Lotharmeyerite, calcium bis(zinc/manganese) bis(arsenate) bis(hydroxide/hydrate), Ca(Zn,Mn3+)2(AsO4)2(H2O,OH)2, is a member of the natrochalcite group of minerals, which are characterized by the general formula AM
2(XO4)2(H2O,OH)2, where A may be occupied by Pb2+, Ca2+, Na+, and Bi3+, M by Fe3+, Mn3+, Cu2+, Zn2+, Co2+, Ni2+, Al3+, and Mg2+, and X by PV, AsV, VV, and SVI. The minerals in the group display either monoclinic or triclinic symmetry, depending on the ordering of chemical components in the M site. Based on single-crystal X-ray diffraction data of a sample from the type locality, Mapimi, Durango, Mexico, this study presents the first structure determination of lotharmeyerite. Lotharmeyerite is isostructural with natrochalcite and tsumcorite. The structure is composed of rutile-type chains of edge-shared MO6 octahedra (site symmetry ) extending along , which are interconnected by XO4 tetrahedra (site symmetry 2) and hydrogen bonds to form [M
2(XO4)2(OH,H2O)2] sheets parallel to (001). These sheets are linked by the larger A cations (site symmetry 2/m), as well as by hydrogen bonds. Bond-valence sums for the M cation, calculated with the parameters for Mn3+ and Mn2+ are 2.72 and 2.94 v.u., respectively, consistent with the occupation of the M site by Mn3+. Two distinct hydrogen bonds are present, one with O⋯O = 2.610 (4) Å and the other O⋯O = 2.595 (3) Å. One of the H-atom positions is disordered over two sites with 50% occupancy, in agreement with observations for other natrochalcite-type minerals, such as natrochalcite and tsumcorite.
In the title compound, [RuCl(C15H11N3)(C12H8N2O4)]ClO4·C2H5OH·H2O, the geometry of the ClN5 coordination set around the RuII atom is close to octahedral, but distorted on account of the limited bite angles of the polypyridyl ligands. The complexes are linked by O—H⋯O hydrogen bonds between the carboxyl groups and the crystal lattice water molecules into chains along . Face-to-face stacking interactions are formed between terpyridine ligands, with interplanar separations of 3.66 (1) and 3.42 (1) Å, and between bipyridine-4,4′-dicarboxylic acid ligands, with interplanar separations of 3.65 (1) and 3.72 (1) Å. Three O atoms of the perchlorate ion are each disordered equally over two positions. The hydroxy group of the ethanol molecule is also disordered over two sites with refined occupancies of 0.794 (9) and 0.206 (9).
The title compound, [Sn(C4H9)2(C9H10NS2)2], features a tetrahedrally coordinated SnIV atom; the dithiocarbamate ligands coordinate in a monodentate fashion, accompanied by two n-butyl chains. The non-coordinating thione S atoms are each proximate to the SnIV atom [3.0136 (7) and 2.9865 (8) Å], giving rise to distortions from the ideal geometry as evident in the wide C—Sn—C bond angle of 139.06 (12) °. In the crystal, C—H⋯S interactions lead to the formation of a linear supramolecular chain along the b axis. The chains are aligned into layers by C—H⋯π interactions, and the layers stack along . One of the ethyl groups is statistically disordered over two sets of sites.
In the title binuclear CoII complex, [Co2(C12H21N2Si)2Cl2], an inversion center is located at the mid-point between the two Co atoms in the dimeric molecule. The bidentate N-silylated anilide ligand coordinates the CoII atom in an N,N′-chelating mode and provides the anilide N atom as a bridge to link two CoII atoms. The two ends of the N—Si—N chelating unit exhibit different affinities for the metal atom. The Co—Nanilide bond is 2.031 (6) Å and Co—Namino bond is 2.214 (6) Å. The four-coordinate Co atom presents a distorted tetrahedral geometry, while the dimeric aggregation exhibits a (CoN)2 rhombus core with 1.998 (6) Å as the shortest sides and shows a ladder structure composed of Co, N and Si atoms.
In the title compound, [Ni(C21H24N2O2)]·H2O, both the complex molecule and the water molecule lie on a twofold rotation axis. The NiII ion is coordinated in a distorted square-planar geometry by the tetradentate ligand. The dihedral angle between the two symmetry-related benzene rings is 47.12 (8)°. In the crystal, pairs of symmetry-related O—H⋯O hydrogen bonds form R
2(6) ring motifs. In addition, there are weak intermolecular C—H⋯O hydrogen bonds, and π–π stacking interactions with a centroid–centroid distance of 3.4760 (8) Å.
In the title complex, [Sn(C7H6F)2(C8H5N2S3)2], including the weak Sn—N interactions, the SnIV atom is situated in a distorted trans-octahedral geometry, and the equatorial plane is defined by two chelating 4-phenyl-5-sulfanylidene-4,5-dihydro-1,3,4-thiodiazole-2-thiolate ligands. The apical positions are occupied by two C atoms of 4-fluorobenzyl groups.
