catena‐Poly[[[tetra­aqua­zinc(II)]‐μ‐4,4′‐bipyridine] bis­(4‐hydroxy­benzene­sulfonate) trihydrate]

In the title compound, {[Zn(C₁₀H₈N₂)(H₂O)₄](C₆H₅O₄S)₂·3H₂O}_n, the Zn atom, the bipyridine ligand and one of water mol­ecules are located on twofold rotation axes. The Zn atom is coordinated by four O atoms from four water mol­ecules and two N atoms from two 4,4′‐bipyridine mol­ecules in a distorted octa­hedral geometry. The Zn²⁺ ions are linked by the 4,4′‐bipyridine mol­ecules to form a one‐dimensional straight chain propagating along the c axis. The 4‐hydroxy­benzene­sulfonate counter‐ions are bridged by the solvent water mol­ecules through hydrogen bonds to generate a two‐dimensional layer featuring large pores. In the crystal packing, the intra­layer pores form one‐dimensional channels along the c axis, in which the one‐dimensional [Zn(C₁₀H₈N₂)(H₂O)₄]²⁺ chains are encapsulated. Electrostatic inter­actions between cations and anions and extensive hydrogen bonds result in a three‐dimensional supra­molecular structure.     

3,4‐Di­hydro‐6‐methyl‐3‐β‐d‐ribo­furan­osyl‐4,5′‐cyclo‐9H‐imidazo[1,2‐a]­purin‐9‐one hydrate

In the title compound, C₁₃H₁₃N₅O₄·H₂O (4,5′‐cyclo­wyosine·H₂O), the cyclization forces a syn arrangement of the aglycon with respect to the sugar moiety. The ribo­furan­ose part of the mol­ecule displays a β‐d configuration with an envelope C1′‐endo pucker. The mol­ecules are arranged in columns along the short a axis and are linked to water mol­ecules through O—H?O and O—H?N hydrogen bonds.     

4‐(4‐Hydro­xy­benzyl­idene­amino)‐4H‐1,2,4‐triazole hemihydrate

In the title compound, 4‐(4H‐1,2,4‐triazol‐4‐yl­imino­methyl)­phenol hemi­hydrate, C₉H₈N₄O·0.5H₂O or (I)·0.5H₂O, mol­ecules of (I) are arranged as layers running along the b axis through intermolecular O—H?N and C—H?O hydrogen bonds. These layers are stabilized by hydrogen‐bonded water mol­ecules to form three‐dimensional networks.     

3,6,9,16,19,22‐Hexa­aza­tri­cyclo[22.2.­2.211,14]­tria­conta‐11,13,24,26(1),27,29‐hexa­ene penta­hydrate

In the title macrocyclic poly­amine, C₂₄H₃₈N₆·5H₂O, the centrosymmetric poly­amine mol­ecules are stacked in rows, and between these mol­ecules there are channels along the a axis. The intermolecular hydrogen bonds formed between the water and poly­amine, together with those formed between water mol­ecules, generate an extensive hydrogen‐bonding network.     

N‐Cyclo­hexyl‐2‐[5‐(4‐pyridyl)‐4‐(p‐tolyl)‐4H‐1,2,4‐triazol‐3‐yl­sulfanyl]­acetamide dihydrate

In the title compound, C₂₂H₂₅N₅OS·2H₂O, the mol­ecules are stacked in columns running along the b axis. In this arrangemant, the mol­ecules are linked to each other by a combination of one two‐centre N—H⋯O hydrogen bond and four two‐centre O—H⋯O hydrogen bonds containing two types of ring motif, viz.R₄⁴(10) and R₃³(11). In the crystal structure, centrosymmetric π–π inter­actions between the triazole rings, with a distance of 3.691 (2) Å between the ring centroids, also affect the packing of the mol­ecules.     

4′‐Hydro­xy­bi­phenyl‐4‐carbo­nitrile

The title compound, C₁₃H₉NO, crystallizes with four mol­ecules in the asymmetric unit. Each of the four crystallographically independent mol­ecules forms a chain parallel to the a axis with symmetry‐equivalent mol­ecules. These chains are held together by similar O—H·NC hydrogen bonds, with approximately linear O—H·N angles and significantly bent H·N—C angles. The four different mol­ecules are related by strong elements of pseudosymmetry. To better describe the pseudosymmetry, the structure has been reported in the non‐standard space group .     

