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Organometallic Chemistry - Science topic

Organometallic chemistry is the study of chemical compounds containing bonds between carbon and a metal.
Questions related to Organometallic Chemistry
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Are there any exceptions to the Irving Williams series in the formation of more stable Zn(II) complexes with tridentate neutral ligands than Cu(II) complexes?
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Yes of course
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With benzene ring as a typical aromatic structure, the uncompromising hydrogenation (ring saturation without altering the non-aromatic functionality such as the -OH and the -C=O) of benzene derivatives: phenol, benzyl alcohol, benzoyl moiety, aniline, etc. is well known.
However, little, if any, is documented about the reverse reaction. Have you come across or thought of the uncompromising dehydrogenation of the corresponding aliphatic (cyclohexane) derivatives to the benzene derivatives? If yes, please share your experiences, papers, weblinks, ideas, and so on.
Thanks in advance!
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Dear Stanislaus O. Okwundu thank you for sharing this very interesting chemical question with the RG community. As a synthetic inorganic chemistry I absolutely not an expert in this area of research. However, I at least found two literature references which at least come close to answering your question in part. Both describe the dehydrogention of cyclohexylamine under formation of aromatic amines. Please have a look at these articles:
A Ni–Mg–Al layered triple hydroxide-supported Pd catalyst for heterogeneous acceptorless dehydrogenative aromatization
and
Versatile routes for synthesis of diarylamines through acceptorless dehydrogenative aromatization catalysis over supported gold–palladium bimetallic nanoparticles
The second paper is even freely available as public full text. You can find and access other related articles by searching the "Publications" section of RG for the term "dehydrogenative aromatization":
Other articles are found when searching for terms like "acceptorless dehydrogenative aromatization". When searching for literature references, I think you should better avoid the term "uncompromising" as in your original question. This word seems to be rather unusual in this context.
I hope this helps. Good luck with your work and best wishes, Frank Edelmann
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The structure is very unusual but we came out with something like a Td with a fifth RCOO- ligand. Formula of the anion  Co(II)2(RCOO)5- each Co(II) is pentacordinated.
We know the J, Delta (small), lamda, E,  D and tau from Xi(DC) measurements.Therefore, there is s tetragonal distortion, sort of.
The EPR Spectra occurs only bellow 15 K, otherwise it is VERY broad. Near 4K is even broader. At 8K I can see the fine structure of Co2(RCOO)5- but only 11 lines emerge.This makes me think the spin-lattice is dominating relaxation.
I can see only one set of 11 lines, therefore I don't believe the distortion is not too large.
There are not many examples of pentacoordinate Co(II), except for proteins.
How can I rationalize these observations?
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mu at (4700 Gauss) does NOT decrease until 4K. It remains constant all the way up to 298K. My Japanese theoretician just asked me if it was a dipole or it was a Single Molecule Magnet? I don't know, yet. Before measuring Xi,I ran an EPR spectra up to 6000Gauss at 298K. Then I ran further spectra at 280K, 20K, 8K and 4K. Sample could have been magnetized. SMM. Sorry, I have never been good at History lessons.
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I have prepared a Co(III)corrole, and the NMR in DCCl3 shows broad signals between 7.30 and 9 ppm. I've read that Co(III)corroles are paramagnetic with S = 1. So I attempted to add MeCN to coordinate the Co ion. It didn't change anything. Then excess triethylammine and although the broad signals move slightly, and some fine signals appear at ~10 ppm, there is still no big change. I thought that maybe I had aggregation, so I greatly diluted the same sample, and although I obtained much weaker signals, they were still broad.
I also prepared the analogous Al(III)corrole, and the NMR is similarly broad, with signals in the same region. That one threw me off.
Does anyone know what could be happening?
Thank you very much!
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Add 5% of NH3 H2O into your NMR sample will solve the problem. Here is the ref:
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I am trying to reduce an organometallic complex that has a tethered diaryl ketone functional group. Unfortunately aqueous or methanolic NaBH4 reduces the ketone functional group as well. 
Any other suggestions would be gratefully acknowledged.
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The mild reducing agent that can operate in water is sodium sulfide which will not reduce ketone.
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While strong catenation is almost exclusively reserved for C, some transition and post-transition elements can oftentimes take part in delocalized electron systems and ring systems. But does the two come together, that is, is there any known aromatic compound that has two adjacent transitional/post-transitional elements in aromatic ring as heteroatoms? If Yes or No, then Why?
Suppose for a 5-valency element, there are two mutually perpendicular pi-orbitals (along with a sigma molecular orbital) that make a triple bond between two atoms, remaining two valency "hands" are used up for taking part in two mutually perpendicular aromatic ring system. Keeping in mind instability of benzyne and ONC (Octanitrocubane), would that structure be chemically stable and permissible by quantum chemistry? If yes, then what kind of novel properties can be expected from the compound and what would be the stability of it? What would the most suitable element for this purpose?
Attached with it is a Lewis structure of a tentative complex of X metal. Note, the two aromatic structures are not coplanar, rather they are orthogonal
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Dear Sumit Bhowmick this is certainly a very interesting and unusual technical question. I have no definite answer to this question and can only speculate about a possible solution. Formally such a molecule would be a "dimetallanaphthalene". I searched the SciFinder for the term "dimetallanaphthalene" and received exactly 0 (zero) answers. Apparently such a molecule has never been prepared experimentally. In my opinion the most suitable element X for forming such a structure would be a Group 6 metal (chromium, molybdenum, or tungsten). These metals are well-known for forming stable "lantern-like" complexes with bridging ligands and multiple bonds between the metal atoms. even quintuple bonds between two Cr or Mo atoms are possible:
(see attached diagram)
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Is it possible for a metal complex to change its coordination mode between solid and solution state?? My crystal data indicates bidentate coordination whereas NMR inidicates monodentate one.
