Molecular Structures of the Products of a Diphosphonate Ester Building Block with Lewis Bases
Abstract
:1. Introduction
2. Results and Discussion
2.1. Supramolecular Structure of 1
2.2. Supramolecular Structure of 2
Compound | C-H···π | Symmetry Code | C···π Centroid-Centroid (Å) | ∠C-H···π (°) |
---|---|---|---|---|
2 | C(14)-H(14B)···Cg(3) | x, −1 + y, z | 3.640 | 149.55 |
C(14)-H(14B)···Cg(3) | 1− x, 1 − y, −z | 3.640 | 149.55 | |
C(17)-H(17B)···Cg(4) | x, y, z | 3.695 | 136.52 | |
C(17)-H(17B)···Cg(4) | − x, 1 − y, 1 − z | 3.695 | 136.52 | |
3 | C(5)-H(5A)···Cg(1) | − x, −½ + y, ½ − z | 4.044 | 164.92 |
C(5)-H(5A)···Cg(1) | x, −½ − y, ½ + z | 4.044 | 164.92 | |
4 | C(2)-H(2B)···Cg(1) | x, y, z | 3.792 | 145.37 |
C(2)-H(2B)···Cg(1) | − x, −y, −z | 3.792 | 145.37 |
2.3. Supramolecular Structure of 3
2.4. Supramolecular Structure of 4
2.5. Fluorescence Properties
3. Experimental Section
3.1. Materials and Methods
3.2. Synthesis of H2[BBPEH2] (1)
3.3. Synthesis of [BBPEH2]2−·[Protonated N,N-dimethylpiperazine]2+·4H2O (2)
3.4. Synthesis of [BBPEH2]2−·[NH4]22+·2H2O (3)
3.5. Synthesis of {[BBPEH2]·[Na2(H2O)6]}∞ (4)
3.6. Single Crystal X-ray Diffraction Studies
Empirical Formula | C6H8O3P | C18H40N2O10P2 | C6 H15NO4P | C12H30Na2O12P2 |
---|---|---|---|---|
M | 159.09 | 506.46 | 196.16 | 474.28 |
crystal size/mm | 0.24 × 0.20 × 0.16 | 0.30 × 0.18 × 0.14 | 0.22 × 0.20 × 0.18 | 0.24 × 0.22 × 0.18 |
T/K | 293(2) | 293(2) | 293(2) | 293(2) |
λ/Å | 0.71073 | 0.71073 | 0.71073 | 0.71073 |
crystal system | monoclinic | centric | centric | centric |
space group | C2 | P-1 | P-1 | Pnma |
a/Å | 13.431(3) | 9.3520(19) | 13.079(3) | 8.2010(16) |
b/Å | 8.8309(18) | 10.458(2) | 9.1170(18) | 28.502(6) |
c/Å | 7.7810(16) | 15.736(3) | 8.9340(18) | 9.7120(19) |
α/deg | 90 | 81.56(3) | 89.88(3) | 90 |
β/deg | 123.98(3) | 82.84(3) | 107.82(3) | 90 |
γ/deg | 90 | 63.46(3) | 90.02(3) | 90 |
V/Å3 | 765.3(3) | 1358.9(5) | 1014.2(4) | 2270.1(8) |
Z | 4 | 2 | 4 | 4 |
ρ calcd/g.cm−3 | 1.381 | 1.238 | 1.285 | 1.352 |
F (000) | 332 | 544 | 420 | 952 |
μ/mm−1 | 0.304 | 0.208 | 0.252 | 0.280 |
θ range/deg | 2.94 to 26.98 | 1.31 to 29.31 | 1.64 to 26.97 | 1.43 to 25.00 |
completeness to θ | 98.7% | 74.9% | 97.2% | 99.6% |
range of h, k, l | −17 ≤ h ≤ 14, −11 ≤ k ≤ 11, 0 ≤ l ≤ 9 | 0 ≤ h ≤ 11, −11 ≤ k ≤ 12, −18 ≤ l ≤ 18 | −15 ≤ h ≤ 15, −10 ≤ k ≤ 10, 0 ≤ l ≤ 10 | 0 ≤ h ≤ 9, −33 ≤ k ≤ 0, 0 ≤ l ≤ 11 |
reflections collected/unique | 1773/881 | 6013/5585 | 4426/2150 | 2035/2035 |
Rint | 0.0334 | 0.1221 | 0.0691 | 0.0000 |
data/restraints/parameters | 881/1/60 | 5585/0/297 | 2150/2/134 | 2035/0/133 |
GOF on F2 | 1.144 | 1.027 | 1.086 | 1.065 |
final R indices [I > 2σ (I)] | R1 = 0.0504 wR2 = 0.1373 | R1 = 0.0574 wR2 = 0.1688 | R1 = 0.0374 wR2 = 0.0994 | R1 = 0.0962 wR2 = 0.2405 |
R indices (all data) | R1 = 0.0545 wR2 = 0.1416 | R1 = 0.0954 wR2 = 0.1946 | R1 = 0.0496 wR2 = 0.1069 | R1 = 0.1459 wR2 = 0.2891 |
peak, hole/e.Å−3 | 0.600 and −0.358 | 0.584 and −0.610 | 0.350 and −0.378 | 1.396 and −1.108 |
Compound | D-H···A | Symmetry Code | D···A (Å) | ∠D-H···A (°) |
---|---|---|---|---|
1 | O(2)-H(1)···O(2) | − x, y, −z | 2.5114 | 165.95 |
2 | N(1)-H(1)···O(2) | x, −1 + y, z | 2.6265 | 175.86 |
O(1w)-H(11W)···O(4W) | −1 + x, y, z | 3.0756 | 126.99 | |
O(2W)-H(12W)···O(1) | −1 + x, y, z | 2.8627 | 155.48 | |
O(3W)-H(13W)···O(2) | 2 − x, 1 − y, −z | 3.0145 | 164.35 | |
O(4W)-H(14W)···O(5) | 1 − x, 1 − y, 1 − z | 2.9162 | 172.15 | |
O(1W)-H(21W)···O(4) | x, −1 + y, z | 2.8216 | 164.14 | |
3 | N (1)-H(1)···O(1) | x, ½ − y, ½ + z | 2.8338 | 168.93 |
O(2W)-H(3)···O(2) | x, ½ − y, ½ + z | 2.7913 | 171.10 | |
N(1)-H(5)···O(2W) | 1 − x, −1/2 + y, ½ − z | 2.8304 | 162.13 | |
N(1)-H(6)···O(2) | 1 − x, ½ + y, ½ − z | 2.7767 | 169.00 |
4. Conclusions
Supplementary Materials
Acknowledgments
Author Contributions
Conflicts of Interest
References
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Li, Y.; Jian, F. Molecular Structures of the Products of a Diphosphonate Ester Building Block with Lewis Bases. Molecules 2015, 20, 14435-14450. https://doi.org/10.3390/molecules200814435
Li Y, Jian F. Molecular Structures of the Products of a Diphosphonate Ester Building Block with Lewis Bases. Molecules. 2015; 20(8):14435-14450. https://doi.org/10.3390/molecules200814435
Chicago/Turabian StyleLi, Yufeng, and Fangfang Jian. 2015. "Molecular Structures of the Products of a Diphosphonate Ester Building Block with Lewis Bases" Molecules 20, no. 8: 14435-14450. https://doi.org/10.3390/molecules200814435