The molecular structure of the neutral mononuclear complex [Fe(NCS)
2(3-bpo)
2(H
2O)
2], in which 3-bpo denotes 2,5-di-3-pyridyl-1,3,4-oxadiazole (C
12H
8N
4O), is centrosymmetric, with Fe
II located on an inversion center. This complex is octahedral, and the Fe
II atom is
trans coordinated by two monodentate NSC
− ligands, two monodentate 3-bpo ligands and two water molecules. Each complex is linked to four others, forming a (011) sheet, by O—H
N hydrogen bonding. Weak C—H
S interactions link each (011) sheet to the two adjacent sheets, hence forming a three-dimensional array. There is also some slipped π stacking within each sheet.
Supporting information
CCDC reference: 271863
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.004 Å
- R factor = 0.041
- wR factor = 0.093
- Data-to-parameter ratio = 12.5
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT199_ALERT_1_C Check the Reported _cell_measurement_temperature 293 K
PLAT200_ALERT_1_C Check the Reported _diffrn_ambient_temperature . 293 K
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C13
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
3 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
1 ALERT type 2 Indicator that the structure model may be wrong or deficient
0 ALERT type 3 Indicator that the structure quality may be low
0 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: Apex II (Bruker, 2003); cell refinement: Apex II; data reduction: SAINT (Bruker, 2001); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 2001) and Diamond (Brandenburg & Berndt, 1999); software used to prepare material for publication: SHELXTL.
Crystal data top
[Fe(C12H8N4O)2(NCS)2(H2O)2] | Z = 1 |
Mr = 656.49 | F(000) = 336 |
Triclinic, P1 | Dx = 1.522 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 8.159 (7) Å | Cell parameters from 697 reflections |
b = 8.712 (7) Å | θ = 2.4–26.0° |
c = 10.531 (9) Å | µ = 0.73 mm−1 |
α = 82.385 (13)° | T = 293 K |
β = 77.494 (13)° | Prism, red |
γ = 80.064 (14)° | 0.20 × 0.18 × 0.14 mm |
V = 716.3 (10) Å3 | |
Data collection top
Bruker Apex II CCD area-detector diffractometer | 2517 independent reflections |
Radiation source: fine-focus sealed tube | 1851 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.023 |
φ and ω scans | θmax = 25.0°, θmin = 2.0° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −9→6 |
Tmin = 0.810, Tmax = 0.903 | k = −10→9 |
3735 measured reflections | l = −12→8 |
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)] = 0.041 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.093 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.02 | w = 1/[σ2(Fo2) + (0.0371P)2 + 0.299P] where P = (Fo2 + 2Fc2)/3 |
2517 reflections | (Δ/σ)max < 0.001 |
202 parameters | Δρmax = 0.33 e Å−3 |
3 restraints | Δρmin = −0.31 e Å−3 |
Special details top
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 | Uiso*/Ueq | |
Fe1 | 0.5000 | 0.5000 | 0.5000 | 0.03567 (19) | |
S1 | 0.16220 (12) | 0.16682 (11) | 0.82089 (10) | 0.0682 (3) | |