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Please check the following free document. My Regards
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MOF-88, MOF-500, ZIP-8, MIL-101 AND MCM-41.
what is meaning of Fe- MOF-88 and how to calculate 88 numbers.
many example i need answer could tell me.
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Please see the following link;
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I have an aryl boronic pinacol ester (Ar-Bpin) which has a phenolic -OH group. I would like to use K2CO3 conditions, as well as NaOH conditions (separate reactions). Question is whether Ar-Bpin can withstand such conditions.
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Gowtham Raj Hi, what do you mean by "got cleaved"? Did you get deprotected B(OH)2 or deboronation product? Thanks!
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During the alkylation step of a Mo(I) compound with a macrocyclic P4 ligand (containing a P-H moiety), the proton of P-H was extracted by n-BuLi (P-H : n-BuLi=1:1). Then R-Br was added in order to finish the alkylation towards P-R structure.
However, the coupling of two P-H moieties happened that dimers of two Mo(I) compound (through the linking between two P4 ligands) were found to be the main product.
So I was wondering what might be a potential mechanism happened during this process instead of desired alkylation.
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Frank T. Edelmann I was thinking the same thing. Allene is stablised. Could well be volatile at reduced temperature, if formed by basic HBr abstraction. Though, you would expect to see at least some cyclohexene formed too. And I still can't rationalise P-P bond formation from forming Propene (I did think of it at the time).
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The background of this is lengthy, but in short, I am an experienced chemist with essentially no experience doing Grignard reactions.
Most recent literature uses mmol scales @ 0.1-1M concentrations. I need to run a ~1mol reaction, but multi-liter is out of the question. Small scale tests showed that concentrated solutions - but still with several equivalents of Mg-coordinating ether - were *extremely* viscous. No crystals or precipitation, but gelatinous to the point of not stirring. The reactions did not proceed as expected.
Very old mole scale literature usually uses Et2O.
Can someone with first hand experience on preparative scale Grignard rxns give me a feel for the maximum concentration of PhMgCl I should make from Mg/PhCl in THF?
I may need to run the reaction in several batches depending on the answer.
Thanks
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Dear all, attached is a book dealing with tips and practices in manipulating air sensitive chemicals. Under the circonstances you want to work, the best option is to work with a continuous lab flow reactor. Please check the link below. My Regards
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Isomers (organic ligands) that contain phosphine (-PH2) moieties have been made and need to be isolated outside the Glove Box by column chromatography (CC). Protection of -PH2 by borane had proved to fail upon exposure to the air.
It seems that -PH2 needs to be oxidized to phosphate first before CC operation.
So would it be possible for phosphate to be isolated by CC despite of its strong polarity as well as the adsorption to silica or aluminium oxide? Or other possible protection method (e.g. sulfuration) can be used for -PH2?
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Dear Jingran Shan , as we know phosphorous-containing ligands are very sensitive to moisture and air. So for the isolation of these types of ligands by column chromatography environment should be moisture-free. And also silica is not good for phosphine ligands separation because of its acidic behavior, it breaks the bond of phosphine resulted in phosphate compounds, So use alumina for CC.
Do not use polar solvents for column as it oxidized phosphines, use only nonpolar solvents. eg, hexane, toluene,
Also, u can do a column in presence of N2 atm , so that less phosphine will be oxidized.
as like we applied air pressure for column u can use N2 pressure for a column. so that u will get a good yield.
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Trying to avoid the use of diborane as precursor for B I am looking for alternative precursors. Essays with Tri isopropyl, 3 etyl and tert buthyl Borate didnt give good results. Also the use of Oxygen during the process make the use of pirophyric precursors (as TMB) quite risky for my level of safety conditions. Any suggestions on the precursors I should try ? (suposing having o2 and heptane already involved on the process)
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Indeed I used 15 years ago meta orto and para. dicarbadodecaborane
However I used as a powder precursor and I got a lot of C within the films. I will try it in toluene
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For complexes, which have red/orange colour, the absorption for dd occurs nears 420-450 nm. However how do we know it is not MLCT but dd.
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Srividya Swaminathan d-d transitions are symmetry forbidden (Laporte selection rule), and therefore less intense. MLCT (or any charge transfer) transitions are far more intense. Typically, molar extinction coefficients for d-d transitions are in the range of 200-500 M-1 cm-1 whereas that for the MLCTs is >1000 M-1cm-1.
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For complex molecules with many heteroatoms, can we predict if the molecule is pi-acceptor or donor? Also if possible can someone suggest a good source to read more about these stuff in detail?
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Almost all ligands are sigma donor, though the extent of donation varies from ligand to ligand. Now the question is when a ligand will act as a pi acceptor or donor. Pi donor ligands are those which have extra non bonding electrons in their valence orbitals (simple example iodine). Now the extent of pi donation depends on the symmetry and energy of those orbitals. The energy difference between vacant metal orbitals and filled ligand orbitals should not be very high and both must have same symmetry. Now to be a pi acceptor a ligand needs to have an empty orbital and here too the extent of pi accepting tendency depends on the energy difference and symmetry of the empty ligand orbital and filled metal orbital.
ref: The Organometallic Chemistry of the Transition Metals by Robert H. Crabtree
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I am preparing LDH with co-precipitation method using aluminium chloride and calcium chloride. Upon addition of NaOH to AlCl3.6H2O and CaCl2.6H2O, not only LDH but also Al(OH)3 is formed. How should I prevent formation of this hydroxide?
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hi
it is all about the ratio of divalent and trivalent cations that you use
keep the ration between 2 to 1 and 4 to 1 this way you may prevent formation of aluminium hydroxide .
check the generic formula for LDH , the value for x must be between 0.2 to 0.33 in that formula ,which corresponds to the above mentioned ratio.