In the crystal structure of the polymeric title complex, [Cd(C11H10O4)(C10H8N2)]n, the CdII cation is chelated by one 2,2-bipyridine ligand and two carboxyl groups from two trimethylisophthalate (TMIPA) anions, and is further coordinated by one carboxylate O atom from a third TMIPA anion, forming a distorted pentagonal–bipyramidal geometry. Each TMIPA anion bridges three CdII cations, forming polymeric complex sheets parallel to (001). Weak C—H⋯O hydrogen bonding occurs between adjacent sheets.
The title mononuclear complex, [Cu(C18H12N2O2)(C12H8N2)]·CH3OH, contains one N′-[(2-oxidonaphthalen-1-yl)methylidene]benzohydrazidate ligand (L
2−), a Cu2+ cation, one 1,10-phenanthroline ligand and a methanol solvent molecule. The CuII ion adopts a CuO2N3 distorted square-pyramidal coordination. An O—H⋯O hydrogen bond is formed between the methanol solvent molecule and the hydrazide O atom of the L
The binuclear title complex, [Zn2(C22H28N3O)2(C3H9OSi)2], has a crystallographic imposed centre of symmetry. The ZnII atom is coordinated by three O and one N atom from one 2-(2H-benzotriazol-2-yl)-4,6-di-tert-pentylphenolate ligand and two bridging trimethylsilanolate anions in a distorted tetrahedral geometry. The dihedral angle between the benzotriazole ring system and the benzene ring is 19.83 (5)°. The tert-pentyl groups are disordered over two orientations with refined site-occupancy ratios of 0.858 (4):0.142 (4) and 0.665 (6):0.335 (6).
The asymmetric unit of the title compound, [Mn2(SO4)2(C6H5NO2)2(H2O)6], comprises half of a centrosymmetric dimer. The MnII atom is coordinated by two O atoms of the monodentate carboxylate ligand, an O atom of the sulfate anion in axial position and three water molecules in a distorted octahedral geometry. In the crystal, molecules are connected through N—H⋯O and O—H⋯O hydrogen bonds, forming a three-dimensional network. The crystal structure is further stabilized by intermolecular π–π interactions [centroid–centroid distance = 3.842 (2) Å].
In the title complex, [Cd(C6H11N2S2)2(C5H5N)2], the CdII ion is hexacoordinated by two N atoms from two pyridine ligands and by four S atoms from two dithiocarbamate ligands in a distorted octahedral geometry. The CdII ion lies on a twofold axis. The piperazine ring is in chair conformation and its least-squares plane makes a dihedral angle of 81.4 (1)° with that of the pyridine ring.
In the title compound, [Zn(C4H6N2)4](BF4)2, the ZnII ion is in a slightly distorted tetrahedral coordination geometry, with Zn—N distances in the range 1.980 (2)–1.991 (2) Å. The tetrahedral angles are in the range 104.93 (9)–118.81 (9)°.
In the title compound, [Cu(CH3CO2)2(C9H7N3)(H2O)]n, the CuII ion is pentacoordinated in a square-pyramidal geometry. The N atoms of the two chelating symmetry-related 5-(pyridin-3-yl)pyrimidine ligands and the O atoms of the two monodentate acetate anions are nearly coplanar, with a mean deviation from the least-squares plane of 0.157 (2) Å and the CuII ion is displaced by 0.050 (3) Å from this plane towards the apical water O atom. Bridging through the bis-monodentate 5-(pyridin-3-yl)pyrimidine ligand forms a one-dimensional coordination polymer extending parallel to . In the crystal, O—H⋯O hydrogen bonds link the molecules into a two-dimensional supramolecular structure parallel to (100). The crystal studied was an inversion twin with a 0.57 (3):0.43 (3) domain ratio.
The crystal structure of the title compound, C9H12ClNTe, contains isolated molecules with no close Te⋯Cl intermolecular contacts and has the same composition as a previously published structure [Engman et al. (2004 ▶). Phosphorus Sulfur Silicon Relat. Elem.
179, 285–292]. However, in this case, the compound has crystallized in a centrosymmetric space group, unlike the previously published structure which contained enantiomerically pure chiral molecules. In all other aspects, the metrical parameters are similar. The molecules with a T-shaped coordination environment about the Te atom are linked into dimers by C—H⋯Cl interactions.
