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CAS No. : | 2449-35-6 | MDL No. : | MFCD00020375 |
Formula : | C14H10O6S | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | SQJQLYOMPSJVQS-UHFFFAOYSA-N |
M.W : | 306.29 | Pubchem ID : | 224167 |
Synonyms : |
|
Num. heavy atoms : | 21 |
Num. arom. heavy atoms : | 12 |
Fraction Csp3 : | 0.0 |
Num. rotatable bonds : | 4 |
Num. H-bond acceptors : | 6.0 |
Num. H-bond donors : | 2.0 |
Molar Refractivity : | 72.3 |
TPSA : | 117.12 Ų |
GI absorption : | High |
BBB permeant : | No |
P-gp substrate : | No |
CYP1A2 inhibitor : | No |
CYP2C19 inhibitor : | No |
CYP2C9 inhibitor : | No |
CYP2D6 inhibitor : | No |
CYP3A4 inhibitor : | No |
Log Kp (skin permeation) : | -6.92 cm/s |
Log Po/w (iLOGP) : | 1.21 |
Log Po/w (XLOGP3) : | 1.76 |
Log Po/w (WLOGP) : | 3.0 |
Log Po/w (MLOGP) : | 2.24 |
Log Po/w (SILICOS-IT) : | 1.14 |
Consensus Log Po/w : | 1.87 |
Lipinski : | 0.0 |
Ghose : | None |
Veber : | 0.0 |
Egan : | 0.0 |
Muegge : | 0.0 |
Bioavailability Score : | 0.56 |
Log S (ESOL) : | -3.01 |
Solubility : | 0.302 mg/ml ; 0.000985 mol/l |
Class : | Soluble |
Log S (Ali) : | -3.84 |
Solubility : | 0.0446 mg/ml ; 0.000146 mol/l |
Class : | Soluble |
Log S (SILICOS-IT) : | -3.57 |
Solubility : | 0.0819 mg/ml ; 0.000267 mol/l |
Class : | Soluble |
PAINS : | 0.0 alert |
Brenk : | 0.0 alert |
Leadlikeness : | 0.0 |
Synthetic accessibility : | 1.87 |
Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H319-H335 | Packing Group: | N/A |
GHS Pictogram: |
* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
65% | With sulfuric acid for 5h; Heating; | |
62% | With sulfuric acid for 6h; Reflux; | |
With sulfuric acid |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
93% | With thionyl chloride; N,N-dimethyl-formamide for 24h; Reflux; | |
78% | With thionyl chloride In N,N-dimethyl-formamide at 90℃; for 3h; | |
With phosphorus pentachloride at 130 - 140℃; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With pyridine; triphenyl phosphite; calcium chloride In 1-methyl-pyrrolidin-2-one at 100℃; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
58% | With NaOH In water High Pressure; mixt. of Ni(CH3CO2)2*4H2O, ligands and NaOH in H2O placed in autoclave, heated to 160°C for 5 d; elem. anal.; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
96% | With potassium hydroxide In ethanol Reflux; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
43% | With 1,2-diaminoethane In water High Pressure; mixt. of Zn(OAc)2*2H2O, levofloxacin hydrochloride, acid and water; adjusted to pH 8.5 with 1,2-diaminoethane, sealed in autoclave, heated at 130°C for 4 d, cooled to room temp.; elem. anal.; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
41.2% | at 150℃; for 48h; High pressure; | Compound 1 can be synthesized by hydrothermal method or microwave syntheses method. In both of the two methods, a reactor comprises a Teflon inner cup and iron outer cup is utilized to synthesizing Compound 1. The difference between hydrothermal method and microwave syntheses method is that the reactor is put into a high temperature furnace for synthesizing in the hydrothermal method but the reactor is put into a microwave reactor for synthesizing in the microwave syntheses method. The hydrothermal method for synthesizing compound 1 is detailed as the following: First, 0.205 g (0.8 mmol) Mg(NO3)2.6H2O, 0.0612 g (0.2 mmol) 4,4′-sulfonyldibenzoic acid (H2SBA), 5.0 mL ethanol (EtOH), and 1.0 mL water (H2O) are put into the Teflon inner cup in order. And then, the Teflon inner cup is put into the iron outer cup and the reactor is put into the high temperature furnace. In the high temperature furnace, the reactor (or the Mg(NO3)2.6H2O, 4,4′-sulfonyldibenzoic acid (H2SBA), ethanol (EtOH), and water (H2O) in the reactor) is heated to 150° C. with 60° Ch-1 and it is maintained at 150° C. for reacting for about 2 days. After, the reactor is cooled to room temperature with 6° Ch-1. And then, compound 1 is gotten through suction filtration, washing with ethanol and water, and drying. The compound 1 is a transparent acicular crystal. The weight of the gotten compound 1 is 0.072 g, and the yield of the compound 1 is 41.2% by calculating with defining the 4,41-sulfonyldibenzoic acid (H2SBA) as a limiting reagent. The weight of the Mg(NO3)2.6H2O, 4,4′-sulfonyldibenzoic acid (H2SBA), ethanol (EtOH), and water (H2O) mentioned above are just taken as an example, and not limited to this. The weight of the Mg(NO3)2.6H2O, 4,4′-sulfonyldibenzoic acid (H2SBA), ethanol (EtOH), and water (H2O) could be increased or decreased with the same ratio of weight mentioned above. |
41.21% | at 150℃; for 0.333333h; Autoclave; Microwave irradiation; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
88.4% | at 150℃; for 48h; High pressure; | Compound 5 also can be synthesized by hydrothermal method or microwave syntheses method. The hydrothermal method for synthesizing compound 5 is detailed as following: First, 0.118 g (0.4 mmol) Zn(NO3)2.6H2O, 0.0612 g (0.2 mmol) 4,4′-sulfonyldibenzoic acid (H2SBA), 5.0 mL ethanol (EtOH), and 1.0 mL water (H2O) are put into the Teflon inner cup in order. And then, the Teflon inner cup is put into the iron outer cup and the reactor is put into the high temperature furnace. In the high temperature furnace, the reactor (or the Zn(NO3)2.6H2O, 4,4′-sulfonyldibenzoic acid (H2SBA), ethanol (EtOH), and water (H2O) in the reactor) is heated to 150° C. with 60° Ch-1 and it is maintained at 150° C. for reacting for about 2 days. After, the reactor is cooled to room temperature with 6° Ch-1. And then, compound 5 is gotten through suction filtration, washing with ethanol and water, and drying. The compound 5 is a transparent acicular crystal. The weight of the gotten compound 5 is 0.0782 g, and the yield of the compound 5 is 88.4% by calculating with defining the 4,4′-sulfonyldibenzoic acid (H2SBA) as a limiting reagent. The weight of the Zn(NO3)2.6H2O, 4,4′-sulfonyldibenzoic acid (H2SBA), ethanol (EtOH), and water (H2O) mentioned above are just taken as an example, and not limited to this. The weight of the Zn(NO3)2.6H2O, 4,4′-sulfonyldibenzoic acid (H2SBA), ethanol (EtOH), and water (H2O) could be increased or decreased with the same ratio of weight mentioned above. |
88.41% | at 180℃; for 0.666667h; Autoclave; Microwave irradiation; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
