Showing papers in "Zeitschrift Fur Kristallographie-new Crystal Structures in 2010"
TL;DR: In this article, the lattice parameters were determined by least-squares refinement of 18 reflections from powder X-ray diffraction data obtained from the annealed PdGa sample.
Abstract: PdGa, cubic, P213 (no. 198), a = 4.89695(6) Å, V = 117.4 Å, Z = 4, Rgt(F) = 0.024, wRref(F) = 0.035, T = 295 K. Source of material Large single crystals of PdGa were obtained by Czochralski growth from the melt as described in [1]. The melt consisted of Pd (99.9 %, ChemPur) and Ga (99.99 %, ChemPur) in an atomic ratio of 45:55. The metals were pre-reacted in glassy carbon crucibles under inert argon atmosphere in a high-frequency induction furnace. Single crystals used in this study were obtained from the bottom of the as grown Czochralski crystal and were annealed at 800 °C for 24 h in dynamic vacuum at 10 mbar prior to the X-ray diffraction experiments. For the lattice parameter determination a small part of the bottom of the large crystal was crushed and annealed as described above. WDXS measurements were performed on a CAMECA SX100 (W filament, 25 kV) with Pd50Ga50 (by chemical analysis via ICP-OES) as standard. Experimental details Single crystal data were collected using a Rigaku R-axis SPIDER diffractometer with monochromated Ag K+ radiation. Determination and refinement of the crystal structure were performed with the SHELX-97 software [2]. Spence [3] defined the two absolute structures of the FeSi type as form A (Fe in 4a with x = 0.1358, Si in 4a with x = 0.844) and form B (Fe in 4a with x = 0.8642, Si in 4a with x = 0.156). Models of both absolute structures were refined for PdGa without twin model and resulted in considerable differences in Rgt,A = 0.028 and Rgt,B = 0.040, respectively. Further refinement of form A as inversion twin resulted in a Flack parameter of 0.05(1), confirming the proper parameter set. Refining site occupancy for both atoms resulted in fully occupied sites within one e.s.d. This excludes mutual site occupation in the crystal as is expected due to the covalent interactions in the compound [4]. To verify the absolute structure refinement, the mean-square Friedel intensity difference was determined according to Flack and Shmueli [5]. The resulting value of 10 ( = 261 is sufficiently high to confirm the selected set of parameters and setting of the crystal structure. The lattice parameters were determined by least-squares refinement of 18 reflections from powder X-ray diffraction data obtained from the annealed PdGa sample (Huber Image Plate Guinier camera G670, Cu K+1 radiation, ! = 1.540562 Å, LaB6 as internal standard, a = 4.15692 Å, WinCSD [6]). WDXS measurements resulted in a composition of Pd51.3(4)Ga48.7(4).
26 citations
TL;DR: In this paper, the title compound is the mononuclear zinc(II) complex of Schiff base and all hydrogen atoms were positioned geometrically (d(C-H) = 0.932(2) and 2.017(3) Å).
Abstract: C28H20Br4N2O2Zn, monoclinic, C12/c1 (no. 15), a = 23.667(5) Å, b = 4.8364(1) Å, c = 24.1941(5) Å, * = 105.672(1)°, V = 2666.4 Å, Z = 4, Rgt(F) = 0.031, wRref(F ) = 0.074, T = 298 K. Source of material 3,5-Dibromosalicyladehyde (56 mg, 0.2 mmol) and benzylamine (21 mg, 0.2 mmol) were dissolved in an aqueous acetonitrile solution (5 mL). The mixture was stirred for 5 min to give an orange solution, which was added to a methanol solution (1 mL) of Zn(NO3)2 · 6H2O (30 mg, 0.1 mmol). The mixture was stirred for another 5 min at room temperature to give a red solution and then filtered. The filtrate was kept in air for 5 d, forming yellow prismlike crystals. The crystals were isolated, washed three times with distilled water and dried in a vacuum desiccator containing anhydrous CaCl2 (yield 73 %). All reagents and solvents were used as obtained without further purification. Experimental details All hydrogen atoms were positioned geometrically (d(C—H) = 0.93 0.97 Å), and refined as riding with Uiso(H) = 1.2 Ueq(C). Discussion Transition metal complexes of Schiff-base ligands have been extensively investigated in the past decades. This is due to their novel structures and potential applications in many fields [1-7]. The title compound is the mononuclear zinc(II) complex of Schiff base. Zn(II) atom has a distorted tetrahedral coordination. Analogous tetrahedral Zn(II) species were also previously reported in the literature [8-10]. The zinc(II) atom is four-coordinated by two N atoms and two O atoms from two Schiff base ligands (figure, top). The average bond distances of Zn—O and Zn—N are 1.932(2) and 2.017(3) Å, respectively. The angles subtended at the Zn(II) ion in (ZnN2O2) is in the range of 95.1(1)° 125.0(1)°. The dihedral angle between the six-membered rings Zn1/O1/C1/C6/C7/N1 and Zn1/O1A/C1A/C6A/C7A/N1A is 86.8(2)°, (symmetry code A: –x,y,1⁄2–z). Some weak interactions play an important role in the crystal structure of the title complex. Z. Kristallogr. NCS 225 (2010) 365-366 / DOI 10.1524/ncrs.2010.0160 365 © by Oldenbourg Wissenschaftsverlag, München
9 citations
TL;DR: In this paper, the title compound, HgCl2 (2.71mg, 0.01 mmol), was prepared using methanol (50 ml), and the mixture was stirred for 10 min at room temperature.
