Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807039177/bt2467sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807039177/bt2467Isup2.hkl |
CCDC reference: 660089
Key indicators
- Single-crystal X-ray study
- T = 295 K
- Mean (C-C) = 0.003 Å
- R factor = 0.037
- wR factor = 0.091
- Data-to-parameter ratio = 15.5
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT230_ALERT_2_B Hirshfeld Test Diff for S1 - C13 .. 7.81 su
Alert level C PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.96 PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.74 PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Fe1 - N1 .. 6.08 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Fe1 - N5_a .. 6.15 su
Alert level G PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K PLAT794_ALERT_5_G Check Predicted Bond Valency for Fe1 (2) 2.05
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 4 ALERT level C = Check and explain 2 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 4 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 0 ALERT type 4 Improvement, methodology, query or suggestion 1 ALERT type 5 Informative message, check
For a review of the coordination chemistry of 3,5-di-2-pyridyl-1,2,4-triazoles and related N-heterocycles, see Klingele & Brooker (2003). For the crystal structure of dinuclear derivatives of the deprotonated ligand, see Chen, Hu et al. (2006) and Chen, Zhou et al. (2006).
4-Amino-3,5-di-2-pyridyl-1,2,4-triazole was purchased from Aldrich Chemical Company. 3,5-di-2-pyridyl-1,2,4-triazole was synthesized by the deammoniation of the compound. Sulfuric acid (2M, 20 ml) was added to a mixture of the compound (11.9 g, 0.05 mol) and sodium nitrite (3.45 g, 0.05 mol) at 273 K. Hypophosphorus acid (0.05 mol) when added gave an immediate precipitate, which was then purified by recrystallization from ethanol (80% yield). 3,5-di-2-pyridyl-1,2,4-triazole, ferrous sulfate and potassium thiocyanate (0.1 mmol each) were suspended in methanol (8 ml). The suspension was heated in a 23-ml, Teflon-lined Parr bomb at 383 K for 96 h. The bomb was then cooled at 5 K h-1 to room temperature. Block-shaped crystals were picked by hand (40% yield).
Carbon-bound H atoms were placed at calculated positions (C–H 0.93 – 0.96 Å) and were included in the refinement in the riding model approximation, with U(H) set to 1.2 – 1.5 times Ueq(C). The hydroxy H atom was located in a difference Fourier map, and its positional and displacement parameters were refined.
The coordination chemistry of the class of 3,5-di-2-pyridyl-1,2,4-triazole N-heterocycles has been reviewed (Klingele & Brooker, 2003). The deprotonated 3,5-di-2-pyridyl-1,2,4-triazole monoanion is capable of using the pyridyl as well as the triazolyl nitrogen atoms to coordinate to more than one metal center, as noted in the trichloridodicopper(I)copper(II) (Chen, Zhou et al., 2006) and tetrachloridodiiron(III) and dichloridodiron(II) (Chen, Hu et al., 2006) complexes. Centrosymmetric dinuclear (C12H8N5)2(CH4O)2(NCS)2Fe2 has the deprotonated ligand using a pair of N'pyridyl/N1 atoms to chelate to one metal atom and its other pair of N"pyridyl/N2 atoms to chelate to the other metal atom, the four nitrogen atoms approximating a square. The six-coordinate environment has the nitrogen atom of the thiocyanate anion and the oxygen atom of the methanol molecule in the other two sites of the octahedron. Intermolecular hydrogen bonding between the hydroxy group and the 4-nitrogen atom of the ligand gives rise to a layer motif.
For a review of the coordination chemistry of 3,5-di-2-pyridyl-1,2,4-triazoles and related N-heterocycles, see Klingele & Brooker (2003). For the crystal structure of dinuclear derivatives of the deprotonated ligand, see Chen, Hu et al. (2006) and Chen, Zhou et al. (2006).
Data collection: SMART (Bruker, 2002); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: X-SEED (Barbour, 2001); software used to prepare material for publication: publCIF (Westrip, 2007).
