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1.  Crystal structure of di­aqua­bis­(4-tert-butyl­benzoato-κO)bis­(nicotinamide-κN 1)cobalt(II) dihydrate 
The asymmetric unit of the monomeric cobalt complex, [Co(C11H13O2)2(C6H6N2O)2(H2O)2]·2H2O, contains one half of the complex mol­ecule, one coordinating and one non-coordinating water, one 4-tert-butyl­benzoate (TBB) ligand and one nicotinamide (NA) ligand; the Co atom lies on an inversion centre. The coordinating water mol­ecules are hydrogen bonded to the carboxyl O atoms [O ⋯ O = 2.6230 (17) Å], enclosing an S(6) hydrogen-bonding motif, while inter­molecular O—H⋯O hydrogen bonds link two of the non-coordinating water mol­ecules to the coordinating water mol­ecules and NA anions. In the crystal, O—H⋯O and N—H⋯O hydrogen bonds link the mol­ecules, enclosing (8), (10) and (12) ring motifs, forming layers parallel to (001).
The asymmetric unit of the mononuclear cobalt complex, [Co(C11H13O2)2(C6H6N2O)2(H2O)2]·2H2O, contains one half of the complex mol­ecule, one coordinating and one non-coordinating water mol­ecule, one 4-tert-butyl­benzoate (TBB) ligand and one nicotinamide (NA) ligand; the Co atom lies on an inversion centre. All ligands coordinating to the Co atom are monodentate. The four nearest O atoms around the Co atom form a slightly distorted square-planar arrangement, with the distorted octa­hedral coordination completed by the two pyridine N atoms of the NA ligands at distances of 2.1638 (11) Å. The coordinating water mol­ecules are hydrogen bonded to the carboxyl O atoms [O ⋯ O = 2.6230 (17) Å], enclosing an S(6) hydrogen-bonding motif, while inter­molecular O—H⋯O hydrogen bonds link two of the non-coordinating water mol­ecules to the coordinating water mol­ecules and NA anions. The dihedral angle between the planar carboxyl­ate group and the adjacent benzene ring is 29.09 (10)°, while the benzene and pyridine rings are oriented at a dihedral angle of 88.53 (4)°. In the crystal, O—H⋯O and N—H⋯O hydrogen bonds link the mol­ecules, enclosing R 2 2(8), R 2 2(10) and R 4 4(12) ring motifs, forming layers parallel to (001). The C and H atoms of the tert-butyl group of the TBB ligand are disordered over two sets of sites with an occupancy ratio of 0.631 (5):0.369 (5).
doi:10.1107/S2056989016008689
PMCID: PMC4992899  PMID: 27555924
crystal structure; cobalt(II); transition metal complexes; benzoic acid; nicotinamide
2.  6-{5-Amino-3-tert-butyl-4-[(E)-(3-methyl-1,2,4-thiadiazol-5-yl)diazen­yl]-1H-pyrazol-1-yl}-1,3,5-triazine-2,4(1H,3H)-dione–1-methyl­pyrrolidin-2-one–water (1/1/1) 
In the title compound, C13H16N10O2S·C5H9NO·H2O, the entire 1-methylpyrrolidin-2-one (NMP) mol­ecule is disordered over two sites with occupancies of 0.488 (5) and 0.512 (5). The six-membered triazine ring and the two five-membered pyrazole and thiadia­zole rings, together with the diazene (–N=N–) linkage are almost coplanar (r.m.s. deviation for the non-H atoms = 0.0256 Å) with methyl groups from the tert-butyl substituent on the pyrazole ring located above and below the plane. Three intra­molecular N—H⋯N hydrogen bonds contribute to the planarity of the system. The O atom of the NMP mol­ecule is hydrogen bonded to an O—H group of water. In turn, the water mol­ecule is hydrogen bonded to the mono-azo skeleton through inter­molecular N—H⋯O and O—H⋯N hydrogen bonds. At both ends of the long mol­ecular axis of the main mol­ecule there are inter­molecular N—H⋯N hydrogen bonds, arranged in a head-to-tail fashion, between the N—H group of the triazine ring of one mol­ecule and the N atom of the thia­diazole ring of a neighboring mol­ecule. These form a polymeric chain along [110] or [10]. The main mol­ecules are stacked alternately along the b axis, which effectively cancels their dipole moments. In addition, pairs of alternate molecules are dimerized via inter­molecular hydrogen bonds involving the solvent mol­ecules.
doi:10.1107/S1600536810010871
PMCID: PMC2983887  PMID: 21580749
3.  Crystal structure of 2-(4-tert-butyl­phen­yl)-3-hydroxy-4H-chromen-4-one 
The title compound is relatively planar with the benzene ring being only slightly twisted with respect to the mean plane of the 4H-chromene-4-one moiety (r.m.s. deviation = 0.0191 Å) by 10.53 (8)°. In the crystal, mol­ecules are linked by pairs of O—H⋯O hydrogen bonds, forming inversion dimers with an (10) ring motif.