Abstract: C24H20Cl4Hg2N4, triclinic, P1 (no. 2), a = 8.058(2) Å, b = 8.744(2) Å, c = 9.867(3) Å, + = 105.80(2)°, * = 100.49(2)°, & = 99.50(2)°, V = 640.6 Å, Z = 1, Rgt(F) = 0.059, wRref(F) = 0.181, T = 298 K. Source of material All reagents were purchased from Merck and used without further purification. For the preparation of the title compound, HgCl2 (2.71mg, 0.01.mmol) and 2-(phenyliminomethyl)pyridine (3.64 g, 0.01 mmol) were dissolved in methanol (50 ml). The mixture was stirred for 10 min at room temperature. The resulting solution was left in air for a few days, giving yellow crystals of the title compound (yield 5.04 g, 79 %; m.p. 298 °C). Discussion Schiff base metal complexes have been known since the 19 century. Investigation on metal organic complexes represents one of the most active areas of material science and chemical research. Schiff base metal complexes play a key role in the development of coordination chemistry [1-3]. Owing to the unique ability of the heterocyclic compounds to form stable chelates with various coordination modes, many crystal structures have been determined [4-8]. Numerous articles have been published on mercury complexes with Schiff base ligands derived by the condensation of pyridinecarbaldehydes and cyclic amines [9,10]. Arylsubstituted iminopyridine complexes have emerged as a powerful class of catalysts for a host of important bond-forming reactions including olefin polymerization, hydrogenation, and hydrosilation [11-13]. It is also now well-established that iminopyridines are both redox [14] and chemically active ligand, [15] participating in electron transfer, addition reactions, and deprotonation chemistry [16]. The crystal structure of the title compound contains a binuclear mercury(II) complex in which the five-coordinated Hg (II) ions have a distorted square pyramidal environment where each of them is surrounded by two (one imino and one pyridine) nitrogen atoms belonging to bidentate chelating iminopyridine ligand and three (two bridge and one terminal) chlorine atoms. The bond lengths of Hg—N fall in the range of 2.322(8) 2.497(7) Å, which are similar to those reported in the literature [10]. The Hg—Nimine distances [2.497(7) Å] are notably longer than the Hg—Npyridine distances [2.322(8) Å]. The C6=N2 and C7—N2 distances of 1.27(1) Å and 1.42(1) Å indicate double and single bonds, respectively. The bond angles around the Hg(II) centre show notable deviations from ideal square-pyramidal geometry. One chlorine atom bridges two Hg(II) centres to form a centrosymmetric binuclear complex with the Hg···Hg distance of 4.71 Å. The planar N1/C5/C6/N2 group forms a dihedral angle of 2.37° with the benzyl group, and the pyridine ring is twisted by about 10.91° out of the N1/C5/C6/N2 plane. The crystal structure of the iminopyridine complex consists of discrete [Hg2Cl4(C12H10N2)2] units held together with stacking interactions between the pyridine and the benzene rings. The centroid-to-centroid distance between benzene and pyridine rings, is 3.852 Å, showing the weak --interaction. Z. Kristallogr. NCS 225 (2010) 717-718 / DOI 10.1524/ncrs.2010.0316 717 © by Oldenbourg Wissenschaftsverlag, München
8 citations
TL;DR: In this article, a mixture of Ca(NO3)2.4 and 2propyl-1H-imidazole-4,5-dicarboxylic acid was stirred into 15 ml of water and the mixture was placed into 25 mL Teflon-lined autoclave and heated under autogenous pressure at 160 °C for 72.h.
