Buy article online - an online subscription or single-article purchase is required to access this article.
The superstructure recently discovered in [Fe(pic)3]Cl2.EtOH at temperatures inside the step region of the high-spin–low-spin transition curve sheds new light on the anomalous transition behaviour in spin crossover compounds. The structure of the metastable LIESST state of [Fe(pic)3]Cl2.EtOH at 10 K has been measured. The decay has been followed by X-ray diffraction using a CCD camera in order to detect reflections of the superstructure building up during the decay. No signal above the noise of the CCD camera was observed, so that even diffuse scattering could not be detected. This finding is in agreement with correlation lengths of pair correlations of molecules in the HS and LS states being very short, as was concluded earlier from the shape of the decay curves of the HS fraction by theoretical considerations [Romstedt et al. (1998). J. Phys. Chem. Solids, 59, 265–275]. The crystal structure inside the step at 118 K has also been studied under continuous irradiation. The temperature range of the superstructure and the degree of order could be changed by continuous irradiation with green laser light, indicating an increase of the lifetime of the HS excited state by several orders of magnitude compared with the temperature regions outside.
Supporting information
CCDC references: 273100; 273101; 273102; 273103; 273104; 273105
Data collection: Enraf Nonius Software V5 for ev_fpic118, fepic100, fepic200, fpic118h; CrysAlis (Oxford Diffraction, 2002) for fpic10k, fpic11hs. Cell refinement: Enraf Nonius Software V5 for ev_fpic118, fepic100, fepic200, fpic118h; STADI4 (Stoe, 1995) for fpic10k, fpic11hs. Data reduction: Corinc (Dräger, 1971) for ev_fpic118, fepic100, fepic200, fpic118h; CrysAlis (Oxford Diffraction, 2002) for fpic10k, fpic11hs. For all compounds, program(s) used to solve structure: SIR92 (Altomare, 1994); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: PLATON (Spek, 2003); software used to prepare material for publication: SHELXL97 (Sheldrick, 1997).
(ev_fpic118) 'tris(2-Picolylamine)-iron(ii) chloride ethanol solvate'
top
Crystal data top
C18H24FeN6·C2H6O·2(Cl) | F(000) = 1040 |
Mr = 497.25 | Dx = 1.392 Mg m−3 |
Monoclinic, P21/c | Cu Kα radiation, λ = 1.54178 Å |
a = 10.8041 (9) Å | Cell parameters from 25 reflections |
b = 21.6945 (14) Å | θ = 21.5–26.8° |
c = 11.395 (4) Å | µ = 7.36 mm−1 |
β = 117.33 (3)° | T = 118 K |
V = 2372.7 (9) Å3 | Block, red |
Z = 4 | 0.46 × 0.12 × 0.12 mm |
Data collection top
CAD4 Enraf Nonius diffractometer | 3612 reflections with I > 2σ(I) |
Radiation source: rotating anode | Rint = 0.053 |
Graphite monochromator | θmax = 73.8°, θmin = 4.1° |
Detector resolution: point detector pixels mm-1 | h = −11→13 |
θ/2ω scans | k = −27→0 |
5041 measured reflections | l = −14→0 |
4798 independent reflections | |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.075 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.197 | Calculated w = 1/[σ2(Fo2) + (0.1071P)2 + 2.315P] where P = (Fo2 + 2Fc2)/3 |
S = 1.13 | (Δ/σ)max < 0.001 |
4798 reflections | Δρmax = 1.36 e Å−3 |
274 parameters | Δρmin = −1.43 e Å−3 |
0 restraints | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0008 (2) |
Crystal data top
C18H24FeN6·C2H6O·2(Cl) | V = 2372.7 (9) Å3 |
Mr = 497.25 | Z = 4 |
Monoclinic, P21/c | Cu Kα radiation |
a = 10.8041 (9) Å | µ = 7.36 mm−1 |
b = 21.6945 (14) Å | T = 118 K |
c = 11.395 (4) Å | 0.46 × 0.12 × 0.12 mm |
β = 117.33 (3)° | |
Data collection top
CAD4 Enraf Nonius diffractometer | 3612 reflections with I > 2σ(I) |
5041 measured reflections | Rint = 0.053 |
4798 independent reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.075 | 0 restraints |
wR(F2) = 0.197 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.13 | Δρmax = 1.36 e Å−3 |
4798 reflections | Δρmin = −1.43 e Å−3 |
274 parameters | |
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 | 0.02844 (7) | 0.13394 (3) | 0.80450 (7) | 0.0227 (2) | |
Cl2 | 0.26469 (11) | 0.27405 (6) | 1.08044 (12) | 0.0336 (3) | |
Cl1 | −0.13622 (12) | 0.06958 (6) | 1.06252 (11) | 0.0309 (3) | |
N6 | −0.1439 (4) | 0.18945 (18) | 0.7646 (4) | 0.0270 (9) | |
N4 | 0.2316 (5) | 0.1009 (2) | 0.8755 (5) | 0.0338 (10) | |
N1 | −0.0619 (4) | 0.0509 (2) | 0.8160 (4) | 0.0299 (9) | |
H1A | −0.1048 | 0.0547 | 0.8726 | 0.036* | |
H1B | 0.0110 | 0.0224 | 0.8396 | 0.036* | |
N5 | 0.0959 (4) | 0.21908 (18) | 0.7674 (4) | 0.0231 (8) | |
H5A | 0.1472 | 0.2338 | 0.8562 | 0.028* | |
H5B | 0.1751 | 0.2215 | 0.7421 | 0.028* | |
N3 | 0.1005 (5) | 0.1429 (3) | 1.0074 (6) | 0.0581 (18) | |
H3A | 0.0379 | 0.1379 | 1.0234 | 0.070* | |
H3B | 0.1224 | 0.1830 | 1.0147 | 0.070* | |
N2 | −0.0502 (4) | 0.10136 (19) | 0.6105 (4) | 0.0247 (8) | |
C2 | −0.1391 (5) | 0.0534 (2) | 0.5792 (5) | 0.0266 (10) | |
C15 | −0.2561 (5) | 0.2855 (2) | 0.6706 (5) | 0.0283 (10) | |
H15 | −0.2559 | 0.3230 | 0.6277 | 0.034* | |
O32 | 0.3050 (5) | 0.3907 (3) | 0.9344 (6) | 0.0660 (14) | |
H32 | 0.280 (2) | 0.344 (4) | 0.983 (4) | 0.099* | |
C18 | −0.2484 (5) | 0.1780 (3) | 0.7948 (5) | 0.0322 (11) | |
H18 | −0.2449 | 0.1409 | 0.8406 | 0.039* | |
C5 | −0.0673 (5) | 0.0941 (2) | 0.3932 (5) | 0.0314 (11) | |
H5 | −0.0409 | 0.1092 | 0.3296 | 0.038* | |
C8 | 0.2991 (5) | 0.0919 (2) | 1.0067 (6) | 0.0347 (12) | |
C13 | −0.0256 (5) | 0.2573 (2) | 0.6800 (5) | 0.0265 (10) | |
H13A | −0.0511 | 0.2483 | 0.5865 | 0.032* | |
H13B | −0.0010 | 0.3015 | 0.6964 | 0.032* | |
C11 | 0.4451 (7) | 0.0848 (3) | 0.8649 (7) | 0.0464 (16) | |
H11 | 0.4935 | 0.0827 | 0.8134 | 0.056* | |
C3 | −0.1947 (6) | 0.0247 (2) | 0.4579 (5) | 0.0336 (11) | |
H3 | −0.2574 | −0.0088 | 0.4394 | 0.040* | |
C14 | −0.1472 (5) | 0.2438 (2) | 0.7058 (5) | 0.0238 (9) | |
C16 | −0.3647 (5) | 0.2716 (2) | 0.6986 (5) | 0.0311 (11) | |
H16 | −0.4411 | 0.2991 | 0.6741 | 0.037* | |
C1 | −0.1752 (5) | 0.0327 (2) | 0.6874 (5) | 0.0310 (11) | |
H1AA | −0.2636 | 0.0522 | 0.6743 | 0.037* | |
H1BB | −0.1875 | −0.0126 | 0.6839 | 0.037* | |
C9 | 0.4400 (6) | 0.0791 (3) | 1.0715 (6) | 0.0402 (13) | |
H9 | 0.4854 | 0.0729 | 1.1644 | 0.048* | |
C6 | −0.0150 (5) | 0.1209 (2) | 0.5168 (5) | 0.0296 (10) | |
H6 | 0.0482 | 0.1544 | 0.5370 | 0.036* | |
C4 | −0.1581 (6) | 0.0453 (3) | 0.3636 (5) | 0.0366 (12) | |
H4 | −0.1951 | 0.0261 | 0.2794 | 0.044* | |
C7 | 0.2103 (6) | 0.0973 (4) | 1.0748 (6) | 0.0525 (19) | |
H7A | 0.1680 | 0.0568 | 1.0747 | 0.063* | |
H7B | 0.2682 | 0.1100 | 1.1678 | 0.063* | |
C12 | 0.3043 (6) | 0.0974 (2) | 0.8068 (7) | 0.0385 (13) | |
H12 | 0.2567 | 0.1038 | 0.7141 | 0.046* | |
C17 | −0.3598 (5) | 0.2168 (2) | 0.7633 (5) | 0.0317 (11) | |
H17 | −0.4320 | 0.2063 | 0.7853 | 0.038* | |
C31 | 0.4475 (7) | 0.3928 (3) | 0.9705 (7) | 0.0524 (16) | |
H31A | 0.4994 | 0.3955 | 1.0680 | 0.063* | |
H31B | 0.4661 | 0.4312 | 0.9344 | 0.063* | |
C30 | 0.5044 (7) | 0.3405 (4) | 0.9271 (7) | 0.061 (2) | |
H30A | 0.4942 | 0.3024 | 0.9681 | 0.091* | |
H30B | 0.6032 | 0.3478 | 0.9538 | 0.091* | |
H30C | 0.4534 | 0.3367 | 0.8308 | 0.091* | |
C10 | 0.5143 (6) | 0.0753 (3) | 1.0008 (7) | 0.0434 (14) | |
H10 | 0.6112 | 0.0663 | 1.0440 | 0.052* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Fe1 | 0.0113 (3) | 0.0267 (4) | 0.0313 (4) | −0.0008 (3) | 0.0108 (3) | −0.0062 (3) |
Cl2 | 0.0172 (5) | 0.0509 (8) | 0.0349 (6) | −0.0059 (5) | 0.0139 (5) | −0.0084 (5) |
Cl1 | 0.0252 (6) | 0.0421 (7) | 0.0282 (5) | 0.0137 (5) | 0.0148 (5) | 0.0027 (5) |
N6 | 0.0109 (17) | 0.025 (2) | 0.040 (2) | 0.0003 (15) | 0.0079 (16) | 0.0057 (17) |
N4 | 0.037 (2) | 0.026 (2) | 0.052 (3) | −0.0109 (18) | 0.033 (2) | −0.0114 (19) |
N1 | 0.025 (2) | 0.039 (2) | 0.025 (2) | 0.0149 (17) | 0.0103 (17) | −0.0003 (16) |
N5 | 0.0163 (17) | 0.026 (2) | 0.0297 (19) | −0.0017 (15) | 0.0130 (15) | −0.0018 (15) |
N3 | 0.027 (2) | 0.087 (4) | 0.074 (4) | −0.024 (3) | 0.034 (3) | −0.050 (3) |
N2 | 0.0191 (18) | 0.036 (2) | 0.0195 (18) | 0.0080 (16) | 0.0094 (15) | 0.0008 (15) |
C2 | 0.024 (2) | 0.031 (2) | 0.026 (2) | 0.0091 (19) | 0.0123 (19) | 0.0045 (18) |
C15 | 0.020 (2) | 0.025 (2) | 0.039 (3) | 0.0015 (18) | 0.012 (2) | 0.0025 (19) |
O32 | 0.047 (3) | 0.070 (3) | 0.089 (4) | 0.010 (2) | 0.038 (3) | 0.014 (3) |
C18 | 0.014 (2) | 0.036 (3) | 0.041 (3) | −0.0027 (19) | 0.008 (2) | 0.008 (2) |
C5 | 0.035 (3) | 0.035 (3) | 0.023 (2) | 0.007 (2) | 0.013 (2) | 0.0025 (19) |
C8 | 0.030 (3) | 0.034 (3) | 0.047 (3) | −0.018 (2) | 0.023 (2) | −0.020 (2) |
C13 | 0.023 (2) | 0.025 (2) | 0.033 (2) | 0.0016 (18) | 0.015 (2) | 0.0004 (18) |
C11 | 0.055 (4) | 0.025 (3) | 0.084 (5) | 0.004 (2) | 0.053 (4) | 0.004 (3) |
C3 | 0.038 (3) | 0.031 (3) | 0.029 (2) | 0.003 (2) | 0.013 (2) | −0.002 (2) |
C14 | 0.020 (2) | 0.020 (2) | 0.031 (2) | −0.0011 (17) | 0.0111 (19) | 0.0020 (17) |
C16 | 0.019 (2) | 0.028 (2) | 0.044 (3) | 0.0058 (19) | 0.013 (2) | 0.002 (2) |
C1 | 0.031 (3) | 0.034 (3) | 0.028 (2) | 0.001 (2) | 0.013 (2) | −0.001 (2) |