2‐Hydroxy‐3‐(3‐oxobut­yl)naphthalene‐1,4‐dione

The title compound, C₁₄H₁₂O₄, forms crystals which appear monoclinic but are actually twinned triclinic. The asymmetric unit consists of two similar mol­ecules, which differ only in the conformation of the 3‐oxobutyl side chain. The mol­ecular conformation is characterized by an intra­molecular O—H⋯O hydrogen bond between the hydroxy group and the adjacent carbonyl O atom. The crystal structure is stabilized by O—H⋯O hydrogen bonds connecting the mol­ecules into zigzag chains running along the b axis.     

l‐Me­thionyl‐l‐alanine–2‐propanol (1/2)

The crystal structure of the title compound, C₈H₁₆N₂O₃S·2C₃H₈O, is divided into hydro­phobic and hydro­philic layers. Two peptide mol­ecules in the asymmetric unit are related by pseudo‐translational symmetry along the a axis, as are two of the four 2‐propanol mol­ecules. The last two 2‐propanol mol­ecules in the asymmetric unit have different relative orientations and hydrogen‐bond interactions.     

Comparison of conventional and synchrotron X‐ray structure deter­minations of the adduct 1,2,4,5‐tetrahydroxybenzene–2,5‐dihydroxy‐1,4‐benzoquinone (1/1) and a conventional X‐ray structure determination of 1,2,4,5‐tetrahydroxybenzene monohydrate

The X‐ray structure of 1,2,4,5‐tetra­hydroxy­benzene (benzene‐1,2,4,5‐tetrol) monohydrate, C₆H₆O₄·H₂O, (I), reveals columns of 1,2,4,5‐tetra­hydroxy­benzene parallel to the b axis that are separated by 3.364 (12) and 3.453 (11) Å. Molecules in adjacent columns are tilted relative to each other by 27.78 (8)°. Water mol­ecules fill the channels between the columns and are involved in hydrogen‐bonding interactions with the 1,2,4,5‐tetra­hydroxy­benzene mol­ecules. The crystal structure of the adduct 1,2,4,5‐tetra­hydroxy­benzene–2,5‐di­hydroxy‐1,4‐benzo­quinone (1/1), C₆H₆O₄·C₆H₄O₄, (II), reveals alternating mol­ecules of 1,2,4,5‐tetra­hydroxy­benzene and 2,5‐di­hydroxy‐1,4‐benzo­quinone (both lying on inversion centers), and a zigzag hydrogen‐bonded network connecting mol­ecules in three dimensions. For compound (II), the conventional X‐ray determination, (IIa), is in very good agreement with the synchrotron X‐ray determination, (IIb). When differences in data collection temperatures are taken into account, even the displacement parameters are in very good agreement.     

C[triple‐bond]C—H systems as hydrogen‐bond donors and acceptors: trans‐1,2‐diethynylcyclo­hexane‐1,2‐diol and trans‐1,4‐diprop‐2‐ynylcyclo­hexane‐1,4‐diol monohydrate

The title 1,2‐diol derivative, C₁₀H₁₂O₂, crystallizes with two independent but closely similar mol­ecules in the asymmetric unit. Only two of the four OH groups are involved in classical hydrogen bonding; the mol­ecules thereby associate to form chains parallel to the short c axis. The other two OH groups are involved in O—H⋯(C[triple‐bond]C) systems. Additionally, three of the four C[triple‐bond]C—H groups act as donors in C—H⋯O inter­actions. The 1,4‐diol derivative crystallizes with two independent half‐mol­ecules of the diol (each associated with an inversion centre) and one water mol­ecule in the asymmetric unit, C₁₂H₁₆O₂·H₂O. Both OH groups and one water H atom act as classical hydrogen‐bond donors, leading to layers parallel to the ac plane. The second water H atom is involved in a three‐centre contact to two C[triple‐bond]C bonds. One acetyl­enic H atom makes a very short `weak' hydrogen bond to a hydr­oxy O atom, and the other is part of a three‐centre system in which the acceptors are a hydroxy O atom and a C[triple‐bond]C bond.     