Fig. 1. Thermal ellipsoid plot of (C12H8N5)2(CH4O)2(NCS)2Fe2. Displacement ellipsoids are drawn at the 70% probability level, and H atoms as spheres of arbitrary radii. |
[Fe2(C12H8N5)2(NCS)2(CH4O)2] | F(000) = 752 |
Mr = 736.41 | Dx = 1.560 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 3100 reflections |
a = 11.5051 (8) Å | θ = 2.3–27.0° |
b = 14.291 (1) Å | µ = 1.11 mm−1 |
c = 9.7794 (7) Å | T = 295 K |
β = 102.885 (1)° | Block, black |
V = 1567.4 (2) Å3 | 0.35 × 0.20 × 0.18 mm |
Z = 2 |
Bruker APEX area-detector diffractometer | 3302 independent reflections |
Radiation source: fine-focus sealed tube | 2827 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.032 |
φ and ω scans | θmax = 27.0°, θmin = 2.3° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −14→13 |
Tmin = 0.698, Tmax = 0.826 | k = −17→18 |
8319 measured reflections | l = −9→12 |
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)] = 0.037 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.092 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.02 | w = 1/[σ2(Fo2) + (0.0535P)2P] where P = (Fo2 + 2Fc2)/3 |
3302 reflections | (Δ/σ)max = 0.001 |
213 parameters | Δρmax = 0.75 e Å−3 |
0 restraints | Δρmin = −0.27 e Å−3 |
[Fe2(C12H8N5)2(NCS)2(CH4O)2] | V = 1567.4 (2) Å3 |
Mr = 736.41 | Z = 2 |
Monoclinic, P21/c | Mo Kα radiation |
a = 11.5051 (8) Å | µ = 1.11 mm−1 |
b = 14.291 (1) Å | T = 295 K |
c = 9.7794 (7) Å | 0.35 × 0.20 × 0.18 mm |
β = 102.885 (1)° |
Bruker APEX area-detector diffractometer | 3302 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 2827 reflections with I > 2σ(I) |
Tmin = 0.698, Tmax = 0.826 | Rint = 0.032 |
8319 measured reflections |
R[F2 > 2σ(F2)] = 0.037 | 0 restraints |
wR(F2) = 0.092 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.02 | Δρmax = 0.75 e Å−3 |
3302 reflections | Δρmin = −0.27 e Å−3 |
213 parameters |
x | y | z | Uiso*/Ueq | ||
Fe1 | 0.64986 (2) | 0.524340 (19) | 0.41164 (3) | 0.01615 (11) | |
S1 | 0.95226 (5) | 0.42521 (5) | 0.81308 (6) | 0.02961 (16) | |
O1 | 0.54102 (13) | 0.57952 (11) | 0.21963 (16) | 0.0211 (3) | |
H1o | 0.541 (2) | 0.636 (2) | 0.207 (3) | 0.038 (8)* | |
N1 | 0.70485 (15) | 0.41319 (12) | 0.26974 (19) | 0.0207 (4) | |
N2 | 0.53238 (15) | 0.40957 (12) | 0.40463 (18) | 0.0178 (4) | |
N3 | 0.44253 (14) | 0.39173 (11) | 0.47076 (18) | 0.0175 (4) | |
N4 | 0.47467 (15) | 0.26108 (11) | 0.35794 (18) | 0.0178 (4) | |
N5 | 0.26895 (15) | 0.32792 (12) | 0.58072 (18) | 0.0199 (4) | |
N6 | 0.78557 (18) | 0.48169 (13) | 0.5746 (2) | 0.0271 (4) | |
C1 | 0.79195 (19) | 0.42006 (16) | 0.2001 (2) | 0.0253 (5) | |