44.5% | In ethanol at 120℃; for 48h; High pressure; | Compound 2 can be synthesized by hydrothermal method or microwave syntheses method. The hydrothermal method for synthesizing compound 2 is detailed as following: First, 0.0945 g (0.4 mmol) Ca(NO3)2.4H2O, 0.0612 g (0.2 mmol) 4,4′-sulfonyldibenzoic acid (H2SBA), 9.0 mL ethanol (EtOH), and 1.0 mL water (H2O) are put into the Teflon inner cup in order. And then, the Teflon inner cup is put into the iron outer cup and the reactor is put into the high temperature furnace. In the high temperature furnace, the reactor (or the Ca(NO3)2.4H2O, 4,4′-sulfonyldibenzoic acid (H2SBA), ethanol (EtOH), and water (H2O) in the reactor) is heated to 120° C. with 60°Ch-1 and it is maintained at 120° C. for reacting for about 2 days. After, the reactor is cooled to room temperature with 6° Ch-1. And then, compound 2 is gotten through suction filtration, washing with ethanol and water, and drying. The compound 2 is a transparent tabular crystal. The weight of the gotten compound 2 is 0.0323 g, and the yield of the compound 2 is 44.5% by calculating with defining the 4,4′-sulfonyldibenzoic acid (H2SBA) as a limiting reagent. The microwave syntheses method for synthesizing compound 2 is detailed as following: First, Ca(NO3)2.4H2O, 4,4′-sulfonyldibenzoic acid (H2SBA), ethanol (EtOH), and water (H2O) with the same weight (or weight ratio) as above mentioned are put into the Teflon inner cup in order. And then, the Teflon inner cup is put into the iron outer cup and the reactor is put into the microwave reactor. In the microwave reactor, the output power of the microwave reactor is set to 400 W, and the reactor (or the Ca(NO3)2.4H2O, 4,4′-sulfonyldibenzoic acid (H2SBA), ethanol (EtOH), and water (H2O) in the reactor) is heated to 150° C. with 60° Ch-1. It is maintained at 150° C. for reacting or synthesizing for 20 minutes. After, the reactor is cooled to room temperature with 6° Ch-1. And then, compound 2 is gotten through suction filtration, washing with ethanol and water, and drying. A compound is produced by heating compound 2 to 200° C. to remove water of crystallization from compound 2. According to powder X-ray diffraction analysis for this compound, it is found that the structures of this compound and compound 2 are almost the same and this compound has a formula [Ca(SBA)]. The weight of the Ca(NO3)2.4H2O, 4,4′-sulfonyldibenzoic acid (H2SBA), ethanol (EtOH), and water (H2O) mentioned above are just taken as an example, and not limited to this. The weight of the Ca(NO3)2.4H2O, 4,4′-sulfonyldibenzoic acid (H2SBA), ethanol (EtOH), and water (H2O) could be increased or decreased with the same ratio of weight mentioned above. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
75.3% | In ethanol at 150℃; for 48h; High pressure; | Compound 3 also can be synthesized by hydrothermal method or microwave syntheses method. The hydrothermal method for synthesizing compound 3 is detailed as following: First, 0.1692 g (0.8 mmol) Sr(NO3)2, 0.0612 g (0.2 mmol) 4,4′-sulfonyldibenzoic acid (H2SBA), 7.0 mL ethanol (EtOH), and 3.0 mL water (H2O) are put into the Teflon inner cup in order. And then, the Teflon inner cup is put into the iron outer cup and the reactor is put into the high temperature furnace. In the high temperature furnace, the reactor (or the Sr(NO3)2, 4,4′-sulfonyldibenzoic acid (H2SBA), ethanol (EtOH), and water (H2O) in the reactor) is heated to 150° C. with 60° Ch-1 and it is maintained at 150° C. for reacting for about 2 days. After, the reactor is cooled to room temperature with 6° Ch-1. And then, compound 3 is gotten through suction filtration, washing with ethanol and water, and drying. The compound 3 is a transparent fringe crystal (or columnar crystal). The weight of the gotten compound 3 is 0.0616 g, and the yield of the compound 3 is 75.3% by calculating with defining the 4,4′-sulfonyldibenzoic acid (H2SBA) as a limiting reagent. The microwave syntheses method for synthesizing compound 3 is detailed as following: First, Sr(NO3)2, 4,4′-sulfonyldibenzoic acid (H2SBA), ethanol (EtOH), and water (H2O) with the same weight (or weight ratio) as above mentioned are put into the Teflon inner cup in order. And then, the Teflon inner cup is put into the iron outer cup and the reactor is put into the microwave reactor. In the microwave reactor, the output power of the microwave reactor is set to 400 W, and the reactor (or the Sr(NO3)2, 4,4′-sulfonyldibenzoic acid (H2SBA), ethanol (EtOH), and water (H2O) in the reactor) is heated to 180° C. with 60° Ch-1. It is maintained at 180° C. for reacting or synthesizing for 20 minutes. After, the reactor is cooled to room temperature with 6° Ch-1. And then, compound 3 is gotten through suction filtration, washing with ethanol and water, and drying. A compound is produced by heating compound 3 to 200° C. to remove water of crystallization from compound 3. According to powder X-ray diffraction analysis for this compound, it is found that the structures of this compound and compound 3 are almost the same and this compound has a formula [Sr(SBA)]. The weight of the Sr(NO3)2, 4,4′-sulfonyldibenzoic acid (H2SBA), ethanol (EtOH), and water (H2O) mentioned above are just taken as an example, and not limited to this. The weight of the Sr(NO3)2, 4,4′-sulfonyldibenzoic acid (H2SBA), ethanol (EtOH), and water (H2O) could be increased or decreased with the same ratio of weight mentioned above. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
87.2% | In water at 150℃; for 48h; High pressure; | Compound 4 also can be synthesized by hydrothermal method or microwave syntheses method. The hydrothermal method for synthesizing compound 4 is detailed as following: First, 0.100 g (0.4 mmol) Mn(NO3)2.4H2O, 0.1224g (0.4 mmol) 4,4′-sulfonyldibenzoic acid (H2SBA), 5.0 mL ethanol (EtOH), and 1.0 mL water (H2O) are put into the Teflon inner cup in order. And then, the Teflon inner cup is put into the iron outer cup and the reactor is put into the high temperature furnace. In the high temperature furnace, the reactor (or the Mn(NO3)2.4H2O, 4,4′-sulfonyldibenzoic acid (H2SBA), ethanol (EtOH), and water (H2O) in the reactor) is heated to 150° C. with 60° Ch-1 and it is maintained at 150° C. for reacting for about 2 days. After, the reactor is cooled to room temperature with 6° Ch-1. And then, compound 4 is gotten through suction filtration, washing with ethanol and water, and drying. The compound 4 is a transparent acicular crystal. The weight of the gotten compound 4 is 0.0705 g, and the yield of the compound 4 is 87.2% by calculating with defining the 4,4′-sulfonyldibenzoic acid (H2SBA) as a limiting reagent. The weight of the Mn(NO3)2.4H2O, 4,4′-sulfonyldibenzoic acid (H2SBA), ethanol (EtOH), and water (H2O) mentioned above are just taken as an example, and not limited to this. The weight of the Mn(NO3)2.4H2O, 4,4′-sulfonyldibenzoic acid (H2SBA), ethanol (EtOH), and water (H2O) could be increased or decreased with the same ratio of weight mentioned above. |
In water at 180℃; for 0.333333h; Autoclave; Microwave irradiation; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
56% | In N,N-dimethyl-formamide at 100℃; for 48h; Sealed tube; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
68% | at 100℃; for 48h; Sealed tube; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
75% | In N,N-dimethyl-formamide at 100℃; for 48h; Sealed tube; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
66% | With sodium hydroxide In methanol; water at 120℃; for 48h; Autoclave; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
64% | With sodium hydroxide In methanol; water at 120℃; for 48h; Autoclave; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
58% | at 95℃; for 72h; High pressure; | A mixture of MnCl2·4H2O (19.8mg, 0.1mmol), sdb (30.4mg, 0.1mmol), and BIBP (28.8mg, 0.1mmol) was dissolved in 2mL of distilled water and 6mL of DMF. The final mixture was sealed in a 15mL Parr Teflon-lined stainless-steel vessel and heated at 95°C for 3days, and then the reaction system was cooled to room temperature. Colorless diamond bulk crystals of 1 were obtained, washed with water, and dried under ambient conditions (yields: 58% for 1 based on BIBP). Elemental analysis (%) calcd for (C70H62Mn3N12O20S2): C, 51.89; H, 3.86; N, 10.37. Found: C, 51.84; H, 3.82; N, 10.33. IR (KBr, cm-1): 1656(w),1634(w), 1597(vs), 1511(s), 1395(vs), 1324(m), 1161(m), 1100(m), 838(m), 738(s), 617(m). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