Yellow–green fluorescent crystals of the title compound, C19H18O3, were obtained by the reaction of hy­droxy­aceto­phenone and 4-tert-butyl­benzaldehyde with hydrogen peroxide as oxidant. The plane of the benzene ring is slightly twisted to the mean plane of the 4H-chromene-4-one moiety (r.m.s. deviation = 0.0191 Å) by 10.53 (8)°. In the crystal, mol­ecules are linked by pairs of O—H⋯O hydrogen bonds, forming inversion dimers with an R 2 2(10) ring motif. The dimers are linked via C—H⋯π inter­actions, forming sheets parallel to (10-1).
doi:10.1107/S2056989015011482
PMCID: PMC4518945  PMID: 26279877
crystal structure; flavonol; hydrogen bonding; fluorescent material
4.  Crystal structures of two hydrazinecarbo­thio­amide derivatives: (E)-N-ethyl-2-[(4-oxo-4H-chromen-3-yl)methyl­idene]hydrazinecarbo­thio­amide hemi­hydrate and (E)-2-[(4-chloro-2H-chromen-3-yl)methyl­idene]-N-phenyl­hydrazinecarbo­thio­amide 
The title compounds, (I) and (II), are hydrazinecarbo­thio­amide derivatives. In the crystal of (I), two independent mol­ecules are linked by bifurcated N—H⋯O and C—H⋯O hydrogen bonds, forming two (6) ring motifs, and (10) and (14) ring motifs. In the crystal of (II), mol­ecules are linked by pairs of N—H⋯S hydrogen bonds, forming inversion dimers with an (8) ring motif.
The title compounds, C13H13N3O2S·0.5H2O, (I), and C17H14ClN3OS, (II), are hydrazinecarbo­thio­amide derivatives. Compound (I) crystallizes with two independent mol­ecules (A and B) and a water mol­ecule of crystallization in the asymmetric unit. The chromene moiety is essentially planar in mol­ecules A and B, with maximum deviations of 0.028 (3) and 0.016 (3) Å, respectively, for the carbonyl C atoms. In (II), the pyran ring of the chromene moiety adopts a screw-boat conformation and the phenyl ring is inclined by 61.18 (9)° to its mean plane. In the crystal of (I), bifurcated N—H⋯O and C—H⋯O hydrogen bonds link the two independent mol­ecules forming A–B dimers with two R 2 1(6) ring motifs, and R 2 2(10) and R 2 2(14) ring motifs. In addition to these, the water mol­ecule forms tetra­furcated hydrogen bonds which alternately generate R 4 4(12) and R 6 6(22) graph-set ring motifs. There are also π–π [inter-centroid distances = 3.5648 (14) and 3.6825 (15) Å] inter­actions present, leading to the formation of columns along the c-axis direction. In the crystal of (II), mol­ecules are linked by pairs of N—H⋯S hydrogen bonds, forming inversion dimers with an R 2 2(8) ring motif. The dimers are linked by C—H⋯π inter­actions, forming ribbons lying parallel to (210).
doi:10.1107/S2056989015003369
PMCID: PMC4350706  PMID: 25844194
crystal structure; hydrazinecarbo­thio­amide; thio­urea derivatives; α-N-heterocycle; hydrogen bonding
5.  Crystal structure of N-[(4-eth­oxy­phen­yl)carbamo­thio­yl]cyclo­hexa­ne­carboxamide 
The asymmetric unit of the title compound, C16H22N2O2S, contains two crystallographically independent mol­ecules (A and B). In mol­ecule A, the cyclo­hexane ring is disordered over two orientations [occupancy ratio 0.841 (10):0.159 (10)]. In each mol­ecule, the central carbonyl thio­urea unit is nearly planar (r.m.s. deviations for all non-H atoms of 0.034 Å in mol­ecule A and 0.094 Å in mol­ecule B). In both mol­ecules, the cyclo­hexane ring adopts a chair conformation. The mean plane of the cyclo­hexane ring makes dihedral angles of 35.8 (4) (mol­ecule A) and 20.7 (3)° (mol­ecule B) with that of the benzene ring. Each mol­ecule features an intra­molecular N—H⋯O hydrogen bond, which closes an S(6) ring motif. In the crystal, mol­ecules are linked via pairs of weak N—H⋯S inter­actions, forming inversion dimers with an R 2 2(8) ring motif for both mol­ecules. The crystal structure also features weak C—H⋯π ring inter­actions.
