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Inhibition of nitric oxide synthase with pyrazole-1-carboxamidine and related compounds.

Guanidines, amidines, S-alkylisothioureas, and other compounds containing the amidine function (-C(=NH)NH2) have been described as inhibitors of the generation of nitric oxide (NO) by NO synthase (NOS). Here we report on the inhibition of the activity of NOS isoforms by compounds in which the amidine function is attached to a nitrogen of 1,2-diazo heterocycles to form N-carboxamidines and related compounds. 1H-Pyrazole-1-carboxamidine HCl (PCA) inhibited the activity of purified inducible NOS (iNOS), endothelial NOS (eNOS), and neuronal NOS (nNOS) isoforms to a similar extent (IC50 = 0.2 microM). 3-Methyl-PCA and 4-methyl-PCA showed reduced potencies, but a preference for iNOS [IC50 = 5 and 2.4 microM, respectively; cf. N(G)-methyl-L-arginine (NMA) IC50 = 6 microM]. Inhibition of purified iNOS by PCAs could be reversed completely by excess L-arginine, while their inhibition of NO production by stimulated RAW macrophages could be reversed by transfer to a drug-free medium. This suggests a competitive mode of inhibition. PCA caused potent concentration-dependent inhibition of the acetylcholine-induced, endothelium-dependent relaxations of precontracted rat thoracic aorta (IC50 = 30 microM). 4-Methyl-PCA inhibited the relaxations only at > or = 300 microM. In contrast, 4-methyl-PCA was more effective than both PCA and NMA in restoring the ex vivo contractility of aortic rings taken from lipopolysaccharide-treated rats. PCA and NMA, but not 4-methyl-PCA, caused marked increases in mean arterial pressure when administered i.v. to anesthetized rats. In conclusion, PCA and related compounds caused potent inhibition of NOS. Substitution of the pyrazole ring reduced potency, but improved selectivity towards iNOS as exemplified by 4-methyl-PCA.

Animals↗

N1-alkyl-D-gluconamidines: are they 'perfect' mimics of the first transition state of glucosidase action?

The inhibition of four beta-glucosidases of plant, fungal, and mammalian origin by N1-butyl- and N1-dodecyl-D-gluconamidine was determined. Comparison with the inhibition by the corresponding N-alkyl-D-glucosylamines revealed that the strongly basic amidines (pKa 10.8) were at the most 10-times more inhibitory than the weakly basic glucosylamines (pKa 6.5). The small enhancement of inhibitory potency, resulting from transforming the tetrahedral C-1 geometry of the glucosylamines to the planar sp2-geometry of the amidines, was ascribed to the inability of the fully protonated amidines to function as hydrogen bond acceptors with the catalytic acid of the enzyme. Additional evidence for the importance of a hydrogen bond for strong inhibition came from the comparison of K1-values of the weakly basic 5-amino-5-deoxyhexopyranoses and 1,5-iminohexitols with those of the corresponding glyconamidrazones (pKa 8.4), which also have a planar C-1 geometry but are largely protonated under the assay conditions and which had similar or up to 10(4)-times larger K1-values than the former. Transition state resemblance was judged from the ratio KS(alkyl beta-glucoside)/K1(alkyl gluconamidine) relative to the rate acceleration factor kcat/kuncat (Wolfenden, Acc, Chem. Res., 5 (1972) 10-16). Compared to ratios of kcat/kuncat from > or = 10(11) to > or = 10(13), the ratios for KS/K1 were only from 10(3) to 2 x 10(4) except for beta-glucosidase A3 from Asp. wentii which had KS/K1 2.8 x 10(6). This enzyme differs from the others by being strongly inhibited by cationic glycon and substrate analogues rather than by basic ones. The pH-dependence of 1/K1 and the 'slow' approach to the inhibition is discussed with respect to transition state resemblance.

Binding Sites↗

Engineering inhibitors highly selective for the S1 sites of Ser190 trypsin-like serine protease drug targets.

