Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807043486/at2391sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807043486/at2391Isup2.hkl |
CCDC reference: 1296492
Crystals of the title compound (I) were synthesized using hydrothermal method in a 23 ml Teflon-lined Parr bomb, which was then sealed. Potassium ferrocyanide trihydrate (84.5 mg, 0.2 mmol), 2,2'-bipyridyl (62.4 mg, 0.4 mmol), potassium thiocyanate (38.9 mg, 0.4 mmol) and distilled water (3 g) were placed into the bomb and sealed. The bomb was then heated under autogenous pressure up to 423 K over the course of 7 d and allowed to cool at room temperature for 24 h. Upon opening the bomb, a clear colourless solution was decanted from small colourless crystals. These crystals were washed with distilled water followed by ethanol, and allowed to air-dry at room temperature.
H atoms were positioned geometrically, with C—H = 0.93 Å, and constrained to ride on their parent atoms, with Uiso(H) = 1.2Ueq(C).
Research on organic-inorganic hybrid materials has attracted much attention owing to their applications in areas including catalysis, materials chemistry and biochemistry (Hill, 1998; Banglin et al., 2001; Ferey, 2001). Weak interactions play an important role in these compounds and many frameworks are linked by different kinds of weak interactions, such as hydrogen bonds and π-π stacking. Several reported crystal structures of metal complexes incorporating the phenanthroline, quinoline and pyridyl ligand have shown the existence of π-π stacking between neighbouring aromatic rings in these structures (Wu et al., 2003; Pan & Xu, 2004; Liu et al., 2004; Li et al., 2005). We report herein the crystal structure of the title compound, (I), and the crystal struture is similar with the structures recently reported (Zhong et al., 2007a,b,c).
In the molecule of (I) (Fig. 1), the ligand bond lengths and angles are within normal ranges (Allen et al., 1987). The six-coordinate environment of the Fe atom is completed by the four N atoms of two 2,2'-bipyridyl ligands and two N atoms of two SCN- ligands (Table 1). The Fe—N bonds [average 2.1654 (15) Å] for the 2,2'-bipyridyl ligands are somewhat greater than the Fe—N bonds [average 2.0769 (18) Å] for the SCN- ligands. The two 2,2'-bipyridyl ligands are nearly perpendicular to each other, with a dihedral angle of 105.4 (3) °.
In the crystal structure, C—H···S and C—H···N non-classical hydrogen bonds between C—H groups of 2,2'-bipyridyl and N and S atoms of neighbouring SCN- ligands, with one C···S and two C···N distances of 3.736 (2), 3.146 (3) and 3.158 (3) Å, respectively, generate a layered hydrogen-bonded network (Table 2). The non-classical hydrogen-bonding interactions and π-π stacking interactions with centroid-centroid distance of 3.619 (7) Å [symmetry code: 1 - x, 2 - y, 2 - z] link the mononuclear complex into a supramolecular network structure (Fig. 2).
For general background, see: Banglin et al. (2001); Ferey (2001); Hill (1998); Li et al. (2005); Liu et al. (2004); Pan & Xu (2004); Wu et al. (2003); Zhong et al. (2007a,b,c). For bond-length data, see: Allen et al. (1987).
Data collection: APEX2 (Bruker, 2005); cell refinement: SAINT (Siemens, 1996); data reduction: SAINT (Siemens, 1996); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Siemens, 1996); software used to prepare material for publication: SHELXTL (Siemens, 1996).