52% | In water at 180℃; for 72h; High pressure; | Synthesis of the complex Zn2(OH)(SDBA)(PTZ) (1) The single crystals of complex 1 were prepared by in situ hydrothermal reaction. A mixture containing Zn(NO3)2*6H2O (59.2 mg, 0.2 mmol), 4-cyanopyridine (10.4 mg, 0.1 mmol), H2SDBA (30.6 mg, 0.1 mmol) and NaN3 (13.2 mg, 0.2 mmol) in 15 mL deionized water was sealed in a 25 mL Teflonlined stainless steel container and heated at 180 °C for 72 h under the autogenous pressure. After the mixture was slowly cooled to room temperature, colorless block crystals suitable for X-ray analysis were obtained directly, which were washed with deionized water and ethanol several times, and dried in air, 31.1 mg, yield 52% based on 4-cyanopyridine. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
58% | In water at 160℃; for 72h; High pressure; | 2.2.3. Synthesis of [Cd(p-phda)(btmx)(H2O)]H2O}n (3) General procedure: A mixture of Cd(NO3)2*4H2O (30.8 mg, 0.1 mmol), btmx (29.8 mg, 0.1 mmol), and p-H2phda (19.4 mg, 0.1 mmol) in 10 mL distilled H2O was sealed in a 25 mL Teflon-lined stainless steel container and heated at 160 °C for 3 days. After the mixture was cooled to room temperature at a rate of 5 °C/h, colorless crystals of 3 were obtained, yield 63% based on Cd. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
42% | In methanol; water at 124.84℃; for 50h; Autoclave; | Synthesis of [Zn2 (SDB)2 (BITMB)]·(THF)2}n (CP3) H2SDB (75 mg, 0.36 mmol), BITMB (70 mg, 0.25 mmol) and Zn(NO3)2·6H2O (100 mg, 0.33 mmol) were dispersed in 12 mL mixed solvent (5 mL water, 5 mL THF and 2 mL methanol) and then sealed in a 23 mL Teflon-lined autoclave, which was heated at 398 K for 50 h. Yield=42%. Elemental analysis (%), Cal.: C, 54.69; H, 4.50; N, 4.81; S, 5.51; found: C, 54.32; H, 4.65; N, 4.68; IR cm-1 (KBr): 3435 (br), 3142 (w), 2924 (w), 2366 (w), 1657 (s), 1562 (w), 1406 (s), 1293 (w), 1223 (w), 1163 (m), 1098 (m), 1014 (w), 870 (w), 740 (s), 619 (w). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
36% | In water at 124.84℃; for 60h; Autoclave; | Synthesis of [Co2(SDB)2(BITMB)]·(dioxane)3}n (CP4) H2SDB (75 mg, 0.36 mmol), BITMB (90 mg, 0.32 mmol) and Co(NO3)2·6H2O (154 mg, 0.52 mmol) were dispersed in a mixture of 3 mL water and 3 mL 1,4-dioxane and then sealed in a 14 mL Teflon-lined autoclave, which was heated at 398 K for 60 h. Yield=36%. Elemental analysis (%), Cal.: C, 53.86; H, 4.76; N, 4.41; S, 5.05; found: C, 53.68; H, 5.02; N, 4.32; IR cm-1 (KBr): 3425 (br), 3105 (w), 2956 (w), 2850 (w), 2375 (w), 1640 (s), 1562 (w), 1406 (s), 1293 (m), 1163 (m), 1112 (s), 1014 (w), 870 (m), 735 (s), 620 (w). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
45% | In 1,4-dioxane; methanol; water at 124.84℃; for 50h; Autoclave; | Synthesis of [Ni(SDB)(BITMB)(H2O)]·H2O}n (CP1) H2SDB (70 mg, 0.33 mmol), BITMB (75 mg, 0.26 mmol) and Ni(NO3)2·6H2O (100 mg, 0.34 mmol) were dispersed in 10 mL mixed solvent (3 mL water, 3 mL methanol and 4 mL 1,4-dioxane) and then sealed in a 23 mL Teflon-lined autoclave, which was heated at 398 K for 50 h. Yield=45%. Elemental analysis (%), Cal.: C, 54.81; H, 4.75; N, 8.25; S, 4.72; found: C, 54.27; H, 4.87; N, 8.12. IR cm-1 (KBr): 3435 (br), 2924 (w), 2362 (w), 1616 (s), 1563 (m), 1394 (s), 1298 (m), 1228 (w), 1164 (m), 1103 (m), 1020 (m), 829 (w), 740 (s), 689 (w), 620 (m). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
67% | In water at 124.84℃; for 98h; Autoclave; | Synthesis of [{Cd(SDB)(BITMB)(H2O)}·(THF)·H2O]n (CP2) H2SDB (60 mg, 0.29 mmol), BITMB (100 mg, 0.35 mmol) and Cd(NO3)2·4H2O (300 mg, 0.97 mmol) were dispersed in 10 mL water/tetrahydrofuran (1:1) and then sealed in a 23 mL Teflon-lined autoclave, which was heated at 398 K for 98 h. Yield=67%. Elemental analysis (%) Cal.: C, 52.21; H, 5.01; N, 6.96; S, 3.98; found: C, 52.48; H, 5.35; N, 6.74; IR cm-1 (KBr): 3412 (br), 3123 (w), 2961 (w), 2367 (w), 1595 (m), 1553 (s), 1398 (s), 1293 (m), 1223 (w), 1158 (w), 1089 (w), 1019 (w), 856 (w), 745 (s), 619 (m). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
51.1% | With sodium hydroxide at 180℃; for 72h; High pressure; | 2.3.4. Synthesisof[Zn2(344-pytpy)2(sfdb)2]n .1.5n(H2O) (4) This compoundwaspreparedinasimilarprocedureas 2, byusing H2sfdb (0.0300g,0.1mmol)inplaceofH2oxandadjustthepH valueofthemixtureto6.0.Thecolorlesscrystalsof 4 wereobtained, washedwithdistilledwater(5mL),anddriedinairtogive0.0709g(yield51.1%basedonZn).Anal.calcd.(%)forC68H47N8O13.5S2Zn2: C,58.88;H,3.42;N,8.08.found:C,58.66;H,3.58;N, 8.68.IR(KBr,cm1): 3588(m),3393(w),3078(s),1608(m)1547(m),1491(s),1408(w),1326(s),1300(s),1169(s),1137(s),1102(s),1069(s),1017(s),866(s),823(w),780(s),739(m),694 (s),583(s),505(m). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
66% | With sodium hydroxide In dimethyl sulfoxide at 120℃; for 48h; Sealed tube; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
78% | With sodium hydroxide In dimethyl sulfoxide at 120℃; for 48h; Sealed tube; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
83% | With sodium hydroxide In dimethyl sulfoxide at 130℃; for 48h; Sealed tube; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
47% | With sodium hydroxide In water at 160℃; for 72h; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
63% | With formic acid In methanol at 110℃; for 72h; Autoclave; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
98% | Stage #1: aluminium(III) chloride hexahydrate; bis(4-carboxyphenyl)sulfone With sodium hydroxide In water at 150℃; for 12h; Autoclave; Stage #2: N,N-dimethyl-formamide at 150℃; for 1h; Microwave irradiation; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
62% | In ethanol at 74.84℃; for 72h; High pressure; | Solvothermal synthesis of I. A reaction mixture of Gd(NO3)3*6H2O (0.015 g, 0.033 mmol), H2Sfdb (0.010 g, 0.033 mmol), DMF (1 mL) and C2H5OH (0.5mL) was stirred for 20 min in air to form a solution, the solution was placed in vial (5 mL), then the vial was sealed and heated at 348 K for three days, followed by slow cooling (5 K/h). The colorless block crystals were washed with DMF and dried in air (the yield was ~62%). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
56% | With sodium carbonate; In water; at 140℃; for 72h; | A mixture of Ni(NO3)2·6H2O(29.1 mg, 0.1 mmol), H2E1 (30.4 mg, 0.1 mmol), Na2CO3 (10.6 mg, 0.1 mmol), and pbtx (24.0 mg, 0.1 mmol) was dissolved in 10 mL of distilled water. The final mixture was sealed in a 15 mL Parr Teflon-lined stainless-steel vessel and heated at 140 C for three days, and then the reaction system was cooled to room temperature. Green crystals were obtained in 56% (35.8 mg) yield (based on Ni). Elemental analysis (EA) (%) Calcd for(C26H24N6Ni1O8S1): C, 48.84; N, 13.14; H, 3.75. Found: C, 48.77; N, 13.25; H, 3.61.FT-IR(KBr, cm-1): 3379(br), 3114(w), 1601(m), 1550(m), 1396(s), 1280(m), 1166(m),1010(m), 866(w), 744(s), 677(m), 616(m), 488(w). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
