Multicomponent Crystal of Metformin and Barbital: Design, Crystal Structure Analysis and Characterization
Abstract
:1. Introduction
2. Results and Discussion
2.1. Single Crystal X-ray Diffraction Analysis of the Crystal Structure
2.2. Characterization of the Crystal Structure
2.3. Characterization of the Moisture Sorption Behavior
3. Conclusions
4. Materials and Methods
4.1. Materials
4.2. Methods
4.2.1. Preparation of Met–Bar
4.2.2. Single Crystal X-ray Diffraction (SCXRD)
4.2.3. Thermal Analysis (TGA and DSC)
4.2.4. Powder X-ray Diffraction (PXRD)
4.2.5. Fourier-Transform Infrared Spectroscopy (FT-IR)
4.2.6. 1H NMR Spectroscopy Analysis
4.2.7. Dynamic Vapor Sorption (DVS)
Author Contributions
Funding
Data Availability Statement
Conflicts of Interest
Sample Availability
References
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Empirical Formula | C14H31N7O5 |
---|---|
Formula weight | 377.46 |
Temperature (K) | 293(2) |
Crystal system | Triclinic |
Space group | P-1 |
a (Å) | 7.3409(7) |
b (Å) | 11.1698(10) |
c (Å) | 13.0980(9) |
α (°) | 74.680(7) |
β (°) | 78.624(7) |
γ (°) | 84.157(8) |
Volume (Å3) | 1014.08(15) |
Z | 2 |
ρcalcg (cm3) | 1.236 |
μ/mm−1 | 0.791 |
F(000) | 408 |
Crystal size (mm3) | 0.12 × 0.1 × 0.09 |
Radiation | CuKα (λ = 1.54184) |
2Θ range for data collection (°) | 7.11 to 134.102 |
Index ranges | −8 ≤ h ≤ 8, −13 ≤ k ≤ 13, −15 ≤ l ≤ 13 |
Reflections collected | 7079 |
Independent reflections | 3627 (Rint = 0.0330, Rsigma = 0.0556) |
Data/restraints/parameters | 3627/0/278 |
Goodness-of-fit on F2 | 1.04 |
Final R indexes (I ≥ 2σ (I)) | R1 = 0.0525, wR2 = 0.1313 |
Final R indexes (all data) | R1 = 0.0805, wR2 = 0.1552 |
Largest diff., peak/hole (e/Å−3) | 0.25/−0.17 |
CCDC deposit number | 2075003 |
D–H···A | d(D–H) (Å) | d(H–A) (Å) | d(D–A) (Å) | D–H–A (°) |
---|---|---|---|---|
N(1)–H(1A)···O(2) 1 | 0.84 | 2.15 | 2.967 | 163 |
N(1)–H(1B)···O(1) | 0.83 | 2.24 | 2.939 | 142 |
N(2)–H(2A)···O(4) | 0.88 | 2.10 | 2.951 | 161 |
N(2)–H(2B)···O(4) 2 | 0.92 | 1.99 | 2.908 | 175 |
N(4)–H(4D)···O(3) 2 | 0.89 | 2.19 | 3.057 | 166 |
N(4)–H(4E)···O(5) 2 | 0.89 | 2.02 | 2.901 | 171 |
N(6)–H(6)···O(1) 1 | 0.80 | 2.13 | 2.931 | 179 |
O(4)–H(4)···N(7) 2 | 0.86 | 1.88 | 2.739 | 172 |
O(5)–H(5)···O(3) 3 | 0.78 | 1.97 | 2.755 | 175 |
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Cai, L.; Jiang, L.; Li, C.; Guan, X.; Zhang, L.; Hu, X. Multicomponent Crystal of Metformin and Barbital: Design, Crystal Structure Analysis and Characterization. Molecules 2021, 26, 4377. https://doi.org/10.3390/molecules26144377
Cai L, Jiang L, Li C, Guan X, Zhang L, Hu X. Multicomponent Crystal of Metformin and Barbital: Design, Crystal Structure Analysis and Characterization. Molecules. 2021; 26(14):4377. https://doi.org/10.3390/molecules26144377
Chicago/Turabian StyleCai, Linhong, Lan Jiang, Cong Li, Xiaoshu Guan, Li Zhang, and Xiangnan Hu. 2021. "Multicomponent Crystal of Metformin and Barbital: Design, Crystal Structure Analysis and Characterization" Molecules 26, no. 14: 4377. https://doi.org/10.3390/molecules26144377