[Fe(NCS)2(C10H8N2)2] | F(000) = 1984 |
Mr = 484.38 | Dx = 1.463 Mg m−3 |
Orthorhombic, Pbca | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ac 2ab | Cell parameters from 11611 reflections |
a = 16.087 (3) Å | θ = 2.4–27.5° |
b = 16.0117 (11) Å | µ = 0.90 mm−1 |
c = 17.0781 (12) Å | T = 273 K |
V = 4399.1 (9) Å3 | Block, colourless |
Z = 8 | 0.36 × 0.34 × 0.22 mm |
Bruker APEXII area-detector diffractometer | 4607 independent reflections |
Radiation source: fine-focus sealed tube | 3440 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.023 |
φ and ω scans | θmax = 26.6°, θmin = 2.2° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −20→20 |
Tmin = 0.738, Tmax = 0.827 | k = −20→20 |
28231 measured reflections | l = −20→21 |
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)] = 0.028 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.104 | H-atom parameters constrained |
S = 0.99 | w = 1/[σ2(Fo2) + (0.0679P)2 + 0.3898P] where P = (Fo2 + 2Fc2)/3 |
4607 reflections | (Δ/σ)max = 0.001 |
280 parameters | Δρmax = 0.26 e Å−3 |
0 restraints | Δρmin = −0.31 e Å−3 |
[Fe(NCS)2(C10H8N2)2] | V = 4399.1 (9) Å3 |
Mr = 484.38 | Z = 8 |
Orthorhombic, Pbca | Mo Kα radiation |
a = 16.087 (3) Å | µ = 0.90 mm−1 |
b = 16.0117 (11) Å | T = 273 K |
c = 17.0781 (12) Å | 0.36 × 0.34 × 0.22 mm |
Bruker APEXII area-detector diffractometer | 4607 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 3440 reflections with I > 2σ(I) |
Tmin = 0.738, Tmax = 0.827 | Rint = 0.023 |
28231 measured reflections |
R[F2 > 2σ(F2)] = 0.028 | 0 restraints |
wR(F2) = 0.104 | H-atom parameters constrained |
S = 0.99 | Δρmax = 0.26 e Å−3 |
4607 reflections | Δρmin = −0.31 e Å−3 |
280 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. |
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. |
x | y | z | Uiso*/Ueq | ||
Fe1 | 0.702218 (14) | 0.384015 (15) | −0.000737 (13) | 0.04495 (11) | |
S1 | 0.57506 (4) | 0.51147 (5) | −0.22505 (4) | 0.0891 (2) | |
S2 | 0.51114 (4) | 0.22577 (4) | 0.15958 (4) | 0.08023 (19) | |
N1 | 0.80962 (9) | 0.46072 (9) | −0.02958 (10) | 0.0536 (4) | |
N2 | 0.69900 (9) | 0.48321 (9) | 0.08364 (9) | 0.0541 (4) | |
N3 | 0.79903 (8) | 0.30887 (10) | 0.05481 (9) | 0.0542 (4) | |
N4 | 0.72299 (9) | 0.28352 (9) | −0.08241 (9) | 0.0513 (3) | |
N5 | 0.62928 (11) | 0.44614 (11) | −0.08248 (11) | 0.0705 (5) | |