doi:10.1107/S205698901501806X
PMCID: PMC4645074  PMID: 26594545
crystals structure; thio­urea derivatives; biological properties; anti­corrosion properties; cyclo­hexa­necarboxamide; C—H⋯π inter­actions
6.  Tetra­kis(μ2-4-amino­benzoato)di-μ3-oxido-tetra­kis[dibutyl­tin(IV)] 
The mol­ecule of the title compound, [Sn4(C4H9)8(C7H6NO2)4O2], lies about an inversion centre and is a tetra­nuclear bis­(tetra­butyl­dicarboxyl­ato­distannoxane) complex containing a planar Sn4O2 core in which two μ3-oxide O atoms connect an Sn2O2 ring to two exocyclic Sn atoms. Each Sn atom has a highly distorted octa­hedral coordination. In the mol­ecule, the carboxyl­ate groups of two amino­benzoate ligands bridge the central and exocyclic Sn atoms, while two further amino­benzoate ligands have highly asymmetric bidentate chelation to the exocyclic Sn atoms plus long O⋯Sn inter­actions with the central Sn atoms. Each Sn atom is also coordinated by two pendant n-butyl ligands, which extend roughly perpendicular to the plane of the Sn4O10 core. Only one of the four unique hydrogen-bond donor sites is involved in a classic N—H⋯O hydrogen bond, and the resulting supra­molecular hydrogen-bonded structure is an extended two-dimensional network which lies parallel to the (100) plane and consists of a checkerboard pattern of four-connected mol­ecular cores acting as nodes. The amine groups not involved in the hydrogen-bonding inter­actions have significant N—H⋯π inter­actions with neighbouring amino­benzene rings.
doi:10.1107/S0108270110003033
PMCID: PMC2855585  PMID: 20203395
7.  (2,6-Bis{5-amino-3-tert-butyl-4-[(3-methyl-1,2,4-thia­diazol-5-yl)diazen­yl]-1H-pyrazol-1-yl}-4-oxo-1,4-dihydro-1,3,5-triazin-1-ido)methanol(phenol)sodium phenol tetra­solvate 
The title compound, [Na(C23H28N17OS2)(CH3OH)(C6H5OH)]·4C6H5OH, is a five-coordinate NaI complex. The Na+ cation is bound to three N atoms of the triazinide ligand, two from each pyrazole ring and one from the central deprotonated triazine ring system. O atoms from a methanol and a phenol mol­ecule complete the five-coordinate NaN3O2 coordination environment. The asymmetric unit also includes three complete and two half phenol mol­ecules, four of which are hydrogen bonded to the N atoms of the thia­diazole ring. Two of the phenol solvent mol­ecules are disordered over two discrete inversion centres. The triazinide ligand is essentially planar (mean deviation from the least-squares plane = 0.0524 Å), with the methyl groups of the tert-butyl substituents on the pyrazole rings located above and below the plane. The planarity of this system is further assisted by the formation of four intra­molecular N—H⋯N hydrogen bonds between the N—H bonds of both amino groups on the pyrazole rings and the N atoms of the triazine ring and also from each of the adjacent diazene (–N=N–) bonds. The highly polar mol­ecules are stacked along the a axis through the central Na atom sandwiched by two kinds of alternating inter­molecular hydrogen bonds: O(carbon­yl)⋯H—O(methanol)/Na/O—H(phenol)⋯O(carbon­yl). These inter­actions form two polymer chains per mol­ecule.
doi:10.1107/S160053681001086X
PMCID: PMC2983962  PMID: 21580548
8.  Crystal structure of (E)-N-{2-[2-(4-methyl­benzyl­idene)hydrazin-1-yl]-2-oxoeth­yl}-p-toluene­sulfonamide 
The title compound, an aryl­sulfonyl glycinyl aryl hydrazone Schiff base, crystallizes with two independent mol­ecules in the asymmetric unit. In the crystal, a series of N—H⋯O and C—H⋯O hydrogen bonds and C—H⋯π and slipped parallel π–π inter­actions link the mol­ecules, forming a three-dimensional structure.
The title acyl­hydrazone derivative, C17H19N3O3S, containing an amino acid moiety and electron-donating substituents attached to both the phenyl rings, crystallized with two independent mol­ecules (A and B) in the asymmetric unit. The mol­ecules are bent at the S atom, with C—SO2—NH—CH2 torsion angles of −67.3 (2) and 67.7 (3)° in mol­ecules A and B, respectively. Further, the dihedral angles between the sulfonyl­glycine segments and the p-toluene­sulfonyl rings are 76.1 (1) and 85.8 (1)° in mol­ecules A and B, respectively. The central hydrazone segments and the toluene rings attached to them are almost co-planar with their mean planes being inclined to one another by 5.2 (2) (mol­ecule A) and 2.9 (2)° (mol­ecule B). The dihedral angles between the benzene rings are 86.83 (12) (mol­ecule A) and 74.00 (14)° (mol­ecule B). In the crystal, the A mol­ecules are linked by a pair of N—H⋯O hydrogen bonds, forming inversion dimers with an R 2 2(8) ring motif. The dimers are linked via three N—H⋯O hydrogen bonds involving the B mol­ecules, forming chains along [100] and enclosing R 2 2(12) and R 4 4(16) ring motifs. The chains are linked via C—H⋯O hydrogen bonds and a C—H⋯π inter­action, forming sheets parallel to (010). There is a further C—H⋯π inter­action and a slipped parallel π–π inter­action [inter-centroid distance = 3.8773 (16) Å] between the sheets, leading to the formation of a three-dimensional framework.