N‐(2‐Amino‐1,6‐di­hydro‐5‐nitro­so‐6‐oxopyrimidin‐4‐yl)‐l‐isoleucine–water (4/1): interplay of molecular and supramolecular structures

In the title compound, 2C₁₀H₁₅N₅O₄·0.5H₂O, there are two independent mol­ecules of the pyrimidinyl­isoleucine in general positions and a water mol­ecule lying on a twofold rotation axis. The bond lengths within the organic moieties demonstrate significant polarization of the electronic structure. Each of the organic mol­ecules participates in 12 intermolecular hydrogen bonds, of O—H?O and N—H?O types, while the water mol­ecule acts as a double donor and as a double acceptor of O—H?O hydrogen bonds. The organic components are linked by the hydrogen bonds into a single three‐dimensional framework, reinforced by the water mol­ecules.     

Methyl 1‐(4‐chloro­benzyl)‐2‐(4‐methyl­piperazin‐1‐yl)‐1H‐benz­imidazole‐5‐carboxyl­ate hemihydrate

The title compound, C₂₁H₂₃ClN₄O₂·0.5H₂O, contains two independent mol­ecules in the asymmetric unit. In each mol­ecule the piperazine ring adopts a chair conformation; the deviations of the piperazine N atoms from the best plane through the remaining four C atoms are ?0.678 (3) and 0.662 (3) Å in mol­ecule A, and 0.687 (3) and ?0.700 (3) Å in mol­ecule B. The mol­ecules are linked by two hydrogen bonds of the O—H?N type involving the O atom of the water mol­ecule of crystallization.     

tert‐Butyl (3S,6R,9R)‐(5‐oxo‐3‐{[1(R)‐phenyl­ethyl]­carbamoyl}‐1,2,3,5,6,7,8,8a‐octa­hydro­indolizin‐6‐yl)­carbamate monohydrate at 95 K

The asymmetric unit of the title compound, C₂₂H₃₁N₃O₄·H₂O, incorporates one water mol­ecule, which is hydrogen bonded to the 3‐oxo O atom of the indolizidinone system. The two rings of the peptidomimetic mol­ecule are trans‐fused, with the six‐membered ring having a slightly distorted half‐chair conformation and the five‐membered ring having a perfect envelope conformation. The structure is stabilized by intermolecular O—H?O interactions between the water and adjacent peptide mol­ecules, and by N—H?O interactions between the peptide mol­ecules, which link the mol­ecules into infinite chains.     

Two novel glycine metal halogenides: catena‐poly[[[diaqua­nickel(II)]‐di‐μ‐glycine] dibromide] and catena‐poly[[[tetra­aqua­magnesium(II)]‐μ‐glycine] dichloride]

In catena‐poly[[[diaqua­nickel(II)]‐di‐μ‐glycine] dibromide], {[Ni(C₂H₅NO₂)₂(H₂O)₂]Br₂}_n, (I), the Ni atom is located on an inversion centre. In catena‐poly[[[tetra­aqua­magnesium(II)]‐μ‐glycine] dichloride], {[Mg(C₂H₅NO₂)(H₂O)₄]Cl₂}_n, (II), the Mg atom and the non‐H atoms of the glycine mol­ecule are located on a mirror plane. All other atoms are located on general positions. The atomic arrangements of both compounds are characterized by [MO₆] octa­hedra (M = Ni or Mg) connected by glycine mol­ecules, with the halogenide ions in the inter­stices. In (I), four of the coordinating O atoms are from glycine and two are from water mol­ecules, building layers of octa­hedra and organic mol­ecules. In (II), two of the coordinating O atoms are from glycine and four are from water mol­ecules. The octa­hedra and organic mol­ecules form chains.     

4‐Acetamido‐3,3,5,5‐[2H4]‐2,2,6,6‐tetra­([2H3]methyl)piperidin‐1‐yloxyl 0.33‐hydrate

The asymmetric unit of the title compound, C₁₁H₅D₁₆N₂O₂·0.33H₂O, is formed by three crystallographically independent piperidin‐1‐yloxyl mol­ecules and a mol­ecule of water. The mol­ecules are crosslinked by nine hydrogen bonds into layers parallel with the ac plane. The water mol­ecule contributes to the stability of the low‐symmetry arrangement by four hydrogen bonds.     