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I am trying to remove THF from a coordinatively saturated metal complex. The THF is not removed under vacuum nor does it comes out upon repeated pentane wash. I am looking for complexes that can attack the THF while not affecting the metal complex.
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Try a solution of elemental sulfur in Toluene or some sulfur compund if it is only important to get rid of the THF-ligand. Metal-Sulfur-bonds are quite favored. If it is important to get a free coordination site, you could try lyophilizing (freeze drying) the solution of the sample. Good luck! P.S.: I worked with a Mn/Re-THF-system + sulfur in my thesis.
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Can I do heck coupling reaction on a compound in salt form without turning it into a free base?
As for example doing Heck coupling on p-chloropyridiniumchlroide.
I don't want to turn my compound into a free base because it contains nitrogen atoms that causes Pd toxicity and inhibit the coupling reaction.
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Hi Abdulrahman Mahgoub, please find attached the Supplementary Information of the Tetrahedron Letters paper to give you some more detailed information. The authors use a number of substituted heterocycles as starting materials for the Heck coupling, but they are all neutral. However, they use DMF as solvent. Chances are that your p-chloropyridiniumchloride is soluble in DMF. So you should just give it a try and run a test reaction on a small scale. Good luck!
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I have done DFT and TD-DFT to obtain singlet excited state, now I want to calculate triplet state also and to check singlet to triplet transition. I have used B3LYP/6-311g(d,p) for singlet state.
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I have done the calculations of triplet energy, but now i want to see my triplet energy values in an out put file, so what is the easiest way to find the triplet energy , please?
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After forming (3-methoxythiophen-2-yl)trimethylsilane, I react it with 1 eq of nBuLi and quench with snbu3cl - obtaining starting material. Is the nBuLi acting the tms group?
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We routinely metalated 1,4-bis(trimethylsilyl)-2,5,7-cyclooctatriene with n-butyllithium and the TMS groups always remained unchanged.
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Ruthenium(III) Chloride, Anhydrous with high assay is not so expensive. Hydrate is hard to measure the exact Ru content. However, hydrate is used for the synthesis of Ru nanoparticles. Wikipedia also says it (https://en.wikipedia.org/wiki/Ruthenium(III)_chloride). What is the advantage of using hydrate?
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The anhydrous RuCl3 is chemically inert and has very low solubility to most of the solvents.
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I wanted to use Titanium (IV) chloride first, but it was explosive with basic solutions. Then I tried Titanium (IV) tert-butoxide. Reaction was held in octanol. I used 50 mg of Sodium Methoxide and 50 mg of strarting phthalonitrile compound. But reaction did not occur. I attached 10 different metals to phthalocyanine core like this, but I can't attach titanium.
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Hello,
I have to optimise [Re(OH2)(CO)3(phen)]+, I have made the structure on gaussview, I have attempted to optimise the complex with B3LYP method in gen mode (SDD/LANL2DZ) for Re and 6-31+g(d,p) for the other atoms) but I keep getting errors. I would appreciate if someone could show me a sample input for gaussian to optimise this complex.
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Probably the format of defining mixed basis set and pseudopotential is incorrect. In fact, the simplest and appropriate keywords for this task is "# B3LYP/def2SVP opt", the def2-SVP quality is adequate for current optimization purpose, and Gaussian will automatically employ proper pseudopotential for Re.
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Hello,
I have to optimise [Re(OH2)(CO)3(phen)]+, I have made the structure on gaussview, I have attempted to optimise the complex with B3LYP method in gen mode (SDD for Re and 6-31g(d,p) for the other atoms) but I keep experiencing problems. I would appreciate if someone could show me a sample input for gaussian to optimise this complex.
Thank you
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Hi. Here is an example of an input using multiple basis set:
#N B3LYP/gen pseudo=read OPT
blank line
name of the complex
blank line
1 1
z-matrix/cartesian
blank line
C O H 0 6-311+G(2d,p) **** Re 0 sdd **** blank line Re0 sdd blank line
blank line
Obviously the blank line means you leave the line empty.
I don't know why but the gaussian input of these type must have two blank lines at the end.
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Tuning luminescence of platinum complexes is well established by variation of cyclometalating ligand. The most common trend I find in literature is a red shift in the emission upon introducing more electron rich rings to the ligand (for example replacing phenyl with thiophene). I am observing the exact opposite, in which more electron rich ligands will result in blue shifted emission and was wondering what might be the possible reason ?
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There is no simple rule in tuning the emission of Pt(II) complexes. Every ligand system is different. What one should consider is whether that (electron-rich) group is placed on a moiety acting as HOMO or LUMO. Usually F is added to the phenyl ring of a cyclometalating ligand to increase the emission energy of the metal complex. But the following paper shows that addition of F to a phenyl ring can lead to red shift. The degree to which the emission is affected also depends on the substitution pattern.
Apart from this, usually we take it for granted that extending the conjugation of a ligand will lead to redshift in emission. But there are also exceptions:
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Hello,
I need to synthesize the Tris(triethylsilyl)bismuthane [(CH3CH2)3Si]3Bi. 
So far I tried an analogous method for Antimony described in DOI:10.1021/cm102904f. I assumed that the chemistry should be similar for bismuth. In the first step, I used Sodium naphthalenide and bismuth powder in DME in order to prepare Na3Bi alloy (reflux 2days). Then injected Chlorotriethylsilane followed by reflux for another two days. However, I noticed, that no Bismuth has been reacted (or maybe small fraction) after refluxing for two days, and I have some mess in flask now...
So my first assumption is that no Na3Bi alloy was formed, and the reaction did not proceed.  Because Bi is also black powder as resulting Na3Bi, I can't visually evaluate if the alloy is formed or not. 
So my question is maybe this method is not appropriate for bismuth? Or something wrong with the starting materials?