doi:10.1107/S2056989015009330
PMCID: PMC4459384  PMID: 26090163
crystal structure; p-toluene­lsulfon­yl; glycin­yl; aryl­hydrazone; hydrogen bonding
9.  Crystal structure of 2-hy­droxy­imino-2-(pyridin-2-yl)-N′-[1-(pyridin-2-yl)ethyl­idene]acetohydrazide 
The mol­ecule of the title compound is approximately planar with the planes of the two pyridine rings inclined to one another by 5.51 (7)°. In the crystal, mol­ecules are linked by bifurcated O—H⋯(O,N) hydrogen bonds, forming inversion dimers, which are in turn linked via C—H⋯O and C—H⋯N hydrogen bonds, forming sheets lying parallel to (502).
The mol­ecule of the title compound, C14H13N5O2, is approximately planar (r.m.s deviation for all non-H atoms = 0.093 Å), with the planes of the two pyridine rings inclined to one another by 5.51 (7)°. The oxime group is syn to the amide group, probably due to the formation of an intra­molecular N—H⋯N hydrogen bond that forms an S(6) ring motif. In the crystal, mol­ecules are linked by pairs of bifurcated O—H⋯(O,N) hydrogen bonds, forming inversion dimers. The latter are linked via C—H⋯O and C—H⋯N hydrogen bonds, forming sheets lying parallel to (502). The sheets are linked via π–π stacking inter­actions [inter-centroid distance = 3.7588 (9) Å], involving the pyridine rings of inversion-related mol­ecules, forming a three-dimensional structure.
doi:10.1107/S1600536814025793
PMCID: PMC4257442  PMID: 25552998
crystal structure; hy­droxy­imino; acetohydrazide; pyridyl­ethyl­idene; hydrogen bonding; π–π stacking inter­actions
10.  2-tert-Butyl 4-methyl 3,5-dimethyl-1H-pyrrole-2,4-dicarboxyl­ate 
In the title mol­ecule, C13H19NO4, except for two C atoms of the tert-butyl group, the non-H atoms are almost coplanar (r.m.s. deviation = 0.2542 Å). In the crystal, mol­ecules are linked into centrosymmetric dimers by two inter­molecular N—H⋯O hydrogen bonds, forming an R 2 2(10) ring motif.
doi:10.1107/S1600536812020120
PMCID: PMC3379292  PMID: 22719490
11.  Crystal structure of 1,2-bis­[(2-tert-butyl­phen­yl)imino]­ethane 
The whole molecule of the title compound, C22H28N2, (I), is generated by inversion symmetry. The mol­ecule is rather similar to that of 2,3-bis­[(2-tert-butyl­phen­yl)imino]­butane, (II), a di­imine ligand comprising similar structural features [Ferreira et al. (2006 ▶). Acta Cryst. E62, o4282–o4284]. Both ligands crystallize with the –N=C(R)—C(R)=N– group around an inversion centre, in a trans configuration. Comparing the two structures, it may be noted that the independent planar groups in both mol­ecules [the central link, –N=C(R)—C(R)=N–, and the terminal aromatic ring] subtend an angle of 69.6 (1)° in (II) and 49.4 (2)° in (I). Ferreira and co-workers proposed that such angle deviation may be ascribed to the presence of two non-classical intra­molecular hydrogen bonds and steric factors. In fact, in (I), similar non-classical hydrogen bonds are observed, and the larger angular deviation in (II) may be assigned to the presence of methyl groups in the di­imino fragment, which can cause steric hindrance due to the presence of bulky tert-butyl substituents in the aromatic rings. The C=N bond lengths are similar in both compounds and agree with comonly accepted values.
doi:10.1107/S2056989015008610
PMCID: PMC4459346  PMID: 26090180
crystal structure; di­imine; non-classical hydrogen bonds; DNA
12.  Poly[[tetra­aqua­bis­(μ3-1H-imidazole-4,5-dicarboxyl­ato)tetra­kis­(μ2-1H-imidazole-4,5-dicarboxyl­ato)tricobalt(II)diytterbium(III)] dihydrate] 
The asymmetric unit of the title compound, {[Co3Yb2(C5H2N2O4)6(H2O)4]·2H2O}n, contains one YbIII ion, two CoII ions (one situated on an inversion centre), three imidazole-4,5-dicarboxyl­ate ligands, two coordinated water mol­ecules and one uncoordinated water mol­ecule. The YbIII ion is seven-coordinated, in a monocapped trigonal prismatic coordination geometry, by six O atoms from three imidazole-4,5-dicarboxyl­ate ligands and one water O atom. Both CoII ions are six-coordinated in a slightly distorted octa­hedral geometry. The CoII ion that is located on an inversion center is coordinated by two O atoms from two water mol­ecules, as well as two O atoms and two N atoms from two imidazole-4,5-dicarboxyl­ate ligands. The second CoII ion is bonded to four O atoms and two N atoms from four imidazole-4,5-dicarboxyl­ate ligands. These metal coordination units are connected by bridging imidazole-4,5-dicarboxyl­ate ligands, generating a three-dimensional network. The crystal structure is further stabilized by N—H⋯O, O—H⋯O and C—H⋯O hydrogen-bonding inter­actions involving the water mol­ecules and the imidazole-4,5-dicarboxyl­ate ligands.