56% | With sodium carbonate; In water; at 140℃; for 72h; | A mixture of Co(NO3)2·6H2O (29.1 mg, 0.1 mmol), H2E1 (30.4 mg, 0.1 mmol), Na2CO3 (10.6 mg, 0.1 mmol), and pbtx (24.0 mg, 0.1 mmol) was dissolved in 10 mL of distilled water. The final mixture was sealed in a 15 mL Parr Teflon-lined stainless-steel vessel and heated at 140 C for three days, and then the reaction system was cooled to room temperature. Purple crystals were obtained in 56% (36.1 mg) yield (based on Co). EA (%) Calcd for (C26H24N6Co1O8S1): C,48.83; N, 13.14; H, 4.07. Found: C, 48.93; N, 13.27; H, 3.98. FT-IR(KBr, cm-1): 3449(br),3148(w), 1595(m), 1544(m), 1393(s), 1278(m), 1166(m), 1018(w), 857(w), 748(s), 677(w),615(w), 490(w). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
78% | In water at 150℃; for 96h; | 2.2.2. Synthesis of [Cd(bmimx)(bdc)H2O]n (2) General procedure: A mixture of Cd(Ac)2*2H2O (26.7 mg, 0.1 mmol), bmimx (32.3 mg, 0.1 mmol) and H2bdc (16.6 mg, 0.1 mmol) in 10 mL distilled H2O was kept in a 25 mL Teflon-lined stainless steel vessel at 150 °C for four days. After the mixture was cooled to room temperature at a rate of 5 °C/h, colorless crystals of 2 were obtained in a yield of 65% (based on Cd). |
Yield | Reaction Conditions | Operation in experiment |
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32% | With sodium hydrogencarbonate; In water; at 160℃; for 72h;Autoclave; | A mixture of Cd(NO3)26H2O (0.030 g, 0.1 mmol), 4,40-H2sdb(0.025 g, 0.1 mmol), NaHCO3 (0.016 g, 0.2 mmol) and H2O (10 mL)was placed in a 23 mL Teflon-lined stainless steel reactor underautogenous pressure at 160 C for 72 h and then cooled to roomtemperature slowly. Colorless block crystals were obtained in 32%yield based on Cd(NO3)24H2O. Anal. calcd. for C50H40Cd2N10O15S2(1309.86): C, 45.81; H, 3.05; N, 10.69%. Found: C, 45.87; H, 3.12; N,10.62%. IR (cm1): 3422(w), 1712(m), 1675(s), 1587(m), 1509(m),1389(m), 1378(m), 1109(w), 1025(w), 958(m), 893(m), 826(m),778(w), 690(w), 674(w), 589(w), 562(w). |
Yield | Reaction Conditions | Operation in experiment |
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56% | In water at 130℃; for 72h; High pressure; Autoclave; | Synthesis of {Eu2(SDB)3(H2O)5}n A mixture of Eu(NO3)3·6H2O (222.982 mg, 0.5 mmol), 4,4-sulfonyldibenzoic acid (H2SDB) (153.145 mg, 0.5 mmol), and deionized water (6 mL) was placed in a 23 mL Teflon-lined stainless steel vessel. The mixture was sealed and heated at 130 °C for three days, and then cooled to room temperature at a rate of 5 °C/h. Yellow block-shaped crystals suitable for X-ray analysis were obtained in 56% yield (based on H2SDB). Anal found/Calcd for C42H34S3Eu2O23: C, 38.55; H, 2.65% (calculated: C, 38.59; H, 2.60%). IR (KBr,cm-1): 3433(m), 2364(m), 1435(m), 1408(s), 1377(s), 1300(s), 1098(s), 1019(w), 850(w),777(w), 736(s), 687(w), 613(m), 576(w). |
Yield | Reaction Conditions | Operation in experiment |
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36% | In water at 130℃; for 72h; High pressure; Autoclave; | Synthesis of {Dy2(SDB)3(H2O)5}n The process was the same as 1 except that Eu(NO3)3·6H2O was replaced by Dy(NO3)3·6H2O (228.5 mg, 0.5 mmol). Yellow block-shaped crystals suitable for X-ray analysis were obtained in 36% yield (based on H2SDB). Anal found/Calcd for C42H34S3Dy2O23: C, 37.95;H, 2.53% (calculated: C, 37.98; H, 2.56%). IR (KBr, cm-1): 3439(w), 2343(w), 1653(2),1592(s), 1419(s), 1300(m), 1166(m), 1099(m), 862(w), 736(s), 613(m). |
Yield | Reaction Conditions | Operation in experiment |
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64% | In water at 130℃; for 72h; High pressure; Autoclave; | Synthesis of {Gd2(SDB)3(H2O)5}n The process was the same as 1 except that the Eu(NO3)3·6H2O was replaced by Gd(NO3)3·6H2O (225.5 mg, 0.5 mmol). Yellow block-shaped crystals suitable for X-ray analysis were obtained in 64% yield (based on H2SDB). Anal found/Calcd for C42H34S3Gd2O23: C, 38.33; H, 2.61 (calculated: C, 38.28; H, 2.58%). IR (KBr, cm-1): 3427(w), 2924(w),2854(w), 2363(m), 1928(w), 1695(w), 1616(w), 1535(m), 1419(s), 1301(m), 1164(m), 1100(m), 933(w), 860(w), 736(s), 612(m). |
Yield | Reaction Conditions | Operation in experiment |
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71% | In water at 130℃; for 72h; High pressure; Autoclave; | Synthesis of {Tb2(SDB)3(H2O)5}n The process was the same as 1 except that the Eu(NO3)3·6H2O was replaced by Tb(NO3)3·6H2O (226.5 mg, 0.5 mmol). White block-shaped crystals suitable for X-ray analysis were obtained in 71% yield (based on H2SDB). Anal found/Calcd for C42H34S3Tb2O23: C, 38.15; H, 2.55% (calculated: C, 38.19; H, 2.58%). IR (KBr, cm-1): 3435(m), 2976(m),2364(s), 1815(m), 1594(m), 1408(s), 1298(w), 1161(s), 1093(m), 861(w), 740(m), 613(m). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
63% | In water at 130℃; for 72h; High pressure; Autoclave; | Synthesis of [Ho2(SDB)3(H2O)4]·H2O}n The process was the same as 1 except that Eu(NO3)3·6H2O was replaced by Ho(NO3)3·6H2O (228.5 mg, 0.5 mmol). Yellow block-shaped crystals suitable for X-rayanalysis were obtained in 63% yield (based on H2SDB). Anal found/Calcd for C42H34S3Ho2O23: C, 37.86; H, 2.58% (calculated: C, 37.84; H, 2.55%). IR (KBr, cm-1): 3425(w), 2364(w), 1624(m), 1535(m), 1419(s), 1300(s), 1168(s), 1099(s), 736(s), 1014(w),866(w), 736(s), 613(s). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
59% | In water at 130℃; for 72h; High pressure; Autoclave; | Synthesis of [Er2(SDB)3(H2O)4]·H2O}n The process was the same as 1 except that Eu(NO3)3·6H2O was replaced by Er(NO3)3·6H2O (230.5 mg, 0.5 mmol). Yellow block-shaped crystals suitable for X-ray analysis were obtained in 59% yield (based on H2SDB). Anal found/Calcd for C42H34S3Er2O23: C, 37.74; H, 2.56% (calculated: C, 37.71; H, 2.54%). IR (KBr, cm-1): 3435(w), 2971(w), 2364(m), 1625(m), 1535(m), 1419(s), 1298(m), 1168(m), 1098(w), 1014(w), 867(w), 740(m), 984(w). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
72% | In water at 130℃; for 72h; High pressure; Autoclave; | Synthesis of [Tm2(SDB)3(H2O)4]·H2O}n The process was the same as 1 except that Eu(NO3)3·6H2O was replaced by Tm(NO3)3·6H2O (231.5 mg, 0.5 mmol). Yellow block-shaped crystals suitable for X-ray analysis were obtained in 72% yield (based on H2SDB). Anal found/Calcd for C42H34S3Tm2O23: C, 37.60; H, 2.50% (calculated: C, 37.62; H, 2.54%). IR (KBr, cm-1): 3435(w), 2976(m), 1625(m), 1531(s), 1415(s), 1298(s), 1167(s), 1098(s), 1051(s), 877(s),736(s), 613(s). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
66% | In water at 130℃; for 72h; High pressure; Autoclave; | Synthesis of [Y2(SDB)3(H2O)4]·H2O}n The process was the same as 1 except that Eu(NO3)3·6H2O was replaced by Y(NO3)3·6H2O (191.5 mg, 0.5 mmol). White block-shaped crystals suitable for X-ray analysis were obtained in 66% yield (based on H2SDB). Anal found/Calcd for C42H34S3Y2O23: C, 42.69;H, 2.85% (calculated: C, 42.72; H, 2.88%). IR (KBr, cm-1): 3430(w), 2364(w), 1624(m),1531(m), 1419(s), 1300(m), 1168(m), 1099(m), 1014(w), 866(w), 736(m), 613(w). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
78% | In water at 130℃; for 72h; High pressure; Autoclave; | Synthesis of [Lu2(SDB)3·(H2O)3]·4H2O}n The process was the same as 1 except that Eu(NO3)3·6H2O was replaced by Lu(NO3)3·6H2O (234.5 mg, 0.5 mmol). Yellow block-shaped crystals suitable for X-ray analysis were obtained in 78% yield (based on H2SDB). Anal found/Calcd for C42H38S3Lu2O25: C, 36.34; H, 2.76% (calculated: C, 36.31; H, 2.74%). IR (KBr, cm-1): 3433(m), 2971(w), 2364(w), 1612(s), 1562(m), 1419(s), 1296(m), 1165(s), 1098(m), 1014(m), 871(m), 782(m), 734(s), 692(m), 608(m). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