H1 | 0.8348 | 0.4757 | 0.2064 | 0.030* | |
C2 | 0.82160 (19) | 0.34804 (17) | 0.1186 (2) | 0.0264 (5) | |
H2 | 0.8822 | 0.3559 | 0.0706 | 0.032* | |
C3 | 0.7597 (2) | 0.26473 (16) | 0.1102 (2) | 0.0251 (5) | |
H3 | 0.7786 | 0.2152 | 0.0573 | 0.030* | |
C4 | 0.66880 (18) | 0.25605 (14) | 0.1818 (2) | 0.0214 (5) | |
H4 | 0.6258 | 0.2006 | 0.1778 | 0.026* | |
C5 | 0.64317 (18) | 0.33118 (14) | 0.2593 (2) | 0.0192 (4) | |
C6 | 0.54899 (17) | 0.33112 (14) | 0.3386 (2) | 0.0165 (4) | |
C7 | 0.41065 (17) | 0.30331 (14) | 0.4418 (2) | 0.0166 (4) | |
C8 | 0.31801 (17) | 0.26428 (14) | 0.5074 (2) | 0.0185 (4) | |
C9 | 0.28571 (18) | 0.17074 (15) | 0.4987 (2) | 0.0224 (5) | |
H9 | 0.3199 | 0.1291 | 0.4459 | 0.027* | |
C10 | 0.20137 (19) | 0.14047 (17) | 0.5702 (2) | 0.0256 (5) | |
H10 | 0.1795 | 0.0777 | 0.5680 | 0.031* | |
C11 | 0.1505 (2) | 0.20409 (17) | 0.6443 (2) | 0.0274 (5) | |
H11 | 0.0937 | 0.1852 | 0.6928 | 0.033* | |
C12 | 0.18556 (18) | 0.29756 (16) | 0.6456 (2) | 0.0247 (5) | |
H12 | 0.1492 | 0.3407 | 0.6937 | 0.030* | |
C13 | 0.85569 (19) | 0.45901 (15) | 0.6734 (2) | 0.0221 (5) | |
C14 | 0.4317 (2) | 0.53995 (17) | 0.1449 (3) | 0.0333 (6) | |
H14A | 0.4008 | 0.5766 | 0.0626 | 0.050* | |
H14B | 0.3752 | 0.5395 | 0.2039 | 0.050* | |
H14C | 0.4453 | 0.4770 | 0.1179 | 0.050* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Fe1 | 0.01877 (17) | 0.01035 (18) | 0.01979 (18) | −0.00042 (11) | 0.00532 (12) | −0.00032 (11) |
S1 | 0.0239 (3) | 0.0385 (4) | 0.0252 (3) | 0.0026 (3) | 0.0028 (2) | 0.0052 (3) |
O1 | 0.0241 (8) | 0.0122 (8) | 0.0251 (8) | −0.0013 (6) | 0.0019 (6) | 0.0026 (6) |
N1 | 0.0213 (9) | 0.0175 (9) | 0.0244 (10) | 0.0008 (7) | 0.0076 (7) | 0.0012 (7) |
N2 | 0.0215 (8) | 0.0118 (8) | 0.0216 (9) | −0.0015 (7) | 0.0079 (7) | −0.0002 (7) |
N3 | 0.0201 (8) | 0.0118 (9) | 0.0222 (9) | −0.0008 (7) | 0.0083 (7) | 0.0008 (7) |
N4 | 0.0206 (9) | 0.0121 (9) | 0.0205 (9) | −0.0013 (7) | 0.0043 (7) | −0.0006 (7) |
N5 | 0.0192 (8) | 0.0178 (10) | 0.0219 (9) | −0.0016 (7) | 0.0027 (7) | 0.0001 (7) |
N6 | 0.0282 (10) | 0.0216 (11) | 0.0289 (11) | 0.0028 (8) | 0.0009 (9) | −0.0004 (8) |
C1 | 0.0232 (11) | 0.0216 (12) | 0.0317 (13) | −0.0004 (9) | 0.0076 (9) | 0.0037 (10) |
C2 | 0.0232 (11) | 0.0310 (13) | 0.0270 (12) | 0.0045 (10) | 0.0101 (9) | 0.0016 (10) |
C3 | 0.0310 (12) | 0.0225 (12) | 0.0220 (12) | 0.0077 (10) | 0.0065 (9) | −0.0023 (9) |
C4 | 0.0244 (11) | 0.0161 (11) | 0.0231 (11) | 0.0013 (9) | 0.0042 (9) | −0.0005 (9) |
C5 | 0.0204 (10) | 0.0160 (11) | 0.0206 (11) | 0.0015 (8) | 0.0032 (8) | 0.0017 (8) |