O1 | 0.4221 (2) | 0.7240 (2) | −0.00258 (16) | 0.0367 (5) | |
O2 | 0.6678 (3) | 0.2960 (2) | 0.44115 (17) | 0.0448 (5) | |
H2A | 0.689 (4) | 0.278 (3) | 0.3621 (11) | 0.054* | |
H2B | 0.665 (4) | 0.213 (2) | 0.491 (2) | 0.054* | |
N1 | 0.3255 (3) | 0.4840 (3) | 0.36059 (19) | 0.0344 (5) | |
N2 | 0.2220 (3) | 0.6455 (3) | −0.0771 (2) | 0.0421 (6) | |
N3 | 0.3129 (3) | 0.7396 (3) | −0.1770 (2) | 0.0403 (6) | |
C10 | 0.8144 (5) | 0.9708 (4) | −0.1869 (4) | 0.0700 (11) | |
H10 | 0.9034 | 0.9777 | −0.1466 | 0.084* | |
N5 | 0.3539 (3) | 0.3654 (3) | 0.6457 (2) | 0.0458 (6) | |
C1 | 0.1889 (4) | 0.4127 (3) | 0.3953 (3) | 0.0385 (7) | |
H1 | 0.1671 | 0.3618 | 0.4792 | 0.046* | |
C2 | 0.0782 (4) | 0.4095 (3) | 0.3152 (3) | 0.0436 (8) | |
H2 | −0.0162 | 0.3584 | 0.3448 | 0.052* | |
C3 | 0.1086 (4) | 0.4830 (3) | 0.1900 (3) | 0.0396 (7) | |
H3 | 0.0363 | 0.4822 | 0.1329 | 0.048* | |
C4 | 0.2504 (3) | 0.5580 (3) | 0.1519 (2) | 0.0320 (6) | |
C5 | 0.3545 (3) | 0.5556 (3) | 0.2397 (2) | 0.0342 (6) | |
H5 | 0.4494 | 0.6064 | 0.2132 | 0.041* | |
C6 | 0.2907 (4) | 0.6401 (3) | 0.0219 (2) | 0.0338 (6) | |
C7 | 0.4275 (4) | 0.7829 (3) | −0.1293 (2) | 0.0352 (6) | |
C8 | 0.5604 (4) | 0.8765 (3) | −0.1894 (3) | 0.0382 (7) | |
C12 | 0.5626 (4) | 0.9562 (3) | −0.3123 (3) | 0.0465 (8) | |
H12 | 0.4753 | 0.9509 | −0.3548 | 0.056* | |
N4 | 0.6837 (4) | 1.0398 (3) | −0.3724 (2) | 0.0554 (7) | |
C11 | 0.8064 (5) | 1.0459 (4) | −0.3093 (4) | 0.0642 (10) | |
H11 | 0.8919 | 1.1042 | −0.3502 | 0.077* | |
C9 | 0.6887 (4) | 0.8863 (4) | −0.1262 (3) | 0.0559 (9) | |
H9 | 0.6896 | 0.8356 | −0.0428 | 0.067* | |
C13 | 0.2738 (4) | 0.2827 (3) | 0.7194 (3) | 0.0381 (7) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Fe1 | 0.0386 (4) | 0.0461 (4) | 0.0252 (3) | −0.0194 (3) | −0.0093 (3) | 0.0085 (2) |
S1 | 0.0460 (5) | 0.0661 (6) | 0.0834 (7) | −0.0251 (5) | −0.0043 (5) | 0.0327 (5) |
O1 | 0.0431 (12) | 0.0428 (11) | 0.0267 (9) | −0.0136 (10) | −0.0111 (8) | 0.0037 (8) |
O2 | 0.0637 (15) | 0.0457 (12) | 0.0264 (10) | −0.0149 (11) | −0.0112 (10) | 0.0049 (9) |
N1 | 0.0345 (13) | 0.0436 (14) | 0.0270 (11) | −0.0116 (11) | −0.0097 (10) | 0.0034 (10) |
N2 | 0.0493 (16) | 0.0536 (15) | 0.0273 (12) | −0.0186 (13) | −0.0134 (11) | 0.0055 (11) |
N3 | 0.0490 (16) | 0.0476 (14) | 0.0264 (12) | −0.0148 (12) | −0.0108 (11) | 0.0042 (10) |
C10 | 0.072 (3) | 0.073 (3) | 0.074 (2) | −0.040 (2) | −0.029 (2) | 0.020 (2) |
N5 | 0.0465 (16) | 0.0590 (17) | 0.0353 (13) | −0.0250 (14) | −0.0131 (12) | 0.0133 (12) |
C1 | 0.0385 (17) | 0.0513 (18) | 0.0264 (13) | −0.0152 (14) | −0.0057 (13) | 0.0042 (12) |
C2 | 0.0375 (18) | 0.057 (2) | 0.0386 (16) | −0.0210 (15) | −0.0088 (14) | 0.0067 (14) |
C3 | 0.0364 (17) | 0.0494 (17) | 0.0373 (15) | −0.0113 (14) | −0.0145 (13) | −0.0011 (13) |
C4 | 0.0350 (16) | 0.0349 (15) | 0.0264 (13) | −0.0050 (13) | −0.0086 (12) | −0.0002 (11) |
C5 | 0.0345 (16) | 0.0408 (16) | 0.0291 (14) | −0.0125 (13) | −0.0076 (12) | 0.0014 (12) |
C6 | 0.0348 (16) | 0.0369 (15) | 0.0311 (14) | −0.0093 (13) | −0.0087 (12) | 0.0007 (12) |