Abstract: C16H22CaN4O10, monoclinic, C12/c1 (no. 15), a = 12.724(2) Å, b = 13.030(2) Å, c = 11.703(2) Å, ) = 97.856(2)°, V = 1922.1 Å, Z = 4, Rgt(F) = 0.039, wRref(F) = 0.109, T = 296 K. Source of material The mixture of Ca(NO3)2.·.4H2O (0.024 g, 0.1 mmol) and 2propyl-1H-imidazole-4,5-dicarboxylic acid (H2L, 0.041 g, 0.2.mmol) was stirred into 15 ml of water. Then 3 ml aqueous solution of potassium hydroxide (0.0056 g, 0.1 mmol) was added to deprotonate the dicarboxylic acid. The pH was adjusted to approx. 4 with 1 M solution of nitric acid. After stirring for 20 min in air and then the mixture was placed into 25 mL Teflon-lined autoclave and heated under autogenous pressure at 160 °C for 72.h. The autoclave was cooled over a period of 12 h at a rate 5.°C/h. After the mixture was slowly cooled to room temperature, colourless crystals were obtained, the products are stable in air and insoluble in water (yield 0.017 g, 36 % based on the calcium element). Elemental analysis — found: C, 40.82 %; H, 4.78 %; N, 11.85 %; calculated for C16H22N4O10Ca: C, 40.84 %; H, 4.71 % ; N, 11.90 %. IR data are available in the CIF. Discussion The rational design and construction of coordination polymers with unique structural motifs and unique chemical and physical properties have attracted extensive interest in supramolecular and materials chemistry [1-3]. In the past decade, plenty of metalorganic hybrids exhibiting fascinating structures have been synthesized [4-7]. Some studies on diand multi-carboxyl ligands or multifunctional carboxyl-containing ligands incorporating other coordination groups, such as N, S have been reported [9,10]. Recent years, imidazole dior multi-carboxylate have been intensively employed to provide a variety of topological architectures [9,10]. The title complex consists of one calcium(II) cation, two HL ligands, and two coordinated water molecules. Ca(II) is octacoordinated [CaN2O6], and has in a slightly distorted quadratic anti-prismatic coordination polyhedron formed by four oxygen atoms from the deprotonated carboxylate group of HL ligand, two nitrogen atoms from the imidazole rings, and two oxygen atoms of water molecules. The N1 and O4 atoms chelate the Ca(II) with a five membered ring of N1/C2/C5/O4/Ca1, while O1 of the other carboxylate groups from HL exhibits a monodentate mode to link the Ca(II) ion. The O2 and O3 atoms do not participate in the coordination. The Ca—O distances range from 2.412(2) to 2.608(2) Å. The bond length of Ca1—N is 2.605(2) Å. The angles around the central Ca ∠O1–Ca1–O1, ∠O1–Ca1–O5, and ∠O1–Ca1–O5 are 72.72(9)°, 125.71(6)° and 71.73(6)°, respectively. The angles of ∠O5–Ca1–O5, ∠O1–Ca1–N1, ∠O1–Ca1–N1 are 160.69(8)°, 156.47(5)° and 107.75(6)°, respectively. The dihedral angles between the adjacent imidazole rings attached to the central Ca is 52.39°. The above units are connected through the bridging O1 of 4-carboxylate groups of HL ligand to an edge-sharing dinuclear moiety with a Ca···Ca separation of 4.468 Å. These dinuclear units are grafted on to an infinite zigzag chains with the shortest intra-chain Ca···Ca distance of 9.10(6) Å. The chains are further linked by O4 of 4-carboxylate groups of next HL ligand to layer structure. Between the adjacent parallel layers there are hydrogen bonds interaction between the oxygen atoms of coordination waters and the carboxylate groups, the nitrogen of imidazole rings: O3–H3···O2 [d(O···O) = 2.478(2) Å, ∠O–H···O = 179.2°], O5–H1W···O4 [d(O···O) = 3.089(2) Å, ∠O–H···O = 160.2°], O5–H2W···O2 [d(O···O) = 2.953(2) Å, ∠O–H···O = 173.1°], N2–H2···O4 [d(O···O) = 2.863(2) Å, ∠O–H···O = 171.0°], (symmetry codes i: –x+1,y, –z+1⁄2; ii: –x+1⁄2,y–1⁄2,–z+1⁄2; iii: x+1⁄2,y–1⁄2,z; iv: x–1⁄2,y+1⁄2,z). Z. Kristallogr. NCS 225 (2010) 119-120 / DOI 10.1524/ncrs.2010.0051 119 © by Oldenbourg Wissenschaftsverlag, München
6 citations
TL;DR: In this article, a solution of K2PtCl4 was added acridine (acr, 0.1813 g, 1.012 mmol), and the mixture was refluxed for 7 h. The precipitate was then separated by filtration, washed with acetone and pentane, and dried at 50 °C to give a yellow powder (0.1615 g).