BACKGROUND: Involved or implicated in a wide spectrum of diseases, trypsin-like serine proteases comprise well studied drug targets and anti-targets that can be subdivided into two major classes. In one class there is a serine at position 190 at the S1 site, as in urokinase type plasminogen activator (urokinase or uPA) and factor VIIa, and in the other there is an alanine at 190, as in tissue type plasminogen activator (tPA) and factor Xa. A hydrogen bond unique to Ser190 protease-arylamidine complexes between O gamma(Ser190) and the inhibitor amidine confers an intrinsic preference for such inhibitors toward Ser190 proteases over Ala190 counterparts. RESULTS: Based on the structural differences between the S1 sites of Ser190 and Ala190 protease-arylamidine complexes, we amplified the selectivity of amidine inhibitors toward uPA and against tPA, by factors as high as 220-fold, by incorporating a halo group ortho to the amidine of a lead inhibitor scaffold. Comparison of K(i) values of such halo-substituted and parent inhibitors toward a panel of Ser190 and Ala190 proteases demonstrates pronounced selectivity of the halo analogs for Ser190 proteases over Ala190 counterparts. Crystal structures of Ser190 proteases, uPA and trypsin, and of an Ala190 counterpart, thrombin, bound by a set of ortho (halo, amidino) aryl inhibitors and of non-halo parents reveal the structural basis of the exquisite selectivity and validate the design principle. CONCLUSIONS: Remarkable selectivity enhancements of exceptionally small inhibitors are achieved toward the uPA target over the highly similar tPA anti-target through a single atom substitution on an otherwise relatively non-selective scaffold. Overall selectivities for uPA over tPA as high as 980-fold at physiological pH were realized. The increase in selectivity results from the displacement of a single bound water molecule common to the S1 site of both the uPA target and the tPA anti-target because of the ensuing deficit in hydrogen bonding of the arylamidine inhibitor when bound in the Ala190 protease anti-target.

Animals↗

Structural effects of carbohydrate-containing polycations on gene delivery. 2. Charge center type.

Recent polycation structure-gene delivery studies reveal that subtle changes in the molecular structure of polycations have substantial influences on DNA-binding and condensation and on in vitro toxicity and gene delivery efficiency. In Part 1 of this structure-property study using carbohydrate-containing polycations (1), it is demonstrated that as the amidine charge center is removed further from the carbohydrate unit within the polycation structure, the toxicity increases. Inclusion of larger carbohydrate species within the polycation backbone also reduces the toxicity. Here, the effect that polycation charge center type has on toxicity and gene delivery efficiency is investigated. A series of quaternary ammonium polycations containing N,N,N',N'-tetramethyl-1,6-hexanediamine, d-trehalose, and beta-cyclodextrin are synthesized in order to elucidate the effects of charge center type (by comparison to the data given in Part 1) on gene delivery. In all cases, it is found that the quaternary ammonium analogues exhibit lower gene expression values and similar toxicities to their amidine analogues. Additionally, transfection experiments conducted in the presence of chloroquine reveal increased gene expression from quaternary ammonium containing polycations and not from their amidine analogues.

Animals↗

Neoglycoproteins: in vitro introduction of glycosyl units at glutamines in beta-casein using transglutaminase.