The alternative is to use NaK, but for safety reasons, I prefer to avoid NaK. 
All reactants used right after purchase, used bismuth powder (325 mesh) DME was purchased dry, stored under molecular sieves.
Any tips? suggestions?
I really need your help. 
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Thank you very much for your answers, it helped a lot!
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For some reported metal complexes as anion sensors in the literature, the proposed mechanism is that upon binding of the anion to the metal center, the extent of ICT from ligand to metal is enhanced. My question is what are control experiments that can confirm such claim?
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As a non-native English speaker, I am quite confused about the correct preposition to use after "oxidative addition". Does an oxidative addition take place to, on or onto a metal centre?
Thank you for your help.
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I vote "to". The others seem less accurate or direct.
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A novel Cu-MOFs was synthesized and characterized by CHN, FT-IR, TGA, HSM, UV-VIS, SEM and X-ray crystallography.The X-ray crystallography revealed that the copper ion coordinate to the ligand through the oxygen to form an octahedral complex.
I want to study the fragmentation pattern of this Novel MOFs and I don't know which one will give a better result between GC-EI-MSD and HPLC-ESI-MS. I also need the chromatographic method
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Thanks Dr. Bojidarka B. Ivanova. I know Chromatography is method for separation. It does not provide structural information about fragment ions. My main interest is in the Mass Spectroscopy. The compound in question is pure but I don't have access to only MS, thanks.
Thanks Dr. Fatma Ulusal. But I dont have access to only MS. I only have access to GC-MS and LC-MS..........................
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The proposed mechanism involves an intramolecular PET in a Carboxylate derivative which leads to the formation of an oxiranone derivative and as a result an ISC from triplet to singlet state (S0). The existence of the oxiranone derivative in the ground state was confirmed by DFT studies using M06-HF functional!
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Mr. Tom,
You could pay attention to Gaussian's manual and the reference section (http://gaussian.com/techsupport/, http://gaussian.com/references/). There are given even test files (http://gaussian.com/testjobs/).
In addition, inputs can be found here:
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such as a derivative of ferrocene and ferrocene salt.
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by phase extraction( adding a miscible solvent like acetone) or by adding a salt i think 
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I am trying to synthesise cis-RuCl2(Me2dcbpy)2. I have followed the experimental below but I have not achieved the correct product and I have repeated the experiment twice. The experiment has been done numerous times before am I am being very careful with carrying this out. Does anyone have any suggestions to why I am not getting the correct product? (the nmr shows mostly the unreacted ligand and the MALDI shows something else which I can't work out). 
A solution of Me2dcbpy (0.492 g, 1.64 mmol) and RuCl3.H2O (0.220 g, 0.841 mmol) in DMF (35 mL) was purged with nitrogen for 15 min. The mixture was heated to 125 oC whilst being vigorously stirred in an oil bath (in darkness). After 2.5 h, the reaction was allowed to cool to room temperature and the DMF was removed on a rotary evaporator to leave a black solid. This solid was stirred in methanol (100 mL) overnight under nitrogen at room temperature. A brown precipitate was collected by filtration. 
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what method do you suggest? I attempted to separate on a silica column but the complex was not collected
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I've made a platinum complex but the NMR spectra gave a complicated peaks made of different oligomers. I suspect that I might have got Pt(IV) complex instead of Pt(II). Is there any experiment that I can do to confirm the oxidation state? 
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Hi,
If you know the geometry you can get it. Pt(IV) is octahedral, whereas Pt(II) is square planar. 
You can use 195Pt NMR if you have access to it and someone with experience doing it (it has a large spectral window). 
FYI oxidations from Pt(II) to Pt(IV) usually require a decent oxidant. Oxygen only works for very electron-rich Pt(II) complexes (ex: Pt(bpy)Me2, but not Pt(bpy)Cl2). If you put Pt(II) in, it's probably still Pt(II) unless there was a good oxidant (eg. Cl2, R-I, H2O2) in there. 
If your compound has a Pt-P bond, you can see the coupling constant in the 13P NMR. Generally if it is less than 2000, it is Pt(IV), but if it is more than 2000 it is Pt(II). It depends on the ligands, though.
-Kyle
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Dear all,
       I have carbanion generated in my reaction system. If I add ferrocene derivative (ferrocene carboxaldehyde ) to this system having carbanion, Does nucleophillic attack is possible on cyclopentadienyl ring of  ferrocene? 
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Mr. Rao,
You could pay attention to:
1. ChemPhysChem, 14, 2013, 311-314, Electrochemically controlled proton-transfer-catalyzed reactions at liquid-liquid interfaces: Nucleophilic substitution on ferrocene methanol, Peljo, P. et al.
2. Tetrahedron, 62, 2006, 9038-9042, Unexpected reactions of ferrocene acetal derived from tartaric acid with alkyllithium: competition between proton abstraction and nucleophilic attack, Zhang, W. et al.
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The majority of samples are paramagnetic but some molecules are dimers which might have antiferomagnetic couplings between the transition metals.
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I'm not an expert for SQUID magnetometry, but I'm not sure if this is possible with liquids, at least I have only used solids for SQUID. As antiferromagnetic coupling should require very low temperatures, you will have a frozen solution at this point. This would not really be a solution anymore, so you could as well do measurements in solid state. Furthermore, if you have a large quantity of diamagnetic frozen solvent and dilute paramagnetic analytes, this will probably not be very helpful in SQUID measurements, depite the sensitivity. Preparing the samples in an inert gas glovebox should not be a problem.
However, if you are interested in the magnetic properties in (still liquid) solution, I can recommend using an NMR based approach which was proposed by Evans. This is fairly standard and will work with any NMR spectrometer. You can find some information in the linked publications.
