2A | 111.7 |
N4—C3—H3A | 109.0 | Ni1—O2—H2A | 111.7 |
N3—C3—H3A | 109.0 | O2—C10—H10A | 109.5 |
N4—C3—H3B | 109.0 | O2—C10—H10B | 109.5 |
N3—C3—H3B | 109.0 | H10A—C10—H10B | 109.5 |
H3A—C3—H3B | 107.8 | O2—C10—H10C | 109.5 |
N5—C4—N4 | 111.32 (16) | H10A—C10—H10C | 109.5 |
N5—C4—H4A | 109.4 | H10B—C10—H10C | 109.5 |
N4—C4—H4A | 109.4 | Ni1—O1W—H1WB | 109.9 |
N5—C4—H4B | 109.4 | Ni1—O1W—H1WD | 110.0 |
N4—C4—H4B | 109.4 | H1WB—O1W—H1WD | 108.3 |
H4A—C4—H4B | 108.0 |
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1WB···S2i | 0.85 | 2.61 | 3.431 (2) | 162 |
O1—H1A···N6i | 0.85 | 1.93 | 2.762 (2) | 165 |
O1W—H1WD···N5ii | 0.85 | 2.02 | 2.836 (2) | 162 |
O2—H2A···N4iii | 0.85 | 2.09 | 2.839 (2) | 148 |
C3—H3A···N1 | 0.97 | 2.50 | 3.084 (3) | 119 |
C3—H3B···O2 | 0.97 | 2.53 | 3.130 (3) | 120 |
C7—H7A···O1 | 0.97 | 2.59 | 2.962 (3) | 103 |
C10—H10B···N2 | 0.96 | 2.52 | 3.156 (4) | 123 |
Symmetry codes: (i) x+1/2, y, −z+1/2; (ii) −x+2, y+1/2, −z+1/2; (iii) −x+2, −y+2, −z+1. |
Experimental details
Crystal data | |
Chemical formula | [Ni(SCN)2(C6H14N4)(CH4O)2(H2O)] |
Mr | 397.17 |
Crystal system, space group | Orthorhombic, Pbca |
Temperature (K) | 293 |
a, b, c (Å) | 14.069 (3), 15.312 (3), 16.036 (3) |
V (Å3) | 3454.6 (12) |
Z | 8 |
Radiation type | Mo Kα |
µ (mm−1) | 1.38 |
Crystal size (mm) | 0.25 × 0.20 × 0.20 |
Data collection | |
Diffractometer | Bruker SMART CCD area-detector |
Absorption correction | – |
No. of measured, independent and observed [I > 2σ(I)] reflections | 20196, 3954, 3102 |
Rint | 0.037 |
(sin θ/λ)max (Å−1) | 0.650 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.031, 0.077, 1.02 |
No. of reflections | 3954 |
No. of parameters | 201 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.63, −0.53 |
Computer programs: SMART (Bruker, 2000), SAINT (Bruker, 2000), SHELXTL (Bruker, 2000).
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1WB···S2i | 0.85 | 2.61 | 3.431 (2) | 162.0 |
O1—H1A···N6i | 0.85 | 1.93 | 2.762 (2) | 165.0 |
O1W—H1WD···N5ii | 0.85 | 2.02 | 2.836 (2) | 162.0 |
O2—H2A···N4iii | 0.85 | 2.09 | 2.839 (2) | 148.0 |
C3—H3A···N1 | 0.97 | 2.50 | 3.084 (3) | 119.0 |
C3—H3B···O2 | 0.97 | 2.53 | 3.130 (3) | 120.0 |
C7—H7A···O1 | 0.97 | 2.59 | 2.962 (3) | 103.0 |
C10—H10B···N2 | 0.96 | 2.52 | 3.156 (4) | 123.0 |
Symmetry codes: (i) x+1/2, y, −z+1/2; (ii) −x+2, y+1/2, −z+1/2; (iii) −x+2, −y+2, −z+1. |
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During the past decade, the self-assembly of transition metal ions and organic molecules has become a powerful methodology for the construction of different supramolecular architectures with unusual and 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, Das et al., 2007; Venkateswaran et al., 2007). Among the ligands, hexamethylenetetramine (hmt) as a potential tetradentate ligand or hydrogen bond acceptor seems quite suitable in self-assembly systems. Several groups have reported that Co(II), Mn(II) or Ni(II) complexes with hmt and SCN- as ligands form two- or three-dimensional networks (Liu et al., 2006; Zhang et al., 1999; Meng et al., 2001; Li et al., 2002). Herein, we present a new hmt complex, (I), of nickel(II) with SCN-, Fig 1. The title complex, which contains one nickel center, one hmt, two NCS-, two coordinated methanol molecules and one coordinated water molecule, forms a mononuclear complex (Fig.1). The Ni2+ atom has a distorted octahedral coordination geometry. The N atom of hmt and the O atom of the water molecule, the N atoms of the two isothiocyanates and 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 1). The O1, O2 and O1w atoms form three O—H···N hydrogen bonds with the N6, N4 and N5 atoms of the adjacent hmt ligand, respectively. In addition, an O1w—H···S2 hydrogen bond is also found in the solid state.