11.2% | With potassium hydroxide at 160℃; for 72h; Autoclave; | Synthesis of [Ni(BTX)(SDBA)(H2O)]0.29H2O}n' A mixture of Ni(NO3)2*6H2O (29.1 mg, 0.1 mmol), H2SDBA (30.7 mg, 0.1 mmol), BTX (48.1 mg, 0.2 mmol), and KOH (11.2 mg, 0.2 mmol) in H2O (10 ml) was sealed in a 16 ml Teflon-lined stainless steel container and heated at 160°C for 72 h. After cooling to room temperature, green block crystals ofthe title complex were collected by filtration and washed several times with water and ethanol (yield 11.2%, based on H2SDBA). Elemental analysis for C26H22.58N6NiO7.29S (Mr = 626.46) (%): C 49.85, H 3.63, N 13.41; found (%): 49.95,H 3.65, N 13.44. Selected IR peaks (cm-1): 3412 (m), 1601 (s), 1478 (s), 1225 (s) , 812(w), 779 (w), 721 (w). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
95% | With pyridine; triphenylphosphine In 1-methyl-pyrrolidin-2-one at 120℃; for 3h; |
Yield | Reaction Conditions | Operation in experiment |
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87% | With pyridine; triphenylphosphine In 1-methyl-pyrrolidin-2-one at 120℃; for 3h; |
Yield | Reaction Conditions | Operation in experiment |
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59% | In water; N,N-dimethyl-formamide at 130℃; for 72h; High pressure; Autoclave; | EXPERIMENTAL A mixture of 4,4'-bis(benzimidazole-1-ylmethyl)biphenyl (bbmb), 4,4'-dicarboxyldiphenyl sulfone (dcps) and Zn(NO3)2·6H2O (a molar ratio of 1:1:1) and the solvent of H2O/DMF(3:1, v/v, 4 mL) was sealed in a 20 mL PTFE-lined stainlesssteelvessel under autogenous pressure and heated at 130 °Cfor 72h. Large quantities of colourless block crystals wereobtained and crystals were filtered off, washed with distilledwater and dried under ambient conditions. The yield of thereaction was about 59 % based on Zn. IR: (KBr pellet, cm-1):3410w, 3031w, 1648s, 1564m, 1498m, 1399s, 1296w, 1950w,1160s, 1097m, 1009m, 926m, 850m, 740s, 692w, 619m,577m, 497m. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
50% | With calcium chloride In ethanol at 179.84℃; for 96h; | |
50% | With calcium chloride In ethanol at 180℃; for 120h; | 2 This Example provides specific examples of MCPNs for use in various embodiments and methods of their synthesis. In some embodiments, the MCPN may be a calcium coordination polymer network. One specific, non-limiting example of a calcium coordination polymer network that may be used is [Ca(4,4′-sulfonyldibenzoate)].H2O. The synthesis and structural properties of [Ca(4,4′-sulfonyldibenzoate)].H2O are described in “A Calcium Coordination Framework Having Permanent Porosity and High CO2/N2 Selectivity,” Banerjee et al., Crystal Growth and Design, 2012, 2162-2165, which is incorporated herein by reference in its entirety. Briefly, in one specific example, [Ca(4,4′-sulfonyldibenzoate)].H2O was synthesized according to the following protocol: a mixture of 0.0006 moles of CaCl2 (0.074 g) and 0.0006 moles of 4,4′-SDB (0.198 gram) were dissolved in 10.05 gram of ethanol and stirred for 2 hours to achieve homogeneity [molar ratio of metal chloride:ligand:solvent=1:1:380]. The resultant solution was heated at 180° C. for 5 days. Colorless needle shaped crystals were recovered as products and washed with and ethanol (Yield: 50% based on calcium in anhydrous CaCl2, 0.112 gram). The water in the final product was derived from the 95% ethanol solvent and adsorbed moisture in the CaCl2 reactant. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
77% | In N,N-dimethyl-formamide at 90℃; for 72h; Autoclave; | 4.2 Syntheses of [Cd2(DPDBT)2(DCPS)2(H2O)](H2O)}n (1) A mixture of Co(NO3)2 · 6H2O (58.2 mg, 0.2 mmol), DPDBT (67.6 mg, 0.2 mmol), and 4,4′-dicarboxydiphenyl sulfone (60.12 mg, 0.20 mmol) was dissolved in 15 mL of DMF-H2O (v/v, 1:1). The final mixture was placed in a Parr Teflon-lined stainless steel vessel (25 mL) under autogenous pressure and heated at 90 °C for 3 days. Red crystals of 1 were collectedin 77 % yield based on DPDBT ligand. - Co2C72H48N4O14S4: calcd. C 60.08, H 3.36, N 3.89; found: C 59.97, H 3.43, N 3.81. - IR (KBr, cm-1): 3429 (s), 1672 (s), 1612 (s), 1556 (s), 1470 (m), 1399 (s), 1324 (m), 1295 (s), 1226 (w), 1162 (s), 1136 (w), 1098 (s), 1070 (w), 1014 (w), 839 (w), 807 (s), 780 (w), 742 (s), 720 (w), 697 (w), 621 (s), 580 (s), 464 (w). |
Yield | Reaction Conditions | Operation in experiment |
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42% | With sodium hydrogencarbonate In water at 150℃; for 60h; Autoclave; High pressure; | Synthesis of [Zn(4,40-sdb)(HPPA)]n (1) A mixture of Zn(NO3)2*6H2O (0.06 g, 0.2 mmol), 4,4'-H2sdb (0.061 g, 0.2 mmol), HPPA (0.061 g, 0.2 mmol), NaHCO3 (0.026 g, 0.6 mmol) and H2O (12 ml) was sealed in an 23 ml Teflone lined stainless steel reactor under autogenous pressure at 150 °C for 60 h, and then cooled to room temperature, giving rise the colorless block crystals (Yield: 42% based on Zn(NO3)2*6H2O). Elemental Anal. Calcd. (%) for C28H24N5O9SZn (671.97): C, 50.00; H, 3.57; N,10.42. Found: C, 49.95; H, 3.62; N, 10.46. IR (cm-1, KBr pellet): 3272(w),1612 (s),1443 (m),1352 (m),1271 (s),1147 (m),1021 (s), 964 (s),859 (s), 758 (m), 644 (m). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With nitric acid In ethanol at 150℃; for 72h; Autoclave; | 1 Example 1 In accordanceMetal-organic composite of skeleton structure 1 Metal according to the first embodiment of the present invention in order to manufacture the organic skeletal structure 1, Ba (NO3) 2 0.261g (1.0 mmol), 4,4'- sulfonyl nildayi acid (4,4'-sulfonyldibenzoic acid, H2SBA) 0.307g (1.0mmol), nitric acid (HNO3) were mixed with 0.1mL, 2mL of ethanol, and N, N- dimethylformamide (N, N-dimethylformamide, DMF) 7mL. 4,4 nildayi sulfonic acid (H2SBA) isWere purchased from Sigma-Aldrich Corporation (St. Louis, MO, USA), barium nitrate (Ba (NO3) 2), DMF, ethanol, and HNO3 has been provided from Samchun Chemicals (Korea). All chemical reagents and solvents were used without further purification.The reaction mixture 23mL teflon-lined stainless steel after moving to the autoclave (Teflon-lined stainless steel autoclaves), autoclave was sealed and heated for 3 days at a temperature of 150 .Then, 6 ( 6 h-1) for one hourIt cooled to room temperature uisok road, which was open to the autoclave. Finally, the product was recovered by filtration and washing with DMFW, a metal according to the first embodiment of the present invention the organic skeletal structure 1 (hereinafter, structure 1) was prepared |
Yield | Reaction Conditions | Operation in experiment |
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77% | With sodium hydroxide at 120℃; for 48h; Autoclave; | 2.3.1 Preparation of [Zn(L1)(oba)]·2H2O}n (1) General procedure: ZnBr2 (0.045g, 0.2mmol), H2oba (0.052g, 0.20mmol and L1 (0.060g, 0.20mmol) were placed in a Teflon-lined digestion bomb (internal volume of 23mL) containing 10ml 0.04M NaOH under autogenous pressure. The reaction mixture was then heated at 120°C for 2days, followed by slow cooling at a rate of 6°Ch-1 to room T. The colorless crystals were then collected, washed with H2O and then dried under vacuum. Yield: 0.061g (46%). |