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I want to conduct nucleophilic addition/substitution reaction on ferrocene carboxaldehyde. May I know the feasibility? 
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Aldehydes undergo nucleophilic addition reaction.
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why you do not use derivatives of hydrazones with Ru(II)/Ru(III)?
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Yes........,  but , i asked  about its ability (application ) as anticancer  complexes or inhibition complexes 
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Hello,
I don't have a background in chemistry so I'm struggling with basic things (I think).
I'm trying to make an aqueous solution with MV dichloride hydrate, removing the chloride from it. I would like to get some advices on how to do it without the insertion of any other ions in the solution or that can be easily removed.
Thanks for your attention.
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Thanks all for the comments. Andreas, Yes! I was forgetting about this basic principle. 
Well, I'm studying a system with Ag nanoparticles and I was trying to add MV2+ but the chloride ions strongly react with the Ag nanoparticle. As was suggested hereI will try to use AgNO3. 
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I am willing to optimize  dimer in both, singlet and triplet, excited state. But I don't know whether it is possible from gaussian, and if yes, how to do.
Thanks in advance.
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Dear Indranil,
You are asking about doing eom-ccsd? this is how to do so for two excited states and optimizing with respect to the 1st excited state, the states are singlets as am showing under the title after the 0 charge (neutral molecule) using 1, which is for singlet , for triplet states use 3 instead of 1
opt eomccsd=(nstate=2,root=1)
Title
0 1
But keep in your mind that eom-ccsd analytic gradients are only implemented in the recent Gaussian16 version, older versions will perform numerical gradients, which is extremely expensive
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Both the processes use Metal and oxidant, then what is the basic difference? How one can distinguish between the two processes?
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CDCs are a subset of C-H activation reactions. In general, C-H activation reactions proceed with the general form:
C–H + X–Y  —>  C–Y + H–X
If X = H, then the reaction is considered dehydrogenative.
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Give some references.
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 Dear Stefano,
Unfortunately, I have also close to 40 years of experience with 31P NMR. -:). The determination of the position of P-ligands on transition metals and of the configuration of the formed complexes were always in the focus of our research. If one includes all transition metals and all peculiar P-ligands, it is indeed difficult to set up a simple classification for cis-trans geometry, based solely on 2JPP.  However, as you also know it very well, triphenylphosphine complexes of late transition metals (including cis  and trans assignments) are among the most explored areas in 31P NMR spectroscopy. The range of cis and trans 2JPP of late transition metal complexes of triphenylphosphine, and more specifically, the analogous values for Ru complexes were suggested on this basis.  
Regards,  
                Imre
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I do an 1H-RMN spectra and I see two differents J in my doublets, the first one is 12.8Hz and the second one 9.8 Hz. How I can assign to the cis- or trans- isomer? Is there any database where I can look for?
Thank you for your time
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The J-coupling for trans is larger than that of  cis-isomer. IR will help you to see if it is cis or trans.
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A highly conjugated organic molecule was tried to load to HKUST-1 pores by dissolving the organic substance in ethanol and stirring with HKUST-1 for a day. After a day the sample was centrifuged and the supernatant (without solid HKUST-1) was examined by UV spectrometry and It was observed that the organic molecule has made a complex with Cu in the solution phase. What could be the reasons for Copper to leach to solution? I find the below possibilities probable and would like to know your view about them.  
01. Can HKUST-1 degrade within a day, to leach Cu ?
02. Can the highly conjugated organic molecule replace Cu atoms from the HKUST-1 structure ?
03. Can uncoordinated Copper be trapped within the framework and released in the presence of the organic molecule?
04. Can there be unreacted CuSO4 in the HKUST-1 sample? (However HKUST-1 was solvent exchanged for 10 times with fresh batches of ethanol in order to remove the unreacted Cu, prior to loading)        
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If I correctly understood the theme, Cu was not leached from solution but mainly from HKUST-1 net. This happens even without organic molecules interacting with Cu2+ ion, but merely with the presence of water media. If there are unstructured Cu2+ in the pores of the net, hence they should be displaced to the solvent phase through water/ethanol washings. But if you use adduct or chelating agents the scavenging of the metallic center from the net is driven through adduct, chelate or macrocyclic effect depending on the employed substance that interacts, with Cu in this case. Its own dissolution or coordinating assisted dissolution happens due to the fact that the HKUST-1 crystallites are surface open/labile materials containing -COOH, -COO- and -COOCu sides or functionalities directed to the interaction with the solvent. Therefore having these terminals, these components should displace to the media since Cu is efficiently solvated with water molecules. In this way the displacement of both Cu ions and trimesate or trimesic acid towards water is observed by UV-vis, therefore the loss of material is attained. Having less and larger crystals should diminish the dissolution rate, but if you have more and smaller crystals, the dissolution rate should be higher. I hope to be sufficiently clear in this explanation. If you need further details in order to understand the issue please contact me and looking forward to help in the analysis of your experiments. Best regards. Hiram
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Salam
I want dissolve TTIP in ethanol by drop wising ethanol to TTIP under stirring but sometimes I get a White milky solution and in other cases I get a clear solution.
How I proceed to get a clear solution of TTIP and ethanol? For information I tried pure ethanol and ethanol 96% and always I get a milky solution 
Thanks in advance
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Hi...,
small amount of water can form milky color solution with ethanol therefore  You need to dry (purify) your ethanol and TTIP from water as much as possible avoid any water vapors before and during  making solution,and do not pass saturation limits.
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EPR spectra
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I am trying to use TMAH to under-etch single crystalline Si to form released amorphous Si structures. The width of the under-etch is approximately 10 um. However, as far as I know, TMAH also attacks some metals like Al. Since I want the metal remains on my samples after the wet etching process to make electrical contacts, do you know what types of metals (namely gold, nickel, etc...) I can use?
Thank you.