Exploring different methods for preparing neoglycoproteins with a specific number of oligosaccharides in specific positions, we have used guinea pig liver transglutaminase to incorporate glycosyl units into glutamine residues in beta-casein. In order to prevent epsilon-(gamma-glutamyl)lysine cross-link formation, the lysine residues of beta-casein were first blocked either by amidination with ethyl acetimidate or by acylation with succinic anhydride. The glycosyl donor substrates prepared for this work were maltotriose reductively aminated with cadaverine, N-(Glc-Glc-glucitol-1)-cadaverine, and an asparaginyl nonasaccharide from ovalbumin modified with a 6-aminohexanoyl group at the alpha-amino group. The transglutaminase-catalyzed incorporation of these two donors into the beta-casein derivatives was monitored in comparison to the incorporation of the commonly used transglutaminase substrate dansylcadaverine under conditions of optimal incorporation (multiple additions of enzyme, large excess of donor, and long incubation time). For both dansylcadaverine and Glc-Glc-Glc(OH)-cadaverine, 5 and 8 mol of donor were incorporated per mol of amidinated and succinylated beta-casein, respectively. Competition experiments showed that the two donor substrates are incorporated into the same glutamine sites. Partial sequencing of the glycosylated beta-casein permitted the identification of glutamine residues 56, 79, 167, 175, and 194 as the primary sites of incorporation in amidinated casein with residues 54 and 182 as possible sites for partial glycosylation. The results are consistent with a specific glycosylation of only selected glutamines in this transglutaminase-catalyzed process.(ABSTRACT TRUNCATED AT 250 WORDS)

Acyltransferases↗

Cytochrome b5 induced flip-flop of phospholipids in sonicated vesicles.

Cytochrome b5 induced flip-flop of phosphatidylethanolamine (PE) in sonicated vesicles prepared from a 9:1 mixture of phosphatidylcholine (PC) to phosphatidylethanolamine was determined as follows. First, vesicles having a nonequilibrium distribution of PE across the bilayer were prepared by amidinating the external amino groups with isethionyl acetimidate. Amidinated cytochrome b5 was then added, and after the protein was completely bound, the rate of appearance of fresh PE on the outer surface was determined by removing aliquots at timed intervals and titrating the external amino groups with trinitrobenzenesulfonic acid. The results show an initial rapid phase of flip-flop (especially in the presence of salt) followed by a very slow phase, at 25 degrees C. Similar results were obtained when cytochrome b5 was introduced into the amidinated vesicles by spontaneous transfer from PC donor vesicles. These results indicate that the accumulation of the transferable ("loose") form of cytochrome b5 on the outer surface of a vesicle causes a transient, global destabilization of the bilayer that is relieved by lipid flip-flop. We speculate that this mechanism may be a significant driving force for the transfer of amphipathic molecules across membranes.

Animals↗

Syntheses of mixed-ligand tetranuclear gold(I)-nitrogen clusters by ligand exchange reactions with the dinuclear gold(I) formamidinate complex Au(2)(2,6-Me2Ph-form)2.

The reaction of the sterically crowded dinuclear gold(I) amidinate complex Au2(2,6-Me2Ph-form)2, 1, with the less bulky bidentate nitrogen ligands results in the formation of tetranuclear gold(I) complexes. When the less bulky amidinate, K(4-MePh-form), A, was reacted with 1 in a 1:1 stoichiometric ratio, crystals containing equal amounts of the tetranuclear and dinuclear gold(I) aryl formamidinates, Au4(4-MePh-form)4 and Au2(2,6-Me2Ph-form)2, where 2,6-Me2Ph-form = B, were found in the same unit cell, 2 x 2THF: space group P, a = 10.794(11) A, b = 14.392(15) A, c = 25.75(3) A, alpha = 82.564(17) degrees, beta = 85.443(18) degrees, gamma = 82.614(19) degrees. The reaction of K(4-MePh-form), A, and 1 in a 1:2 ratio (excess) produced the tetranuclear complex only, 3. The potassium salt of the exchanged bulky ligand, K(2,6-Me2Ph-form), formed as a byproduct. The reaction of the dinuclear gold(I) complex Au2(2,6-Me2Ph-form)2 with the 3,5-diphenylpyrazolate salt, K(3,5-Ph2pz), resulted in the formation of two tetranuclear mixed-ligand complexes, Au4(3,5-Ph2pz)2(2,6-Me2Ph-form)2 x 2THF, 4 x 2THF (space group P21/c, a = 11.5747(19) A, b = 25.497(4) A, c = 21.221(3) A, beta = 96.979(3) degrees) and Au4(3,5-Ph2pz)3(2,6-Me2Ph-form) x THF, 5 x THF (space group P21/c, a = 23.058(5) A, b = 14.314(3) A, c = 18.528(4) A, beta = 90.94(3) degrees. The block crystals from the tetranuclear complex, 4 x 2THF, contain mixed ligands with each pyrazolate ring facing an amidinate ring. The tetranuclear mixed ligand complex, 5 x THF, was isolated as needles with ligands alternating above and below the Au4 plane. The two tetranuclear mixed-ligand complexes emit at 490 and 530 nm, respectively, under UV excitation.