doi:10.1107/S1600536811028285
PMCID: PMC3212186  PMID: 22090888
13.  Crystal structure of (E)-N-{2-[2-(2-chloro­benzyl­idene)hydrazin-1-yl]-2-oxoeth­yl}-4-methyl­benzamide monohydrate 
The title compound is twisted in such a way that the almost planar [Car—C(=O)—N(H)—C(H2] and [C(H2)—C(=O)N(H)—N=C(H)—Car] segments are inclined to on another by 77.36 (8)°, while the benzene rings are inclined to one another by 89.69 (9)°. In the crystal, mol­ecules are linked via pairs of N—H⋯O hydrogen bonds, forming inversion dimers which are linked by O—H⋯O hydrogen bonds, involving the crystal water mol­ecule, forming chains propagating along the a-axis direction.
The title compound, C17H16ClN3O2·H2O, an acyl­hydrazone derivative, contains a glycine moiety and two substituted benzene rings on either end of the chain. It crystallized as a monohydrate. The mol­ecules adopt an E conformation with respect to the C=N double bond, as indicated by the N—N=C—C torsion angle of 179.38 (14)°. The mol­ecule is twisted in such a way that the almost planar Car—C(=O)—N(H)—C(H2) and C(H2)—C(=O)N(H)—N=C—Car [r.m.s deviations = 0.009 and 0.025 Å, respectively] segments are inclined to on another by 77.36 (8)°, while the benzene rings are normal to one another, making a dihedral angle of 89.69 (9)°. In the crystal, the water mol­ecule links three mol­ecules through two O—H⋯O and one N—H⋯O hydrogen bonds. The mol­ecules are linked via pairs of N—H⋯O hydrogen bonds, forming inversion dimers with an R 2 2(14) ring motif. The dimers are linked by O—H⋯O hydrogen bonds, involving two mol­ecules of water, forming chains along [100], enclosing R 2 2(14) and R 2 2(18) ring motifs. The chains are linked through C—H⋯O inter­actions, forming sheets parallel to (010). Within the sheets, there are C—H⋯π and parallel slipped π–π stacking inter­actions present [inter-centroid distance = 3.6458 (12) Å].
doi:10.1107/S2056989015011147
PMCID: PMC4518978  PMID: 26279870
crystal structure; glycinyl hydrazone; monohydrate; hydrogen bonding
14.  Crystal structures of three indole derivatives: 3-ethnyl-2-methyl-1-phenyl­sulfonyl-1H-indole, 4-phenyl­sulfonyl-3H,4H-cyclo­penta­[b]indol-1(2H)-one and 1-{2-[(E)-2-(5-chloro-2-nitro­phen­yl)ethen­yl]-1-phenyl­sulfonyl-1H-indol-3-yl}ethan-1-one chloro­form monosolvate 
The title compounds, (I), (II) and (III), are indole derivatives. Compounds (I) and (II) present two independent moieties in the asymmetric unit, and their packing is led by C—H⋯O hydrogen bonds and C—H⋯π inter­actions. In compound (III), the C—H⋯O hydrogen bonds form (22) inversion dimers.
The title compounds, C17H13NO2S, (I), C17H13NO3S, (II), and C24H17ClN2O5S·CHCl3, (III), are indole derivatives. Compounds (I) and (II) crystalize with two independent mol­ecules in the asymmetric unit. The indole ring systems in all three structures deviate only slightly from planarity, with dihedral angles between the planes of the pyrrole and benzene rings spanning the tight range 0.20 (9)–1.65 (9)°. These indole ring systems, in turn, are almost orthogonal to the phenyl­sulfonyl rings [range of dihedral angles between mean planes = 77.21 (8)–89.26 (8)°]. In the three compounds, the mol­ecular structure is stabilized by intra­molecular C—H⋯O hydrogen bonds, generating S(6) ring motifs with the sulfone O atom. In compounds (I) and (II), the two independent mol­ecules are linked by C—H⋯O hydrogen bonds and C—H⋯π inter­actions, while in compound (III), the mol­ecules are linked by C—H⋯O hydrogen bonds, generating R 2 2(22) inversion dimers.