C7 | 0.0429 (18) | 0.0342 (15) | 0.0273 (14) | −0.0047 (13) | −0.0081 (13) | 0.0017 (12) |
C8 | 0.0444 (18) | 0.0345 (15) | 0.0340 (15) | −0.0072 (14) | −0.0060 (13) | 0.0012 (12) |
C12 | 0.052 (2) | 0.0460 (18) | 0.0412 (17) | −0.0141 (16) | −0.0091 (15) | 0.0051 (14) |
N4 | 0.064 (2) | 0.0508 (17) | 0.0482 (16) | −0.0211 (15) | −0.0051 (15) | 0.0123 (12) |
C11 | 0.059 (2) | 0.059 (2) | 0.073 (2) | −0.0293 (19) | −0.005 (2) | 0.0109 (18) |
C9 | 0.065 (2) | 0.060 (2) | 0.0488 (19) | −0.0274 (19) | −0.0217 (17) | 0.0137 (16) |
C13 | 0.0337 (17) | 0.0454 (17) | 0.0377 (16) | −0.0115 (14) | −0.0136 (13) | 0.0048 (13) |
Geometric parameters (Å, º) top
Fe1—N5 | 2.089 (2) | C1—C2 | 1.369 (4) |
Fe1—O2 | 2.122 (2) | C1—H1 | 0.9300 |
Fe1—N1 | 2.287 (2) | C2—C3 | 1.378 (4) |
S1—C13 | 1.612 (3) | C2—H2 | 0.9300 |
O1—C7 | 1.359 (3) | C3—C4 | 1.384 (4) |
O1—C6 | 1.360 (3) | C3—H3 | 0.9300 |
O2—H2A | 0.843 (10) | C4—C5 | 1.380 (4) |
O2—H2B | 0.841 (10) | C4—C6 | 1.456 (4) |
N1—C1 | 1.328 (3) | C5—H5 | 0.9300 |
N1—C5 | 1.333 (3) | C7—C8 | 1.453 (4) |
N2—C6 | 1.279 (3) | C8—C9 | 1.376 (4) |
N2—N3 | 1.404 (3) | C8—C12 | 1.383 (4) |
N3—C7 | 1.282 (4) | C12—N4 | 1.328 (4) |
C10—C9 | 1.362 (4) | C12—H12 | 0.9300 |
C10—C11 | 1.375 (5) | N4—C11 | 1.327 (4) |
C10—H10 | 0.9300 | C11—H11 | 0.9300 |
N5—C13 | 1.159 (3) | C9—H9 | 0.9300 |
| | | |
N5—Fe1—O2i | 89.22 (11) | C4—C3—H3 | 121.1 |
N5—Fe1—O2 | 90.78 (11) | C5—C4—C3 | 119.1 (2) |
N5—Fe1—N1i | 90.38 (10) | C5—C4—C6 | 119.5 (2) |
O2—Fe1—N1i | 86.75 (9) | C3—C4—C6 | 121.4 (2) |
N5—Fe1—N1 | 89.62 (10) | N1—C5—C4 | 123.1 (3) |
O2—Fe1—N1 | 93.25 (9) | N1—C5—H5 | 118.4 |
C7—O1—C6 | 102.8 (2) | C4—C5—H5 | 118.4 |
Fe1—O2—H2A | 119.6 (19) | N2—C6—O1 | 112.8 (2) |
Fe1—O2—H2B | 119 (2) | N2—C6—C4 | 129.9 (3) |
H2A—O2—H2B | 111 (2) | O1—C6—C4 | 117.3 (2) |
C1—N1—C5 | 116.9 (2) | N3—C7—O1 | 111.8 (2) |
C1—N1—Fe1 | 123.42 (17) | N3—C7—C8 | 130.8 (2) |
C5—N1—Fe1 | 119.61 (18) | O1—C7—C8 | 117.3 (2) |
C6—N2—N3 | 105.7 (2) | C9—C8—C12 | 118.3 (3) |
C7—N3—N2 | 106.9 (2) | C9—C8—C7 | 120.8 (3) |
C9—C10—C11 | 118.2 (3) | C12—C8—C7 | 120.9 (3) |
C9—C10—H10 | 120.9 | N4—C12—C8 | 123.0 (3) |
C11—C10—H10 | 120.9 | N4—C12—H12 | 118.5 |
C13—N5—Fe1 | 174.7 (2) | C8—C12—H12 | 118.5 |
N1—C1—C2 | 124.1 (2) | C11—N4—C12 | 117.2 (3) |
N1—C1—H1 | 118.0 | N4—C11—C10 | 123.8 (3) |
C2—C1—H1 | 118.0 | N4—C11—H11 | 118.1 |
C1—C2—C3 | 119.0 (3) | C10—C11—H11 | 118.1 |
C1—C2—H2 | 120.5 | C10—C9—C8 | 119.4 (3) |
C3—C2—H2 | 120.5 | C10—C9—H9 | 120.3 |
C2—C3—C4 | 117.8 (3) | C8—C9—H9 | 120.3 |
C2—C3—H3 | 121.1 | N5—C13—S1 | 179.5 (3) |
Symmetry code: (i) −x+1, −y+1, −z+1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O2—H2A···N3ii | 0.84 (1) | 1.98 (1) | 2.807 (4) | 167 (3) |
O2—H2B···N4iii | 0.84 (1) | 1.95 (1) | 2.775 (3) | 168 (3) |
C10—H10···S1iv | 0.93 | 2.83 | 3.575 (4) | 138 |
C9—H9···S1i | 0.93 | 2.85 | 3.625 (4) | 141 |
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) −x+1, −y+1, −z; (iii) x, y−1, z+1; (iv) x+1, y+1, z−1. |