C9 | 0.032 (3) | 0.035 (3) | 0.056 (3) | −0.008 (2) | 0.023 (3) | −0.010 (2) |
C6 | 0.024 (2) | 0.038 (3) | 0.029 (2) | 0.006 (2) | 0.014 (2) | 0.000 (2) |
C4 | 0.050 (3) | 0.038 (3) | 0.020 (2) | 0.006 (2) | 0.015 (2) | −0.003 (2) |
C7 | 0.028 (3) | 0.103 (6) | 0.029 (3) | −0.022 (3) | 0.014 (2) | −0.024 (3) |
C12 | 0.048 (3) | 0.023 (3) | 0.066 (4) | 0.006 (2) | 0.044 (3) | 0.004 (2) |
C17 | 0.017 (2) | 0.036 (3) | 0.044 (3) | −0.0025 (19) | 0.015 (2) | 0.006 (2) |
C31 | 0.037 (3) | 0.059 (4) | 0.059 (4) | 0.002 (3) | 0.020 (3) | 0.006 (3) |
C30 | 0.048 (4) | 0.091 (6) | 0.045 (4) | 0.027 (4) | 0.023 (3) | 0.013 (4) |
C10 | 0.034 (3) | 0.025 (3) | 0.079 (4) | 0.000 (2) | 0.033 (3) | −0.003 (3) |
Geometric parameters (Å, º) top
Fe1—N3 | 2.082 (6) | C2—C1 | 1.522 (6) |
Fe1—N1 | 2.082 (5) | C15—C16 | 1.384 (7) |
Fe1—N6 | 2.085 (4) | C15—C14 | 1.389 (6) |
Fe1—N4 | 2.087 (5) | O32—C31 | 1.400 (7) |
Fe1—N2 | 2.094 (4) | C18—C17 | 1.375 (7) |
Fe1—N5 | 2.099 (4) | C5—C4 | 1.377 (8) |
N6—C18 | 1.346 (6) | C5—C6 | 1.382 (7) |
N6—C14 | 1.347 (6) | C8—C9 | 1.382 (8) |
N4—C12 | 1.341 (6) | C8—C7 | 1.489 (7) |
N4—C8 | 1.344 (7) | C13—C14 | 1.501 (6) |
N1—C1 | 1.468 (6) | C11—C12 | 1.378 (8) |
N5—C13 | 1.484 (6) | C11—C10 | 1.392 (10) |
N3—C7 | 1.462 (9) | C3—C4 | 1.378 (7) |
N2—C2 | 1.348 (6) | C16—C17 | 1.387 (7) |
N2—C6 | 1.355 (6) | C9—C10 | 1.376 (8) |
C2—C3 | 1.377 (7) | C31—C30 | 1.480 (10) |
| | | |
N3—Fe1—N1 | 87.6 (2) | C6—N2—Fe1 | 127.0 (4) |
N3—Fe1—N6 | 91.71 (19) | N2—C2—C3 | 123.0 (4) |
N1—Fe1—N6 | 96.67 (15) | N2—C2—C1 | 115.4 (4) |
N3—Fe1—N4 | 79.09 (19) | C3—C2—C1 | 121.6 (5) |
N1—Fe1—N4 | 96.82 (16) | C16—C15—C14 | 119.1 (5) |
N6—Fe1—N4 | 163.30 (16) | N6—C18—C17 | 123.8 (5) |
N3—Fe1—N2 | 165.3 (2) | C4—C5—C6 | 118.9 (5) |
N1—Fe1—N2 | 78.43 (16) | N4—C8—C9 | 121.7 (5) |
N6—Fe1—N2 | 94.34 (16) | N4—C8—C7 | 114.7 (5) |
N4—Fe1—N2 | 97.96 (16) | C9—C8—C7 | 123.6 (6) |
N3—Fe1—N5 | 98.9 (2) | N5—C13—C14 | 110.1 (4) |
N1—Fe1—N5 | 172.15 (15) | C12—C11—C10 | 118.3 (5) |
N6—Fe1—N5 | 78.78 (15) | C2—C3—C4 | 119.1 (5) |
N4—Fe1—N5 | 88.81 (15) | N6—C14—C15 | 122.7 (4) |
N2—Fe1—N5 | 95.43 (16) | N6—C14—C13 | 116.2 (4) |
C18—N6—C14 | 117.0 (4) | C15—C14—C13 | 121.1 (4) |
C18—N6—Fe1 | 127.4 (3) | C15—C16—C17 | 118.6 (4) |
C14—N6—Fe1 | 115.5 (3) | N1—C1—C2 | 108.9 (4) |
C12—N4—C8 | 118.5 (5) | C10—C9—C8 | 119.7 (6) |
C12—N4—Fe1 | 126.0 (4) | N2—C6—C5 | 122.8 (5) |
C8—N4—Fe1 | 114.7 (3) | C5—C4—C3 | 119.1 (5) |
C1—N1—Fe1 | 111.7 (3) | N3—C7—C8 | 109.9 (6) |
C13—N5—Fe1 | 110.2 (3) | N4—C12—C11 | 122.9 (6) |
C7—N3—Fe1 | 108.7 (3) | C18—C17—C16 | 118.7 (4) |
C2—N2—C6 | 117.1 (4) | O32—C31—C30 | 116.5 (6) |
C2—N2—Fe1 | 115.8 (3) | C9—C10—C11 | 118.9 (6) |
(fepic100) 'tris(2-Picolylamine)-iron(ii) chloride ethanol solvate'
top
Crystal data top
C18H24FeN6·C2H6O·2(Cl) | F(000) = 1040 |
Mr = 497.25 | Dx = 1.408 Mg m−3 |
Monoclinic, P21/c | Cu Kα radiation, λ = 1.54178 Å |
a = 10.7098 (17) Å | Cell parameters from 25 reflections |
b = 21.5711 (13) Å | θ = 21.5–26.8° |
c = 11.356 (4) Å | µ = 7.44 mm−1 |
β = 116.62 (3)° | T = 100 K |
V = 2345.5 (9) Å3 | Block, red |
Z = 4 | 0.46 × 0.12 × 0.12 mm |
Data collection top
CAD4 Enraf Nonius diffractometer | 4752 independent reflections |
Radiation source: rotating anode | 3699 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.056 |
Detector resolution: point detector pixels mm-1 | θmax = 74.0°, θmin = 4.1° |
θ/2ω scans | h = −11→13 |
Absorption correction: ψ scan ? | k = −26→0 |
Tmin = 0.399, Tmax = 0.411 | l = −14→0 |
4994 measured reflections | |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.064 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.173 | Calculated w = 1/[σ2(Fo2) + (0.1071P)2 + 2.315P] where P = (Fo2 + 2Fc2)/3 |
S = 1.04 | (Δ/σ)max < 0.001 |
4752 reflections | Δρmax = 1.20 e Å−3 |
274 parameters | Δρmin = −1.34 e Å−3 |
0 restraints | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0009 (2) |
Crystal data top
C18H24FeN6·C2H6O·2(Cl) | V = 2345.5 (9) Å3 |
Mr = 497.25 | Z = 4 |
Monoclinic, P21/c | Cu Kα radiation |
a = 10.7098 (17) Å | µ = 7.44 mm−1 |
b = 21.5711 (13) Å | T = 100 K |
c = 11.356 (4) Å | 0.46 × 0.12 × 0.12 mm |
β = 116.62 (3)° | |
Data collection top
CAD4 Enraf Nonius diffractometer | 4752 independent reflections |
Absorption correction: ψ scan ? | 3699 reflections with I > 2σ(I) |
Tmin = 0.399, Tmax = 0.411 | Rint = 0.056 |
4994 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.064 | 0 restraints |
wR(F2) = 0.173 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.04 | Δρmax = 1.20 e Å−3 |
4752 reflections | Δρmin = −1.34 e Å−3 |
274 parameters | |
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 | 0.02566 (6) | 0.13334 (3) | 0.80177 (6) | 0.01536 (19) | |
Cl2 | 0.26794 (10) | 0.27443 (5) | 1.08067 (10) | 0.0233 (2) | |
Cl1 | −0.13660 (10) | 0.07046 (5) | 1.06507 (10) | 0.0209 (2) | |
N6 | −0.1446 (3) | 0.18489 (16) | 0.7613 (3) | 0.0193 (7) | |
N4 | 0.2194 (4) | 0.10005 (16) | 0.8678 (4) | 0.0209 (7) | |
N1 | −0.0579 (3) | 0.05174 (16) | 0.8199 (3) | 0.0189 (7) | |
H1A | −0.1007 | 0.0556 | 0.8766 | 0.023* | |
H1B | 0.0151 | 0.0233 | 0.8436 | 0.023* | |
N5 | 0.0973 (3) | 0.21639 (16) | 0.7700 (4) | 0.0194 (7) | |
H5A | 0.1486 | 0.2311 | 0.8588 | 0.023* | |
H5B | 0.1765 | 0.2188 | 0.7447 | 0.023* | |
N3 | 0.0913 (4) | 0.14741 (17) | 0.9965 (4) | 0.0223 (8) | |
H3A | 0.0286 | 0.1424 | 1.0125 | 0.027* | |
H3B | 0.1131 | 0.1875 | 1.0038 | 0.027* | |
N2 | −0.0475 (3) | 0.10278 (16) | 0.6146 (3) | 0.0184 (7) | |
C2 | −0.1369 (4) | 0.05401 (19) | 0.5837 (4) | 0.0181 (8) | |
C15 | −0.2559 (4) | 0.2827 (2) | 0.6729 (4) | 0.0220 (9) | |
H15 | −0.2551 | 0.3209 | 0.6318 | 0.026* | |
O32 | 0.3055 (4) | 0.3910 (2) | 0.9324 (5) | 0.0490 (11) | |
H32 | 0.2865 (14) | 0.347 (3) | 0.980 (3) | 0.073* | |
C18 | −0.2507 (4) | 0.1727 (2) | 0.7913 (4) | 0.0223 (9) | |
H18 | −0.2487 | 0.1348 | 0.8346 | 0.027* | |
C5 | −0.0655 (4) | 0.0971 (2) | 0.3966 (4) | 0.0232 (9) | |
H5 | −0.0381 | 0.1125 | 0.3333 | 0.028* | |
C8 | 0.2899 (4) | 0.09322 (19) | 0.9997 (4) | 0.0211 (8) | |
C13 | −0.0221 (4) | 0.2552 (2) | 0.6820 (4) | 0.0214 (9) | |
H13A | −0.0449 | 0.2465 | 0.5890 | 0.026* | |
H13B | 0.0026 | 0.2996 | 0.6995 | 0.026* | |
C11 | 0.4336 (5) | 0.0815 (2) | 0.8548 (5) | 0.0293 (10) | |
H11 | 0.4814 | 0.0776 | 0.8021 | 0.035* | |
C3 | −0.1933 (5) | 0.0263 (2) | 0.4619 (4) | 0.0240 (9) | |
H3 | −0.2560 | −0.0076 | 0.4439 | 0.029* | |
C14 | −0.1461 (4) | 0.24092 (19) | 0.7060 (4) | 0.0192 (8) | |
C16 | −0.3655 (4) | 0.2682 (2) | 0.7001 (5) | 0.0245 (9) | |
H16 | −0.4421 | 0.2958 | 0.6767 | 0.029* | |
C1 | −0.1709 (4) | 0.0325 (2) | 0.6919 (4) | 0.0203 (8) | |
H1AA | −0.2605 | 0.0508 | 0.6800 | 0.024* | |
H1BB | −0.1803 | −0.0132 | 0.6891 | 0.024* | |
C9 | 0.4314 (5) | 0.0809 (2) | 1.0631 (5) | 0.0292 (10) | |
H9 | 0.4779 | 0.0767 | 1.1562 | 0.035* | |
C6 | −0.0132 (4) | 0.12332 (19) | 0.5200 (4) | 0.0195 (8) | |
H6 | 0.0495 | 0.1573 | 0.5398 | 0.023* | |
C4 | −0.1586 (5) | 0.0479 (2) | 0.3654 (4) | 0.0251 (9) | |
H4 | −0.1973 | 0.0295 | 0.2804 | 0.030* | |
C7 | 0.2016 (4) | 0.1015 (2) | 1.0703 (4) | 0.0233 (9) | |
H7A | 0.1589 | 0.0615 | 1.0751 | 0.028* | |
H7B | 0.2598 | 0.1164 | 1.1612 | 0.028* | |
C12 | 0.2915 (5) | 0.0939 (2) | 0.7968 (5) | 0.0246 (9) | |
H12 | 0.2431 | 0.0983 | 0.7038 | 0.030* | |
C17 | −0.3618 (4) | 0.2122 (2) | 0.7626 (4) | 0.0228 (9) | |
H17 | −0.4345 | 0.2014 | 0.7851 | 0.027* | |
C31 | 0.4488 (6) | 0.3963 (3) | 0.9675 (6) | 0.0422 (13) | |
H31A | 0.5007 | 0.4001 | 1.0645 | 0.051* | |
H31B | 0.4643 | 0.4349 | 0.9287 | 0.051* | |
C30 | 0.5076 (6) | 0.3428 (3) | 0.9241 (6) | 0.0438 (14) | |
H30A | 0.4971 | 0.3046 | 0.9656 | 0.066* | |
H30B | 0.6068 | 0.3502 | 0.9502 | 0.066* | |
H30C | 0.4572 | 0.3386 | 0.8281 | 0.066* | |
C10 | 0.5047 (5) | 0.0748 (2) | 0.9898 (6) | 0.0322 (11) | |
H10 | 0.6020 | 0.0661 | 1.0315 | 0.039* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Fe1 | 0.0088 (3) | 0.0154 (3) | 0.0229 (3) | 0.0001 (2) | 0.0081 (2) | −0.0003 (2) |
Cl2 | 0.0133 (4) | 0.0248 (5) | 0.0335 (5) | −0.0025 (4) | 0.0120 (4) | −0.0050 (4) |
Cl1 | 0.0170 (5) | 0.0228 (5) | 0.0265 (5) | 0.0039 (4) | 0.0129 (4) | 0.0024 (4) |
N6 | 0.0119 (16) | 0.0197 (17) | 0.0257 (18) | 0.0011 (13) | 0.0079 (14) | 0.0025 (14) |
N4 | 0.0175 (17) | 0.0151 (16) | 0.034 (2) | −0.0005 (13) | 0.0152 (15) | −0.0007 (14) |
N1 | 0.0140 (16) | 0.0172 (17) | 0.0268 (18) | 0.0013 (13) | 0.0105 (14) | −0.0005 (13) |
N5 | 0.0135 (16) | 0.0184 (17) | 0.0268 (18) | −0.0010 (13) | 0.0093 (14) | −0.0001 (14) |
N3 | 0.0156 (17) | 0.0239 (19) | 0.033 (2) | −0.0001 (14) | 0.0162 (15) | −0.0027 (15) |
N2 | 0.0127 (15) | 0.0210 (17) | 0.0229 (17) | 0.0030 (13) | 0.0094 (14) | −0.0006 (14) |
C2 | 0.0137 (18) | 0.020 (2) | 0.0207 (19) | 0.0015 (15) | 0.0074 (16) | 0.0028 (15) |
C15 | 0.019 (2) | 0.017 (2) | 0.030 (2) | 0.0003 (16) | 0.0099 (17) | 0.0020 (16) |
O32 | 0.037 (2) | 0.040 (2) | 0.074 (3) | 0.0109 (18) | 0.028 (2) | 0.016 (2) |