Journal Article↗

Catalytic addition of terminal alkynes to carbodiimides by half-sandwich rare earth metal complexes.

The catalytic addition of terminal alkynes to carbodiimides has been achieved for the first time by use of half-sandwich rare earth metal complexes, such as {Me2Si(C5Me4)(NPh)}Y(CH2SiMe3)(THF)2, which offers a straightforward, atom-economic route to the N,N'-disubstituted propiolamidines which contain a conjugated C-C triple bond, a new family of amidines which were difficult to prepare by other means. A rare earth metal amidinate species was confirmed to be a true catalytic species in this process, thus demonstrating for the first time that an amidinate unit, though being often used as an ancillary ligand for various organometallic complexes, can itself participate in a catalytic reaction under appropriate conditions.

Journal Article↗

Spectroscopic determination of proton position in the proton-coupled electron transfer pathways of donor-acceptor supramolecule assemblies.

A homologous set of porphyrin derivatives possessing an isocyclic five-membered ring appended with an amidinium functionality has been used to examine proton-coupled electron transfer (PCET) through well-characterized amidine-carboxylic acid interfaces. Conjugation between the porphyrin chromophore and the amidinium interface can be altered by selective reduction of the isocyclic ring of an amidinium-purpurin to produce an amidinium-chlorin. The highly conjugated amidinium-purpurin displays large spectral shifts in the visible region upon alteration of the amidinium/amidine protonation state; no such change is observed for the chlorin homologue. Analysis of the UV-vis absorption and emission profiles of the amidinium-purpurin upon deprotonation allows for the measurement of the porphyrinic-amidinium acidity constant for the ground state (pKa = 9.55 +/- 0.1 in CH3CN) and excited state (pKa)= 10.40 +/- 0.1 in CH3CN). The absorption spectrum of the purpurin also provides a convenient handle for determining the protonation state of assembled interfaces. In this way, the purpurin macrocycle provides a general tool for PCET studies because it can be used to determine the location of a proton within PCET interfaces formed from carboxylic acid electron acceptors including dinitrobenzenes (DNBs) and naphthalenediimide (NI), which have been used extensively in previous PCET studies. An amidine-carboxylic acid interface is observed for electron-rich acceptors, whereas the ionized amidinium-carboxylate interface is observed for electron-poor acceptors. The PCET kinetics for purpurin/chlorin associated to NI are consistent with an amidine-carboxylic acid interface, which is also verified spectrally.

Algorithms↗

Noncovalent interactions between tetrazole and an N,N'-diethyl-substituted benzamidine.