C6 | 0.0189 (10) | 0.0122 (10) | 0.0178 (10) | −0.0002 (8) | 0.0028 (8) | 0.0012 (8) |
C7 | 0.0184 (9) | 0.0122 (10) | 0.0190 (10) | −0.0010 (8) | 0.0037 (8) | 0.0000 (8) |
C8 | 0.0193 (10) | 0.0173 (11) | 0.0179 (11) | 0.0000 (8) | 0.0019 (8) | 0.0024 (8) |
C9 | 0.0245 (11) | 0.0181 (11) | 0.0242 (11) | −0.0022 (9) | 0.0045 (9) | −0.0012 (9) |
C10 | 0.0255 (11) | 0.0229 (12) | 0.0269 (12) | −0.0083 (9) | 0.0023 (9) | 0.0017 (10) |
C11 | 0.0229 (11) | 0.0317 (14) | 0.0285 (12) | −0.0087 (10) | 0.0078 (9) | 0.0033 (10) |
C12 | 0.0225 (11) | 0.0279 (13) | 0.0247 (11) | −0.0014 (10) | 0.0071 (9) | −0.0013 (10) |
C13 | 0.0248 (11) | 0.0165 (11) | 0.0274 (12) | −0.0013 (9) | 0.0107 (10) | −0.0024 (9) |
C14 | 0.0347 (13) | 0.0219 (13) | 0.0362 (14) | −0.0059 (11) | −0.0071 (11) | 0.0029 (11) |
Fe1—O1 | 2.160 (2) | C2—C3 | 1.380 (3) |
Fe1—N1 | 2.289 (2) | C2—H2 | 0.9300 |
Fe1—N2 | 2.117 (2) | C3—C4 | 1.388 (3) |
Fe1—N3i | 2.106 (2) | C3—H3 | 0.9300 |
Fe1—N5i | 2.303 (2) | C4—C5 | 1.383 (3) |
Fe1—N6 | 2.059 (2) | C4—H4 | 0.9300 |
S1—C13 | 1.630 (2) | C5—C6 | 1.467 (3) |
O1—C14 | 1.423 (3) | C7—C8 | 1.471 (3) |
O1—H1o | 0.82 (3) | C8—C9 | 1.385 (3) |
N1—C1 | 1.335 (3) | C9—C10 | 1.386 (3) |
N1—C5 | 1.362 (3) | C9—H9 | 0.9300 |
N2—C6 | 1.329 (3) | C10—C11 | 1.372 (3) |
N2—N3 | 1.360 (2) | C10—H10 | 0.9300 |
N4—C6 | 1.357 (2) | C11—C12 | 1.394 (3) |
N4—C7 | 1.359 (3) | C11—H11 | 0.9300 |
N5—C12 | 1.335 (3) | C12—H12 | 0.9300 |
N5—C8 | 1.356 (3) | C14—H14A | 0.9600 |
N6—C13 | 1.158 (3) | C14—H14B | 0.9600 |
C1—C2 | 1.390 (3) | C14—H14C | 0.9600 |
C1—H1 | 0.9300 | ||
N6—Fe1—N3i | 97.69 (7) | C2—C3—C4 | 118.9 (2) |
N6—Fe1—N2 | 99.45 (7) | C2—C3—H3 | 120.5 |
N3i—Fe1—N2 | 93.59 (6) | C4—C3—H3 | 120.5 |
N6—Fe1—O1 | 166.75 (7) | C5—C4—C3 | 118.93 (19) |
N3i—Fe1—O1 | 90.08 (6) | C5—C4—H4 | 120.5 |
N2—Fe1—O1 | 90.71 (6) | C3—C4—H4 | 120.5 |
N6—Fe1—N1 | 89.98 (7) | N1—C5—C4 | 122.55 (19) |
N3i—Fe1—N1 | 165.34 (6) | N1—C5—C6 | 113.25 (18) |
N2—Fe1—N1 | 72.75 (6) | C4—C5—C6 | 124.20 (19) |
O1—Fe1—N1 | 84.91 (6) | N2—C6—N4 | 113.04 (17) |
N6—Fe1—N5i | 90.82 (7) | N2—C6—C5 | 117.38 (17) |
N3i—Fe1—N5i | 73.18 (6) | N4—C6—C5 | 129.58 (18) |
N2—Fe1—N5i | 164.32 (6) | N3—C7—N4 | 112.96 (17) |
O1—Fe1—N5i | 81.13 (6) | N3—C7—C8 | 117.37 (18) |
N1—Fe1—N5i | 119.40 (6) | N4—C7—C8 | 129.61 (18) |
C14—O1—Fe1 | 125.15 (14) | N5—C8—C9 | 122.85 (19) |
C14—O1—H1o | 109.9 (18) | N5—C8—C7 | 113.81 (18) |
Fe1—O1—H1o | 118.5 (19) | C9—C8—C7 | 123.32 (19) |
C1—N1—C5 | 117.57 (18) | C8—C9—C10 | 118.6 (2) |
C1—N1—Fe1 | 126.76 (15) | C8—C9—H9 | 120.7 |
C5—N1—Fe1 | 115.65 (13) | C10—C9—H9 | 120.7 |