C18 | 0.0117 (19) | 0.026 (2) | 0.029 (2) | −0.0019 (16) | 0.0087 (17) | 0.0019 (17) |
C5 | 0.024 (2) | 0.026 (2) | 0.022 (2) | 0.0007 (18) | 0.0123 (18) | 0.0015 (16) |
C8 | 0.019 (2) | 0.0148 (19) | 0.030 (2) | −0.0047 (15) | 0.0113 (18) | −0.0044 (15) |
C13 | 0.021 (2) | 0.018 (2) | 0.029 (2) | 0.0018 (16) | 0.0140 (18) | 0.0012 (16) |
C11 | 0.024 (2) | 0.020 (2) | 0.053 (3) | 0.0011 (18) | 0.026 (2) | 0.000 (2) |
C3 | 0.021 (2) | 0.022 (2) | 0.030 (2) | −0.0010 (17) | 0.0115 (19) | −0.0019 (17) |
C14 | 0.019 (2) | 0.017 (2) | 0.022 (2) | −0.0017 (15) | 0.0095 (17) | 0.0024 (15) |
C16 | 0.015 (2) | 0.022 (2) | 0.035 (2) | 0.0030 (16) | 0.0105 (18) | −0.0003 (18) |
C1 | 0.017 (2) | 0.022 (2) | 0.024 (2) | −0.0027 (16) | 0.0106 (17) | −0.0008 (16) |
C9 | 0.022 (2) | 0.024 (2) | 0.040 (3) | −0.0021 (18) | 0.012 (2) | −0.0031 (19) |
C6 | 0.0163 (19) | 0.018 (2) | 0.027 (2) | −0.0012 (15) | 0.0125 (17) | 0.0000 (16) |
C4 | 0.022 (2) | 0.028 (2) | 0.022 (2) | 0.0014 (18) | 0.0069 (18) | −0.0008 (17) |
C7 | 0.0151 (19) | 0.032 (2) | 0.020 (2) | 0.0026 (17) | 0.0048 (16) | −0.0014 (17) |
C12 | 0.021 (2) | 0.021 (2) | 0.036 (2) | 0.0016 (17) | 0.0169 (19) | −0.0006 (17) |
C17 | 0.0134 (19) | 0.025 (2) | 0.032 (2) | −0.0016 (16) | 0.0121 (17) | 0.0015 (17) |
C31 | 0.030 (3) | 0.040 (3) | 0.055 (3) | −0.001 (2) | 0.017 (3) | 0.002 (3) |
C30 | 0.036 (3) | 0.056 (4) | 0.040 (3) | 0.020 (3) | 0.018 (2) | 0.011 (3) |
C10 | 0.015 (2) | 0.023 (2) | 0.057 (3) | −0.0004 (17) | 0.015 (2) | −0.004 (2) |
Geometric parameters (Å, º) top
Fe1—N4 | 1.997 (4) | C2—C1 | 1.504 (5) |
Fe1—N6 | 2.006 (3) | C15—C16 | 1.378 (6) |
Fe1—N2 | 2.019 (4) | C15—C14 | 1.392 (6) |
Fe1—N3 | 2.021 (4) | O32—C31 | 1.406 (6) |
Fe1—N1 | 2.026 (4) | C18—C17 | 1.378 (6) |
Fe1—N5 | 2.044 (4) | C5—C6 | 1.377 (6) |
N6—C18 | 1.350 (5) | C5—C4 | 1.390 (6) |
N6—C14 | 1.359 (5) | C8—C9 | 1.381 (6) |
N4—C12 | 1.349 (5) | C8—C7 | 1.500 (6) |
N4—C8 | 1.350 (6) | C13—C14 | 1.503 (6) |
N1—C1 | 1.475 (5) | C11—C10 | 1.381 (8) |
N5—C13 | 1.479 (5) | C11—C12 | 1.387 (6) |
N3—C7 | 1.480 (5) | C3—C4 | 1.386 (6) |
N2—C6 | 1.355 (5) | C16—C17 | 1.393 (6) |
N2—C2 | 1.358 (5) | C9—C10 | 1.384 (7) |
C2—C3 | 1.373 (6) | C31—C30 | 1.500 (8) |
| | | |
N4—Fe1—N6 | 166.03 (15) | C2—N2—Fe1 | 114.9 (3) |
N4—Fe1—N2 | 97.21 (15) | N2—C2—C3 | 122.6 (4) |
N6—Fe1—N2 | 93.19 (14) | N2—C2—C1 | 115.4 (4) |
N4—Fe1—N3 | 81.38 (15) | C3—C2—C1 | 122.0 (4) |
N6—Fe1—N3 | 90.12 (15) | C16—C15—C14 | 119.6 (4) |
N2—Fe1—N3 | 169.12 (15) | N6—C18—C17 | 123.7 (4) |
N4—Fe1—N1 | 94.66 (14) | C6—C5—C4 | 119.4 (4) |
N6—Fe1—N1 | 96.17 (14) | N4—C8—C9 | 122.5 (4) |
N2—Fe1—N1 | 80.95 (14) | N4—C8—C7 | 114.0 (4) |
N3—Fe1—N1 | 88.39 (15) | C9—C8—C7 | 123.4 (4) |
N4—Fe1—N5 | 88.41 (14) | N5—C13—C14 | 109.2 (3) |
N6—Fe1—N5 | 81.27 (14) | C10—C11—C12 | 119.3 (4) |
N2—Fe1—N5 | 95.72 (15) | C2—C3—C4 | 119.8 (4) |
N3—Fe1—N5 | 95.03 (15) | N6—C14—C15 | 122.3 (4) |
N1—Fe1—N5 | 175.72 (14) | N6—C14—C13 | 115.9 (4) |
C18—N6—C14 | 116.9 (4) | C15—C14—C13 | 121.8 (4) |
C18—N6—Fe1 | 128.0 (3) | C15—C16—C17 | 118.6 (4) |
C14—N6—Fe1 | 114.9 (3) | N1—C1—C2 | 109.0 (3) |
C12—N4—C8 | 117.8 (4) | C8—C9—C10 | 119.4 (5) |
C12—N4—Fe1 | 126.0 (3) | N2—C6—C5 | 122.8 (4) |
C8—N4—Fe1 | 115.2 (3) | C3—C4—C5 | 118.2 (4) |
C1—N1—Fe1 | 110.5 (3) | N3—C7—C8 | 108.2 (4) |
C13—N5—Fe1 | 109.6 (3) | N4—C12—C11 | 122.4 (4) |
C7—N3—Fe1 | 108.5 (3) | C18—C17—C16 | 118.8 (4) |
C6—N2—C2 | 117.3 (4) | O32—C31—C30 | 114.2 (5) |
C6—N2—Fe1 | 127.8 (3) | C11—C10—C9 | 118.6 (4) |
(fepic200) 'tris(2-Picolylamine)-iron(ii) chloride ethanol solvate'
top
Crystal data top
C18H24FeN6·C2H6O·2(Cl) | F(000) = 1040 |
Mr = 497.25 | Dx = 1.353 Mg m−3 |
Monoclinic, P21/c | Cu Kα radiation, λ = 1.54178 Å |
a = 10.9348 (7) Å | Cell parameters from 25 reflections |
b = 21.9329 (16) Å | θ = 21.5–26.8° |
c = 11.484 (5) Å | µ = 7.15 mm−1 |
β = 117.59 (2)° | T = 200 K |
V = 2441.0 (11) Å3 | Block, yellow |
Z = 4 | 0.46 × 0.12 × 0.12 mm |
Data collection top
CAD4 Enraf Nonius diffractometer | 3585 reflections with I > 2σ(I) |
Radiation source: rotating anode | Rint = 0.057 |
Graphite monochromator | θmax = 73.6°, θmin = 4.0° |
Detector resolution: point detector pixels mm-1 | h = −12→13 |
θ/2ω scans | k = −27→0 |
5190 measured reflections | l = −14→0 |
4939 independent reflections | |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.076 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.199 | Calculated w = 1/[σ2(Fo2) + (0.1071P)2 + 2.315P] where P = (Fo2 + 2Fc2)/3 |
S = 1.09 | (Δ/σ)max < 0.001 |
4939 reflections | Δρmax = 1.15 e Å−3 |
274 parameters | Δρmin = −1.28 e Å−3 |
0 restraints | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0010 (3) |
Crystal data top
C18H24FeN6·C2H6O·2(Cl) | V = 2441.0 (11) Å3 |
Mr = 497.25 | Z = 4 |
Monoclinic, P21/c | Cu Kα radiation |
a = 10.9348 (7) Å | µ = 7.15 mm−1 |
b = 21.9329 (16) Å | T = 200 K |
c = 11.484 (5) Å | 0.46 × 0.12 × 0.12 mm |
β = 117.59 (2)° | |
Data collection top
CAD4 Enraf Nonius diffractometer | 3585 reflections with I > 2σ(I) |
5190 measured reflections | Rint = 0.057 |
4939 independent reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.076 | 0 restraints |
wR(F2) = 0.199 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.09 | Δρmax = 1.15 e Å−3 |
4939 reflections | Δρmin = −1.28 e Å−3 |
274 parameters | |
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 | 0.02826 (7) | 0.13452 (3) | 0.80631 (7) | 0.0252 (2) | |
Cl2 | 0.25376 (13) | 0.27338 (6) | 1.07564 (14) | 0.0414 (3) | |
Cl1 | −0.13745 (12) | 0.06834 (6) | 1.05956 (12) | 0.0327 (3) | |
N6 | −0.1474 (4) | 0.19467 (19) | 0.7692 (4) | 0.0292 (9) | |
N4 | 0.2416 (4) | 0.10346 (19) | 0.8798 (5) | 0.0333 (9) | |
N1 | −0.0694 (4) | 0.04893 (18) | 0.8119 (4) | 0.0286 (9) | |
H1A | −0.1122 | 0.0528 | 0.8686 | 0.034* | |
H1B | 0.0036 | 0.0205 | 0.8356 | 0.034* | |
N5 | 0.0884 (4) | 0.22268 (19) | 0.7611 (4) | 0.0317 (9) | |
H5A | 0.1397 | 0.2374 | 0.8499 | 0.038* | |
H5B | 0.1676 | 0.2251 | 0.7358 | 0.038* | |
N3 | 0.1093 (4) | 0.1376 (2) | 1.0195 (4) | 0.0329 (9) | |
H3A | 0.0466 | 0.1326 | 1.0354 | 0.039* | |
H3B | 0.1311 | 0.1777 | 1.0268 | 0.039* | |
N2 | −0.0571 (4) | 0.09854 (19) | 0.6039 (4) | 0.0287 (9) | |
C2 | −0.1430 (5) | 0.0509 (2) | 0.5757 (5) | 0.0296 (10) | |
C15 | −0.2613 (6) | 0.2875 (3) | 0.6678 (6) | 0.0415 (13) | |
H15 | −0.2627 | 0.3240 | 0.6226 | 0.050* | |
O32 | 0.3060 (7) | 0.3868 (3) | 0.9371 (8) | 0.109 (3) | |
H32 | 0.279 (3) | 0.340 (5) | 0.985 (5) | 0.163* | |
C18 | −0.2509 (5) | 0.1836 (2) | 0.7985 (5) | 0.0354 (11) | |
H18 | −0.2467 | 0.1475 | 0.8460 | 0.042* | |
C5 | −0.0731 (6) | 0.0900 (3) | 0.3890 (5) | 0.0407 (13) | |
H5 | −0.0475 | 0.1045 | 0.3254 | 0.049* | |
C8 | 0.3076 (5) | 0.0909 (2) | 1.0106 (6) | 0.0333 (11) | |
C13 | −0.0335 (6) | 0.2599 (2) | 0.6768 (6) | 0.0389 (13) | |
H13A | −0.0616 | 0.2507 | 0.5834 | 0.047* | |
H13B | −0.0090 | 0.3036 | 0.6920 | 0.047* | |
C11 | 0.4551 (6) | 0.0886 (3) | 0.8723 (8) | 0.0511 (17) | |
H11 | 0.5041 | 0.0886 | 0.8222 | 0.061* | |
C3 | −0.1977 (6) | 0.0212 (3) | 0.4551 (5) | 0.0400 (12) | |
H3 | −0.2590 | −0.0122 | 0.4378 | 0.048* | |
C14 | −0.1520 (5) | 0.2471 (2) | 0.7054 (5) | 0.0324 (11) | |
C16 | −0.3675 (6) | 0.2745 (3) | 0.6961 (7) | 0.0444 (14) | |
H16 | −0.4436 | 0.3016 | 0.6696 | 0.053* | |
C1 | −0.1786 (6) | 0.0313 (3) | 0.6830 (5) | 0.0382 (12) | |
H1AA | −0.2665 | 0.0505 | 0.6683 | 0.046* | |
H1BB | −0.1909 | −0.0135 | 0.6799 | 0.046* | |
C9 | 0.4465 (5) | 0.0765 (3) | 1.0741 (7) | 0.0438 (14) | |
H9 | 0.4904 | 0.0675 | 1.1654 | 0.053* | |
C6 | −0.0228 (6) | 0.1174 (3) | 0.5098 (5) | 0.0355 (11) | |
H6 | 0.0386 | 0.1509 | 0.5287 | 0.043* | |
C4 | −0.1620 (6) | 0.0409 (3) | 0.3613 (6) | 0.0451 (14) | |
H4 | −0.1979 | 0.0211 | 0.2784 | 0.054* | |
C7 | 0.2204 (5) | 0.0921 (3) | 1.0793 (5) | 0.0372 (12) | |
H7A | 0.1796 | 0.0513 | 1.0742 | 0.045* | |
H7B | 0.2786 | 0.1022 | 1.1731 | 0.045* | |
C12 | 0.3165 (6) | 0.1022 (3) | 0.8145 (7) | 0.0425 (13) | |
H12 | 0.2712 | 0.1112 | 0.7232 | 0.051* | |
C17 | −0.3626 (5) | 0.2215 (3) | 0.7636 (6) | 0.0410 (13) | |
H17 | −0.4343 | 0.2117 | 0.7852 | 0.049* | |
C31 | 0.4467 (9) | 0.3881 (4) | 0.9739 (11) | 0.086 (3) | |
H31A | 0.4982 | 0.3884 | 1.0710 | 0.103* | |
H31B | 0.4674 | 0.4269 | 0.9424 | 0.103* | |
C30 | 0.4979 (11) | 0.3391 (6) | 0.9270 (9) | 0.111 (4) | |
H30A | 0.4950 | 0.3012 | 0.9709 | 0.167* | |
H30B | 0.5933 | 0.3478 | 0.9460 | 0.167* | |
H30C | 0.4405 | 0.3348 | 0.8319 | 0.167* | |
C10 | 0.5213 (6) | 0.0750 (3) | 1.0049 (8) | 0.0527 (17) | |
H10 | 0.6166 | 0.0649 | 1.0476 | 0.063* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Fe1 | 0.0198 (4) | 0.0244 (4) | 0.0352 (4) | 0.0008 (3) | 0.0160 (3) | 0.0006 (3) |
Cl2 | 0.0346 (6) | 0.0417 (7) | 0.0565 (8) | −0.0068 (5) | 0.0285 (6) | −0.0093 (6) |
Cl1 | 0.0310 (6) | 0.0343 (6) | 0.0419 (6) | 0.0047 (5) | 0.0247 (5) | 0.0029 (5) |
N6 | 0.0238 (19) | 0.026 (2) | 0.040 (2) | 0.0002 (16) | 0.0165 (17) | 0.0029 (17) |