Amidines have long been known to form strong noncovalent complexes with carboxylates and phosphates. However, their interaction with tetrazoles, which are acidic heterocycles and important bioisosteric replacements for carboxylic acids in medicinal chemistry, has remained unexplored so far. The binding of a tetrazole to an N,N'-diethyl-substituted benzamidine has been studied for the first time by X-ray crystallography, solution NMR methods, and electrospray mass spectrometry. The amidinium group of model complex 3 was found to prefer an E,Z configuration in the crystal. Benzamidinium and tetrazolate groups alternate along an infinite chain of hydrogen bonds and salt bridges between the amidine-NH groups and the two tetrazole-N atoms next to the ring carbon. In solution, a 1:1 complex was evident from Job's method of continuous variation, and an association constant of 4.0 x 10(3) +/- 1.6 x 10(3) M(-)(1) (in CDCl(3)/CD(3)CN, 6:1) could be determined by (1)H NMR dilution experiments. Tetrazolate was not only found to be a weaker ligand than carboxylates but, surprisingly, the binding mode also changed with concentration in neat CDCl(3). At low concentrations, the amidine group in complex 3 adapted an E,E configuration as it does in a related carboxylic acid complex 4. With increasing concentration, the E,Z isomer starts to predominate. A free activation enthalpy DeltaG(298)() of 64 +/- 1 kJ mol(-)(1) for the E,E to E,Z isomerization was determined by line shape analysis at different magnetic fields. Binding strength was further probed in a competition experiment between a bisamidine, a carboxylate, and a tetrazolate by electrospray mass spectrometry.

Benzamidines↗

Experimental and theoretical evidence of basic site preference in polyfunctional superbasic amidinazine: N(1),N(1)-dimethyl-N(2)-beta-(2-pyridylethyl)formamidine.

The gas-phase basicity (GB) of the flexible polyfunctional N(1),N(1)-dimethyl-N(2)-beta-(2-pyridylethyl)formamidine (1) containing two potential basic sites (the ring N-aza and the chain N-imino) is obtained from proton-transfer equilibrium constant measurements, using Fourier-transform ion-cyclotron resonance mass spectrometry. Comparison of the experimental GB obtained for 1 with those reported for model amidines and azines indicates that the chain N-imino in the amidine group is the favored site of protonation. Semiempirical (AM1) and ab initio calculations (HF, MP2, and DFT), performed for 1 and its protonated forms, confirm this interpretation. These results are in contrast to those found previously for N(1),N(1)-dimethyl-N(2)-azinylformamidines (containing the amidine function directly linked to the azinyl ring), in which the ring N-aza is the most basic site in the gas phase. The separation of the two potential basic sites in 1 by the ethylene chain interrupts the resonance conjugation between the two functions and changes their relative basicities and, thus, the preferable site of protonation. It also increases the chelation effect against the proton and the gas-phase basicity of 1 in such a magnitude that consequently 1 may be classified as a superbase (GB = 241.1 kcal mol(-)(1)). A transition state corresponding to the internal transfer of the proton (ITP) between the ring N-aza and the chain N-imino in 1 is investigated at the DFT(B3LYP)/6-31G level. The energy barrier calculated for the ITP between the two basic sites is small and vanishes when zero-point vibrational terms and thermal corrections are applied to obtain the enthalpy or Gibbs energy of activation for the proton transfer. Additional calculations at the DFT(MPW1K)/6-31G level confirm this behavior. This indicates that the quantum-chemical ITP in 1 has a single-well character. The proton is located on the N-imino site, and the H-bond is formed with the N-aza site.

Journal Article↗

Lipid mixing between lipoplexes and plasma lipoproteins is a major barrier for intravenous transfection mediated by cationic lipids.