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Thank Hyun-Sue! Do you have any idea about the etching rate of each metal?
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Dear All,
I would like to ask that whether it could be possible to perform a reaction in complete inert condition under ball-milling, if it is then how?
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For inert atmosphere, argon is used  - it is heavy and replace air from vessels. SF6 is also suitable, excluding work with alkali metals ( molten Mg and Al do not react). Powders should be degassed by 2-3x  pressure swing (vacuum-inert gas) .
As inert fluids you can use perfluorinated fluids, but they are reactive under milling with many metals, hydrides , metalorganics; hydrocarbon-based fluids (vaseline oil)  are reactive with oxidizers. For  mutual compatibility rough estimation  -  milling ball shock is equal to short-term 400oC generation. 
Cryomilling (in  liquid nitrogen, LN2) do not have disadvantages of all above-mentioned mediums and is suitable for high energy materials milling; lab-scale equipment is available, but simple porcelain mortar and pestle are also functional
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Would it be OK to briefly expose this substance to ambient atmosphere or will it all oxidize immediately?
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Do you actually mean PhPH2 ?  If so, it oxidizes very quickly and should not be exposed to air.  If you mean Ph3P, or triphenylphosphine, brief exposure is fine.
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I have a [Ru(SO2)(NH3)4Cl]Cl2 and I want to change at least two of the ammine groups of the complex for H2O or another Cl. Any suggestions?
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You can by choosen strong  ligand more than ammine
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Ligand:Thioamide Ligands
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Thioamides are better ligands and more likely to cleave than amides. The Ru could activate the thioamide to nucleophilic attack by solvent or adventitious water if you in a non-aqueous solution. 
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what is the restriction to form M-M bond through produce an organometallic  complex for S and P block elements?
and when form single or double or triple bond between M - M for S and P block elements?
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More reduced states open the door for closer distances between the metal atoms. Higher order bonds require the metals to be in very low oxidation states so they can get very close to each other. Moreover, lower oxidation states result in larger orbitals which allows them to have a much better overlap.
Additionally, we can use very bulky ligands to protect such bonds. 
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Dear All, 
Here's a query, please clarify, 
Given a compound, how to predict the likelihood of its chelating property? Are there any webservers/programs available to predict whether a compound will  have chelating property?
Please let me know 
Thanks 
srinivas 
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For the compound to act as a chelating ligand, it would ideally have two donor atoms positioned in such a way that when both atoms bind to a metal, a five- or six-membered ring is formed e.g. 2,2`-bipyridine binds to a metal to form a 5 membered C-N-M-N-C-C ring, while acac binds to metals to give a 6 mebered C-C-O-M-O-C-C ring.
Does this help?
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As I have used DMF for the synthesis process of HKUST-1, I had to activate it in the oven at 110 0C after solvent exchanging with ethanol, prior to applications. while it was in the oven the colour of HKUST-1 turned from light blue to dark blue. when it was cooled to room temperature dark blue turned to the lighter colour as before.
Is the change in color due to the loss of solvent molecules during the activation process ? or has the MOF dissociated during the activation step ? or are there any other reasons for the change of colour ?  
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The change of colour from light to dark is due to the removal of the axial ligand (ethanol, DMF or water) from the copper acetate lantern, then the dark to light colour change is due to atmospheric water binding onto this coordination site. I find it's a good way to visually identify whether the activated samples have been exposed to air.
At 110 degrees Celcius, HKUST-1 should not have degraded, but it is worth checking by PXRD anyway. I have never done this desolvation when the sample wasn't under vacuum, so I'm not sure whether the air interacts with HKUST-1 at these comparatively low temperatures.
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I have a chemical compound may used as indicator, how i can prepare a film from it such as litmus paper to detect some metals with different colors ?    
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what functional groups does the compound have?
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my complex is pentanuclear cobalt schiff base that is highly soluble in methanol ,acetonitrile, DCM. i tried a no of times with methanol , acetonirile solvent using slow evaporation technique in low temperature  but i could not get it.plz give suggestion.
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if slow evaporation fails, you can try other methods like diffusing other solvents, layering method, vapor diffusion etc
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I am doing Hydroboration of aldehyde with HBpin. I want to know the easiest method for hydrolysis of resultant boronte ester to alcohol.
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Dear Milan,
The hydrolysis of boronic esters to the boronic acid and the corresponding alcohol can take place by thionyl chloride and pyridine. Aryl boronic acids or esters can be hydrolyzed to the corresponding phenols by treating with hydroxylamine at RT.
References:
New asymmetric syntheses with boronic esters and fluoroboranes Donald S. Matteson Pure Appl. Chem., Vol. 75, No. 9, pp. 1249–1253, 2003.
A mild conversion of arylboronic acids and their pinacolyl boronate esters into phenols using hydroxylamine Ebrahim Kianmehr , Tetrahedron Letters ,vol. 48 , Issue 15 , 9 April 2007.
Hoping this will be helpful,
Rafik
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I am intending to optimize an organometallic complex with Gaussian and M06-2X functional. I am dissociating a bond (between two oxygen atoms), so the correspondent bond is frozen. However, I encountered the problem that tells "Cannot scale VSX exchange in M06-2X". I did not have any issue when proceeding with B3LYP. Hence, the problem might be due to the starting geometry and the exchange of the functional used. Nevertheless, is there anyway I could proceed with such an optimization imposing the constraint at the bond and employing the M062X funtional?
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Hello Enrique,
Thanks a lot for your reply! Actually, I have tried to perform optimization with both M06-HF and the pure functional M06-L. However, the obtained result is invariant. Therefore, the error must be due to another factor
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In catalytic oxidation of alkene reaction, aromatic, cyclic and longer chain alkenes gave aldehyde as a sole product [Ru catalyst, NaIO4 (oxidant), ACN/EtOAc/H2O].