N4 | 0.025 (2) | 0.029 (2) | 0.050 (3) | −0.0007 (17) | 0.0219 (19) | −0.0023 (19) |
N1 | 0.029 (2) | 0.026 (2) | 0.037 (2) | 0.0011 (16) | 0.0202 (18) | −0.0008 (16) |
N5 | 0.026 (2) | 0.036 (2) | 0.041 (2) | −0.0028 (17) | 0.0222 (18) | −0.0011 (18) |
N3 | 0.030 (2) | 0.034 (2) | 0.042 (2) | −0.0009 (18) | 0.0223 (19) | −0.0030 (18) |
N2 | 0.026 (2) | 0.031 (2) | 0.030 (2) | −0.0015 (17) | 0.0141 (17) | −0.0004 (16) |
C2 | 0.023 (2) | 0.034 (3) | 0.031 (2) | −0.0001 (19) | 0.012 (2) | −0.0014 (19) |
C15 | 0.037 (3) | 0.032 (3) | 0.060 (4) | 0.008 (2) | 0.026 (3) | 0.011 (2) |
O32 | 0.090 (5) | 0.086 (5) | 0.179 (8) | 0.028 (4) | 0.086 (5) | 0.045 (5) |
C18 | 0.027 (2) | 0.035 (3) | 0.047 (3) | −0.001 (2) | 0.020 (2) | 0.002 (2) |
C5 | 0.048 (3) | 0.046 (3) | 0.035 (3) | 0.002 (3) | 0.025 (3) | 0.004 (2) |
C8 | 0.025 (2) | 0.026 (2) | 0.048 (3) | −0.0032 (19) | 0.016 (2) | −0.008 (2) |
C13 | 0.049 (3) | 0.026 (3) | 0.057 (3) | 0.006 (2) | 0.038 (3) | 0.008 (2) |
C11 | 0.041 (3) | 0.032 (3) | 0.099 (5) | 0.000 (2) | 0.049 (4) | −0.001 (3) |
C3 | 0.035 (3) | 0.042 (3) | 0.040 (3) | −0.007 (2) | 0.014 (2) | −0.008 (2) |
C14 | 0.034 (3) | 0.026 (2) | 0.042 (3) | 0.002 (2) | 0.021 (2) | 0.002 (2) |
C16 | 0.033 (3) | 0.033 (3) | 0.072 (4) | 0.012 (2) | 0.029 (3) | 0.008 (3) |
C1 | 0.035 (3) | 0.046 (3) | 0.037 (3) | −0.011 (2) | 0.019 (2) | −0.002 (2) |
C9 | 0.025 (3) | 0.036 (3) | 0.061 (4) | 0.000 (2) | 0.013 (2) | −0.006 (3) |
C6 | 0.036 (3) | 0.039 (3) | 0.037 (3) | 0.000 (2) | 0.022 (2) | 0.002 (2) |
C4 | 0.050 (3) | 0.047 (3) | 0.036 (3) | −0.001 (3) | 0.018 (3) | −0.005 (2) |
C7 | 0.031 (3) | 0.039 (3) | 0.035 (3) | 0.002 (2) | 0.011 (2) | −0.001 (2) |
C12 | 0.037 (3) | 0.041 (3) | 0.065 (4) | 0.005 (2) | 0.036 (3) | 0.005 (3) |
C17 | 0.027 (2) | 0.043 (3) | 0.062 (4) | 0.002 (2) | 0.028 (3) | 0.006 (3) |
C31 | 0.072 (6) | 0.077 (6) | 0.115 (8) | 0.006 (5) | 0.049 (6) | 0.009 (6) |
C30 | 0.120 (8) | 0.155 (11) | 0.075 (6) | 0.086 (8) | 0.059 (6) | 0.044 (6) |
C10 | 0.024 (3) | 0.037 (3) | 0.093 (5) | 0.001 (2) | 0.024 (3) | −0.006 (3) |
Geometric parameters (Å, º) top
Fe1—N1 | 2.175 (4) | C2—C1 | 1.516 (7) |
Fe1—N5 | 2.181 (4) | C15—C16 | 1.374 (8) |
Fe1—N3 | 2.185 (4) | C15—C14 | 1.386 (7) |
Fe1—N4 | 2.190 (4) | O32—C31 | 1.395 (10) |
Fe1—N6 | 2.203 (4) | C18—C17 | 1.375 (7) |
Fe1—N2 | 2.210 (4) | C5—C6 | 1.372 (8) |
N6—C18 | 1.344 (6) | C5—C4 | 1.386 (8) |
N6—C14 | 1.352 (6) | C8—C9 | 1.383 (7) |
N4—C12 | 1.342 (6) | C8—C7 | 1.493 (7) |
N4—C8 | 1.360 (7) | C13—C14 | 1.503 (7) |
N1—C1 | 1.459 (6) | C11—C12 | 1.377 (8) |
N5—C13 | 1.477 (7) | C11—C10 | 1.382 (10) |
N3—C7 | 1.472 (6) | C3—C4 | 1.375 (8) |
N2—C2 | 1.340 (6) | C16—C17 | 1.383 (8) |
N2—C6 | 1.362 (6) | C9—C10 | 1.379 (9) |
C2—C3 | 1.390 (7) | C31—C30 | 1.426 (13) |
| | | |
N1—Fe1—N5 | 168.06 (16) | C6—N2—Fe1 | 126.0 (4) |
N1—Fe1—N3 | 86.73 (16) | N2—C2—C3 | 122.4 (5) |
N5—Fe1—N3 | 103.24 (17) | N2—C2—C1 | 116.1 (4) |
N1—Fe1—N4 | 99.79 (16) | C3—C2—C1 | 121.5 (5) |
N5—Fe1—N4 | 89.01 (16) | C16—C15—C14 | 119.7 (5) |
N3—Fe1—N4 | 76.76 (16) | N6—C18—C17 | 123.7 (5) |
N1—Fe1—N6 | 97.27 (15) | C6—C5—C4 | 118.8 (5) |
N5—Fe1—N6 | 75.81 (15) | N4—C8—C9 | 121.3 (5) |
N3—Fe1—N6 | 93.62 (16) | N4—C8—C7 | 116.0 (4) |
N4—Fe1—N6 | 159.82 (16) | C9—C8—C7 | 122.7 (5) |
N1—Fe1—N2 | 75.46 (15) | N5—C13—C14 | 111.2 (4) |
N5—Fe1—N2 | 95.36 (16) | C12—C11—C10 | 118.4 (6) |
N3—Fe1—N2 | 160.68 (16) | C4—C3—C2 | 119.1 (5) |
N4—Fe1—N2 | 98.64 (16) | N6—C14—C15 | 121.5 (5) |
N6—Fe1—N2 | 95.99 (16) | N6—C14—C13 | 117.2 (4) |
C18—N6—C14 | 117.7 (4) | C15—C14—C13 | 121.3 (5) |
C18—N6—Fe1 | 127.1 (3) | C15—C16—C17 | 119.3 (5) |
C14—N6—Fe1 | 115.1 (3) | N1—C1—C2 | 110.6 (4) |
C12—N4—C8 | 117.6 (5) | C10—C9—C8 | 120.1 (6) |
C12—N4—Fe1 | 127.4 (4) | N2—C6—C5 | 122.8 (5) |
C8—N4—Fe1 | 114.5 (3) | C3—C4—C5 | 119.2 (5) |
C1—N1—Fe1 | 112.4 (3) | N3—C7—C8 | 110.9 (4) |
C13—N5—Fe1 | 111.4 (3) | N4—C12—C11 | 123.8 (6) |
C7—N3—Fe1 | 108.7 (3) | C18—C17—C16 | 118.0 (5) |
C2—N2—C6 | 117.7 (4) | O32—C31—C30 | 116.2 (10) |
C2—N2—Fe1 | 116.1 (3) | C9—C10—C11 | 118.8 (5) |
(fpic10k) tris(2-Picolylamine)-iron(ii) chloride ethanol solvate
top
Crystal data top
C18H24FeN6·C2H6O·2(Cl) | F(000) = 1040 |
Mr = 497.25 | Dx = 1.421 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
a = 10.7322 (14) Å | Cell parameters from 60 reflections |
b = 21.5055 (7) Å | θ = 30–40° |
c = 11.323 (2) Å | µ = 0.90 mm−1 |
β = 117.184 (17)° | T = 10 K |
V = 2324.7 (5) Å3 | Block, red |
Z = 4 | 0.4 × 0.3 × 0.2 mm |
Data collection top
CCD Oxford Diffraction diffractometer | 5154 independent reflections |
Radiation source: fine-focus rotating anode | 4302 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.105 |
ϕ–scans | θmax = 27.9°, θmin = 3.9° |
Absorption correction: multi-scan ? | h = −13→13 |
Tmin = 0.730, Tmax = 0.835 | k = −26→27 |
20473 measured reflections | l = −14→13 |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.060 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.130 | Calculated w = 1/[σ2(Fo2) + (0.0401P)2 + 5.8012P] where P = (Fo2 + 2Fc2)/3 |
S = 1.11 | (Δ/σ)max = 0.001 |
5154 reflections | Δρmax = 0.62 e Å−3 |
274 parameters | Δρmin = −0.57 e Å−3 |
0 restraints | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0044 (8) |
Crystal data top
C18H24FeN6·C2H6O·2(Cl) | V = 2324.7 (5) Å3 |
Mr = 497.25 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 10.7322 (14) Å | µ = 0.90 mm−1 |
b = 21.5055 (7) Å | T = 10 K |
c = 11.323 (2) Å | 0.4 × 0.3 × 0.2 mm |
β = 117.184 (17)° | |
Data collection top
CCD Oxford Diffraction diffractometer | 5154 independent reflections |
Absorption correction: multi-scan ? | 4302 reflections with I > 2σ(I) |
Tmin = 0.730, Tmax = 0.835 | Rint = 0.105 |
20473 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.060 | 0 restraints |
wR(F2) = 0.130 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.11 | Δρmax = 0.62 e Å−3 |
5154 reflections | Δρmin = −0.57 e Å−3 |
274 parameters | |
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 | 0.02410 (5) | 0.13315 (2) | 0.80247 (5) | 0.00395 (14) | |
Cl2 | 0.26959 (8) | 0.27370 (4) | 1.08624 (8) | 0.00741 (18) | |
Cl1 | −0.14068 (8) | 0.06988 (4) | 1.06312 (8) | 0.00677 (18) | |
N6 | −0.1460 (3) | 0.18464 (13) | 0.7601 (3) | 0.0061 (5) | |
N4 | 0.2172 (3) | 0.09936 (12) | 0.8709 (3) | 0.0059 (5) | |
N1 | −0.0586 (3) | 0.05172 (13) | 0.8208 (3) | 0.0057 (5) | |
H1A | −0.1015 | 0.0556 | 0.8774 | 0.007* | |
H1B | 0.0143 | 0.0233 | 0.8444 | 0.007* | |
N5 | 0.0966 (3) | 0.21592 (13) | 0.7730 (3) | 0.0069 (6) | |
H5A | 0.1479 | 0.2306 | 0.8618 | 0.008* | |
H5B | 0.1758 | 0.2183 | 0.7477 | 0.008* | |
N3 | 0.0886 (3) | 0.14735 (13) | 0.9983 (3) | 0.0066 (5) | |
H3A | 0.0260 | 0.1424 | 1.0143 | 0.008* | |
H3B | 0.1105 | 0.1875 | 1.0056 | 0.008* | |
N2 | −0.0462 (3) | 0.10272 (13) | 0.6159 (3) | 0.0052 (5) | |
C2 | −0.1364 (3) | 0.05417 (15) | 0.5830 (3) | 0.0062 (6) | |
C15 | −0.2553 (3) | 0.28348 (15) | 0.6753 (3) | 0.0080 (6) | |
H15 | −0.2536 | 0.3222 | 0.6359 | 0.010* | |
O32 | 0.3013 (2) | 0.39001 (12) | 0.9307 (3) | 0.0124 (5) | |
H32 | 0.2893 (8) | 0.3609 (18) | 0.962 (2) | 0.019* | |
C18 | −0.2523 (3) | 0.17177 (15) | 0.7898 (3) | 0.0063 (6) | |
H18 | −0.2513 | 0.1331 | 0.8310 | 0.008* | |
C5 | −0.0631 (3) | 0.09669 (15) | 0.3965 (3) | 0.0072 (6) | |
H5 | −0.0352 | 0.1122 | 0.3337 | 0.009* | |
C8 | 0.2874 (3) | 0.09266 (15) | 1.0044 (3) | 0.0065 (6) | |
C13 | −0.0225 (3) | 0.25513 (15) | 0.6834 (3) | 0.0069 (6) | |
H13A | −0.0456 | 0.2464 | 0.5898 | 0.008* | |
H13B | 0.0028 | 0.2996 | 0.7013 | 0.008* | |
C11 | 0.4347 (3) | 0.08196 (15) | 0.8623 (3) | 0.0088 (7) | |
H11 | 0.4836 | 0.0785 | 0.8107 | 0.011* | |
C3 | −0.1923 (3) | 0.02574 (15) | 0.4601 (3) | 0.0075 (7) | |
H3 | −0.2551 | −0.0082 | 0.4413 | 0.009* | |
C14 | −0.1474 (3) | 0.24112 (15) | 0.7065 (3) | 0.0060 (6) | |
C16 | −0.3657 (3) | 0.26896 (16) | 0.7021 (3) | 0.0082 (6) | |
H16 | −0.4417 | 0.2969 | 0.6794 | 0.010* | |
C1 | −0.1724 (3) | 0.03229 (16) | 0.6909 (3) | 0.0070 (6) | |
H1AA | −0.2624 | 0.0508 | 0.6776 | 0.008* | |
H1BB | −0.1822 | −0.0135 | 0.6878 | 0.008* | |
C9 | 0.4298 (3) | 0.08029 (15) | 1.0699 (3) | 0.0082 (6) | |
H9 | 0.4756 | 0.0754 | 1.1637 | 0.010* | |
C6 | −0.0119 (3) | 0.12317 (15) | 0.5212 (3) | 0.0061 (6) | |
H6 | 0.0506 | 0.1574 | 0.5416 | 0.007* | |
C4 | −0.1558 (3) | 0.04726 (15) | 0.3640 (3) | 0.0080 (6) | |
H4 | −0.1934 | 0.0286 | 0.2786 | 0.010* | |
C7 | 0.1982 (3) | 0.10096 (16) | 1.0740 (3) | 0.0076 (6) | |
H7A | 0.1546 | 0.0609 | 1.0776 | 0.009* | |
H7B | 0.2562 | 0.1157 | 1.1660 | 0.009* | |
C12 | 0.2917 (3) | 0.09409 (15) | 0.8016 (3) | 0.0066 (6) | |
H12 | 0.2443 | 0.0989 | 0.7079 | 0.008* | |
C17 | −0.3620 (3) | 0.21236 (16) | 0.7630 (3) | 0.0079 (6) | |
H17 | −0.4341 | 0.2017 | 0.7860 | 0.009* | |
C31 | 0.4471 (4) | 0.39605 (16) | 0.9684 (4) | 0.0124 (7) | |
H31A | 0.4993 | 0.4001 | 1.0661 | 0.015* | |
H31B | 0.4623 | 0.4346 | 0.9288 | 0.015* | |