It has been previously shown that transfection activity of cationic liposome/DNA lipoplexes delivered systemically is drastically inhibited by lipoproteins (Tandia, B. M., Vandenbranden, M., Wattiez, R., Lakhdar, Z., Ruysschaert, J. M., and Elouahabi, A. (2003) Mol Ther. 8, 264-273). In this work, we have compared the binding/uptake and transfection activities of DOTAP (N-[1-(2,3-dioleoyloxy)propyl]-N,N,N-trimethylammonium chloride) and diC14-amidine (3-tetradecylamino-N-tert-butyl-N'-tetra-decylpropionamidine)-containing lipoplexes in the presence or absence of purified low density lipoproteins and high density lipoprotein. Binding/uptake of both lipoplexes by the mouse lung endothelial cell line was inhibited to a similar extent in the presence of lipoproteins. In contrast, transfection activity of diC14-amidine-containing lipoplexes was almost completely inhibited (approximately by 95%), whereas approximately 40% transfection activity of DOTAP-containing lipoplexes was preserved in the presence of lipoproteins. Interestingly, the ability of lipoproteins to inhibit the transfection efficiency of lipoplexes was well correlated with their ability to undergo lipid mixing with the cationic lipid bilayer as revealed by fluorescence resonance energy transfer assay. Incubation of lipoplexes with increased doses of lipoproteins resulted in enhanced lipid mixing and reduced transfection activity of the lipoplexes in mouse lung endothelial cells. The role of lipid mixing in transfection was further demonstrated using lipid-mixing inhibitor, lyso-phosphatidylcholine, or activator (dioleoylphosphatidylethanolamine). Incorporation of Lyso-PC into diC14-amidine-containing lipoplexes completely abolished their capacity to undergo lipid mixing with lipoproteins and allowed them to reach a high transfection efficiency in the presence of lipoproteins. On the other hand, the incorporation of dioleoylphosphatidylethanolamine into DOTAP/DNA lipoplex activated lipid mixing with the lipoproteins and was shown to be detrimental toward the transfection activity of these lipoplexes. Taken together, these results indicate that fusion of lipoplexes with lipoproteins is a limiting factor for in vivo transfection.

Animals↗

Lysines of histone 1 represent the principal target for covalent binding of microsomally activated benzo[a]pyrene in vitro.

The principal target amino acid residue for covalent binding of metabolically activated [3H]benzo[a]pyrene (B[a]P) to histone 1 (H1) has been identified. Highly purified calf thymus H1 was modified by incubation with [3H]B[a]P in the presence of rat liver microsomes. The relative distribution of [3H]B[a]P versus specific amino acids among the N-bromo-succinimide peptides of H1 suggested that lysine may be the target. This was tested by selectively blocking the nucleophilic amino groups of lysine by amidination prior to [3H]B[a]P binding. Increasing levels of amidination of H1 resulted in corresponding decreases in the reactivity of this histone toward [3H]B[a]P. Amidination of 93% of the lysines blocked 87% of the [3H]B[a]P binding indicating that lysine was the principal target. N-terminal amino acid sequencing of [3H]B[a]P-modified H1 confirmed that lysine residues had bound [3H]B[a]P.

Benzopyrenes↗

4-Amino-N-isopropylbenzamidinium chloride ethanol solvate.

The title compound, C10H16N3+.Cl-.C2H6O, is an important intermediate in the convergent synthesis of amidine-substituted polycyclic heterocycles, a class of compounds that shows significant anticancer activity. The molecule of (I) is not planar, having a dihedral angle of 25.00 (7) degrees between the aniline and amidine (-C-NH=C=NH2) groups. The protonation of the amidine molecular fragment is accompanied by delocalized C-N bond distances of 1.320 (2) and 1.317 (2) A. The cations and chloride anions are involved in a network of hydrogen bonds, resulting in the formation of infinite chains propagating along the b direction. The chains are further grouped within the ab plane, in such a way that the structure is segregated into layers dominated by hydrophobic interactions involving N-isopropyl residues and layers dominated by N-H...Cl [N...Cl = 3.275 (2)-3.596 (2) A], O-H...Cl [O...Cl = 3.229 (3) A] and N-H...O [N...O = 2.965 (3) A] hydrogen bonds.

Benzamidines↗

Identification of a class of lysines within the non-specific DNA-binding site of RNA polymerase core enzyme from Escherichia coli.

The imido ester, methyl acetimidate, which specifically amidinates lysine residues, modifies RNA polymerase core enzyme, leading to rapid loss of activity. Calf thymus DNA partially protects the enzyme against this inactivation, an effect which disappears at high salt concentration. DNA protects 17 +/- 6 lysines from amidination at low salt concentration. The dependence of amidination on methyl acetimidate concentration is examined in the presence of DNA at high and low salt concentration. Analysis of the data suggests a class of approximately 12 lysines which are protected by DNA, consistent with the above estimate. These lysines are approximately 5--10-fold more reactive than most other available lysine residues.