C6—N2—N3 | 106.25 (16) | C11—C10—C9 | 119.2 (2) |
C6—N2—Fe1 | 120.63 (13) | C11—C10—H10 | 120.4 |
N3—N2—Fe1 | 132.64 (13) | C9—C10—H10 | 120.4 |
C7—N3—N2 | 106.24 (16) | C10—C11—C12 | 118.9 (2) |
C7—N3—Fe1i | 120.61 (13) | C10—C11—H11 | 120.6 |
N2—N3—Fe1i | 133.04 (13) | C12—C11—H11 | 120.6 |
C6—N4—C7 | 101.51 (16) | N5—C12—C11 | 123.0 (2) |
C12—N5—C8 | 117.44 (19) | N5—C12—H12 | 118.5 |
C12—N5—Fe1i | 127.71 (15) | C11—C12—H12 | 118.5 |
C8—N5—Fe1i | 114.73 (13) | N6—C13—S1 | 178.7 (2) |
C13—N6—Fe1 | 174.49 (19) | O1—C14—H14A | 109.5 |
N1—C1—C2 | 123.1 (2) | O1—C14—H14B | 109.5 |
N1—C1—H1 | 118.4 | H14A—C14—H14B | 109.5 |
C2—C1—H1 | 118.4 | O1—C14—H14C | 109.5 |
C3—C2—C1 | 118.9 (2) | H14A—C14—H14C | 109.5 |
C3—C2—H2 | 120.5 | H14B—C14—H14C | 109.5 |
C1—C2—H2 | 120.5 | ||
N6—Fe1—O1—C14 | 143.2 (3) | C1—N1—C5—C6 | −179.54 (18) |
N3i—Fe1—O1—C14 | −90.68 (18) | Fe1—N1—C5—C6 | 2.0 (2) |
N2—Fe1—O1—C14 | 2.91 (18) | C3—C4—C5—N1 | −1.0 (3) |
N1—Fe1—O1—C14 | 75.52 (17) | C3—C4—C5—C6 | 179.54 (19) |
N5i—Fe1—O1—C14 | −163.64 (18) | N3—N2—C6—N4 | −0.3 (2) |
N6—Fe1—N1—C1 | −82.18 (18) | Fe1—N2—C6—N4 | 172.72 (12) |
N3i—Fe1—N1—C1 | 156.0 (2) | N3—N2—C6—C5 | −179.34 (17) |
N2—Fe1—N1—C1 | 177.91 (19) | Fe1—N2—C6—C5 | −6.3 (2) |
O1—Fe1—N1—C1 | 85.58 (18) | C7—N4—C6—N2 | 0.0 (2) |
N5i—Fe1—N1—C1 | 8.7 (2) | C7—N4—C6—C5 | 178.9 (2) |
N6—Fe1—N1—C5 | 96.12 (15) | N1—C5—C6—N2 | 2.5 (3) |
N3i—Fe1—N1—C5 | −25.7 (3) | C4—C5—C6—N2 | −177.98 (19) |
N2—Fe1—N1—C5 | −3.79 (14) | N1—C5—C6—N4 | −176.37 (19) |
O1—Fe1—N1—C5 | −96.12 (15) | C4—C5—C6—N4 | 3.2 (3) |
N5i—Fe1—N1—C5 | −172.96 (13) | N2—N3—C7—N4 | −0.5 (2) |
N6—Fe1—N2—C6 | −81.62 (16) | Fe1i—N3—C7—N4 | 176.19 (13) |
N3i—Fe1—N2—C6 | 179.96 (16) | N2—N3—C7—C8 | 176.88 (16) |
O1—Fe1—N2—C6 | 89.84 (16) | Fe1i—N3—C7—C8 | −6.4 (2) |
N1—Fe1—N2—C6 | 5.39 (15) | C6—N4—C7—N3 | 0.3 (2) |
N5i—Fe1—N2—C6 | 148.1 (2) | C6—N4—C7—C8 | −176.7 (2) |
N6—Fe1—N2—N3 | 89.26 (18) | C12—N5—C8—C9 | −0.4 (3) |
N3i—Fe1—N2—N3 | −9.1 (2) | Fe1i—N5—C8—C9 | 175.95 (16) |
O1—Fe1—N2—N3 | −99.28 (18) | C12—N5—C8—C7 | −178.85 (17) |
N1—Fe1—N2—N3 | 176.27 (19) | Fe1i—N5—C8—C7 | −2.5 (2) |
N5i—Fe1—N2—N3 | −41.0 (3) | N3—C7—C8—N5 | 5.7 (3) |
C6—N2—N3—C7 | 0.5 (2) | N4—C7—C8—N5 | −177.49 (19) |
Fe1—N2—N3—C7 | −171.37 (14) | N3—C7—C8—C9 | −172.74 (19) |
C6—N2—N3—Fe1i | −175.62 (14) | N4—C7—C8—C9 | 4.1 (3) |
Fe1—N2—N3—Fe1i | 12.5 (3) | N5—C8—C9—C10 | −1.3 (3) |
C5—N1—C1—C2 | 0.1 (3) | C7—C8—C9—C10 | 176.91 (19) |
Fe1—N1—C1—C2 | 178.33 (16) | C8—C9—C10—C11 | 1.6 (3) |
N1—C1—C2—C3 | −0.9 (3) | C9—C10—C11—C12 | −0.1 (3) |