C30 | 0.5053 (4) | 0.34127 (17) | 0.9248 (4) | 0.0135 (7) | |
H30A | 0.5000 | 0.3037 | 0.9711 | 0.020* | |
H30B | 0.6033 | 0.3495 | 0.9465 | 0.020* | |
H30C | 0.4504 | 0.3353 | 0.8288 | 0.020* | |
C10 | 0.5049 (3) | 0.07500 (15) | 0.9987 (4) | 0.0092 (7) | |
H10 | 0.6027 | 0.0668 | 1.0424 | 0.011* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Fe1 | 0.0041 (2) | 0.0037 (2) | 0.0039 (2) | −0.00008 (16) | 0.00172 (18) | −0.00002 (17) |
Cl2 | 0.0070 (4) | 0.0068 (4) | 0.0082 (4) | −0.0002 (3) | 0.0033 (3) | −0.0004 (3) |
Cl1 | 0.0073 (3) | 0.0069 (4) | 0.0067 (4) | 0.0007 (3) | 0.0037 (3) | 0.0004 (3) |
N6 | 0.0072 (13) | 0.0068 (13) | 0.0028 (13) | −0.0022 (10) | 0.0009 (11) | −0.0008 (11) |
N4 | 0.0060 (12) | 0.0037 (13) | 0.0077 (14) | −0.0005 (10) | 0.0029 (11) | −0.0004 (10) |
N1 | 0.0039 (12) | 0.0072 (13) | 0.0062 (14) | −0.0004 (10) | 0.0023 (11) | −0.0024 (11) |
N5 | 0.0062 (13) | 0.0075 (13) | 0.0072 (14) | −0.0001 (10) | 0.0032 (11) | 0.0004 (11) |
N3 | 0.0055 (12) | 0.0059 (13) | 0.0105 (14) | −0.0012 (10) | 0.0053 (11) | 0.0011 (11) |
N2 | 0.0050 (12) | 0.0055 (13) | 0.0041 (13) | 0.0011 (10) | 0.0012 (11) | 0.0009 (11) |
C2 | 0.0049 (14) | 0.0069 (15) | 0.0064 (16) | 0.0018 (12) | 0.0022 (13) | 0.0008 (12) |
C15 | 0.0079 (15) | 0.0060 (15) | 0.0073 (16) | −0.0001 (12) | 0.0012 (13) | 0.0004 (13) |
O32 | 0.0095 (12) | 0.0097 (12) | 0.0193 (14) | 0.0024 (9) | 0.0077 (11) | 0.0064 (11) |
C18 | 0.0049 (14) | 0.0077 (15) | 0.0048 (15) | −0.0010 (12) | 0.0009 (13) | −0.0009 (12) |
C5 | 0.0059 (14) | 0.0083 (16) | 0.0075 (16) | 0.0024 (12) | 0.0032 (13) | 0.0023 (13) |
C8 | 0.0088 (15) | 0.0027 (14) | 0.0076 (16) | −0.0009 (12) | 0.0032 (13) | 0.0006 (12) |
C13 | 0.0057 (14) | 0.0072 (15) | 0.0085 (16) | 0.0011 (12) | 0.0038 (13) | 0.0008 (13) |
C11 | 0.0114 (16) | 0.0060 (15) | 0.0123 (17) | 0.0008 (12) | 0.0081 (14) | −0.0006 (13) |
C3 | 0.0062 (15) | 0.0075 (16) | 0.0080 (16) | 0.0008 (12) | 0.0026 (13) | 0.0006 (13) |
C14 | 0.0084 (15) | 0.0058 (15) | 0.0019 (15) | −0.0008 (12) | 0.0007 (12) | 0.0000 (12) |
C16 | 0.0081 (15) | 0.0093 (16) | 0.0063 (16) | 0.0029 (12) | 0.0026 (13) | −0.0004 (13) |
C1 | 0.0075 (15) | 0.0076 (15) | 0.0073 (16) | −0.0024 (12) | 0.0046 (13) | −0.0016 (13) |
C9 | 0.0081 (15) | 0.0063 (16) | 0.0074 (16) | 0.0002 (12) | 0.0011 (13) | 0.0006 (13) |
C6 | 0.0047 (14) | 0.0062 (15) | 0.0058 (16) | 0.0001 (12) | 0.0009 (12) | 0.0007 (12) |
C4 | 0.0090 (15) | 0.0077 (16) | 0.0062 (16) | 0.0011 (12) | 0.0027 (13) | 0.0005 (13) |
C7 | 0.0057 (14) | 0.0098 (16) | 0.0049 (15) | 0.0006 (12) | 0.0002 (13) | 0.0002 (13) |
C12 | 0.0103 (15) | 0.0030 (14) | 0.0079 (16) | −0.0017 (12) | 0.0053 (13) | −0.0025 (12) |
C17 | 0.0070 (15) | 0.0096 (16) | 0.0083 (16) | 0.0001 (12) | 0.0045 (13) | −0.0015 (13) |
C31 | 0.0095 (16) | 0.0115 (17) | 0.0147 (18) | −0.0006 (13) | 0.0042 (14) | 0.0012 (14) |
C30 | 0.0106 (16) | 0.0175 (18) | 0.0113 (17) | 0.0065 (14) | 0.0040 (14) | 0.0027 (15) |
C10 | 0.0058 (14) | 0.0060 (16) | 0.0135 (17) | 0.0008 (12) | 0.0024 (13) | 0.0017 (13) |
Geometric parameters (Å, º) top
Fe1—N4 | 1.989 (3) | C2—C1 | 1.515 (4) |
Fe1—N6 | 1.997 (3) | C15—C14 | 1.387 (4) |
Fe1—N2 | 2.001 (3) | C15—C16 | 1.385 (5) |
Fe1—N1 | 2.017 (3) | O32—C31 | 1.427 (4) |
Fe1—N3 | 2.022 (3) | C18—C17 | 1.384 (4) |
Fe1—N5 | 2.031 (3) | C5—C6 | 1.382 (5) |
N6—C18 | 1.357 (4) | C5—C4 | 1.386 (5) |
N6—C14 | 1.355 (4) | C8—C9 | 1.385 (4) |
N4—C8 | 1.354 (4) | C8—C7 | 1.503 (4) |
N4—C12 | 1.357 (4) | C13—C14 | 1.508 (4) |
N1—C1 | 1.479 (4) | C11—C10 | 1.383 (5) |
N5—C13 | 1.480 (4) | C11—C12 | 1.389 (5) |
N3—C7 | 1.480 (4) | C3—C4 | 1.393 (4) |
N2—C2 | 1.355 (4) | C16—C17 | 1.391 (5) |
N2—C6 | 1.356 (4) | C9—C10 | 1.382 (5) |
C2—C3 | 1.381 (5) | C31—C30 | 1.518 (5) |
| | | |
N4—Fe1—N6 | 166.30 (11) | C6—N2—Fe1 | 128.4 (2) |
N4—Fe1—N2 | 96.60 (11) | N2—C2—C3 | 123.0 (3) |
N6—Fe1—N2 | 93.74 (11) | N2—C2—C1 | 115.6 (3) |
N4—Fe1—N1 | 94.13 (11) | C3—C2—C1 | 121.5 (3) |
N6—Fe1—N1 | 96.25 (11) | C14—C15—C16 | 119.6 (3) |
N2—Fe1—N1 | 81.56 (11) | N6—C18—C17 | 123.0 (3) |
N4—Fe1—N3 | 81.60 (11) | C6—C5—C4 | 119.3 (3) |
N6—Fe1—N3 | 89.85 (11) | N4—C8—C9 | 122.2 (3) |
N2—Fe1—N3 | 169.25 (11) | N4—C8—C7 | 114.2 (3) |
N1—Fe1—N3 | 87.97 (11) | C9—C8—C7 | 123.6 (3) |
N4—Fe1—N5 | 88.56 (11) | N5—C13—C14 | 109.0 (3) |
N6—Fe1—N5 | 81.46 (11) | C10—C11—C12 | 119.2 (3) |
N2—Fe1—N5 | 95.79 (11) | C2—C3—C4 | 119.5 (3) |
N1—Fe1—N5 | 176.41 (11) | N6—C14—C15 | 122.7 (3) |
N3—Fe1—N5 | 94.76 (11) | N6—C14—C13 | 115.3 (3) |
C18—N6—C14 | 117.1 (3) | C15—C14—C13 | 122.0 (3) |
C18—N6—Fe1 | 127.4 (2) | C15—C16—C17 | 118.2 (3) |
C14—N6—Fe1 | 115.2 (2) | N1—C1—C2 | 108.4 (3) |
C8—N4—C12 | 117.6 (3) | C10—C9—C8 | 119.9 (3) |
C8—N4—Fe1 | 115.0 (2) | N2—C6—C5 | 123.3 (3) |
C12—N4—Fe1 | 126.1 (2) | C5—C4—C3 | 118.1 (3) |
C1—N1—Fe1 | 110.2 (2) | N3—C7—C8 | 107.7 (3) |
C13—N5—Fe1 | 109.64 (19) | N4—C12—C11 | 122.6 (3) |
C7—N3—Fe1 | 108.5 (2) | C18—C17—C16 | 119.3 (3) |
C2—N2—C6 | 116.8 (3) | O32—C31—C30 | 113.0 (3) |
C2—N2—Fe1 | 114.8 (2) | C9—C10—C11 | 118.5 (3) |
(fpic118h) 'tris(2-Picolylamine)-iron(ii) chloride ethanol solvate'
top
Crystal data top
C18H24FeN6·C2H6O·2(Cl) | F(000) = 2080 |
Mr = 994.50 | Dx = 1.392 Mg m−3 |
Monoclinic, P21/n | Cu Kα radiation, λ = 1.54178 Å |
a = 21.6080 (18) Å | Cell parameters from 25 reflections |
b = 21.6945 (14) Å | θ = 21.5–26.8° |
c = 11.395 (4) Å | µ = 7.36 mm−1 |
β = 117.33 (3)° | T = 118 K |
V = 4745.4 (17) Å3 | Block, red |
Z = 4 | 0.46 × 0.12 × 0.12 mm |
Data collection top
CAD4 Enraf Nonius diffractometer | 5558 reflections with I > 2σ(I) |
Radiation source: rotating anode | Rint = 0.062 |
Graphite monochromator | θmax = 73.8°, θmin = 3.1° |
Detector resolution: point detector pixels mm-1 | h = −23→26 |
θ/2ω scans | k = −27→0 |
10076 measured reflections | l = −14→0 |
9586 independent reflections | |
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)] = 0.085 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.254 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.00 | Calculated w = 1/[σ2(Fo2) + (0.1507P)2] where P = (Fo2 + 2Fc2)/3 |
9586 reflections | (Δ/σ)max < 0.001 |
543 parameters | Δρmax = 1.78 e Å−3 |
0 restraints | Δρmin = −1.58 e Å−3 |
Crystal data top
C18H24FeN6·C2H6O·2(Cl) | V = 4745.4 (17) Å3 |
Mr = 994.50 | Z = 4 |
Monoclinic, P21/n | Cu Kα radiation |
a = 21.6080 (18) Å | µ = 7.36 mm−1 |
b = 21.6945 (14) Å | T = 118 K |
c = 11.395 (4) Å | 0.46 × 0.12 × 0.12 mm |
β = 117.33 (3)° | |
Data collection top
CAD4 Enraf Nonius diffractometer | 5558 reflections with I > 2σ(I) |
10076 measured reflections | Rint = 0.062 |
9586 independent reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.085 | 0 restraints |
wR(F2) = 0.254 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.00 | Δρmax = 1.78 e Å−3 |
9586 reflections | Δρmin = −1.58 e Å−3 |
543 parameters | |
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 | 0.23626 (5) | 0.13797 (4) | 0.20150 (9) | 0.0173 (2) | |
Fe1A | 0.26474 (5) | −0.12980 (4) | −0.18916 (10) | 0.0191 (2) | |
Cl2 | 0.31489 (8) | 0.07458 (7) | −0.06222 (15) | 0.0248 (3) | |
Cl1 | −0.11672 (8) | −0.23200 (7) | −0.41747 (16) | 0.0268 (3) | |
Cl2A | 0.17877 (8) | −0.06458 (7) | 0.06276 (15) | 0.0240 (3) | |
Cl1A | 0.61866 (8) | 0.21996 (7) | 0.42182 (16) | 0.0269 (3) | |
N4 | 0.1384 (3) | 0.1049 (2) | 0.1319 (6) | 0.0253 (12) | |
N1 | 0.2772 (3) | 0.0558 (2) | 0.1841 (5) | 0.0207 (10) | |
H1A | 0.2427 | 0.0263 | 0.1535 | 0.025* | |
H1B | 0.2941 | 0.0596 | 0.1237 | 0.025* | |
N5 | 0.2022 (3) | 0.2214 (2) | 0.2341 (5) | 0.0219 (11) | |
H5A | 0.1777 | 0.2418 | 0.1552 | 0.026* | |
H5B | 0.1729 | 0.2154 | 0.2716 | 0.026* | |
N2A | 0.2224 (3) | −0.0968 (2) | −0.3889 (5) | 0.0222 (11) | |
N2 | 0.2727 (3) | 0.1055 (2) | 0.3898 (5) | 0.0188 (10) | |
N6A | 0.1790 (3) | −0.1901 (2) | −0.2254 (5) | 0.0231 (11) | |
C12A | 0.4073 (4) | −0.0960 (3) | −0.1837 (8) | 0.0369 (18) | |
H12A | 0.3837 | −0.1031 | −0.2763 | 0.044* | |
N1A | 0.2149 (3) | −0.0456 (2) | −0.1845 (5) | 0.0245 (11) | |
H1AA | 0.1977 | −0.0493 | −0.1245 | 0.029* | |
H1AB | 0.2474 | −0.0145 | −0.1561 | 0.029* | |
C6 | 0.2548 (3) | 0.1252 (3) | 0.4824 (6) | 0.0252 (13) | |
H6 | 0.2247 | 0.1598 | 0.4633 | 0.030* | |
C15A | 0.1232 (3) | −0.2855 (3) | −0.3228 (7) | 0.0272 (14) | |
H15A | 0.1239 | −0.3228 | −0.3658 | 0.033* | |
C5A | 0.2117 (3) | −0.0916 (3) | −0.6091 (6) | 0.0270 (14) | |
H5A2 | 0.2247 | −0.1070 | −0.6728 | 0.032* | |
C17 | 0.4298 (3) | 0.2149 (3) | 0.2441 (7) | 0.0274 (14) | |
H17 | 0.4655 | 0.2037 | 0.2213 | 0.033* | |
N3A | 0.3036 (3) | −0.1335 (3) | 0.0218 (6) | 0.0343 (14) | |
H3AA | 0.2681 | −0.1257 | 0.0429 | 0.041* | |
H3AB | 0.3212 | −0.1720 | 0.0526 | 0.041* | |
N5A | 0.2979 (3) | −0.2165 (2) | −0.2308 (5) | 0.0220 (11) | |
H5AA | 0.3251 | −0.2098 | −0.2724 | 0.026* | |
H5AB | 0.3246 | −0.2369 | −0.1529 | 0.026* | |
C4A | 0.1647 (4) | −0.0442 (3) | −0.6400 (7) | 0.0320 (15) | |
H4A | 0.1450 | −0.0261 | −0.7254 | 0.038* | |