Animals↗

The potential effects of new synthetic drugs against Leishmania amazonensis and Trypanosoma cruzi.

Amidine derivatives, never used before on trypanosomatids, were tested against Leishmania amazonensis and Trypanosoma cruzi. These drugs in doses up to 500 mg/kg inoculated into Swiss mice did not show any toxic effect (Santos, 1993). The in vitro effect of N,N'-diphenyl-4-R- benzamidine was evaluated. L. amazonensis promastigotes, epimastigotes and blood forms of T. cruzi, were assayed with/without the drugs in axenic media, using pentamidine isethionate and benznidazole, as reference drugs. The results were very promising for L. amazonensis, showing that the most active compounds were the metoxy and Br-derivatives, with LD50 of 20 microM and 22 microM, respectively. In general the amidines showed lower activity against T. cruzi than L. amazonensis. The most active compounds against blood trypomastigotes were the same metoxy and Br-derivatives, but in much higher concentrations, e.g. as LD50 of 59 nM and 251 nM, respectively. All amidines had a very low activity against epimastigotes, and the only active compounds were the halogen-derivatives with LD50 = 424 nM for the Br-derivative and LD50 of 474 nM for the C1-derivative.

Animals↗

Syntheses and selective inhibitory activities of terphenyl-bisamidines for serine proteases.

Biphenyl nitriles 5a-c, terphenyl dinitriles 11a-d, and naphthalene-bis(benzonitrile) 11c were prepared by palladium-catalyzed cross coupling reactions and subsequently converted to biphenyl amidines 8a-c and bis(benzamidines) 4a-e. Among the biphenyl amidines 8 only the meta-derivative 8b inhibits factor Xa and trypsin (Ki = 10 microM). The terphenyl bisamidine 4c does not inhibit factor Xa, trypsin, thrombin, and plasmin, while 4a and 4d are almost equipotent inhibitors of these enzymes (Ki 1-6 microM), and 4b and 4e are selective for trypsin (Ki = 0.2 and 0.3 microM; but Ki > 1 microM for factor Xa, thrombin, and plasmin). X-ray analysis of crystals of 4b complexed with bovine trypsin revealed a unique binding mode: one benzamidino group binds in the S1 site to the side chain carboxylate of Arg189. The central phenyl group is twisted away from the S2/S3 sites and the second amidino group contacts the Asn143 side chain.

Amidines↗

Hydrogen bonding in sulfonamides.

The hydrogen-bond connectivity in 39 sulfonamide crystal structures has been deciphered and described using graph set notation. The hydrogen-bond connectivity observed is used to gain information on hydrogen-bond preferences of specific donor and acceptor atoms of related sulfonamide molecules. The amido protons show a greater preference for hydrogen bonding to amidine nitrogens and cocrystal guests, whereas the amino protons show a greater preference for hydrogen bonding to sulfonyl oxygens, forming the only dominant hydrogen-bond pattern, a chain with an eight atom repeat unit. Preferential hydrogen bonding between the amidine group and the guest carboxyl group was observed in five cocrystal structures of sulfamethazine. Sulfamoxole displays a conformation and a hydrogen-bond motif not seen in any other structures. Sulfamerazine and sulfamethazine, differing by a methyl group, show no similarity in hydrogen-bond pattern, whereas sulfamethoxydiazine and sulfamethoxymethazine, which have sterically similar but chemically different heterocycles, show a striking similarity in hydrogen-bond pattern. Sulfamethoxydiazine, sulfamethoxymethazine, and sulfamethoxazole also show a large variation in hydrogen-bond pattern between polymorphs. Studies such as this, by revealing details of hydrogen-bonding patterns in closely related organic crystal structures, can potentially provide predictive capability among the crystal structures of pharmaceutical solids.

Algorithms↗