C1—C2—C3—C4 | 0.9 (3) | C8—N5—C12—C11 | 2.0 (3) |
C2—C3—C4—C5 | 0.0 (3) | Fe1i—N5—C12—C11 | −173.83 (16) |
C1—N1—C5—C4 | 0.9 (3) | C10—C11—C12—N5 | −1.8 (3) |
Fe1—N1—C5—C4 | −177.56 (16) |
Symmetry code: (i) −x+1, −y+1, −z+1. |
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1o···N4ii | 0.82 (3) | 1.89 (3) | 2.698 (2) | 169 (3) |
Symmetry code: (ii) −x+1, y+1/2, −z+1/2. |
Experimental details
Crystal data | |
Chemical formula | [Fe2(C12H8N5)2(NCS)2(CH4O)2] |
Mr | 736.41 |
Crystal system, space group | Monoclinic, P21/c |
Temperature (K) | 295 |
a, b, c (Å) | 11.5051 (8), 14.291 (1), 9.7794 (7) |
β (°) | 102.885 (1) |
V (Å3) | 1567.4 (2) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 1.11 |
Crystal size (mm) | 0.35 × 0.20 × 0.18 |
Data collection | |
Diffractometer | Bruker APEX area-detector |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.698, 0.826 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 8319, 3302, 2827 |
Rint | 0.032 |
(sin θ/λ)max (Å−1) | 0.639 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.037, 0.092, 1.02 |
No. of reflections | 3302 |
No. of parameters | 213 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 0.75, −0.27 |
Computer programs: SMART (Bruker, 2002), SAINT (Bruker, 2002), SAINT, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), X-SEED (Barbour, 2001), publCIF (Westrip, 2007).
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1o···N4i | 0.82 (3) | 1.89 (3) | 2.698 (2) | 169 (3) |
Symmetry code: (i) −x+1, y+1/2, −z+1/2. |
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The coordination chemistry of the class of 3,5-di-2-pyridyl-1,2,4-triazole N-heterocycles has been reviewed (Klingele & Brooker, 2003). The deprotonated 3,5-di-2-pyridyl-1,2,4-triazole monoanion is capable of using the pyridyl as well as the triazolyl nitrogen atoms to coordinate to more than one metal center, as noted in the trichloridodicopper(I)copper(II) (Chen, Zhou et al., 2006) and tetrachloridodiiron(III) and dichloridodiron(II) (Chen, Hu et al., 2006) complexes. Centrosymmetric dinuclear (C12H8N5)2(CH4O)2(NCS)2Fe2 has the deprotonated ligand using a pair of N'pyridyl/N1 atoms to chelate to one metal atom and its other pair of N"pyridyl/N2 atoms to chelate to the other metal atom, the four nitrogen atoms approximating a square. The six-coordinate environment has the nitrogen atom of the thiocyanate anion and the oxygen atom of the methanol molecule in the other two sites of the octahedron. Intermolecular hydrogen bonding between the hydroxy group and the 4-nitrogen atom of the ligand gives rise to a layer motif.