But in case of cis 2-heptene and allylcyclopentane gave their corresponding acid as s sole product using the above same condition. Please explain the reason for over-oxidation. 
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Dear,
The conditions mentioned by you clearly indicates that you are bound to get carboxylic acid as a product.
I am a little amazed that you got aldehyde in some cases. 
Anyway, the problem is due to moisture, you have H2O so clearly it is bound to give carboxylic acid product.
If your goal is to get the aldehyde product I suggest you use Tetrapropylammonium perruthenate,  N-methylmorpholine N-oxide & molecular sieves.
Molecular sieves should be activated as they will absorb the moisture in it. 
I have personally performed this oxidation, so I told you about my experience. 
A link has been attached for you and it is called ley griffith oxidation
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1) Suggest a method for calculation of Critical Micelle concentration (CMC) value from peak wavelength obtained from Absorption v/s wavelength plot generated using Near Infrared Spectroscopy
2) For measuring surfactant under NIR Spectroscopy. I am considering wavelength range of 1400-2200 nm based on previous work. Please comment
3) Please have a look at the plot for better understanding of question
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 Important to choose the right range of wavelength for  calculation.
Don"t you satisfied by results? It is  good.
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Hexacarbonylcobalt-alkyne complex was the key intermediate in Nicholas reaction. The NMR characterization of these kind of organometalic compounds has been reported by hundreds of papers. When I was trying to character one of these compounds on bruker 400 MHz instrument  for 1H NMR, the shim process became quite problematic, a warning: "the signal to noise is too low" was come out after an autoshim process. Though I have tried to add more compound or used a mannual shim program, the peaks were still so wide that cannot be treated as a reliable spectrum. Can anyone help me on this sort of things?
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Hi, I think Pedro got the right answer and you have paramagnetic species in your sample. The other option would be convection in the sample that can also affect topshim. Try "topshim convcomp". This compensates for convection. If this still does not help it is most likely the paramagnetism.
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It is my understanding that the observed magnetic susceptibility (Xobs) of a material from SQUID magnetomtery data (MvT) is composed of several components
Xobs = Xpara + Xdia + Xtip
Where the paramagentic contribution (Xpara) is the key part to Curie/Curie Weiss law and for calculating the effective magnetic moment of a material. Thus the Diamagnetic contribution (Xdia) and Temperature independent paramagnetism contribution (Xtip) must be accounted for and subtracted from the Xobs in order to have an accurate description of the unpaired electrons.
The diamagnetic contribution (Xdia) from the electrons in the core orbitals can subtracted from the observed molar susceptibility by calculating from Pascals constants.
It my understanding plotting Xobs vs 1/T of a paramagnetic material will give Xtip as the intercept of the Y-axis i.e. X = C*1/T + Xtip, and thus one can easily subtract and get a nice curie plot and further calculate the effective magnetic moment.
However, I am unsure how to find/subtract the Xtip from an antiferromagnetic (or ferromagnetic for that matter) material without loosing the Weiss Constant (W). Surely if one subtracts the Y intercept then W=0 when we plot 1/Xp vs T.... what is the usual procedure for subtracting this so that one can accurately calculate W and more importantly the effective magnetic moment.....
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May be the attached article can help you
Best regards,
Pedro
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usually one calculates from their SQUID magnetometry MvT data
Ueff = 2.828*SQRT(Xp*T)
Where Ueff is the effective magnetic moment, Xp is the corrected paramagnetic susceptibility, and T is temperature
However do we need account for the Weiss constant also to get the correct result when considering ferro/antiferromagnetic materials?
so 
Ueff = 2.828*SQRT(Xp*(T-weiss constant)
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Yes, you would have to take it into account!
I usually go by the inverse susceptibility. It should be proportional to the temperature (which is easily checked) and you can get the (squared) effective moment from the slope. In such a plot the paramagnetic Curie-Weiss temperature corresponds just to a horizontal displacement of the curve and not a fit parameter since that does not affect the slope. Nevertheless you can read it off directly from the intersect of the straight with the temperature axis!.
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in case of organic ligand there r several techniques for purification,but in case of metal complex(Cr,Mn,Fe,Co) with schiff base  i have not seen any literature for the purification of them except recrystallization. give some suggestion..
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As has been already referred  that Imine bond in schiff bases is prone to hydrolysis. The rate of hydrolysis gets speeded up in presence of acid or base. The stationary phase used in column like silica or alumina have acidic sites which prompt the acid hydrolysis of the imine leading to the loss of product imine (in general case) so column chromatography is not sometimes  a good choice in case of schiff bases or imines.
This may or may not be true in your case as i donot know the exact nature of your compounds. I can recommend  purification through  solvent washing's. That is say for a hypothetical case we have an unreacted aldehyde   or  unreacted amine or ligand along with the product complex. Choose a dried solvent in which the product  is most soluble than the reactant aldehyde and ammine do multiple washings with solvent/ solvent system( work out such system over TLC for your case)  and remove the solvent to get the pure imine product.
in another case use multiple solvents first the one  in which aldeyde or amine of ligand is soluble to remove one of the reactants selectively then use another dried solvent to remove the second reactant selectively to purify  the final product.
You may have to optimize the work up protocol for your system
Selective Distillation separation can also be used if the boiling points of the components of mixture are different.
If the product imine is totally insoluble in some solvent, then best method would be purification by product crystallization.
i have tried to give  general approaches, hope any of these works for your system
good luck.
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can anybody tell the eualent base catalyst for Potassium tertiary butoxide for cyclisation reaction in Etoricoxib preparation ?
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thank you sir, could you plaese tell me more detailed 
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how can i remove HCl in a reaction which was formed as byproduct in chlorination reaction Thionyl chloride Used as chlorination  Agent, Solevt was toluene , Distillation at 80°C u/vacuum , but HCl content remains as 3 to 4 % , need to nullify the HCl content, can any body help?
co-distillation is possible? or Not ?