doi:10.1107/S2056989015014917
PMCID: PMC4555396  PMID: 26396842
crystal structure; phenyl­sulfon­yl; indole derivatives; hydrogen bonding
15.  1-(2-Chloro-5-nitro­phen­yl)-3-(2,2-di­methyl­propion­yl)thio­urea 
With the exception of the C atoms of two of the methyl groups of the tert-butyl substituent, all of the non-H atoms of the title compound, C12H14ClN3O3S, lie on a mirror plane. The 2-chloro-5-nitro­phenyl and 2,2-dimethyl­propionyl substituents are, respectively, cis and trans relative to the thio­carbonyl S atom across the two C—N bonds. Intra­molecular N—H⋯O and C—H⋯S hydrogen bonds form S(6) ring motifs, also in the mirror plane. Despite the presence of two N—H subsituents, no inter­molecular hydrogen bonds are observed in the crystal structure. Weak π–π contacts [centroid–centroid distances of 4.2903 (17) Å] involving adjacent aromatic rings link the mol­ecules in a head-to-tail fashion above and below the mol­ecular plane.
doi:10.1107/S1600536809024672
PMCID: PMC2977335  PMID: 21583450
16.  Poly[tetra­deca­aqua­tetra­kis­(μ3-1H-imidazole-4,5-dicarboxyl­ato)tetra-μ3-sulfato-cobalt(II)hexa­gadolinium(III)] 
The asymmetric unit of the title compound, [CoGd6(C5H2N2O4)4(SO4)6(H2O)14]n, contains a CoII ion (site symmetry ), three GdIII ions, two imidazole-4,5-dicarboxyl­ate ligands, three SO4 2− anions, and seven coordinated water mol­ecules. The CoII ion is six-coordinated by two O atoms from water mol­ecules, two O atoms and two N atoms from two imidazole-4,5-dicarboxyl­ate ligands, giving a slightly distorted octa­hedral geometry. The GdIII ions exhibit three types of coordination environments. One Gd ion is eight-coordinated in a bicapped trigonal–prismatic geometry by four O atoms from two imidazole-4,5-dicarboxyl­ate ligands, two O atoms from two SO4 2− anions and two coordinated water mol­ecules. The other Gd ions are nine-coordinated in a tricapped trigonal–prismatic geometry; one of these Gd ions is bonded to four O atoms from two imidazole-4,5-dicarboxyl­ate ligands, three O atoms from three SO4 2− anions and two water O atoms and the other Gd ion is coordinated by one O atom and one N atom from one imidazole-4, 5-dicarboxyl­ate ligand, five O atoms from three SO4 2− anions as well as two coordinated water mol­ecules. These metal coordination units are connected by bridging imidazole-4,5-dicarboxyl­ate and sulfate ligands, generating a three-dimensional network. The crystal structure is further stabilized by N—H⋯O, O—H⋯O, and C—H⋯O hydrogen-bonding inter­actions between water mol­ecules, SO4 2− anions, and imidazole-4,5-dicarboxyl­ate ligands.
doi:10.1107/S1600536811026821
PMCID: PMC3212143  PMID: 22090845
17.  Crystal structures of methyl (E)-3-(2-chloro­phen­yl)-2-({2-[(E)-2-nitro­vin­yl]phen­oxy}meth­yl)acrylate and methyl (E)-2-({4-chloro-2-[(E)-2-nitro­vin­yl]phen­oxy}meth­yl)-3-(2-chloro­phen­yl)acrylate 
In the title compounds, (I) and (II), both of which crystallize in the monoclinic space group P21/n, the methyl acrylate and nitro­vinyl units are relatively planar with an E conformation about the C=C bonds. The two aromatic rings are inclined to one another by 74.87 (9) and 75.65 (2)° for compounds (I) and (II), respectively. In the crystal of (I), chains along the b axis are formed via C—H⋯O hydrogen bonds. In the crystal of (II), mol­ecules are linked by C—H⋯O hydrogen bonds, forming sheets parallel to the ac plane.
The title compounds, C19H16ClNO5, (I), and C19H15Cl2NO5, (II), both crystallize in the monoclinic space group P21/n. They differ essentially in the orientation of the methyl acetate group, with the C=O bond directed towards the NO2 group in (I) but away from it in (II). In compound (I), the mean plane of the methyl acrylate unit is planar, with a maximum deviation of 0.0044 (2) Å for the methyl C atom, while in (II) this deviation is 0.0147 Å. The inter­planar angles between the two aromatic rings are 74.87 (9) and 75.65 (2)° for compounds (I) and (II), respectively. In both compounds, the methyl acrylate and nitro­vinyl groups each adopt an E conformation about the C=C bond. In the crystal of (I), mol­ecules are linked by C—H⋯O hydrogen bonds forming chains along the b axis. The chains are linked via C—H⋯Cl hydrogen bonds, forming sheets parallel to the ab plane. The sheets are linked via C—H⋯π inter­actions, forming a three-dimensional structure. In the crystal of (II), mol­ecules are linked by pairs of C—H⋯O hydrogen bonds, forming inversion dimers with an R 2 2(30) ring motif. The dimers are linked via C—H⋯O hydrogen bonds, forming sheets parallel to the ac plane and enclosing R 4 4(28) ring motifs. The sheets are linked via parallel slipped π–π inter­actions (inter­centroid distances are both ca 3.86 Å), forming a three-dimensional structure.