Abstract: C26H18Cl2N2Pt, monoclinic, C12/c1 (no. 15), a = 16.051(1) Å, b = 8.4946(5) Å, c = 17.222(1) Å, * = 115.984(1)°, V = 2110.8 Å, Z = 4, Rgt(F) = 0.028, wRref(F ) = 0.079, T = 200 K. Source of material To a solution of K2PtCl4 (0.1993 g, 0.480 mmol) in H2O (20 ml) was added acridine (acr, 0.1813 g, 1.012 mmol), and the mixture was refluxed for 7 h. The precipitate was then separated by filtration, washed with acetone and pentane, and dried at 50 °C to give a yellow powder (0.1615 g). Crystals suitable for X-ray diffraction analysis were obtained by slow evaporation of a dimethyl sulfoxide solution at 80 °C. Experimental details Hydrogen atoms were positioned geometrically and allowed to ride on their parent atoms [d(C—H) = 0.95 Å and Uiso(H) = 1.2 Ueq(C)]. The highest peak (1.92 e·Å) and the deepest hole (–0.84 e·Å) in the difference Fourier map are located 1.04 Å and 0.84 Å from the Pt1 atom, respectively. Discussion In the title complex, the Pt(II) ion is four-coordinated in a slightly distorted square-planar manner by two N atoms from two acridine ligands and two chloride ions (figure, top). The Pt atom is located on an inversion center and thus the asymmetric unit contains one half of the complex. The nearly planar acridine ligands, with a maximum deviation of 0.068(5) Å (C11) from the leastsquares plane, are parallel. The Cl atoms are in trans conformation with respect to each other and almost perpendicular to the acridine planes, with the bond angle ∠N1–Pt1–Cl1 = 89.1(1)°. In the crystal structure, the complexes are arranged in a V-shaped packing pattern and stacked in two distinct columns along [010] (figure, bottom). The packing pattern is considerably similar to that of the most stable polymorph of acridine [1]. In the columns, numerous intermolecular --interactions between adjacent sixmembered rings are present. The shortest distance between Cg1 (the centroid of ring N1-C13) and Cg2 (ring C1-C6; symmetry code i: 1⁄2–x,1⁄2–y,–z) is 3.601(4) Å, and the dihedral angle between the ring planes is 1.0(3)°. Z. Kristallogr. NCS 225 (2010) 323-324 / DOI 10.1524/ncrs.2010.0141 323 © by Oldenbourg Wissenschaftsverlag, München Crystal: yellow block, size 0.06 × 0.18 × 0.20 mm Wavelength: Mo K+ radiation (0.71073 Å) .: 69.18 cm−1 Diffractometer, scan mode: Bruker SMART 1000 CCD, #/' 2,max: 56.56° N(hkl)measured, N(hkl)unique: 7355, 2567 Criterion for Iobs, N(hkl)gt: Iobs > 2 )(Iobs), 1801 N(param)refined: 142 Programs: SHELXS-97 [2], SHELXL-97 [3], ORTEP-III [4], PLATON [5] Table 1. Data collection and handling. H(2) 8f 0.0009 0.2131 −0.0640 0.036 H(3) 8f 0.0154 −0.0438 −0.1001 0.041 H(4) 8f 0.1573 −0.1798 −0.0321 0.043 H(5) 8f 0.2832 −0.0582 0.0745 0.042 H(7) 8f 0.3529 0.1750 0.1666 0.038 H(9) 8f 0.4222 0.4134 0.2551 0.048 H(10) 8f 0.4114 0.6778 0.2795 0.050 H(11) 8f 0.2667 0.8068 0.2066 0.044 H(12) 8f 0.1395 0.6786 0.1087 0.041 Table 2. Atomic coordinates and displacement parameters (in Å). Atom Site x y z Uiso
6 citations
TL;DR: In this article, the authors described a compound from 1-hydroxyimidazole-3oxide, benzyl bromide, and sodium hydrogen carbonate, which was prepared from a mixture of 1-H17BrN2O2 and 1-hexafluorophosphate.