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A few things to note: firstly, HCl is not soluble in toluene, and therefore to say "the HCl content remains as 3-4%" does not sound correct.  In fact, toluene is used as a solvent precisely for this reason (as opposed to THF / Et2O /dioxane, which dissolve HCl; commercial solutions of HCl in these solvents are available ).
2. How do you know you see "3-4% HCl?" NMR? Give some info here.
3. You are working with pyridines; it is very likely whatever you see as "HCl" is the pyridinium salt. Heating and vac distillation probably won't help your cause. You will need to use an external base to deprotonate.
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I'm not sure of how it occurs. Thank you. :)
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OK, thank you very much for your answer :)
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I have synthesized Ru(II)thiosemicarbazone complexes with two different coordination modes. The H substituted thiosemicarbazone ligands gave Ru(II) hydride complexes NS donor having pseudo octahedral environment . But In the case of Phenyl substituent ligands results Cyclometallated Ru(II) thiosemicarbazone complexes with CNS coordination mode resulting octahedral geometry.
Both of the complexes has been synthesized in the same experimental conditions. What is the mechanism behind these two unusual coordination modes of thiosemicarbazone ligands?  Kindly related to literature reports
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May be this publication helps you
Organometallics 2008, 27, 175–180
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Can anyone help me understand the reaction mechanism of the synthesis of [trans-FeCl2(imidazole)4]Cl•THF•H2O ?
The complex is synthesized by first adding Fecl3 to THF. To that solution imidazol is added and then 2,2-dimethyl-1,3-propandiol. I dont think I quite understand how it works.
thankyou
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thankyou for your answer
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I have used hydrazine monohydrate as reducing agent with the Te powder and FeCl3 and reacting them at 600C by magnetic stirring for 2 hours but all i got peaks of Te in XRD.
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Mr. Swain,
For obtaining of Te-glasses you can read the following paper given as ref. 1. The procedure, however is different.
1. T. Kolev, B.Koleva, B. Schivachev, Oriented solids as a colloid suspension in nematic liquid
crystal – New tool for IR-spectroscopic and structural elucidation
of inorganic compounds and glasses, Inorganica Chimica Acta 361 (2008) 2002–2012
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Relates the reported literature.....
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Dear Ramasamy Raj Kumar
Kindly find this paper of your interest....
Journal of Coordination Chemistry, 2015
Regards
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I want to know which is the adequate force field for an organometallic system and how I can  create this topology file. I was working in some tutorials in gromacs with proteins but now I want to work in my own system.
Thank you in advance
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thanks for  your answers!
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You see MOs for a molecular system. Which is HOMO and which is LUMO orbital, since we have an half filled MO there? What do you think? 104 to 105 ? or ?
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More specifically, when there is one or more singly-occupied molecular orbital (SOMO), then the label SOMO is preferred instead of HOMO, since HOMO usually implies the highest doubly-occupied molecular orbital - likewise, LUMO is the lowest completely-unoccupied molecular orbital, so not the SOMO, but the next one
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Anyone tell me more about the chemical pathways of bioaccumulation of METALS in aquatic life? Interested in chemistry than toxic effects.
I am interested in how certain plankton or bivalves accumulate metals in their body, I am trying to understand the organometallic chemistry as well as the kinetics.
E.g.Wang et al 2008
or Emmanuel et al 2011 (on bacterial accumulation). 
doi: 10.1007/s12088-011-0111-8
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PS - Some of these processes are discussed in: http://www.sciencedirect.com/science/article/pii/S0045653513006942
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I'm looking for the criteria to folllow in the following topic. I'm not looking for a recipe.
I have a 3,5-pyridinedicarboxylic acid and Zn, Cu and Mg nitrate salts to make a MOF but the carboxylate only connect in a monodentate fashion instead of bidentate. Then I cannot form a cluster. Does anyone have a suggestion?
Thank you
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From data I looked up, there is NO SBU which has the requisite bidentate mode of chelation with 3,5-PDC. You only have the monodentate version. So maybe you have to rethink this. Unless you can find an SBU with the bidentate mode of chelation, this is going to be a tough ask, unless you alter your reaction conditions totally like Dr. Paech has suggested. Good luck on the hunt.
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I am taking cm and Columbus values. but not getting final result. So please inform. Peak under the curve in equation, where have to substitute (in which unit).
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Dear Rajamouli Boddula,
The following link contains a publication which depicts the units of the parameters in  Judd-Ofelt equations (theory):
Hoping this will be helpful,
rafik
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I have synthesized the Ruthenium(II) thioamide complexes containing OS donor. In the complex structure the pyrrolidine ring  attached with C-N bond undergoes cleavage( pyrrolidine ring escape) resulting the octahedral ruthenium OS donor complexes. What is the experimental observations for the C-N bond cleavage upon complex formation. Could you correlate the literature reports?
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Dear Sudarsan/
C-N activation or amide C-N bond cleavage?
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I've already attempted using a normal plasma cleaner for up to 30 minutes. It seems much of the sample is still covered in Carbon.
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Plasma cleaning will help for a typical carbon coating.  You may have to mill the carbon away with a FIB, but good luck, as Carbon is quite resilient to the FIB beam.  Curious to know results!
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I am fabricating an electrode which has platinum deposited on glass. on that organic compound is deposited using electrochemical method. Adhesion of the film on platinum is not good. I have also tried titanium to improve adhesion between glass and platinum. still the film of the organic compound is peeling off.
Any suggestion to improve the adhesion of the film on platinum would be appreciable. 
Thank you
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Not exactly. one reason of poor adhesion can be the oxide layer formation on the platinum surface.
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