doi:10.1107/S2056989016001493
PMCID: PMC4770962  PMID: 26958402
crystal structure; 2-cyano­acrylates; phenyl acrylates; cinnamic acid derivatives; C—H⋯O hydrogen bonding
18.  Crystal structure of (2-{[3,5-bis­(1,1-di­methyl­eth­yl)-4-hy­droxy­phen­yl](5-methyl-2H-pyrrol-2-yl­idene)meth­yl}-5-methyl-1H-pyrrolido-κ2 N,N′)di­fluoridoboron 
The title compound, C25H31BF2N2O, is a potential boron tracedrug in boron neutron capture therapy (BNCT), in which the B atom adopts a distorted BN2F2 tetra­hedral geometry: it is soluble in dimethyl sulfoxide, di­methyl­formamide and methanol. The pyrrolyl­idene­methyl­pyrrole triple fused ring system is almost planar (r.m.s. deviation = 0.031 Å) and subtends a dihedral angle of 47.09 (5)° with the plane of the pendant phenol ring. The phenol –OH group is blocked from forming hydrogen bonds by the adjacent bulky tert-butyl groups. In the crystal, inversion dimers linked by pairs of very weak C—H⋯F inter­actions generate R 2 2(22) loops.
doi:10.1107/S2056989015015789
PMCID: PMC4555381  PMID: 26396909
crystal structure; boron tracedrug; boron neutron capture therapy (BNCT)
19.  4,6-Dimeth­oxy-2-(methyl­sulfan­yl)pyrimidine–4-hy­droxy­benzoic acid (1/1) 
The base mol­ecule of the title co-crystal, C7H10N2O2S·C7H6O3, is essentially planar, with a maximum deviation of 0.0806 (14) Å for all non-H atoms. The acid mol­ecule is also nearly planar, with a dihedral angle of 8.12 (14)° between the benzene ring and the carb­oxy group. In the crystal, the acid mol­ecules form an inversion dimer through a pair of O—H⋯O hydrogen bonds with an R 2 2(8) ring motif. The pyrimidine mol­ecules are linked on both sides of the dimer into a heterotetra­mer via O—H⋯N and C—H⋯O hydrogen bonds with R 2 2(8) ring motifs. The heterotetra­mers are further linked by weak C—H⋯O hydrogen bonds, forming a tape structure along [1-10].
doi:10.1107/S1600536812046338
PMCID: PMC3589001  PMID: 23476237
20.  5-Chloro-N-(4,5-dihydro-1H-imidazol-2-yl)-2,1,3-benzothia­diazol-4-amine (tizanidine) 
There are two independent mol­ecules (A and B) with similar conformations in the asymmetric unit of the title compound, C9H8ClN5S. The benzothia­diazole ring systems of both mol­ecules are essentially planar [maximum deviation = 0.021 (2) Å in mol­ecule A and 0.022 (1) Å in mol­ecule B] and make dihedral angles of 68.78 (9) and 54.39 (8)°, respectively, with the mean planes of their 4,5-dihydro-1H-imidazole rings. An intra­molecular N—H⋯Cl hydrogen bond occurs in mol­ecule B. In the crystal, both mol­ecules form centrosymmetric dimers through π-stacking of their benzothia­diazole rings, with inter­planar distances of 3.3174 (7) and 3.2943 (6) Å. These dimers are further linked via pairs of N—H⋯N hydrogen bonds with the dihydro­imidazole rings as the hydrogen-bonding donors and one of the benzothia­diazole N atoms as the acceptors, generating R 2 2(16) ring motifs. The A 2 and B 2 dimers in turn form additional N—H⋯N hydrogen bonds with the secondary amine as the H-atom donor and the dihydro­imidazole N atom as the acceptor. These R 2 2(8)-type inter­actions connect the A 2 and B 2 dimers with each other, forming infinite chains along [11].
doi:10.1107/S1600536811008348
PMCID: PMC3100067  PMID: 21754121
21.  N-tert-Butyl-3-hydr­oxy-5-androstene-17-carboxamide monohydrate 
In the title compound, C24H39NO2·H2O, the A and C rings of the pregnolene derivative sterol adopt chair conformations, with the B ring in a flattened chair conformation and the five-membered ring in an envelope conformation twisted about the C/D ring junction. The N-tert-butyl­carboxamide substituent is equatorial. The 3β-hydr­oxy H atom and one H atom of the water mol­ecule are disordered over two positions with equal occupancies. In the crystal structure, O—H⋯O hydrogen bonds between the 3β-hydr­oxy groups of neighbouring mol­ecules form dimers in the bc plane and these dimers are stacked along the a axis by additional O—H⋯O hydrogen bonds involving the water mol­ecules. The steric effect of the bulky tert-butyl substituent in the carboxamide chain precludes hydrogen-bond formation by the N—H group.