The title compound, C9H13Br2ClNTe, was synthesized by reacting [2-(dimethylaminomethyl)phenyl]tellurium(II) chloride with Br2. As a consequence, the Cl and Br atoms are not well ordered but distributed over the three possible positions such that the overall stiochiometry is two Br atoms and one Cl atom. The scrambling of the Br and Cl atoms indicates a small energy barrier for the exchange process between the apical and equatorial positions. Overall, the Te atom geometry is slightly distorted square pyramidal (τ = 0.052 for the major component). However, there is a weak secondary interaction between the Te atoms and the disordered Br/Cl atoms of a nearby molecule. The Te—Br and Te—Cl distances in both disorder components fall into two groups; a longer distance for the Br/Cl involved in this secondary interaction [2.6945 (17) Å for Br and 2.601 (9)Å for Cl] and shorter bond distances to the remaining halogen atoms, indicating that this interaction has slightly weakened the Te—X bond, as is the case in the previously reported tribromido structure [Singh et al. (1990). J. Chem. Soc. Dalton Trans. pp. 907–913]. Otherwise, the metrical parameters in the two structures are not significantly different. An intermolecular C—H⋯Br interaction occurs.
In the title compound, C16H21N2O5, the benzene ring is nearly perpendicular to the imidazole ring, making a torsion angle of 88.6 (8)°·The crystal structure is stabilized by non-classical C—H⋯O and C—H⋯π interactions, which build up a three-dimensional network.
In the title compound, C15H21N2O5, the imidazoline ring displays a twisted conformation. The mean plane of the imidazoline ring makes a dihedral angle of 22.55 (5)° with the benzene ring. In the crystal, O—H⋯O and C—H⋯O hydrogen bonds link the molecules into a layer parallel to the bc plane.
The title molecule, C9H6ClNO2, is essentially planar; the maximum deviation of the indoline ring system is 0.027 (3) Å and the substituents do not deviate by more than 0.075 (2) Å from this plane. Intermolecular C—H⋯O hydrogen bonds consolidate the crystal structure.
The molecule of the title compound, C16H16N2O4, exists in the E configuration with respect to the central C=N double bond. The dihedral angle between the two benzene rings is 2.17 (9) Å. In the crystal, molecules are linked via O—H⋯N hydrogen bonds into chains that propagate along the b-axis direction. There is also π–π stacking of inversion-related molecules, with interplanar spacings of 3.479 (5) Å and ring centroid–centroid distances of 3.876 (4) Å.
In the title compound, C11H12ClNO3, the conformation of the N—H bond in the amide segment is syn with respect to the ortho-Cl atom. The amide and carboxyl C=O groups are syn to each other. Furthermore, the C=O and O—H bonds of the carboxyl group are in syn positions with respect to each other. The dihedral angle between the benzene ring and the amide group is 47.8 (2)°. In the crystal, molecules are connected by pairs of O—H⋯O hydrogen bonds, forming inversion dimers. The dimers are further linked by N—H⋯O hydrogen bonds into double chains along the b-axis direction.
In the title compound, C12H6F2N2O2, the 2,2-difluoro-1,3-benzodioxole ring system is approximately planar [maximum deviation = 0.012 (2) Å] and its mean plane is twisted with respect to the pyrrole ring, making a dihedral angle of 2.51 (9)°. In the crystal, N—H⋯N hydrogen bonds link the molecules into chains running along the a axis. π–π stacking is also observed between parallel benzene rings of adjacent molecules, the centroid–centroid distance being 3.7527 (13) Å.
In the title compound, C2H10N2
2−, the two acetate groups of the cation form dihedral angles of 74.2 (4) and 63.9 (5)° with the central benzene ring. In the crystal, N—H⋯O hydrogen bonds link the cations and anions into layers parallel to the ab plane.
In the title compound, C4H5N3OS2·2C2H6OS, the five-membered heterocyclic ring and the N—(C=O)—C plane of the acetamide group are essentially co-planar, with a dihedral angle of 1.25 (3)°. Intermolecular N—H⋯O hydrogen bonds between the acetamide compound and the dimethyl sulfoxide molecules stabilize the crystal structure. The two dimethyl sulfoxide molecules are each disordered over two positions with occupancy ratios of 0.605 (2):0.395 (2) and 0.8629 (18):0.1371 (18).
In the title compound, CH3NH3
−·C12H24O6, the methylammonium cation makes three N—H⋯O hydrogen bonds to the 18-crown-6 molecule. The –NH3
+ and –CH3 groups of the cation adopt a staggered conformation. The F atoms of the tetrafluoridoborate anion are disordered over two sets of sites in a 0.519 (11):0.481 (11) ratio. Weak C—H⋯F interactions occur in the crystal, which possibly correlate with the anion disorder.
In the title compound, C15H17N3O3, the dihedral angle between the pyrimidine and benzene rings is 87.0 (7)°. In the crystal, molecules are linked into inversion dimers with R
2(8) graph-set motifs by a pair of N—H⋯O hydrogen bonds. Weak C—H⋯O hydrogen bonds and intermolecular π–π interactions [centroid–centroid distance = 3.544 (1) Å] are also observed.