Table 2.
X-ray crystallographic data for compounds 7-12 (Chart 1) at 100 Ka
| Compounds | 7·3DMF·Et2O | 8·2DMF | 9·2DMF | 10·4MeCN | 11·DMF | 12·2DMF |
|---|---|---|---|---|---|---|
| Formula | C105H150B4 F16Fe5 N25O13 |
C92H116B2 F8Fe4 N22O9 |
C92H112B2 F8Fe4N22O8 |
C51H62B2 F8Fe N14O |
C48H60B2 F8Fe2 N12O3 |
C55H78B3 F12Fe2 N14O7 |
| formula weight | 2596.99 | 2071.09 | 2051.06 | 1116.62 | 1138.40 | 1419.44 |
| crystal system | triclinic | triclinic | triclinic | orthorhombic | monoclinic | Triclinic |
| space group | Pī | Pī | Pī | Pbcn | P21/n | Pī |
| a, Å | 17.548(2) | 15.092(2) | 17.282(1) | 23.978(2) | 13.879(1) | 12.821(4) |
| b, Å | 18.524(2) | 17.612(3) | 17.599(1) | 11.555(8) | 23.342(2) | 17.528(6) |
| c, Å | 20.896(2) | 27.955(4) | 23.455(3) | 19.580(1) | 15.968(1) | 17.703(6) |
| α, deg | 78.952(2) | 85.993(3) | 100.636(2) | 73.288 (1) | ||
| β, deg | 71.109(2) | 80.605(2) | 95.959(2) | 97.122(2) | 76.650(1) | |
| γ, deg | 69.479(2) | 64.731(2) | 116.188(1) | 79.532(1) | ||
| V, Å3 | 5995.2(1) | 6629.1(2) | 6151.0(1) | 5425.0(6) | 5133.0(8) | 3678.9(2) |
| Z | 2 | 2 | 2 | 4 | 4 | 2 |
| ρcalcd, gm/cm3 | 1.439 | 1.257 | 1.107 | 1.367 | 1.473 | 1.281 |
| μ, mm−1 | 0.684 | 0.506 | 0.527 | 0.357 | 0.649 | 0.478 |
| θ range, deg | 1.63-25.76 | 1.48-25.80 | 1.61-24.75 | 1.70-25.71 | 1.55-25.69 | 1.49-25.70 |
| completeness to θ , % |
99.1 | 99.0 | 98.6 | 100.0 | 100.0 | 99.8 |
| reflections collected |
95976 | 25264 | 92034 | 84107 | 83460 | 58867 |
| independent reflections |
22796 | 107121 | 20801 | 5165 | 9751 | 13988 |
| R(int) | 0.0585 | 0.0630 | 0.0457 | 0.0422 | 0.0469 | 0.0365 |
| drestraints | 16 | 6 | 3 | 3 | 46 | 17 |
| Parameters | 1509 | 1269 | 1161 | 360 | 668 | 791 |
| max., min. transmission |
0.9731, 0.8210 | 0.9899, 0.8629 |
0.9691, 0.8169 |
0.9858, 0.9385 | 0.9745, 0.9262 |
0.9811, 0.9104 |
| R1b(wR2)c [I>2sigma(I)] |
0.0841 (0.2271) |
0.0809 (0.2559) |
0.0762 (0.2433) |
0.0652 (0.1622) |
0.0912 (0.2200) |
0.0848 (0.2554) |
| R1b(wR2)c | 0.1140 (0.2484) |
0.1157(0.278 9) |
0.0959 (0.2587) |
0.0776 (0.1737) |
0.1089 (0.2335) |
0.1110 (0.2771) |
| GOF(F2)d | 1.073 | 1.116 | 1.096 | 1.057 | 1.051 | 1.143 |
|
emax, min peaks, e.Å−3 |
1.821 , −1.137 |
1.096, −0.675 | 1.118, −1.136 | 1.467, −0.951 |
1.232, −1.101 |
1.473, −1.418 |
Mo Kα radiation (λ = 0.71073 Å).
R1 = Σ∥Fo∣-∣Fc∥/Σ∣Fo∣.
wR2 = {Σ[w(Fo2-Fc2)2]/Σ[w(Fo2)2]}1/2.
GOF = {Σ[w(Fo2–Fc2)2]/(n–p)}1/2, where n is the number of data and p is the number of refined parameters.
7, disordered DMF (2), diethyl ether (1); 8, disordered DMF (2), N-Et group (2); 9, disordered DMF(1), N-Et group (1); 10, MeCN (3); 11, disordered DMF (1), BF4− (2), N-Et (2), N-CH (4); 12, disordered DMF (1), perchlorate (3).
7, near one BF4−, disorder modeling was not reasonable; 8, near iron; 9, near BF4−, disorder modeling was not helpful; 10, near alkoxide group, not taken into account; 11, near severely disordered benzimidazole; 12, near hydroxide groups, no meaningful disorder modeling found; 13, near one of the perchlorates, disorder modeling was not helpful.