Yield | Reaction Conditions | Operation in experiment |
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67% | With dapsone at 65℃; for 96h; Autoclave; | 2.1.1 Synthesis of [Cd(OBA)(μ-H2O)(H2O)]n, 1 General procedure: Cd(NO3)2·4H2O (0.154g, 0.50mmol), H2OBA (0.102g, 0.40mmol) and 4-Aminophenyl sulfone (0.100g, 0.40mmol) were mixed in 6mL of DMF and 3mL of H2O. The mixture was homogenized for 30min at room temperature, transferred into a 23mL PTFE lined stainless steel autoclave, sealed and heated at 65°C for 4 days under autogenous pressure. The final product contained large quantities of colorless block shaped crystals, which were filtered under vacuum, washed with deionized water and dried under ambient conditions. |
Yield | Reaction Conditions | Operation in experiment |
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67% | In water; N,N-dimethyl-formamide at 95℃; for 72h; Autoclave; High pressure; | Syntheses of complexes [Cd2(DPDBT)2(DCPS)2(H2O)](H2O)}n (1) A mixture of Cd(NO3)26H2O (30.1mg, 0.1mmol), DPDBT (33.8mg, 0.1mmol) and 4,4′-dicarboxydiphenyl sulfone (30.6mg, 0.10mmol) was dissolved in 15mL of DMF/H2O (V/V, 1/1). The final mixture was placed in a Parr Teflon-lined stainless steel vessel (25mL) under autogenous pressure and heated at 95°C for 3d. Pale yellow crystals of 1 were collected in 67% yield (based on DPDBT ligand). Calcd for Cd2C72H48N4O14S4: C, 55.93%; H, 3.13%; N, 3.62%. Found: C, 55.90%; H, 3.18%; N, 3.61%. IR(KBr, cm-1): 3419 (s), 2962 (m), 2362 (w), 1594 (s), 1468 (m), 1396 (s), 1354 (s), 1286 (m), 1220 (w), 1165 (w), 1072 (w), 1036 (m), 1014 (w), 839 (m), 803 (s), 772 (w), 674 (w), 568 (w), 544 (w), 470 (w), 447 (w). |
Yield | Reaction Conditions | Operation in experiment |
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48% | With sodium hydroxide In water at 160℃; for 96h; | 4 2.4. [Ni2(sdc)2(ibpi)2(H2O)2]H2O (4) A mixture of Ni(NO3)26H2O (0.0298 g, 0.1 mmol), H2sdc(0.0306 g, 0.1 mmol), ibpi (0.0316 g, 0.1 mmol), 0.1 molL1 NaOH(2 ml) and H2O (8 ml) was placed in a Teflon reactor (20 ml) andheated at 160 C for 4 days. After gradually cooled to room temperatureat a rate of 10 Ch1, green crystals of 4 were obtained with48% yield based on ibpi. Anal. Calcd for C66H54N8Ni2O17S2: C, 56.11;H, 3.85; N, 7.93. Found: C, 56.20; H, 3.74; N, 7.99. IR (KBr, cm1):3125 (s), 1592 (m), 1520 (s), 1417 (s), 1385 (s), 1294 (m), 1268(m), 1229 (m), 1159 (s), 1133 (m), 1100 (m), 1061 (m), 1010 (m),964 (m), 938 (m), 861 (m), 828 (m), 784 (m), |
Yield | Reaction Conditions | Operation in experiment |
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56% | In water; N,N-dimethyl-formamide at 100℃; for 48h; | 2.2. Synthesis of [Cd(sdc)(ibpi)]*H2O (2) General procedure: A mixture of Cd(NO3)24H2O (0.0308 g, 0.1 mmol), H2cba(0.0270 g, 0.1 mmol), ibpi (0.0316 g, 0.1 mmol), DMF (8 ml) andH2O (2 ml) was placed in a Teflon reactor (20 ml) and heated at100 C for 2 days. After gradually cooled to room temperature, colorless crystals of 1 were obtained with 54% yield based on ibpi |
Yield | Reaction Conditions | Operation in experiment |
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88% | With ammonium nitrate In methanol at 160℃; for 4h; Autoclave; High pressure; |
Yield | Reaction Conditions | Operation in experiment |
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35.6% | In N,N-dimethyl-formamide at 100℃; for 72h; | Preparation of [Zn(SDBA)(1,3-BMIB)H2O]n (1) A mixture of 1,3-BMIB (11.9 mg, 0.05 mmol), H2SDBA (15.3 mg,0.05 mmol), Zn(NO3)2*6H2O (14.9 mg, 0.05 mmol), DMF (l.5 mL)and H2O (0.5 mL) was placed in a Teflon-lined stainless steel vessel,heated to 100 C for 3 days, and then cooled to 40 C over 12 h.Transparent crystals of 1 were obtained. Yield: 35.6% based on Zn(NO3)2*6H2O. Elemental analysis (%) calcd for C56H48N8O14S2Zn2:C, 53.72; H, 3.86; N, 8.95. Found: C, 53.74; H, 3.86; N, 8.97. IR(cm1): 3459 m, 3116 m, 1634 s, 1505 s, 1354 s, 1158 s, 1099 s,1011 m, 869 w, 842 w, 744 s, 688 m, 624 m, 571 m, 465 m. |
Yield | Reaction Conditions | Operation in experiment |
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43% | In N,N-dimethyl-formamide at 95℃; for 72h; Sealed tube; | General procedure for the preparation of [Cd(L1)(sdb)]·H2O}n 1 A mixture of Cd(NO3)2·4H2O (30.8 mg, 0.1 mmol), L1 (31.8 mg,0.1 mmol), and 4,4'-H2sdb (30.6 mg, 0.1 mmol) was dissolved in 6 ml ofdistilled water and 3 ml of DMF. The final mixture was sealed in a 15 mlParr Teflon-lined stainless-steel vessel and heated at 95°C for threedays and then cooled to room temperature. Colorless block crystals of 1obtained were washed with water and dried under ambient conditions.Yield 43% for 1 based on L1. Found (%): C, 61.62; H, 3.66; N, 3.37.Calc. for C42H30CdN2O7S (%): C, 61.58; H, 3.69; N, 3.41. |
Yield | Reaction Conditions | Operation in experiment |
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85% | With nitric acid at 150℃; for 288h; Sealed tube; | 2 Example 2 0.10 mmol of 2,5-bis (4-pyridyl) pyrimidine ligand and 0.10 mmol of 4,4'-sulfonyl dibenzoic acid ligand were mixed, And then with 0.20-0.30mmol of Cd (CH3COOH) 2 · 2H2O together into a small glass bottle, 3.0 ml of N, N'-dimethylformamide organic solvent and 2.0 ml of ionized water were added, Dropping 6 drops of nitric acid solution, Measured the pH of 6, At this point the solution is clear. The sealed vials were placed in a blast oven and heated to 150 ° C, Constant temperature heating time of 12 days, And then reduced to room temperature at a rate of 10 ° C / At this point a small glass bottle with colorless rod-like crystal precipitation, Then washed with DMF solution, To obtain pure colorless crystals, Yield: 85%. |
Yield | Reaction Conditions | Operation in experiment |
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80% | With sodium hydroxide In water; dimethyl sulfoxide at 20 - 120℃; for 56h; |
Yield | Reaction Conditions | Operation in experiment |
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70% | With sodium hydroxide In water; dimethyl sulfoxide; N,N-dimethyl-formamide at 20 - 120℃; for 56h; Sealed tube; |
Yield | Reaction Conditions | Operation in experiment |
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40% | at 160℃; for 72h; High pressure; | 2.5 Synthesis of [Zn(sdc)(bmis)]2·3H2O (5) A mixture of Zn(OAc)2·2H2O (0.0220g, 0.1mmol), H2sdc (0.0306g, 0.1mmol), bmis (0.0378g, 0.1mmol) and H2O (6ml) was placed in a Teflon reactor (20ml) and heated at 160°C for 3days. After gradually cooled to room temperature at a rate of 10°C·h-1, colorless crystals of 5 were obtained with 40% yield based on bmis. Anal. Calcd for C68H58N8O19S4Zn2: C, 52.69; H, 3.77; N, 7.23. Found: C, 52.77; H, 3.88; N, 7.20. IR (KBr, cm-1): 3138 (m), 2258 (w), 1643 (s), 1592 (m), 1573 (m), 1508 (s), 1359 (s), 1301 (s), 1159 (s), 1107 (s), 1010 (m), 874 (m), 835 (m), 770 (s), 738 (s), 693 (m), 615 (s), 576 (m), 472 (s) |
Yield | Reaction Conditions | Operation in experiment |