N6 | 0.60985 (10) | 0.31801 (10) | 0.05743 (11) | 0.0667 (4) | |
C1 | 0.86327 (13) | 0.44587 (14) | −0.08809 (12) | 0.0700 (5) | |
H1 | 0.8545 | 0.3992 | −0.1194 | 0.084* | |
C2 | 0.93059 (14) | 0.49603 (17) | −0.10431 (14) | 0.0861 (7) | |
H2 | 0.9665 | 0.4837 | −0.1454 | 0.103* | |
C3 | 0.94281 (14) | 0.56411 (17) | −0.05820 (16) | 0.0880 (7) | |
H3 | 0.9875 | 0.5996 | −0.0678 | 0.106* | |
C4 | 0.88890 (15) | 0.58084 (16) | 0.00311 (13) | 0.0759 (6) | |
H4 | 0.8968 | 0.6276 | 0.0346 | 0.091* | |
C5 | 0.82295 (12) | 0.52690 (11) | 0.01694 (11) | 0.0544 (4) | |
C6 | 0.76284 (11) | 0.53793 (11) | 0.08202 (10) | 0.0526 (4) | |
C7 | 0.77061 (13) | 0.59913 (14) | 0.13863 (12) | 0.0693 (5) | |
H7 | 0.8158 | 0.6353 | 0.1379 | 0.083* | |
C8 | 0.71093 (15) | 0.60623 (16) | 0.19610 (14) | 0.0821 (7) | |
H8 | 0.7162 | 0.6466 | 0.2349 | 0.098* | |
C9 | 0.64395 (15) | 0.55372 (15) | 0.19585 (13) | 0.0786 (6) | |
H9 | 0.6019 | 0.5593 | 0.2329 | 0.094* | |
C10 | 0.64025 (13) | 0.49220 (13) | 0.13928 (12) | 0.0653 (5) | |
H10 | 0.5954 | 0.4555 | 0.1396 | 0.078* | |
C11 | 0.83790 (13) | 0.32758 (13) | 0.12300 (12) | 0.0674 (5) | |
H11 | 0.8168 | 0.3709 | 0.1533 | 0.081* | |
C12 | 0.90694 (15) | 0.28565 (16) | 0.14962 (15) | 0.0832 (7) | |
H12 | 0.9317 | 0.2997 | 0.1970 | 0.100* | |
C13 | 0.93838 (14) | 0.22198 (17) | 0.10378 (18) | 0.0909 (8) | |
H13 | 0.9854 | 0.1927 | 0.1197 | 0.109* | |
C14 | 0.89971 (13) | 0.20211 (15) | 0.03439 (16) | 0.0756 (6) | |
H14 | 0.9207 | 0.1596 | 0.0029 | 0.091* | |
C15 | 0.82893 (11) | 0.24598 (12) | 0.01150 (11) | 0.0550 (4) | |
C16 | 0.78122 (11) | 0.22718 (11) | −0.06158 (12) | 0.0545 (4) | |
C17 | 0.79405 (13) | 0.15627 (14) | −0.10565 (14) | 0.0735 (6) | |
H17 | 0.8349 | 0.1181 | −0.0914 | 0.088* | |
C18 | 0.74578 (17) | 0.14220 (15) | −0.17115 (14) | 0.0812 (7) | |
H18 | 0.7537 | 0.0942 | −0.2008 | 0.097* | |
C19 | 0.68650 (14) | 0.19881 (14) | −0.19234 (14) | 0.0723 (6) | |
H19 | 0.6534 | 0.1902 | −0.2363 | 0.087* | |
C20 | 0.67727 (12) | 0.26850 (12) | −0.14697 (12) | 0.0607 (5) | |
H20 | 0.6374 | 0.3076 | −0.1614 | 0.073* | |
C21 | 0.60591 (11) | 0.47321 (11) | −0.14205 (13) | 0.0589 (5) | |
C22 | 0.56819 (11) | 0.28039 (11) | 0.10015 (12) | 0.0540 (4) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Fe1 | 0.04535 (16) | 0.04334 (17) | 0.04615 (18) | −0.00323 (10) | 0.00046 (9) | −0.00113 (10) |