C18A | 0.1258 (3) | −0.1797 (3) | −0.1958 (7) | 0.0270 (14) | |
H18A | 0.1270 | −0.1430 | −0.1494 | 0.032* | |
C16A | 0.0688 (4) | −0.2727 (3) | −0.2948 (7) | 0.0302 (15) | |
H16A | 0.0308 | −0.3006 | −0.3206 | 0.036* | |
N6 | 0.3226 (3) | 0.1891 (2) | 0.2449 (5) | 0.0219 (11) | |
N4A | 0.3705 (3) | −0.0969 (2) | −0.1164 (6) | 0.0295 (13) | |
C1 | 0.3334 (3) | 0.0364 (3) | 0.3116 (6) | 0.0248 (13) | |
H1A2 | 0.3779 | 0.0554 | 0.3257 | 0.030* | |
H1B2 | 0.3387 | −0.0090 | 0.3134 | 0.030* | |
C2 | 0.3153 (3) | 0.0565 (3) | 0.4192 (6) | 0.0220 (13) | |
C13A | 0.2375 (3) | −0.2553 (3) | −0.3160 (7) | 0.0257 (14) | |
H13A | 0.2506 | −0.2994 | −0.2999 | 0.031* | |
H13B | 0.2235 | −0.2463 | −0.4100 | 0.031* | |
C14A | 0.1770 (3) | −0.2429 (3) | −0.2873 (6) | 0.0214 (13) | |
C8 | 0.1042 (3) | 0.0970 (3) | 0.0007 (7) | 0.0259 (14) | |
C13 | 0.2633 (3) | 0.2592 (3) | 0.3242 (6) | 0.0243 (13) | |
H13Z | 0.2748 | 0.2503 | 0.4172 | 0.029* | |
H13X | 0.2517 | 0.3036 | 0.3077 | 0.029* | |
C3A | 0.1462 (4) | −0.0228 (3) | −0.5457 (7) | 0.0283 (14) | |
H3A | 0.1137 | 0.0099 | −0.5652 | 0.034* | |
C15 | 0.3792 (3) | 0.2856 (3) | 0.3356 (7) | 0.0262 (14) | |
H15 | 0.3795 | 0.3235 | 0.3776 | 0.031* | |
C10 | −0.0027 (4) | 0.0756 (3) | 0.0065 (9) | 0.0383 (18) | |
H10 | −0.0507 | 0.0652 | −0.0364 | 0.046* | |
C30A | 0.0031 (5) | −0.1644 (5) | −0.5707 (9) | 0.065 (3) | |
H30A | −0.0033 | −0.2024 | −0.5311 | 0.098* | |
H30B | 0.0529 | −0.1574 | −0.5408 | 0.098* | |
H30C | −0.0209 | −0.1681 | −0.6672 | 0.098* | |
C2A | 0.1762 (3) | −0.0505 (3) | −0.4224 (6) | 0.0223 (12) | |
C9A | 0.4745 (4) | −0.0756 (3) | 0.0802 (9) | 0.0378 (17) | |
H9A | 0.4973 | −0.0687 | 0.1729 | 0.045* | |
C16 | 0.4336 (3) | 0.2706 (3) | 0.3078 (7) | 0.0284 (15) | |
H16 | 0.4722 | 0.2975 | 0.3316 | 0.034* | |
C4 | 0.3230 (4) | 0.0466 (3) | 0.6333 (6) | 0.0285 (14) | |
H4 | 0.3406 | 0.0265 | 0.7165 | 0.034* | |
C17A | 0.0703 (3) | −0.2189 (3) | −0.2285 (7) | 0.0289 (15) | |
H17A | 0.0341 | −0.2092 | −0.2063 | 0.035* | |
C14 | 0.3245 (3) | 0.2447 (3) | 0.3014 (6) | 0.0218 (13) | |
C1A | 0.1580 (4) | −0.0291 (3) | −0.3136 (6) | 0.0269 (14) | |
H1AZ | 0.1509 | 0.0161 | −0.3190 | 0.032* | |
H1AX | 0.1143 | −0.0491 | −0.3255 | 0.032* | |
C7A | 0.3581 (4) | −0.0874 (4) | 0.0824 (7) | 0.0338 (16) | |
H7AA | 0.3866 | −0.0970 | 0.1773 | 0.041* | |
H7AB | 0.3369 | −0.0462 | 0.0754 | 0.041* | |
C10A | 0.5121 (4) | −0.0749 (3) | 0.0093 (9) | 0.0394 (19) | |
H10A | 0.5609 | −0.0673 | 0.0530 | 0.047* | |
O32A | −0.0954 (4) | −0.1151 (3) | −0.5604 (9) | 0.086 (3) | |
H32A | −0.1023 | −0.1463 | −0.5241 | 0.128* | |
C31 | 0.5261 (4) | 0.1025 (4) | 0.5289 (9) | 0.0438 (19) | |
H31A | 0.5156 | 0.0639 | 0.5625 | 0.053* | |
H31B | 0.5009 | 0.1010 | 0.4312 | 0.053* | |
C18 | 0.3743 (3) | 0.1764 (3) | 0.2145 (7) | 0.0268 (14) | |
H18 | 0.3723 | 0.1389 | 0.1701 | 0.032* | |
C11A | 0.4785 (4) | −0.0852 (3) | −0.1243 (10) | 0.045 (2) | |
H11A | 0.5034 | −0.0849 | −0.1748 | 0.054* | |
C7 | 0.1478 (4) | 0.1066 (3) | −0.0678 (7) | 0.0307 (15) | |
H7A | 0.1690 | 0.0670 | −0.0736 | 0.037* | |
H7B | 0.1183 | 0.1217 | −0.1587 | 0.037* | |
C6A | 0.2397 (3) | −0.1164 (3) | −0.4842 (6) | 0.0252 (13) | |
H6A | 0.2727 | −0.1488 | −0.4630 | 0.030* | |
C8A | 0.4037 (4) | −0.0864 (3) | 0.0153 (7) | 0.0278 (14) | |
N3 | 0.2030 (3) | 0.1520 (3) | 0.0060 (6) | 0.0302 (13) | |
H3A1 | 0.1858 | 0.1914 | −0.0167 | 0.036* | |
H3B | 0.2394 | 0.1472 | −0.0139 | 0.036* | |
C9 | 0.0339 (4) | 0.0822 (3) | −0.0641 (8) | 0.0331 (16) | |
H9 | 0.0112 | 0.0767 | −0.1572 | 0.040* | |
C11 | 0.0326 (4) | 0.0846 (3) | 0.1444 (8) | 0.0371 (17) | |
H11 | 0.0089 | 0.0813 | 0.1965 | 0.044* | |
C3 | 0.3409 (3) | 0.0267 (3) | 0.5381 (6) | 0.0263 (14) | |
H3 | 0.3711 | −0.0077 | 0.5550 | 0.032* | |
O32 | 0.5982 (3) | 0.1045 (3) | 0.5686 (6) | 0.0465 (14) | |
H32 | 0.6076 | 0.1366 | 0.5388 | 0.070* | |
C5 | 0.2788 (3) | 0.0966 (3) | 0.6046 (6) | 0.0266 (14) | |
H5 | 0.2649 | 0.1112 | 0.6676 | 0.032* | |
C30 | 0.4990 (5) | 0.1559 (4) | 0.5755 (9) | 0.051 (2) | |
H30Z | 0.5278 | 0.1614 | 0.6708 | 0.077* | |
H30X | 0.4507 | 0.1477 | 0.5569 | 0.077* | |
H30V | 0.5007 | 0.1934 | 0.5291 | 0.077* | |
C12 | 0.1022 (4) | 0.0984 (3) | 0.2010 (8) | 0.0316 (16) | |
H12 | 0.1263 | 0.1036 | 0.2941 | 0.038* | |
C31A | −0.0261 (5) | −0.1120 (4) | −0.5302 (11) | 0.056 (2) | |
H31Z | 0.0012 | −0.1072 | −0.4334 | 0.067* | |
H31X | −0.0191 | −0.0742 | −0.5713 | 0.067* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Fe1 | 0.0092 (5) | 0.0184 (4) | 0.0256 (5) | −0.0003 (3) | 0.0093 (4) | 0.0004 (3) |
Fe1A | 0.0121 (5) | 0.0180 (5) | 0.0291 (5) | 0.0004 (4) | 0.0112 (4) | 0.0016 (4) |
Cl2 | 0.0225 (8) | 0.0277 (7) | 0.0289 (8) | −0.0052 (6) | 0.0158 (6) | −0.0017 (6) |
Cl1 | 0.0150 (7) | 0.0324 (8) | 0.0350 (8) | −0.0024 (6) | 0.0132 (6) | −0.0052 (6) |
Cl2A | 0.0187 (7) | 0.0287 (7) | 0.0287 (8) | −0.0067 (6) | 0.0144 (6) | −0.0033 (6) |
Cl1A | 0.0179 (7) | 0.0293 (8) | 0.0362 (8) | −0.0039 (6) | 0.0145 (7) | −0.0059 (6) |
N4 | 0.022 (3) | 0.021 (3) | 0.038 (3) | 0.002 (2) | 0.018 (3) | 0.006 (2) |
N1 | 0.015 (2) | 0.024 (3) | 0.024 (3) | −0.004 (2) | 0.009 (2) | 0.001 (2) |
N5 | 0.015 (3) | 0.020 (2) | 0.034 (3) | 0.0025 (19) | 0.014 (2) | 0.002 (2) |
N2A | 0.019 (3) | 0.027 (3) | 0.024 (3) | −0.003 (2) | 0.013 (2) | 0.000 (2) |
N2 | 0.014 (2) | 0.025 (3) | 0.017 (2) | −0.0023 (19) | 0.007 (2) | −0.0020 (18) |
N6A | 0.013 (3) | 0.025 (3) | 0.030 (3) | 0.000 (2) | 0.009 (2) | −0.004 (2) |
C12A | 0.048 (5) | 0.028 (4) | 0.059 (5) | −0.008 (3) | 0.045 (4) | −0.006 (3) |
N1A | 0.022 (3) | 0.025 (3) | 0.027 (3) | −0.005 (2) | 0.012 (2) | −0.002 (2) |
C6 | 0.020 (3) | 0.028 (3) | 0.031 (3) | 0.002 (2) | 0.015 (3) | 0.003 (3) |
C15A | 0.017 (3) | 0.027 (3) | 0.036 (4) | 0.001 (3) | 0.011 (3) | −0.002 (3) |
C5A | 0.022 (3) | 0.035 (4) | 0.021 (3) | −0.002 (3) | 0.008 (3) | −0.001 (3) |
C17 | 0.016 (3) | 0.034 (4) | 0.033 (4) | 0.006 (3) | 0.012 (3) | −0.004 (3) |
N3A | 0.022 (3) | 0.037 (3) | 0.053 (4) | 0.011 (2) | 0.025 (3) | 0.018 (3) |
N5A | 0.018 (3) | 0.026 (3) | 0.025 (3) | 0.001 (2) | 0.013 (2) | 0.002 (2) |
C4A | 0.035 (4) | 0.036 (4) | 0.024 (3) | 0.000 (3) | 0.014 (3) | 0.006 (3) |
C18A | 0.012 (3) | 0.037 (4) | 0.033 (4) | 0.002 (3) | 0.011 (3) | −0.005 (3) |
C16A | 0.019 (3) | 0.031 (4) | 0.039 (4) | −0.004 (3) | 0.012 (3) | 0.002 (3) |
N6 | 0.009 (2) | 0.028 (3) | 0.026 (3) | 0.000 (2) | 0.005 (2) | −0.003 (2) |
N4A | 0.031 (3) | 0.017 (3) | 0.052 (4) | 0.003 (2) | 0.030 (3) | 0.002 (2) |
C1 | 0.019 (3) | 0.024 (3) | 0.031 (3) | 0.003 (2) | 0.011 (3) | 0.001 (2) |
C2 | 0.017 (3) | 0.025 (3) | 0.026 (3) | −0.005 (2) | 0.012 (3) | −0.003 (2) |
C13A | 0.026 (4) | 0.024 (3) | 0.032 (4) | −0.006 (3) | 0.017 (3) | −0.003 (3) |
C14A | 0.019 (3) | 0.022 (3) | 0.024 (3) | 0.000 (2) | 0.010 (3) | −0.004 (2) |
C8 | 0.015 (3) | 0.019 (3) | 0.041 (4) | 0.006 (2) | 0.010 (3) | 0.009 (2) |
C13 | 0.019 (3) | 0.024 (3) | 0.030 (3) | 0.004 (2) | 0.012 (3) | 0.000 (2) |
C3A | 0.024 (3) | 0.031 (3) | 0.027 (3) | 0.006 (3) | 0.009 (3) | 0.004 (3) |
C15 | 0.021 (3) | 0.024 (3) | 0.032 (4) | −0.003 (3) | 0.011 (3) | −0.001 (2) |
C10 | 0.021 (3) | 0.026 (4) | 0.066 (5) | −0.004 (3) | 0.018 (4) | −0.001 (3) |
C30A | 0.058 (6) | 0.096 (8) | 0.045 (5) | 0.043 (6) | 0.026 (5) | 0.018 (5) |
C2A | 0.016 (3) | 0.026 (3) | 0.026 (3) | 0.000 (2) | 0.010 (3) | −0.002 (2) |
C9A | 0.026 (4) | 0.031 (4) | 0.056 (5) | 0.007 (3) | 0.018 (4) | 0.006 (3) |
C16 | 0.017 (3) | 0.027 (3) | 0.038 (4) | −0.008 (3) | 0.010 (3) | −0.003 (3) |
C4 | 0.030 (4) | 0.034 (4) | 0.018 (3) | −0.004 (3) | 0.009 (3) | 0.003 (2) |
C17A | 0.018 (3) | 0.034 (4) | 0.039 (4) | 0.000 (3) | 0.016 (3) | −0.004 (3) |
C14 | 0.020 (3) | 0.020 (3) | 0.026 (3) | 0.002 (2) | 0.010 (3) | −0.002 (2) |
C1A | 0.026 (4) | 0.031 (3) | 0.027 (3) | 0.011 (3) | 0.015 (3) | 0.005 (3) |
C7A | 0.020 (3) | 0.053 (5) | 0.026 (3) | 0.011 (3) | 0.008 (3) | 0.009 (3) |
C10A | 0.029 (4) | 0.025 (4) | 0.073 (6) | 0.001 (3) | 0.031 (4) | 0.004 (3) |
O32A | 0.073 (6) | 0.055 (5) | 0.151 (8) | 0.015 (4) | 0.070 (6) | 0.026 (5) |
C31 | 0.033 (4) | 0.049 (5) | 0.046 (5) | 0.003 (4) | 0.015 (4) | 0.002 (4) |
C18 | 0.016 (3) | 0.032 (3) | 0.028 (3) | 0.001 (3) | 0.006 (3) | −0.004 (3) |
C11A | 0.051 (5) | 0.024 (4) | 0.086 (7) | −0.007 (3) | 0.054 (5) | −0.008 (4) |
C7 | 0.024 (4) | 0.041 (4) | 0.024 (3) | 0.004 (3) | 0.008 (3) | 0.003 (3) |
C6A | 0.018 (3) | 0.030 (3) | 0.028 (3) | −0.001 (3) | 0.012 (3) | 0.000 (3) |
C8A | 0.031 (4) | 0.021 (3) | 0.035 (4) | 0.011 (3) | 0.018 (3) | 0.011 (2) |
N3 | 0.025 (3) | 0.034 (3) | 0.040 (3) | 0.004 (2) | 0.022 (3) | 0.012 (2) |
C9 | 0.020 (3) | 0.032 (4) | 0.045 (4) | −0.001 (3) | 0.013 (3) | 0.004 (3) |
C11 | 0.031 (4) | 0.025 (3) | 0.063 (5) | −0.001 (3) | 0.028 (4) | 0.000 (3) |
C3 | 0.020 (3) | 0.029 (3) | 0.027 (3) | 0.001 (3) | 0.008 (3) | 0.002 (3) |
O32 | 0.035 (3) | 0.044 (3) | 0.066 (4) | 0.013 (3) | 0.027 (3) | 0.016 (3) |