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58% | In water at 160℃; for 72h; Autoclave; High pressure; | 2.2. Synthesis of [M2((μ3-OH)(trz)(sdba)(H2O)]·3H2O}∞ (M = Ni for1, Zn for 2) For 1, a mixture of Ni(NO3)2·6H2O (0.3 mmol, 87 mg), Htrz(0.3 mmol, 21 mg), H2sdba (0.1 mmol, 31 mg) and NaOH (5.2 mL,0.1 mol/L) in deionized water (3 mL) was sealed in a Teflon reactor autoclave and heated to 160 °C for 3 days. After the autoclave was cooled to room temperature, green block crystals suitable for single crystal X-ray crystallographic analysis were obtained. Yield: 58% based on Ni(II). Anal. Calc. for C16H19N3O11SNi2 (578.82): C, 33.20; H, 3.31;N, 7.26%. Found: C, 33.16; H, 3.35; N, 7.31%. IR (KBr, cm-1):3550(νH2O), 3403(νOH-), 1623(νCOO-), 1572(νCOO-), 1532(νCOO-),1516(νCOO-), 1409(νSO), 1165(νSO), 1104(νSO), 738(νC-H), 683(νC-H). |
Yield | Reaction Conditions | Operation in experiment |
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47% | In water at 160℃; for 72h; Autoclave; High pressure; | 2.2. Synthesis of [M2((μ3-OH)(trz)(sdba)(H2O)]·3H2O}∞ (M = Ni for1, Zn for 2) General procedure: For 1, a mixture of Ni(NO3)2·6H2O (0.3 mmol, 87 mg), Htrz(0.3 mmol, 21 mg), H2sdba (0.1 mmol, 31 mg) and NaOH (5.2 mL,0.1 mol/L) in deionized water (3 mL) was sealed in a Teflon reactor autoclave and heated to 160 °C for 3 days. After the autoclave was cooled to room temperature, green block crystals suitable for single crystal X-ray crystallographic analysis were obtained. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
51.7% | With sodium hydroxide In methanol; water at 160℃; for 72h; | 2.2. Preparation of [Co(pytpy)(sfdb)]n (1) A mixture of CoCl26H2O (0.0238 g, 0.1 mmol), pytpy (0.0312 g,0.1 mmol), H2sfdb (0.0306 g 0.2 mmol) in methanol (2.5 mL) and distilled water (10 mL) was placed in a Teflon-lined stainless steel vessel and adjusted the pH value of the mixture to 6.0 with 0.5 mol L-1 NaOH aqueous solution. The reaction system was heated at 160 °C for 72 h, followed by slowly cooling down to room temperature at a rate of 5 °C· h-1. Finally, red block crystals were obtained and dried in air, 34.8 mg, yield: 51.7% based on Co.Elemental anal. calcd for C34H22CoN4O6S (%): C 60.63, H 3.29, N8.32; found: C 60.52, H 3.17, N 8.43. IR (KBr, cm1): 3424 m, 3063 w,1690 m, 1598 s, 1554 m, 1403 s, 1295 m, 1161 s, 1101 m, 1069 m, 1016w, 865 m, 826 m, 783 m, 773 w, 741 m, 692 m, 618m, 572 w, 524 m. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
63.2% | With sodium hydroxide In methanol; water at 160℃; for 72h; | 2.2. Preparation of [Co(pytpy)(sfdb)]n (1) General procedure: A mixture of CoCl26H2O (0.0238 g, 0.1 mmol), pytpy (0.0312 g,0.1 mmol), H2sfdb (0.0306 g 0.2 mmol) in methanol (2.5 mL) and distilled water (10 mL) was placed in a Teflon-lined stainless steel vessel and adjusted the pH value of the mixture to 6.0 with 0.5 mol L-1 NaOH aqueous solution. The reaction system was heated at 160 °C for 72 h, followed by slowly cooling down to room temperature at a rate of 5 °C· h-1. Finally, red block crystals were obtained and dried in air, 34.8 mg, yield: 51.7% based on Co. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
66.8% | With sodium hydroxide In methanol; water at 160℃; for 72h; | 2.2. Preparation of [Co(pytpy)(sfdb)]n (1) General procedure: A mixture of CoCl26H2O (0.0238 g, 0.1 mmol), pytpy (0.0312 g,0.1 mmol), H2sfdb (0.0306 g 0.2 mmol) in methanol (2.5 mL) and distilled water (10 mL) was placed in a Teflon-lined stainless steel vessel and adjusted the pH value of the mixture to 6.0 with 0.5 mol L-1 NaOH aqueous solution. The reaction system was heated at 160 °C for 72 h, followed by slowly cooling down to room temperature at a rate of 5 °C· h-1. Finally, red block crystals were obtained and dried in air, 34.8 mg, yield: 51.7% based on Co. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
54% | With sodium carbonate; In water; at 140℃; for 72h;Autoclave; | CdNO3·4H2O (30.8 mg, 0.1 mmol),4,4-sulfonyldibenzoic acid (30.4 mg, 0.1 mmol),Na2CO3 (10.6 mg, 0.1 mmol),Tmb (24.0 mg, 0.1 mmol) was dissolved in 10 ml of water, and then placed in a 25 ml autoclave, and the reactor was placed in an oven.The reaction was carried out for 3 days at 140 C, and then it was cooled to room temperature.Produce colorless crystals, filter, wash,After drying, a colorless crystalline product is obtained.The yield calculated based on Cd(NO3)2·4H2O was 54%. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
In methanol; water; N,N-dimethyl-formamide at 80℃; for 48h; Autoclave; | Synthesis of [Cd2(bpdc)2(bief)2]xsolvent (1) General procedure: A mixture of Cd(NO3)2·4H2O (0.0308 g, 0.1 mmol), H2bpdc (0.0242 g, 0.1 mmol), bief (0.0354 g, 0.1 mmol), DMF (8 ml), CH3OH (1 ml) and H2O (1 ml) was placed in a Teflon reactor (20 ml) and heated at 80 °C for 2 days. After gradually cooled to room temperature, colorless crystals of 1 were obtained. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
50% | With sodium hydroxide In water at 119.84℃; for 72h; Autoclave; High pressure; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With oxalic acid; In ethanol; water; for 0.5h; | General procedure: 4,40-Sulfonyldibenzoic acid (SDA, 98%, A.R.) is commerciallyavailable from Alfa Aesar. Oxalic acid (A.R.), boric acid(A.R.) and <strong>[4499-86-9]tetrapropylammonium hydroxide</strong> (25% aqueoussolution, C.R.) were obtained from Aladdin Industrial Inc.SDA (25 mmol, 0.7657 g), oxalic acid and tetrapropylammoniumhydroxide were dissolved in a 1:2:2 molar ratio insmall quantities of water-ethanol (1:2 v/v). The mixture, in a10 ml glass bottle, was stirred for about half an hour. Thebottle containing the clean solution was sealed with abreathable film and set aside under ambient conditions tocrystallize, yielding colourless block-shaped crystals of 1.These crystals were suitable for single-crystal X-ray diffractionanalysis after about 15 d, and oxalic acid was absent from thefinal crystal structure. The preparation of salt 2 was almost thesame as for 1, except that oxalic acid was replaced with boricacid. The absence of oxalic acid in 1 may be down to the factthat deprotonated oxalic acid under the experimental alkalineconditions cannot efficiently interact with the depronated hostanion to form the related host framework. Oxalic acid isessential to the formation of crystals of 1 because crystalscannot be obtained without oxalic acid, i.e. when only SDAand <strong>[4499-86-9]tetrapropylammonium hydroxide</strong> were mixed togetherusing the same procedure. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
In ethanol; water; for 0.5h; | General procedure: 4,40-Sulfonyldibenzoic acid (SDA, 98%, A.R.) is commerciallyavailable from Alfa Aesar. Oxalic acid (A.R.), boric acid(A.R.) and <strong>[4499-86-9]tetrapropylammonium hydroxide</strong> (25% aqueoussolution, C.R.) were obtained from Aladdin Industrial Inc.SDA (25 mmol, 0.7657 g), oxalic acid and tetrapropylammoniumhydroxide were dissolved in a 1:2:2 molar ratio insmall quantities of water-ethanol (1:2 v/v). The mixture, in a10 ml glass bottle, was stirred for about half an hour. Thebottle containing the clean solution was sealed with abreathable film and set aside under ambient conditions tocrystallize, yielding colourless block-shaped crystals of 1.These crystals were suitable for single-crystal X-ray diffractionanalysis after about 15 d, and oxalic acid was absent from thefinal crystal structure. The preparation of salt 2 was almost thesame as for 1, except that oxalic acid was replaced with boricacid. The absence of oxalic acid in 1 may be down to the factthat deprotonated oxalic acid under the experimental alkalineconditions cannot efficiently interact with the depronated hostanion to form the related host framework. Oxalic acid isessential to the formation of crystals of 1 because crystalscannot be obtained without oxalic acid, i.e. when only SDAand <strong>[4499-86-9]tetrapropylammonium hydroxide</strong> were mixed togetherusing the same procedure. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