S1 | 0.0815 (4) | 0.1094 (5) | 0.0763 (4) | −0.0105 (3) | −0.0249 (3) | 0.0132 (3) |
S2 | 0.0866 (4) | 0.0743 (4) | 0.0797 (4) | −0.0121 (3) | 0.0266 (3) | 0.0007 (3) |
N1 | 0.0555 (8) | 0.0551 (9) | 0.0501 (8) | −0.0065 (7) | 0.0031 (7) | 0.0005 (7) |
N2 | 0.0557 (8) | 0.0530 (8) | 0.0535 (9) | −0.0036 (7) | 0.0025 (7) | −0.0036 (7) |
N3 | 0.0517 (8) | 0.0587 (9) | 0.0523 (9) | −0.0046 (6) | −0.0025 (7) | 0.0072 (7) |
N4 | 0.0515 (8) | 0.0495 (8) | 0.0528 (9) | −0.0019 (6) | 0.0016 (7) | −0.0019 (6) |
N5 | 0.0783 (11) | 0.0576 (10) | 0.0756 (12) | 0.0020 (8) | −0.0177 (9) | 0.0028 (9) |
N6 | 0.0614 (9) | 0.0605 (9) | 0.0781 (11) | −0.0086 (8) | 0.0105 (9) | −0.0036 (8) |
C1 | 0.0714 (12) | 0.0796 (14) | 0.0588 (12) | −0.0141 (11) | 0.0133 (10) | −0.0054 (10) |
C2 | 0.0759 (14) | 0.114 (2) | 0.0682 (15) | −0.0253 (14) | 0.0221 (12) | −0.0036 (14) |
C3 | 0.0738 (14) | 0.0989 (18) | 0.0913 (17) | −0.0338 (13) | 0.0144 (13) | 0.0035 (14) |
C4 | 0.0699 (14) | 0.0731 (14) | 0.0848 (17) | −0.0226 (12) | −0.0003 (11) | −0.0058 (11) |
C5 | 0.0526 (10) | 0.0528 (10) | 0.0578 (11) | −0.0057 (8) | −0.0061 (8) | 0.0040 (8) |
C6 | 0.0529 (9) | 0.0526 (10) | 0.0524 (10) | −0.0002 (8) | −0.0086 (8) | −0.0007 (8) |
C7 | 0.0687 (12) | 0.0690 (13) | 0.0704 (14) | −0.0076 (10) | −0.0090 (11) | −0.0145 (11) |
C8 | 0.0902 (17) | 0.0883 (17) | 0.0677 (15) | −0.0053 (13) | −0.0026 (12) | −0.0289 (13) |
C9 | 0.0847 (15) | 0.0872 (15) | 0.0640 (13) | −0.0010 (13) | 0.0134 (11) | −0.0174 (12) |
C10 | 0.0684 (12) | 0.0655 (12) | 0.0620 (12) | −0.0058 (10) | 0.0105 (10) | −0.0081 (9) |
C11 | 0.0722 (12) | 0.0690 (13) | 0.0611 (12) | −0.0089 (10) | −0.0102 (10) | 0.0084 (10) |
C12 | 0.0768 (14) | 0.0893 (17) | 0.0836 (17) | −0.0152 (13) | −0.0283 (13) | 0.0204 (14) |
C13 | 0.0591 (13) | 0.0988 (19) | 0.115 (2) | 0.0037 (12) | −0.0204 (14) | 0.0276 (17) |
C14 | 0.0565 (11) | 0.0773 (14) | 0.0929 (17) | 0.0088 (10) | 0.0021 (12) | 0.0125 (13) |
C15 | 0.0467 (9) | 0.0546 (10) | 0.0638 (12) | −0.0002 (8) | 0.0078 (8) | 0.0097 (8) |
C16 | 0.0532 (9) | 0.0533 (10) | 0.0569 (11) | 0.0000 (8) | 0.0102 (8) | 0.0007 (8) |
C17 | 0.0804 (14) | 0.0623 (12) | 0.0779 (15) | 0.0136 (10) | 0.0085 (11) | −0.0067 (11) |
C18 | 0.1001 (18) | 0.0680 (14) | 0.0754 (16) | 0.0067 (13) | 0.0120 (14) | −0.0194 (11) |
