Self-Assembly of a 1D Hydrogen-Bonded Polymer from a Hexamethyltetraaza Macrocyclic Nickel(II) Complex and Isophthalic Acid
Abstract
:1. Introduction
2. Results and Discussion
2.1. Description of the Structure
Bond lengths and angles | |||
---|---|---|---|
Bond lengths | |||
Ni(1)-N(1) | 2.130(7) | Ni(1)-N(2) | 2.009(7) |
Ni(1)-O(1) | 2.056(6) | Ni(2)-N(3) | 1.913(7) |
Ni(2)-N(4) | 1.878(8) | C(9)-O(1) | 1.254(11) |
C(9)-O(1) | 1.238(11) | C(16)-O(3) | 1.196(12) |
C(16)-O(4) | 1.239(12) | Ni(1)…Ni(2) | 11.641(8) |
Ni(1)…Ni(2)i | 9.607(4) | ||
Bond angles | |||
N(1)-Ni(1)-N(2) | 87.0(3) | N(1)-Ni(1)-N(2)iii | 93.0(3) |
N(1)-Ni(1)-O(1) | 89.7(3) | N(1)iii-Ni(1)-O(1) | 90.3(3) |
N(2)-Ni(1)-O(1) | 85.6(3) | N(2)iii-Ni(1)-O(1) | 94.4(3) |
N(3)-Ni(2)-N(4) | 91.3(4) | N(3)-Ni(2)-N(4)iv | 88.7(4) |
Ni(1)-O(1)-C(9) | 133.7(6) | O(1)-C(9)-O(2) | 127.7(8) |
O(3)-C(16)-O(4) | 122.6(9) |
D-H…A | D-H (Å) | H…A (Å) | D…A (Å) | D-H…A (°) |
---|---|---|---|---|
N(1)-H(1)…O(2)iii | 0.91 | 1.95 | 2.804(10) | 154.6 |
N(3)-H(3)…O(4) | 0.91 | 1.98 | 2.869(10) | 164.0 |
N(4)-H(4)…O(3) | 0.91 | 1.98 | 2.841(11) | 157.8 |
Ow(1)-HO(1)…O(4) | 1.07(10) | 1.65(11) | 2.676(11) | 160(9) |
Ow(2)-HO(3)…O(2) | 1.00(11) | 1.76(11) | 2.734(12) | 163(9) |
Ow(2)-HO(4)…Ow(1) | 0.89(13) | 1.92(13) | 2.706(14) | 147(11) |
Ow(4)-HO(8)…Ow(1)iv | 0.82(13) | 2.12(14) | 2.829(17) | 145(13) |
2.2. Chemical Properties
Complex | State | λmax/nm (ε/M−1 cm−1) |
---|---|---|
[Ni(L)](ClO4)2 b | H2O | 463(80) |
CH3CN | 469(63) | |
Solid | 262, 468 | |
[Ni(L)(isoph)2][Ni(L)]∙8H2O (1) | H2O | 260(5.2 × 103), 458(71) |
Solid | 325(sh), 474, 696 |
Complex | Potentials(V) Ag/AgCl |
---|---|
Ni(II)/Ni(I) | |
[Ni(L)](ClO4)2 b,a | −1.29 |
[Ni(L)(isoph)2][Ni(L)]∙8H2O (1) | −0.76(i) c |
3. Experimental
3.1. Materials and Physical Measurements
3.2. Synthesis of [Ni(L)(isoph)2][Ni(L)]·8H2O (1)
3.3. X-ray Crystallography
Data and refinement | |
---|---|
Empirical formula | C48H96N8Ni2O16 |
Formula weight | 1157.94 |
Temperature (K) | 293(2) |
Crystal color/habit | Brown/prism |
Crystal system | Triclinic |
Space group | P-1 |
Unit cell dimensions | |
a (Å) | 8.602(2) |
b (Å) | 10.684(7) |
c (Å) | 16.550(3) |
α (°) | 91.04(4) |
β (°) | 94.09(2) |
γ (°) | 111.09(4) |
V (Å3) | 1413.9(10) |
Z | 1 |
Dcalc (Mg m−3) | 1.360 |
Absorption coefficient (mm−1) | 0.738 |
F(000) | 624 |
Crystal size (mm3) | 0.40 × 0.30 × 0.10 |
θ range (°) | 1.23 to 26.37 |
Limiting indices | −10 ≤ h ≤ 10, −13 ≤ k≤ 13, −1 ≤ l≤ 19 |
Reflection collected/unique | 5729/5137 (Rint = 0.0817) |
Absorption correction | ψ-scan |
Max./min. transmission | 0.9145 and 0.7122 |
Data/restraints/parameters | 5137/0/369 |
Goodness of fit on F2 | 1.184 |
Final R indices (I>2σ(I)) | R1a = 0.0811, wR2b = 0.2224 |
R indices (all data) | R1 = 0.1742, wR2 = 0.3391 |
Weighting scheme | w = 1/[σ2(Fo2) + (0.20000P)2 +0.0000P] |
rgest difference peak and hole (eÅ−3) | with P = (Fo2 + 2Fc2)/3 |
1.731 and −1.199 |
4. Conclusions
Supplementary Materials
Conflicts of Interest
References
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Lim, I.-T.; Choi, K.-Y. Self-Assembly of a 1D Hydrogen-Bonded Polymer from a Hexamethyltetraaza Macrocyclic Nickel(II) Complex and Isophthalic Acid. Molecules 2013, 18, 6608-6619. https://doi.org/10.3390/molecules18066608
Lim I-T, Choi K-Y. Self-Assembly of a 1D Hydrogen-Bonded Polymer from a Hexamethyltetraaza Macrocyclic Nickel(II) Complex and Isophthalic Acid. Molecules. 2013; 18(6):6608-6619. https://doi.org/10.3390/molecules18066608
Chicago/Turabian StyleLim, In-Taek, and Ki-Young Choi. 2013. "Self-Assembly of a 1D Hydrogen-Bonded Polymer from a Hexamethyltetraaza Macrocyclic Nickel(II) Complex and Isophthalic Acid" Molecules 18, no. 6: 6608-6619. https://doi.org/10.3390/molecules18066608