50% | With water In water at 150℃; for 96h; Autoclave; High pressure; | Synthesis of [Zn(dbim) (H2sdba)]n (5) A mixture of Zn(Ac)2·2H2O (0.2mmol), dbim (0.1mmol), H2sdba (0.2mmol), and NaOH (0.2mmol) in H2O (10mL) was kept in a 25mL Teflon-lined stainless steel vessel at 150°C for four days. After the mixture was cooled to room temperature at a rate of 5°C/h, colorless crystals suitable for X-ray diffraction were obtained with a yield of 50% (based on Zn). Anal. calcd for C40H34N4O6SZn (%): C, 62.86; H, 4.48; N, 7.33. Found: C, 62.84; H, 4.46; N, 7.35. IR (KBr, cm-1): 3037.34(w), 2865.70(w), 1652.70(m), 1562.06(m), 1519.63(m), 1488.78(w), 1405.85(s), 1330.64(m), 1295.93(m), 1162.87(s), 1135.87(m), 1101.15(s), 1014.37(m), 869.74(m), 782.96(m), 744.39(s), 698.10(m), 622.89(m), 576.61(m), 501.40(w). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
54% | Stage #1: nickel(II) nitrate hexahydrate; 2,5-bis(4-pyridyl)-1,3,4-thiadiazole; bis(4-carboxyphenyl)sulfone With triethylamine In ethanol; water at 20℃; for 0.333333h; Stage #2: In ethanol; water at 145℃; for 72h; Autoclave; High pressure; | Synthesis of [Ni(bpt)(sdba)(H2O)3]n (1) A mixture of Ni(NO3)26H2O (0.1 mmol, 29.1 mg), H2sdba(0.1 mmol, 30.6 mg), and bpt (0.1 mmol, 24.0 mg) was dissolvedin water/methanol (8/2 mL). Two drops of triethylaminewere added to the solution and the mixture wasstirred at room temperature for 20 min, then transferredinto a Teflon-lined stainless steel vessel (25 mL). The sealedvessel was heated at 145 C for 3 days under autogenouspressure, then cooled slowly to room temperature over 48 h.Green block crystals of 1 were collected with a 54% yieldbased on Ni. Anal. Calc. (%) for C26H16N4NiO9S2: C, 47.95;H, 2.48; N, 8.60. Found: C, 47.86; H, 2.56; N, 8.73. IR spectrum(cm1, KBr pellet): 3455 s, 3210 m, 2958 m, 1698 m,1627 s, 1506 m, 1412 s, 1340 m, 1213w, 1164 m, 905 m,865 m, 732 m, 621w. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
15.15% | With potassium hydroxide In water at 150℃; for 72h; Sealed tube; | Synthesis of [Zn2(SDBA)2(DPA)2*2H2O] A mixture of Zn(NO3)26H2O (29.8 mg, 0.1 mmol), H2SDBA (30.6 mg,0.1 mmol), DPA (34.2 mg, 0.2 mmol), and KOH (11.2 mg, 0.2 mmol) in H2O (8 ml) was sealed in a 16-ml Teflon-lined stainless steel container and heated at 150 °C for 72 h. After cooling to room temperature, colorless block crystals of complex 1 were separated by filtration and washed several times with water and ethanol (yield 15.15%, based on Zn). Elemental analysis for C48H38N6O14S2Zn2 (FW = 1117.74): C 51.58, N 7.52, H 3.43%; found: C 51.71, N 7.53, H 3.43%. Selected IRpeaks (cm-1): 3441(w), 3146(w), 2913(w), 1586(m), 1391(s), 1282(m), 1212(w), 1121(m), 1083(m), 1056(w), 989(w),873(w), 772(w), 679(w), 632(m) |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
58% | In N,N-dimethyl-formamide; at 95℃; for 72h;High pressure; | A solvothermal reaction of <strong>[1366291-62-4]TPPA</strong> (9.5 mg, 0.02 mmol), H2sdba(12.3 mg, 0.04 mmol), Co(NO3)2·6H2O (43.7 mg, 0.15 mmol), H2O(6 mL), N,N-dimethylformamide (DMF, 2 mL) and acetonitrile (2 mL) were sealed in a Teflon-lined stainless-steel vessel andheated to 95 C for 72 h, and then cooled to room temperature naturally.Black block-shaped crystals were obtained (yield: 58% basedon Co). Elemental analysis calculated (%) for C61H36Co2N4O12S2: C,61.11; H, 3.03; N, 4.67. Found: C, 61.15; H, 3.06; N, 4.64. IR (KBr,cm-1): 3417(m), 1637(s), 1596(s), 1489(w), 1406(s), 1325(w),1294(w), 1222(w), 1165(s), 1099(w), 813(w), 736(s). The IR spectrum of compound 1 is existed in the Supporting Information(Fig. S3). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
52% | With hydrogenchloride at 90℃; for 72h; | Preparation of [Gd2(H2O)3(SDBA)3](DMA)3] In a 50 mL breaker was placed Gd(NO3)36H2O (45 mg,0.1 mmol),H2SDBA (31 mg, 0.1 mmol),DMA(6 mL), andH2O(1.5 mL). After the addition of 0.2 mL of HCl (2 M, aq), thesolution was vigorously stirred for 30 min at room temperatureto obtain a clear solution. The clear solution was transferred intoa 20 mL vial and heated at 908C for 72 h. Yellow sheet-likecrystalline products of 1 were obtained by removing the solvent,the products were washed withH2Oand left in the air for one dayto dry. Yield 52% on the basis of the H2SDBA ligand. Anal.Calc. for C40H43Gd2N3O15S2 (1184.4): C 40.56, H 3.66, N 3.55;Found: C 40.28, H 3.98, N 3.45 %. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
0.31% | In N,N-dimethyl-formamide at 100℃; for 72h; Autoclave; High pressure; | Synthesis of compound 2 A mixture of Cd(NO3)2·4H2O (0.0155 g, 0.05 mmol),H2sdba(0.0153 g, 0.05 mmol) and L (0.0155 g, 0.05 mmol)in DMF (2 mL), H2O(1 mL) and 150 μL of HCl (6 mol/L) was sealed in an autoclave equipped with a Teflon liner(25 mL). The mixture was heated at 100 °C for 3 days andthen cooled to room temperature. Colorless block single crystals of 2 were collected in ca. 31% yield based on L.Elemental analysis for C54H36Cl2N8SCd2O6 calcd (%): C,53.1; H, 3.0; N, 9.2. Found (%): C, 52.4; H, 3.0; N, 9.0. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
48% | With calcium(II) chloride dihydrate at 150℃; for 96h; High pressure; Autoclave; | 2.1.3. [Ca4(SBA)4(DMF)2].2DMF (3) A mixture of CaCl2·2H2O (147 mg, 1 mmol), H2SBA (153 mg, 0.5 mmol) and 15 mL DMF was stirred for 30 min at room temperature. The resulted homogeneous solution was transferred into a 10 mL PTFE lined stainless steel autoclave, sealed and heated at 150 °C for 4 days under autogenous pressure. After slow cooling at room temperature block-shaped transparent crystals were isolated which were filtered under vacuum, washed with DMF and dried under ambient condition. The yield is 48% (102 mg) based on SBA ligand. Elemental analysis calcd. for C68H60Ca4N4O28S4 (3): C, 48.91; H, 3.40; N, 3.36%. Found: C, 49.12; H, 3.62; N, 3.86%. FTIR (KBr pellets, cm-1): 2151(w); 1660(m); 1591(s); 1392(s); 1300 (m,s); 1161(m); 1092 (m); 747(m). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
61.2% | In water at 99.84℃; for 72h; | 2.1. Synthesis and crystallization A mixture of BMIOPE (16.5 mg, 0.05 mmol), H2SDBA(15.3 mg, 0.05 mmol), Zn(NO3)26H2O (14.8 mg, 0.05 mmol)and H2O (2.5 ml) was placed in a Teflon-lined stainless steel vessel, heated to 373 K for 3 d and then cooled to roomtemperature over a period of 24 h. Colourless block-shapedcrystals were obtained after cooling the container to roomtemperature undisturbed. The crystals were filtered off,washed with H2O and dried in air [yield 61.2%, based onZn(NO3)26H2O]. Elemental analysis (%) calculated forC34H26N4O7SZn: C 58.33, H 3.74, N 8.00; found: C 58.45, H3.75, N 8.02. IR (KBr, cm1): 3129 (w), 3058 (w), 1636 (s),1565 (m), 1505 (s), 1358 (s), 1292 (s), 1245 (s), 1160 (s),1101 (m), 1007 (w), 848 (m), 743 (w), 690 (w), 623 (w), 545 (w). |