C19 | 0.0844 (14) | 0.0712 (13) | 0.0613 (13) | −0.0083 (11) | 0.0001 (11) | −0.0125 (10) |
C20 | 0.0624 (10) | 0.0608 (11) | 0.0587 (12) | −0.0039 (9) | −0.0014 (9) | −0.0042 (9) |
C21 | 0.0508 (9) | 0.0505 (10) | 0.0753 (14) | 0.0006 (8) | −0.0090 (9) | −0.0096 (9) |
C22 | 0.0496 (9) | 0.0500 (9) | 0.0623 (12) | 0.0004 (8) | 0.0022 (9) | −0.0094 (8) |
Fe1—N1 | 2.1762 (15) | C5—C6 | 1.484 (3) |
Fe1—N2 | 2.1452 (15) | C6—C7 | 1.382 (3) |
Fe1—N3 | 2.1847 (15) | C7—C8 | 1.378 (3) |
Fe1—N4 | 2.1555 (15) | C7—H7 | 0.9300 |
Fe1—N5 | 2.0773 (18) | C8—C9 | 1.367 (3) |
Fe1—N6 | 2.0765 (17) | C8—H8 | 0.9300 |
S1—C21 | 1.622 (2) | C9—C10 | 1.381 (3) |
S2—C22 | 1.624 (2) | C9—H9 | 0.9300 |
N1—C5 | 1.342 (2) | C10—H10 | 0.9300 |
N1—C1 | 1.342 (2) | C11—C12 | 1.375 (3) |
N2—C10 | 1.348 (2) | C11—H11 | 0.9300 |
N2—C6 | 1.350 (2) | C12—C13 | 1.381 (4) |
N3—C15 | 1.339 (2) | C12—H12 | 0.9300 |
N3—C11 | 1.355 (2) | C13—C14 | 1.376 (4) |
N4—C20 | 1.347 (2) | C13—H13 | 0.9300 |
N4—C16 | 1.348 (2) | C14—C15 | 1.394 (3) |
N5—C21 | 1.168 (2) | C14—H14 | 0.9300 |
N6—C22 | 1.159 (2) | C15—C16 | 1.496 (3) |
C1—C2 | 1.376 (3) | C16—C17 | 1.378 (3) |
C1—H1 | 0.9300 | C17—C18 | 1.380 (3) |
C2—C3 | 1.359 (3) | C17—H17 | 0.9300 |
C2—H2 | 0.9300 | C18—C19 | 1.365 (3) |
C3—C4 | 1.386 (3) | C18—H18 | 0.9300 |
C3—H3 | 0.9300 | C19—C20 | 1.367 (3) |
C4—C5 | 1.388 (3) | C19—H19 | 0.9300 |
C4—H4 | 0.9300 | C20—H20 | 0.9300 |
N1—Fe1—N2 | 75.72 (6) | C7—C6—C5 | 123.32 (17) |
N1—Fe1—N3 | 80.97 (6) | C8—C7—C6 | 119.59 (19) |
N1—Fe1—N4 | 98.73 (6) | C8—C7—H7 | 120.2 |
N1—Fe1—N5 | 91.50 (7) | C6—C7—H7 | 120.2 |
N1—Fe1—N6 | 164.50 (7) | C9—C8—C7 | 119.8 (2) |
N2—Fe1—N3 | 97.66 (6) | C9—C8—H8 | 120.1 |
N2—Fe1—N4 | 172.35 (5) | C7—C8—H8 | 120.1 |
N2—Fe1—N5 | 94.78 (6) | C8—C9—C10 | 118.4 (2) |
N2—Fe1—N6 | 92.19 (6) | C8—C9—H9 | 120.8 |
N3—Fe1—N4 | 76.08 (6) | C10—C9—H9 | 120.8 |
N3—Fe1—N5 | 163.37 (7) | N2—C10—C9 | 122.62 (19) |
N3—Fe1—N6 | 91.27 (6) | N2—C10—H10 | 118.7 |
N4—Fe1—N5 | 90.58 (6) | C9—C10—H10 | 118.7 |
N4—Fe1—N6 | 92.32 (6) | N3—C11—C12 | 123.3 (2) |
N5—Fe1—N6 | 99.27 (7) | N3—C11—H11 | 118.4 |
C5—N1—C1 | 118.56 (16) | C12—C11—H11 | 118.4 |
C5—N1—Fe1 | 116.02 (13) | C11—C12—C13 | 118.0 (2) |
C1—N1—Fe1 | 125.40 (13) | C11—C12—H12 | 121.0 |
C10—N2—C6 | 118.59 (16) | C13—C12—H12 | 121.0 |
C10—N2—Fe1 | 124.72 (13) | C14—C13—C12 | 119.6 (2) |