C5 | 0.028 (4) | 0.030 (3) | 0.022 (3) | −0.003 (3) | 0.012 (3) | −0.001 (2) |
C30 | 0.040 (5) | 0.073 (6) | 0.045 (5) | 0.024 (4) | 0.022 (4) | 0.014 (4) |
C12 | 0.031 (4) | 0.020 (3) | 0.052 (5) | −0.008 (3) | 0.027 (4) | −0.003 (3) |
C31A | 0.040 (5) | 0.052 (5) | 0.079 (7) | 0.000 (4) | 0.029 (5) | 0.013 (5) |
Geometric parameters (Å, º) top
Fe1—N4 | 2.018 (5) | N3A—C7A | 1.455 (9) |
Fe1—N3 | 2.025 (6) | N5A—C13A | 1.481 (8) |
Fe1—N6 | 2.027 (5) | C4A—C3A | 1.387 (9) |
Fe1—N1 | 2.040 (5) | C18A—C17A | 1.375 (9) |
Fe1—N2 | 2.042 (5) | C16A—C17A | 1.383 (9) |
Fe1—N5 | 2.052 (5) | N6—C18 | 1.340 (8) |
Fe1A—N1A | 2.132 (5) | N6—C14 | 1.358 (7) |
Fe1A—N5A | 2.142 (5) | N4A—C8A | 1.352 (9) |
Fe1A—N6A | 2.147 (5) | C1—C2 | 1.512 (8) |
Fe1A—N2A | 2.149 (5) | C2—C3 | 1.368 (9) |
Fe1A—N3A | 2.153 (6) | C13A—C14A | 1.510 (8) |
Fe1A—N4A | 2.162 (6) | C8—C9 | 1.387 (9) |
N4—C8 | 1.341 (9) | C8—C7 | 1.488 (9) |
N4—C12 | 1.348 (8) | C13—C14 | 1.496 (8) |
N1—C1 | 1.464 (8) | C3A—C2A | 1.385 (9) |
N5—C13 | 1.491 (8) | C15—C14 | 1.382 (9) |
N2A—C2A | 1.342 (8) | C15—C16 | 1.389 (9) |
N2A—C6A | 1.369 (8) | C10—C9 | 1.370 (11) |
N2—C2 | 1.344 (8) | C10—C11 | 1.410 (12) |
N2—C6 | 1.350 (8) | C30A—C31A | 1.473 (13) |
N6A—C14A | 1.336 (7) | C2A—C1A | 1.535 (8) |
N6A—C18A | 1.356 (8) | C9A—C8A | 1.380 (10) |
C12A—N4A | 1.336 (8) | C9A—C10A | 1.384 (11) |
C12A—C11A | 1.388 (11) | C4—C3 | 1.379 (9) |
N1A—C1A | 1.465 (8) | C4—C5 | 1.381 (9) |
C6—C5 | 1.390 (9) | C7A—C8A | 1.498 (9) |
C15A—C16A | 1.382 (9) | C10A—C11A | 1.371 (12) |
C15A—C14A | 1.392 (9) | O32A—C31A | 1.375 (10) |
C5A—C4A | 1.375 (10) | C31—O32 | 1.409 (9) |
C5A—C6A | 1.374 (9) | C31—C30 | 1.501 (11) |
C17—C18 | 1.372 (9) | C7—N3 | 1.476 (9) |
C17—C16 | 1.392 (9) | C11—C12 | 1.369 (9) |
| | | |
N4—Fe1—N3 | 80.9 (2) | C5A—C4A—C3A | 119.6 (6) |
N4—Fe1—N6 | 166.2 (2) | N6A—C18A—C17A | 124.3 (6) |
N3—Fe1—N6 | 90.5 (2) | C15A—C16A—C17A | 119.1 (6) |
N4—Fe1—N1 | 94.2 (2) | C18—N6—C14 | 117.2 (5) |
N3—Fe1—N1 | 88.6 (2) | C18—N6—Fe1 | 127.4 (4) |
N6—Fe1—N1 | 96.4 (2) | C14—N6—Fe1 | 115.2 (4) |
N4—Fe1—N2 | 96.9 (2) | C12A—N4A—C8A | 118.8 (7) |
N3—Fe1—N2 | 168.1 (2) | C12A—N4A—Fe1A | 126.0 (5) |
N6—Fe1—N2 | 93.7 (2) | C8A—N4A—Fe1A | 114.2 (4) |
N1—Fe1—N2 | 79.9 (2) | N1—C1—C2 | 108.4 (5) |
N4—Fe1—N5 | 89.2 (2) | N2—C2—C3 | 122.7 (6) |
N3—Fe1—N5 | 95.2 (2) | N2—C2—C1 | 115.4 (5) |
N6—Fe1—N5 | 80.8 (2) | C3—C2—C1 | 121.9 (6) |
N1—Fe1—N5 | 175.2 (2) | N5A—C13A—C14A | 110.3 (5) |
N2—Fe1—N5 | 96.4 (2) | N6A—C14A—C15A | 122.9 (6) |
N1A—Fe1A—N5A | 168.9 (2) | N6A—C14A—C13A | 116.6 (5) |
N1A—Fe1A—N6A | 97.2 (2) | C15A—C14A—C13A | 120.6 (5) |
N5A—Fe1A—N6A | 76.70 (19) | N4—C8—C9 | 122.1 (7) |
N1A—Fe1A—N2A | 76.5 (2) | N4—C8—C7 | 114.1 (6) |
N5A—Fe1A—N2A | 94.7 (2) | C9—C8—C7 | 123.8 (7) |
N6A—Fe1A—N2A | 95.1 (2) | N5—C13—C14 | 109.8 (5) |
N1A—Fe1A—N3A | 86.9 (2) | C2A—C3A—C4A | 118.2 (6) |
N5A—Fe1A—N3A | 102.5 (2) | C14—C15—C16 | 119.2 (6) |
N6A—Fe1A—N3A | 93.0 (2) | C9—C10—C11 | 118.5 (7) |
N2A—Fe1A—N3A | 162.3 (2) | N2A—C2A—C3A | 123.7 (6) |
N1A—Fe1A—N4A | 99.5 (2) | N2A—C2A—C1A | 115.4 (5) |
N5A—Fe1A—N4A | 88.4 (2) | C3A—C2A—C1A | 120.9 (6) |
N6A—Fe1A—N4A | 160.2 (2) | C8A—C9A—C10A | 119.6 (8) |
N2A—Fe1A—N4A | 99.0 (2) | C15—C16—C17 | 118.0 (6) |
N3A—Fe1A—N4A | 77.4 (2) | C3—C4—C5 | 118.2 (6) |
C8—N4—C12 | 117.8 (6) | C18A—C17A—C16A | 118.0 (6) |
C8—N4—Fe1 | 115.2 (4) | N6—C14—C15 | 122.7 (6) |
C12—N4—Fe1 | 126.3 (5) | N6—C14—C13 | 115.7 (5) |
C1—N1—Fe1 | 110.7 (4) | C15—C14—C13 | 121.7 (6) |
C13—N5—Fe1 | 109.4 (4) | N1A—C1A—C2A | 109.2 (5) |
C2A—N2A—C6A | 116.4 (6) | N3A—C7A—C8A | 110.2 (6) |
C2A—N2A—Fe1A | 116.8 (4) | C11A—C10A—C9A | 119.5 (7) |
C6A—N2A—Fe1A | 126.7 (4) | O32—C31—C30 | 114.6 (7) |
C2—N2—C6 | 117.8 (5) | N6—C18—C17 | 123.4 (6) |
C2—N2—Fe1 | 115.1 (4) | C10A—C11A—C12A | 118.2 (7) |
C6—N2—Fe1 | 126.9 (4) | N3—C7—C8 | 109.6 (6) |
C14A—N6A—C18A | 116.6 (5) | N2A—C6A—C5A | 123.3 (6) |
C14A—N6A—Fe1A | 116.0 (4) | N4A—C8A—C9A | 121.1 (7) |
C18A—N6A—Fe1A | 127.3 (4) | N4A—C8A—C7A | 115.2 (6) |
N4A—C12A—C11A | 122.9 (8) | C9A—C8A—C7A | 123.7 (7) |
C1A—N1A—Fe1A | 112.7 (4) | C7—N3—Fe1 | 108.2 (4) |
N2—C6—C5 | 122.1 (6) | C10—C9—C8 | 119.8 (7) |
C16A—C15A—C14A | 119.1 (6) | C12—C11—C10 | 118.1 (7) |
C4A—C5A—C6A | 118.7 (6) | C2—C3—C4 | 119.9 (6) |
C18—C17—C16 | 119.4 (6) | C4—C5—C6 | 119.2 (6) |
C7A—N3A—Fe1A | 108.7 (4) | N4—C12—C11 | 123.6 (7) |
C13A—N5A—Fe1A | 111.1 (4) | O32A—C31A—C30A | 117.3 (9) |
(fpic11hs) 'tris(2-Picolylamine)-iron(ii) chloride ethanol solvate'
top
Crystal data top
C18H24FeN6·C2H6O·2(Cl) | F(000) = 1040 |
Mr = 497.25 | Dx = 1.388 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
a = 10.949 (3) Å | Cell parameters from 60 reflections |
b = 21.825 (5) Å | θ = 30–40° |
c = 11.370 (2) Å | µ = 0.88 mm−1 |
β = 118.85 (2)° | T = 10 K |
V = 2379.9 (10) Å3 | Block, yellow |
Z = 4 | 0.4 × 0.3 × 0.2 mm |
Data collection top
CCD Oxford Diffraction diffractometer | 5279 independent reflections |
Radiation source: fine-focus rotating anode | 4081 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.142 |
ϕ–scans | θmax = 27.8°, θmin = 3.8° |
Absorption correction: multi-scan ? | h = −14→13 |
Tmin = 0.735, Tmax = 0.838 | k = −27→27 |
19183 measured reflections | l = −14→13 |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.139 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.308 | Calculated w = 1/[σ2(Fo2) + (0.074P)2 + 44.0563P] where P = (Fo2 + 2Fc2)/3 |
S = 1.18 | (Δ/σ)max < 0.001 |
5279 reflections | Δρmax = 0.95 e Å−3 |
274 parameters | Δρmin = −1.42 e Å−3 |
0 restraints | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0051 (17) |
Crystal data top
C18H24FeN6·C2H6O·2(Cl) | V = 2379.9 (10) Å3 |
Mr = 497.25 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 10.949 (3) Å | µ = 0.88 mm−1 |
b = 21.825 (5) Å | T = 10 K |
c = 11.370 (2) Å | 0.4 × 0.3 × 0.2 mm |
β = 118.85 (2)° | |
Data collection top
CCD Oxford Diffraction diffractometer | 5279 independent reflections |
Absorption correction: multi-scan ? | 4081 reflections with I > 2σ(I) |
Tmin = 0.735, Tmax = 0.838 | Rint = 0.142 |
19183 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.139 | 0 restraints |
wR(F2) = 0.308 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.18 | Δρmax = 0.95 e Å−3 |
5279 reflections | Δρmin = −1.42 e Å−3 |
274 parameters | |
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 | 0.02784 (12) | 0.13510 (5) | 0.80841 (13) | 0.0144 (4) | |
Cl2 | 0.2583 (2) | 0.27291 (9) | 1.0835 (2) | 0.0176 (5) | |
Cl1 | −0.1442 (2) | 0.06714 (9) | 1.0540 (2) | 0.0165 (5) | |
N6 | −0.1496 (7) | 0.1952 (3) | 0.7665 (7) | 0.0169 (15) | |
N4 | 0.2453 (7) | 0.1034 (3) | 0.8899 (8) | 0.0177 (15) | |
N1 | −0.0713 (7) | 0.0489 (3) | 0.8111 (7) | 0.0149 (14) | |
H1A | −0.1142 | 0.0527 | 0.8678 | 0.018* | |
H1B | 0.0016 | 0.0204 | 0.8348 | 0.018* | |
N5 | 0.0889 (7) | 0.2236 (3) | 0.7640 (7) | 0.0146 (14) | |
H5A | 0.1402 | 0.2383 | 0.8528 | 0.018* | |
H5B | 0.1681 | 0.2260 | 0.7387 | 0.018* | |
N3 | 0.1088 (7) | 0.1378 (3) | 1.0259 (8) | 0.0177 (15) | |
H3A | 0.0462 | 0.1329 | 1.0419 | 0.021* | |
H3B | 0.1307 | 0.1780 | 1.0332 | 0.021* | |
N2 | −0.0567 (7) | 0.0996 (3) | 0.6005 (7) | 0.0146 (14) | |
C2 | −0.1458 (8) | 0.0510 (4) | 0.5700 (9) | 0.0136 (16) | |
C15 | −0.2610 (8) | 0.2909 (4) | 0.6717 (9) | 0.0156 (17) | |
H15 | −0.2602 | 0.3286 | 0.6303 | 0.019* | |
O32 | 0.2989 (6) | 0.3873 (3) | 0.9360 (7) | 0.0213 (14) | |
H32 | 0.279 (3) | 0.354 (5) | 0.965 (4) | 0.032* | |
C18 | −0.2517 (8) | 0.1839 (4) | 0.7987 (9) | 0.0158 (17) | |
H18 | −0.2470 | 0.1471 | 0.8454 | 0.019* | |
C5 | −0.0673 (9) | 0.0891 (4) | 0.3862 (9) | 0.0160 (17) | |
H5 | −0.0402 | 0.1040 | 0.3237 | 0.019* | |
C8 | 0.3077 (8) | 0.0897 (4) | 1.0211 (8) | 0.0137 (16) | |
C13 | −0.0359 (8) | 0.2606 (3) | 0.6748 (8) | 0.0104 (15) | |
H13A | −0.0665 | 0.2502 | 0.5799 | 0.012* | |
H13B | −0.0117 | 0.3047 | 0.6877 | 0.012* | |
C11 | 0.4613 (8) | 0.0892 (4) | 0.8879 (9) | 0.0158 (17) | |
H11 | 0.5121 | 0.0895 | 0.8397 | 0.019* | |
C3 | −0.1947 (8) | 0.0197 (4) | 0.4495 (9) | 0.0174 (17) | |
H3 | −0.2544 | −0.0147 | 0.4312 | 0.021* | |
C14 | −0.1546 (9) | 0.2482 (4) | 0.7060 (9) | 0.0189 (18) | |
C16 | −0.3675 (9) | 0.2773 (4) | 0.6992 (10) | 0.0194 (18) | |
H16 | −0.4438 | 0.3047 | 0.6722 | 0.023* | |
C1 | −0.1830 (9) | 0.0329 (4) | 0.6757 (9) | 0.0185 (18) | |
H1AA | −0.2702 | 0.0539 | 0.6586 | 0.022* | |
H1BB | −0.2000 | −0.0118 | 0.6707 | 0.022* | |
C9 | 0.4487 (9) | 0.0740 (4) | 1.0904 (9) | 0.0191 (18) | |
H9 | 0.4909 | 0.0633 | 1.1828 | 0.023* | |
C6 | −0.0188 (8) | 0.1172 (4) | 0.5105 (8) | 0.0134 (16) | |
H6 | 0.0444 | 0.1506 | 0.5323 | 0.016* | |
C4 | −0.1557 (9) | 0.0391 (4) | 0.3544 (10) | 0.0200 (18) | |
H4 | −0.1888 | 0.0185 | 0.2709 | 0.024* | |
C7 | 0.2164 (8) | 0.0899 (4) | 1.0862 (9) | 0.0165 (17) | |
H7A | 0.1713 | 0.0494 | 1.0743 | 0.020* | |
H7B | 0.2741 | 0.0976 | 1.1837 | 0.020* | |
C12 | 0.3191 (9) | 0.1040 (4) | 0.8237 (9) | 0.0177 (17) | |