doi:10.1107/S1600536809020984
PMCID: PMC2969220  PMID: 21582804
22.  Ethyl 5-hy­droxy-6-oxo-4-phenyl-5,6-dihydro-4H-cyclo­penta­[b]thio­phene-5-carboxyl­ate 
In the title mol­ecule, C16H14O4S, the dihydro­cyclo­penta­thio­phenone ring system is almost planar, with an r.m.s. deviation of 0.060 Å from the best fit plane through all nine non-H atoms. The cyclo­penta­none ring adopts a severely flattened envelope conformation with the C atom carrying the OH and ethylcarboxylate substituents at the flap. This atom lies only 0.185 (3) Å from the plane through the other four C atoms. The phenyl substituent is inclined at 43.37 (5)° to the dihydro­cyclo­penta­thio­phenone mean plane. In the crystal, mol­ecules are linked by pairs of O—H⋯O hydrogen bonds, forming inversion dimers with R 2 2(10) ring motifs. Weak C—H⋯O hydrogen bonds also link mol­ecules into chains along c, while an approximately orthogonal set of C—H⋯O contacts form chains along b, resulting in layers lying parallel to (100). Inversion dimers also form through weaker R 2 2(12) C—H⋯S contacts, which combine with C—H⋯O contacts to form stacks along b.
doi:10.1107/S1600536811037032
PMCID: PMC3201281  PMID: 22058815
23.  2-Amino-5-methyl­pyridinium 1H-pyrazole-3,5-dicarboxyl­ate trihydrate 
In the title compound, 2C6H9N2 +·C5H2N2O4 2−·3H2O, the 1H-pyrazole-3,5-dicarboxyl­ate anion is close to planar [maximum deviation = 0.208 (1) Å]. The two distinct 2-amino-5-methyl­pyridinium cations are also almost planar, with maximum deviations of 0.018 (2) and 0.014 (2) Å. In the crystal, pairs of inter­molecular N—H⋯O and O—H⋯O hydrogen bonds connect neighbouring mol­ecules into dimers, generating R 2 2(8) and R 2 4(8) ring motifs, respectively. Further inter­molecular N—H⋯O, O—H⋯O and C—H⋯O hydrogen bonds link the mol­ecules into a three-dimensional network.
doi:10.1107/S1600536810041644
PMCID: PMC3008987  PMID: 21589058
24.  4,4′-[Ethylenebis(nitrilomethylidyne)]dibenzonitrile 
The mol­ecule of the title Schiff base compound, C18H14N4, lies across a crystallographic inversion centre and adopts an E configuration with respect to the azomethine (C=N) bonds. The imino groups are coplanar with the aromatic rings with a maximum deviation of 0.1574 (12) Å for the N atom. Within the mol­ecule, the planar units are parallel, but extend in opposite directions from the dimethyl­ene bridge. In the crystal structure, pairs of inter­molecular C—H⋯N hydrogen bonds link neighbouring mol­ecules into centrosymmetric dimers with R 2 2(10) ring motifs. An inter­esting feature of the crystal structure is the short inter­molecular C⋯C inter­action with a distance of 3.3821 (13) Å, which is shorter than the sum of the van der Waals radius of a carbon atom.
doi:10.1107/S1600536809007284
PMCID: PMC2969074  PMID: 21582425
25.  (E)-2-[1-(1-Benzothio­phen-2-yl)ethyl­idene]-N-phenyl­hydrazinecarboxamide 
The title compound, C17H15N3OS, crystallizes with two unique mol­ecules, denoted 1 and 2, in the asymmetric unit. The two mol­ecules are closely similar and overlay with an r.m.s. deviation of 0.053 Å. Both mol­ecules adopt E configurations with respect to the C=N bonds. The dihedral angles between the benzothio­phene groups and N-bound phenyl rings are 36.36 (9)° for mol­ecule 1 and 29.71 (9)° for mol­ecule 2. The C=N—NH—C(O)NH ethyl­idene–hydrazinecarboxamide units are also reasonably planar, with r.m.s. deviations of 0.061 and 0.056 Å, respectively, for the two mol­ecules. The methyl substituents lie 0.338 (3) and 0.396 (3) Å, respectively, from these planes. The C=N—NH—C(O)NH planes are inclined to the phenyl rings at 13.65 (11) and 15.56 (11)°, respectively, in mol­ecules 1 and 2. This conformation is enhanced by weak intra­molecular C—H⋯O hydrogen bonds between ortho-H atoms of the two phenyl rings and the carbonyl O atoms, which generate S(6) rings in each mol­ecule. In the crystal, pairs of mol­ecules are linked by pairs of inter­molecular N—H⋯O hydrogen bonds into dimers. Alternating dimers are further inter­connected by weak C—H⋯O contacts into zigzag rows along b. The rows are stacked along a by C—H⋯π contacts involving the benzene ring from molecule 2 and the thiophene ring from molecule 1 of adjacent benzothio­phene units.
doi:10.1107/S1600536811037457
PMCID: PMC3201294  PMID: 22058789

Results 1-25 (659540)