C6—N2—Fe1 | 116.63 (12) | C14—C13—H13 | 120.2 |
C15—N3—C11 | 118.37 (17) | C12—C13—H13 | 120.2 |
C15—N3—Fe1 | 115.50 (12) | C13—C14—C15 | 119.6 (2) |
C11—N3—Fe1 | 125.47 (14) | C13—C14—H14 | 120.2 |
C20—N4—C16 | 118.42 (16) | C15—C14—H14 | 120.2 |
C20—N4—Fe1 | 125.33 (12) | N3—C15—C14 | 121.2 (2) |
C16—N4—Fe1 | 115.87 (12) | N3—C15—C16 | 115.34 (16) |
C21—N5—Fe1 | 160.89 (17) | C14—C15—C16 | 123.5 (2) |
C22—N6—Fe1 | 168.26 (17) | N4—C16—C17 | 120.75 (19) |
N1—C1—C2 | 123.5 (2) | N4—C16—C15 | 116.23 (16) |
N1—C1—H1 | 118.2 | C17—C16—C15 | 123.01 (18) |
C2—C1—H1 | 118.2 | C16—C17—C18 | 119.5 (2) |
C3—C2—C1 | 117.7 (2) | C16—C17—H17 | 120.2 |
C3—C2—H2 | 121.1 | C18—C17—H17 | 120.2 |
C1—C2—H2 | 121.1 | C19—C18—C17 | 120.0 (2) |
C2—C3—C4 | 120.2 (2) | C19—C18—H18 | 120.0 |
C2—C3—H3 | 119.9 | C17—C18—H18 | 120.0 |
C4—C3—H3 | 119.9 | C18—C19—C20 | 117.9 (2) |
C3—C4—C5 | 119.1 (2) | C18—C19—H19 | 121.1 |
C3—C4—H4 | 120.4 | C20—C19—H19 | 121.1 |
C5—C4—H4 | 120.4 | N4—C20—C19 | 123.4 (2) |
N1—C5—C4 | 120.85 (19) | N4—C20—H20 | 118.3 |
N1—C5—C6 | 115.68 (16) | C19—C20—H20 | 118.3 |
C4—C5—C6 | 123.47 (18) | N5—C21—S1 | 179.0 (2) |
N2—C6—C7 | 120.96 (18) | N6—C22—S2 | 178.66 (18) |
N2—C6—C5 | 115.71 (15) |
D—H···A | D—H | H···A | D···A | D—H···A |
C2—H2···S1i | 0.93 | 2.85 | 3.736 (2) | 159 |
C10—H10···N6 | 0.93 | 2.62 | 3.158 (3) | 117 |
C20—H20···N5 | 0.93 | 2.60 | 3.146 (3) | 118 |
Symmetry code: (i) x+1/2, y, −z−1/2. |
Experimental details
Crystal data | |
Chemical formula | [Fe(NCS)2(C10H8N2)2] |
Mr | 484.38 |
Crystal system, space group | Orthorhombic, Pbca |
Temperature (K) | 273 |
a, b, c (Å) | 16.087 (3), 16.0117 (11), 17.0781 (12) |
V (Å3) | 4399.1 (9) |
Z | 8 |
Radiation type | Mo Kα |
µ (mm−1) | 0.90 |
Crystal size (mm) | 0.36 × 0.34 × 0.22 |
Data collection | |
Diffractometer | Bruker APEXII area-detector diffractometer |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.738, 0.827 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 28231, 4607, 3440 |
Rint | 0.023 |
(sin θ/λ)max (Å−1) | 0.630 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.028, 0.104, 0.99 |
No. of reflections | 4607 |
No. of parameters | 280 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.26, −0.31 |
Computer programs: APEX2 (Bruker, 2005), SAINT (Siemens, 1996), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL (Siemens, 1996).