H12 | 0.2738 | 0.1147 | 0.7313 | 0.021* | |
C17 | −0.3632 (9) | 0.2236 (4) | 0.7664 (10) | 0.0206 (19) | |
H17 | −0.4336 | 0.2142 | 0.7896 | 0.025* | |
C31 | 0.4464 (9) | 0.3895 (4) | 0.9810 (9) | 0.0212 (19) | |
H31A | 0.4975 | 0.3902 | 1.0804 | 0.025* | |
H31B | 0.4682 | 0.4280 | 0.9488 | 0.025* | |
C30 | 0.4973 (10) | 0.3359 (5) | 0.9324 (11) | 0.027 (2) | |
H30A | 0.4939 | 0.2985 | 0.9785 | 0.041* | |
H30B | 0.5934 | 0.3435 | 0.9518 | 0.041* | |
H30C | 0.4375 | 0.3310 | 0.8354 | 0.041* | |
C10 | 0.5270 (8) | 0.0741 (4) | 1.0245 (9) | 0.0188 (18) | |
H10 | 0.6233 | 0.0641 | 1.0710 | 0.023* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Fe1 | 0.0112 (6) | 0.0101 (6) | 0.0201 (7) | 0.0007 (4) | 0.0062 (5) | 0.0010 (5) |
Cl2 | 0.0150 (9) | 0.0145 (10) | 0.0222 (11) | −0.0013 (7) | 0.0081 (8) | −0.0011 (8) |
Cl1 | 0.0144 (9) | 0.0137 (9) | 0.0213 (11) | −0.0002 (7) | 0.0085 (8) | 0.0004 (8) |
N6 | 0.012 (3) | 0.013 (3) | 0.023 (4) | −0.004 (3) | 0.006 (3) | −0.002 (3) |
N4 | 0.015 (3) | 0.009 (3) | 0.024 (4) | 0.001 (3) | 0.005 (3) | −0.002 (3) |
N1 | 0.008 (3) | 0.011 (3) | 0.023 (4) | 0.003 (3) | 0.005 (3) | 0.002 (3) |
N5 | 0.010 (3) | 0.012 (3) | 0.019 (4) | 0.000 (3) | 0.005 (3) | 0.003 (3) |
N3 | 0.012 (3) | 0.010 (3) | 0.030 (4) | −0.001 (3) | 0.010 (3) | −0.002 (3) |
N2 | 0.013 (3) | 0.010 (3) | 0.022 (4) | 0.001 (3) | 0.010 (3) | 0.001 (3) |
C2 | 0.011 (4) | 0.006 (3) | 0.019 (4) | 0.002 (3) | 0.003 (3) | −0.001 (3) |
C15 | 0.012 (4) | 0.009 (4) | 0.022 (4) | 0.002 (3) | 0.005 (3) | 0.003 (3) |
O32 | 0.013 (3) | 0.014 (3) | 0.037 (4) | 0.005 (2) | 0.012 (3) | 0.007 (3) |
C18 | 0.017 (4) | 0.010 (4) | 0.018 (4) | −0.001 (3) | 0.006 (3) | −0.002 (3) |
C5 | 0.016 (4) | 0.015 (4) | 0.018 (4) | 0.001 (3) | 0.010 (3) | 0.002 (3) |
C8 | 0.007 (3) | 0.014 (4) | 0.017 (4) | 0.002 (3) | 0.004 (3) | −0.002 (3) |
C13 | 0.013 (4) | 0.006 (3) | 0.012 (4) | 0.003 (3) | 0.006 (3) | 0.003 (3) |
C11 | 0.010 (4) | 0.014 (4) | 0.023 (4) | 0.004 (3) | 0.007 (3) | 0.006 (3) |
C3 | 0.012 (4) | 0.018 (4) | 0.019 (4) | 0.006 (3) | 0.005 (3) | 0.003 (3) |
C14 | 0.019 (4) | 0.015 (4) | 0.021 (5) | 0.002 (3) | 0.008 (4) | 0.004 (3) |
C16 | 0.013 (4) | 0.011 (4) | 0.034 (5) | −0.001 (3) | 0.010 (4) | 0.003 (4) |
C1 | 0.017 (4) | 0.013 (4) | 0.024 (5) | −0.004 (3) | 0.008 (4) | 0.002 (3) |
C9 | 0.019 (4) | 0.008 (4) | 0.025 (5) | 0.000 (3) | 0.007 (4) | 0.002 (3) |
C6 | 0.011 (4) | 0.014 (4) | 0.016 (4) | 0.003 (3) | 0.007 (3) | 0.002 (3) |
C4 | 0.018 (4) | 0.014 (4) | 0.026 (5) | 0.001 (3) | 0.009 (4) | 0.001 (4) |
C7 | 0.012 (4) | 0.011 (4) | 0.017 (4) | 0.005 (3) | 0.000 (3) | 0.005 (3) |
C12 | 0.019 (4) | 0.014 (4) | 0.022 (5) | 0.001 (3) | 0.012 (4) | 0.000 (3) |
C17 | 0.024 (4) | 0.014 (4) | 0.032 (5) | 0.003 (3) | 0.019 (4) | −0.001 (4) |
C31 | 0.011 (4) | 0.026 (5) | 0.023 (5) | 0.001 (3) | 0.005 (4) | 0.008 (4) |
C30 | 0.016 (4) | 0.025 (5) | 0.037 (6) | 0.006 (4) | 0.009 (4) | 0.003 (4) |
C10 | 0.011 (4) | 0.018 (4) | 0.025 (5) | −0.003 (3) | 0.007 (4) | −0.005 (4) |
Geometric parameters (Å, º) top
Fe1—N1 | 2.181 (7) | C2—C1 | 1.496 (12) |
Fe1—N5 | 2.182 (7) | C15—C16 | 1.376 (12) |
Fe1—N3 | 2.189 (8) | C15—C14 | 1.392 (11) |
Fe1—N6 | 2.197 (7) | O32—C31 | 1.440 (10) |
Fe1—N4 | 2.208 (7) | C18—C17 | 1.394 (12) |
Fe1—N2 | 2.221 (7) | C5—C4 | 1.386 (12) |
N6—C14 | 1.334 (11) | C5—C6 | 1.390 (12) |
N6—C18 | 1.356 (11) | C8—C9 | 1.395 (11) |
N4—C8 | 1.342 (11) | C8—C7 | 1.503 (11) |
N4—C12 | 1.344 (11) | C13—C14 | 1.528 (11) |
N1—C1 | 1.473 (11) | C11—C10 | 1.401 (13) |
N5—C13 | 1.487 (10) | C11—C12 | 1.401 (11) |
N3—C7 | 1.474 (10) | C3—C4 | 1.406 (12) |
N2—C6 | 1.333 (10) | C16—C17 | 1.389 (12) |
N2—C2 | 1.369 (10) | C9—C10 | 1.384 (12) |
C2—C3 | 1.386 (12) | C31—C30 | 1.510 (13) |
| | | |
N1—Fe1—N5 | 167.9 (3) | C2—N2—Fe1 | 114.8 (5) |
N1—Fe1—N3 | 86.6 (3) | N2—C2—C3 | 121.3 (8) |
N5—Fe1—N3 | 103.6 (3) | N2—C2—C1 | 116.0 (7) |
N1—Fe1—N6 | 97.1 (3) | C3—C2—C1 | 122.6 (7) |
N5—Fe1—N6 | 76.0 (3) | C16—C15—C14 | 118.6 (8) |
N3—Fe1—N6 | 93.6 (3) | N6—C18—C17 | 123.1 (8) |
N1—Fe1—N4 | 99.6 (3) | C4—C5—C6 | 119.4 (8) |
N5—Fe1—N4 | 89.2 (3) | N4—C8—C9 | 120.9 (8) |
N3—Fe1—N4 | 76.6 (3) | N4—C8—C7 | 116.4 (7) |
N6—Fe1—N4 | 159.9 (3) | C9—C8—C7 | 122.7 (8) |
N1—Fe1—N2 | 76.1 (3) | N5—C13—C14 | 110.5 (6) |
N5—Fe1—N2 | 94.5 (3) | C10—C11—C12 | 118.6 (8) |
N3—Fe1—N2 | 161.1 (3) | C2—C3—C4 | 119.8 (8) |
N6—Fe1—N2 | 96.1 (3) | N6—C14—C15 | 123.1 (8) |
N4—Fe1—N2 | 98.5 (3) | N6—C14—C13 | 116.5 (7) |
C14—N6—C18 | 117.6 (7) | C15—C14—C13 | 120.5 (7) |
C14—N6—Fe1 | 116.2 (6) | C15—C16—C17 | 119.9 (8) |
C18—N6—Fe1 | 126.2 (6) | N1—C1—C2 | 111.5 (7) |
C8—N4—C12 | 120.3 (7) | C10—C9—C8 | 120.0 (8) |
C8—N4—Fe1 | 113.8 (5) | N2—C6—C5 | 123.0 (8) |
C12—N4—Fe1 | 125.5 (6) | C5—C4—C3 | 117.9 (9) |
C1—N1—Fe1 | 110.9 (5) | N3—C7—C8 | 110.2 (7) |
C13—N5—Fe1 | 110.8 (5) | N4—C12—C11 | 121.6 (8) |
C7—N3—Fe1 | 107.7 (5) | C16—C17—C18 | 117.6 (8) |
C6—N2—C2 | 118.5 (7) | O32—C31—C30 | 113.1 (8) |
C6—N2—Fe1 | 126.3 (6) | C9—C10—C11 | 118.7 (8) |
Experimental details
| (ev_fpic118) | (fepic100) | (fepic200) | (fpic10k) |
Crystal data |
Chemical formula | C18H24FeN6·C2H6O·2(Cl) | C18H24FeN6·C2H6O·2(Cl) | C18H24FeN6·C2H6O·2(Cl) | C18H24FeN6·C2H6O·2(Cl) |
Mr | 497.25 | 497.25 | 497.25 | 497.25 |
Crystal system, space group | Monoclinic, P21/c | Monoclinic, P21/c | Monoclinic, P21/c | Monoclinic, P21/c |
Temperature (K) | 118 | 100 | 200 | 10 |
a, b, c (Å) | 10.8041 (9), 21.6945 (14), 11.395 (4) | 10.7098 (17), 21.5711 (13), 11.356 (4) | 10.9348 (7), 21.9329 (16), 11.484 (5) | 10.7322 (14), 21.5055 (7), 11.323 (2) |
β (°) | 117.33 (3) | 116.62 (3) | 117.59 (2) | 117.184 (17) |
V (Å3) | 2372.7 (9) | 2345.5 (9) | 2441.0 (11) | 2324.7 (5) |
Z | 4 | 4 | 4 | 4 |
Radiation type | Cu Kα | Cu Kα | Cu Kα | Mo Kα |
µ (mm−1) | 7.36 | 7.44 | 7.15 | 0.90 |
Crystal size (mm) | 0.46 × 0.12 × 0.12 | 0.46 × 0.12 × 0.12 | 0.46 × 0.12 × 0.12 | 0.4 × 0.3 × 0.2 |
|
Data collection |
Diffractometer | CAD4 Enraf Nonius diffractometer | CAD4 Enraf Nonius diffractometer | CAD4 Enraf Nonius diffractometer | CCD Oxford Diffraction diffractometer |
Absorption correction | – | ψ scan | – | Multi-scan |
Tmin, Tmax | – | 0.399, 0.411 | – | 0.730, 0.835 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 5041, 4798, 3612 | 4994, 4752, 3699 | 5190, 4939, 3585 | 20473, 5154, 4302 |
Rint | 0.053 | 0.056 | 0.057 | 0.105 |
(sin θ/λ)max (Å−1) | 0.623 | 0.623 | 0.622 | 0.657 |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | 0.075, 0.197, 1.13 | 0.064, 0.173, 1.04 | 0.076, 0.199, 1.09 | 0.060, 0.130, 1.11 |
No. of reflections | 4798 | 4752 | 4939 | 5154 |
No. of parameters | 274 | 274 | 274 | 274 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement | H atoms treated by a mixture of independent and constrained refinement | H atoms treated by a mixture of independent and constrained refinement | H atoms treated by a mixture of independent and constrained refinement |
| Calculated w = 1/[σ2(Fo2) + (0.1071P)2 + 2.315P] where P = (Fo2 + 2Fc2)/3 | Calculated w = 1/[σ2(Fo2) + (0.1071P)2 + 2.315P] where P = (Fo2 + 2Fc2)/3 | Calculated w = 1/[σ2(Fo2) + (0.1071P)2 + 2.315P] where P = (Fo2 + 2Fc2)/3 | Calculated w = 1/[σ2(Fo2) + (0.0401P)2 + 5.8012P] where P = (Fo2 + 2Fc2)/3 |
Δρmax, Δρmin (e Å−3) | 1.36, −1.43 | 1.20, −1.34 | 1.15, −1.28 | 0.62, −0.57 |
| (fpic118h) | (fpic11hs) |
Crystal data |
Chemical formula | C18H24FeN6·C2H6O·2(Cl) | C18H24FeN6·C2H6O·2(Cl) |
Mr | 994.50 | 497.25 |
Crystal system, space group | Monoclinic, P21/n | Monoclinic, P21/c |
Temperature (K) | 118 | 10 |
a, b, c (Å) | 21.6080 (18), 21.6945 (14), 11.395 (4) | 10.949 (3), 21.825 (5), 11.370 (2) |
β (°) | 117.33 (3) | 118.85 (2) |
V (Å3) | 4745.4 (17) | 2379.9 (10) |
Z | 4 | 4 |
Radiation type | Cu Kα | Mo Kα |
µ (mm−1) | 7.36 | 0.88 |
Crystal size (mm) | 0.46 × 0.12 × 0.12 | 0.4 × 0.3 × 0.2 |
|
Data collection |
Diffractometer | CAD4 Enraf Nonius diffractometer | CCD Oxford Diffraction diffractometer |
Absorption correction | – | Multi-scan |
Tmin, Tmax | – | 0.735, 0.838 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 10076, 9586, 5558 | 19183, 5279, 4081 |
Rint | 0.062 | 0.142 |
(sin θ/λ)max (Å−1) | 0.623 | 0.656 |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | 0.085, 0.254, 1.00 | 0.139, 0.308, 1.18 |
No. of reflections | 9586 | 5279 |
No. of parameters | 543 | 274 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement | H atoms treated by a mixture of independent and constrained refinement |
| Calculated w = 1/[σ2(Fo2) + (0.1507P)2] where P = (Fo2 + 2Fc2)/3 | Calculated w = 1/[σ2(Fo2) + (0.074P)2 + 44.0563P] where P = (Fo2 + 2Fc2)/3 |
Δρmax, Δρmin (e Å−3) | 1.78, −1.58 | 0.95, −1.42 |
Subscribe to Journal of Applied Crystallography
The full text of this article is available to subscribers to the journal.
If you have already registered and are using a computer listed in your registration details, please email
support@iucr.org for assistance.