Abstract: C17H17BrN2O2, orthorhombic, Pca21 (no. 29), a = 13.1672(3) Å, b = 14.5045(4) Å, c = 8.9452(2) Å, V = 1708.4 Å, Z = 4, Rgt(F) = 0.040, wRref(F) = 0.103, T = 173 K. Source of material The title compound was prepared from 1-hydroxyimidazole-3oxide, benzyl bromide and sodium hydrogencarbonate, as described in [1]. Notably, the reaction did not work with benzyl chloride [2]. The resulting clear syrup crystallized after three months at room temperature. The low melting temperature range of 60 70 °C qualifies this salt as an ‘ionic liquid’. Discussion As mentioned earlier [3], imidazolium salts with an N-O moiety are quite rare [1-6]. Different conformations of 1,3-di(alkyloxy)imidazolium cations have been reported [1,5]. Interestingly, in the present case of the bromide, the benzyl groups adopt an anti conformation. This is in contrast to the recently described hexafluorophosphate where they exhibit a syn conformation [1]. Thus, the O1—C4 bond is rotated out of the ring plane by 56.8°, the O2—C11 bond by 82.6° on opposite sides of the heterocyclic ring. A hydrogen bond is observed between the most acidic proton of the imidazolium cation and the bromide anion: C1–H···Br1 (H···acceptor distance 2.61 Å and donor···acceptor distance 3.485 Å, donor–H···acceptor angle 153°). The bromide accepts another hydrogen bond from C2–H (2.64 Å and 3.571 Å, 168°) and also three weak contacts from C11–H (2.88 Å and 3.834 Å, 162°), C8–H (2.99 Å and 3.892 Å, 160°), and C4–H (2.99 Å and 3.816 Å, 142°); symmetry codes i: x,y, –1+z; ii: 1–x,–y,–1/2+z; iii: 1–x,1–y,–1/2+z; iv: 3/2–x,y,–1/2+z. Z. Kristallogr. NCS 225 (2010) 759-760 / DOI 10.1524/ncrs.2010.0334 759 © by Oldenbourg Wissenschaftsverlag, München Crystal: colourless plate-like fragment, size 0.02 × 0.09 × 0.14 mm Wavelength: Cu K+ radiation (1.5418 Å) .: 33.47 cm−1 Diffractometer, scan mode: Xcalibur, Ruby, Gemini ultra, % 2,max: 134.86° N(hkl)measured, N(hkl)unique: 18441, 3006 Criterion for Iobs, N(hkl)gt: Iobs > 2 )(Iobs), 2661 N(param)refined: 200 Programs: SIR2002 [7], SHELXL-97 [8] Table 1. Data collection and handling. H(2) 4a 0.6380 0.1332 1.0354 0.045 H(3) 4a 0.6706 −0.0182 0.9112 0.041 H(11A) 4a 0.5473 0.0080 0.4926 0.043 H(11B) 4a 0.5384 −0.0658 0.6260 0.043 H(15) 4a 0.6612 −0.3097 0.1725 0.068 H(14) 4a 0.6356 −0.1612 0.0820 0.066 H(13) 4a 0.6046 −0.0405 0.2483 0.052 H(17) 4a 0.6162 −0.2197 0.5938 0.055 H(1) 4a 0.6440 0.1736 0.5876 0.040 H(16) 4a 0.6540 −0.3390 0.4284 0.066 H(4A) 4a 0.7520 0.3209 0.8828 0.070 H(4B) 4a 0.6823 0.3006 1.0270 0.070 H(6) 4a 0.7291 0.4663 0.7464 0.090 H(10) 4a 0.5545 0.4083 1.1004 0.082 H(8) 4a 0.5366 0.6571 0.9162 0.124 H(7) 4a 0.6610 0.6182 0.7399 0.125 H(9) 4a 0.4904 0.5561 1.0981 0.107 Table 2. Atomic coordinates and displacement parameters (in Å). Atom Site x y z Uiso
6 citations
TL;DR: In this article, the authors proposed a method for removing aquabis(acetylacetonato-\"O,O')(diacetylmethanido-\"C)iridium(III) in acetonitrile to form saturated solution at 70 °C, and then filtered off.