Fe1—N1 | 2.1762 (15) | Fe1—N4 | 2.1555 (15) |
Fe1—N2 | 2.1452 (15) | Fe1—N5 | 2.0773 (18) |
Fe1—N3 | 2.1847 (15) | Fe1—N6 | 2.0765 (17) |
N1—Fe1—N2 | 75.72 (6) | N2—Fe1—N6 | 92.19 (6) |
N1—Fe1—N3 | 80.97 (6) | N3—Fe1—N4 | 76.08 (6) |
N1—Fe1—N4 | 98.73 (6) | N3—Fe1—N5 | 163.37 (7) |
N1—Fe1—N5 | 91.50 (7) | N3—Fe1—N6 | 91.27 (6) |
N1—Fe1—N6 | 164.50 (7) | N4—Fe1—N5 | 90.58 (6) |
N2—Fe1—N3 | 97.66 (6) | N4—Fe1—N6 | 92.32 (6) |
N2—Fe1—N4 | 172.35 (5) | N5—Fe1—N6 | 99.27 (7) |
N2—Fe1—N5 | 94.78 (6) |
D—H···A | D—H | H···A | D···A | D—H···A |
C2—H2···S1i | 0.93 | 2.85 | 3.736 (2) | 159 |
C10—H10···N6 | 0.93 | 2.62 | 3.158 (3) | 117 |
C20—H20···N5 | 0.93 | 2.60 | 3.146 (3) | 118 |
Symmetry code: (i) x+1/2, y, −z−1/2. |
Research on organic-inorganic hybrid materials has attracted much attention owing to their applications in areas including catalysis, materials chemistry and biochemistry (Hill, 1998; Banglin et al., 2001; Ferey, 2001). Weak interactions play an important role in these compounds and many frameworks are linked by different kinds of weak interactions, such as hydrogen bonds and π-π stacking. Several reported crystal structures of metal complexes incorporating the phenanthroline, quinoline and pyridyl ligand have shown the existence of π-π stacking between neighbouring aromatic rings in these structures (Wu et al., 2003; Pan & Xu, 2004; Liu et al., 2004; Li et al., 2005). We report herein the crystal structure of the title compound, (I), and the crystal struture is similar with the structures recently reported (Zhong et al., 2007a,b,c).
In the molecule of (I) (Fig. 1), the ligand bond lengths and angles are within normal ranges (Allen et al., 1987). The six-coordinate environment of the Fe atom is completed by the four N atoms of two 2,2'-bipyridyl ligands and two N atoms of two SCN- ligands (Table 1). The Fe—N bonds [average 2.1654 (15) Å] for the 2,2'-bipyridyl ligands are somewhat greater than the Fe—N bonds [average 2.0769 (18) Å] for the SCN- ligands. The two 2,2'-bipyridyl ligands are nearly perpendicular to each other, with a dihedral angle of 105.4 (3) °.
In the crystal structure, C—H···S and C—H···N non-classical hydrogen bonds between C—H groups of 2,2'-bipyridyl and N and S atoms of neighbouring SCN- ligands, with one C···S and two C···N distances of 3.736 (2), 3.146 (3) and 3.158 (3) Å, respectively, generate a layered hydrogen-bonded network (Table 2). The non-classical hydrogen-bonding interactions and π-π stacking interactions with centroid-centroid distance of 3.619 (7) Å [symmetry code: 1 - x, 2 - y, 2 - z] link the mononuclear complex into a supramolecular network structure (Fig. 2).