A one‐dimensional coordination polymer with metal–metal inter­actions: catena‐poly­[[tri­aqua­barium(II)]‐μ‐aqua‐κ2O:O‐di‐μ‐thio­salicyl­ato‐κ4O:O]

In the title compound, [Ba(C₇H₅O₂S)₂(H₂O)₄]_n, the Ba^II atom lies on a mirror plane and is nine‐coordinated by four bridging carboxylate O atoms of the thio­salicyl­ate ligands, two bridging water mol­ecules and three terminal water mol­ecules. There is an intramolecular S—H⋯O hydrogen bond between the S and O atoms in the thio­salicyl­ate ligand. A one‐dimensional coordination polymer is formed via weak metal–metal interactions along polymeric zigzag chains.     

Bis(μ‐diphenyl­phosphinato‐κ2O:O′)bis­[aqua­(diphenyl­phosphinato‐κO)bis­(pyridine‐κN)cobalt(II)]

In the centrosymmetric title compound, [Co₂(C₁₂H₁₀O₂P)₄(C₅H₅N)₄(H₂O)₂], each approximately octa­hedral Co atom features two trans‐coordinated pyridine mol­ecules, one water mol­ecule, a terminally coordinated monodentate diphenyl­phosphinate ligand, and two bidentate diphenyl­phosphinate ligands that bridge the two Co atoms across a centre of inversion to form a dimeric binuclear complex. The discrete mol­ecules are linked by double hydrogen bonds between the terminally coordinated diphenyl­phosphinate ligand and the water mol­ecule to form a continuous chain along the crystallographic b axis.     

Solvent water tapes in two hydrates of μ‐oxo‐bis­[bis­(2,2′‐bipyridine‐κ2N,N′)(sulfato‐κO)iron(III)]

The title compound, [Fe₂O(SO₄)₂(C₁₀H₈N₂)₄], crystallizes as two different hydrates, viz. 11H₂O, (I), and 15H₂O, (II). The complex is binuclear, in which the two Fe^III atoms are coordinated in an octa­hedral geometry to four N atoms from the two bipyridine ligands, to one O atom from the sulfate ion and to an oxide ion on a twofold axis, which acts as a bridge between the symmetry‐related units. The Fe⋯Fe separation is 3.556 (4) Å and the Fe—O—Fe angle is 161.6 (2)° in (I); the corresponding values are 3.544 (1) Å and 165.8 (2)° in (II). In (II), one of the O atoms of the sulfate ion is disordered over two positions. In both compounds, the solvent water mol­ecules form slightly different one‐dimensional hydrogen‐bonded networks which pass along the c axis of the unit cell. In (I), three solvent water mol­ecules and, in (II), one solvent water mol­ecule, are situated on the twofold axis. In both (I) and (II), the central O atom of the metal complex lies on a twofold axis.     

[(4,4‐Dimethyl‐2‐oxo‐1,3‐oxazolidin‐3‐yl)methyl]phosphonic acid

The title compound, C₆H₁₂NO₅P, was synthesized as an inter­mediate phase in a search for new N‐(phosphono­methyl)glycine derivatives. The mol­ecules are held together by O—H⋯O hydrogen bonds, forming chains along the b axis in the crystal structure. The observed mol­ecular structure is compared with that calculated by the density functional theory method.     

A new estra‐1,3,5(10)‐triene‐3,17β‐diol solvate: estradiol–methanol–water (3/2/1)

The title solvate of the steroid 17β‐estradiol (E₂) with methanol and water, C₁₈H₂₄O₂·0.67CH₄O·0.33H₂O, is the first E₂ derivative to contain three crystallographically independent mol­ecules in the asymmetric unit. The three steroid mol­ecules, along with two methanol mol­ecules and a water mol­ecule, create a three‐dimensional hydrogen‐bonded system. Three‐sided columns are formed, with the estradiol mol­ecules aligned lengthwise parallel to (101), and joined by solvent mol­ecules at both hydro­philic ends. The three estradiol mol­ecules differ slightly in their ring‐bowing angles, i.e. the angle between the mean plane of the A ring and that of the BCD ring; this angle ranges from 7.1 to 12.2°.