Abstract: C17H27IrNO7.50, monoclinic, C12/c1 (no. 15), a = 27.563(3) Å, b = 9.2294(9) Å, c = 20.462(2) Å, * = 126.993(1)°, V = 4157.7 Å, Z = 8, Rgt(F) = 0.028, wRref(F) = 0.054, T = 298 K. Source of material The titled complex was prepared by dissolving aquabis(acetylacetonato-\"O,O')(diacetylmethanido-\"C)iridium(III) in acetonitrile to form saturated solution at 70 °C, and then the insoluble substance was filtered off. The filtrate was slowly cooled to room temperature. Upon cooling, a yelleow crystalline product precipitated. Single crystals were selected from the product for the X-ray diffraction analysis. Experimental details The carbon-bound H atoms were positioned geometrically with d(C—H) = 0.93 0.98 Å, d(O—H) = 0.85 Å, and refined as riding with Uiso(H) = 1.2 Ueq(C), Uiso(H) = 1.5 Ueq(O). Discussion The Ir atom is six-coordinated and situated in a slightly distorted octahedral environment, formed by four oxygen atoms of two acetyacetone ligands, one carbon atom of one acetylacetone ligand and one N atom of acetonitrile. The average Ir—O bond length of two acetylacetone ligands is 2.0175(3) Å, the Ir—C bond length is found to be 2.133(4) Å, which agree with the literature data of Ir(C5H7O2)3 and Ir(C5H7O2)3(H2O) [1-3]. The Ir—N bond length is found to be 2.074(3) Å. The molecule packing is stablilized by extensive hydrogen bonds formed between water molecules and O atoms of the acetylacetone ligand with d(O···O) of 2.897(4) Å, 2.808(5) Å and 2.789(4) Å. Z. Kristallogr. NCS 225 (2010) 667-668 / DOI 10.1524/ncrs.2010.0292 667 © by Oldenbourg Wissenschaftsverlag, München Crystal: yellow block, size 0.12 × 0.21 × 0.26 mm Wavelength: Mo K+ radiation (0.71073 Å) .: 64.61 cm−1 Diffractometer, scan mode: Bruker SMART CCD, #/% 2θmax: 55° N(hkl)measured, N(hkl)unique: 13614, 4703 Criterion for Iobs, N(hkl)gt: Iobs > 2 )(Iobs), 3572 N(param)refined: 248 Programs: SHELXS-97, SHELXL-97 [4], DIAMOND [5] Table 1. Data collection and handling. H(1WA) 8f 0.9158 0.0844 0.1432 0.172 H(1WB) 8f 0.8846 −0.0536 0.1385 0.172 H(2A) 8f 0.1137 0.2637 0.0391 0.105 H(2B) 8f 0.0618 0.3473 −0.0393 0.105 H(2C) 8f 0.0488 0.2734 0.0177 0.105 H(3) 8f 0.0540 0.5905 −0.0317 0.066 H(5A) 8f 0.0522 0.9331 0.0269 0.106 H(5B) 8f 0.0298 0.8350 −0.0489 0.106 H(5C) 8f 0.0948 0.9041 0.0016 0.106 H(7A) 8f 0.2857 0.9399 0.4140 0.094 H(7B) 8f 0.2959 0.8566 0.4882 0.094 H(7C) 8f 0.2342 0.9363 0.4252 0.094 H(8) 8f 0.2987 0.6131 0.4715 0.062 Table 2. Atomic coordinates and displacement parameters (in Å). Atom Site x y z Uiso
5 citations
TL;DR: In this article, the effect of intermolecular hydrogen bonds on the assembly process of complex cations was investigated using CoCl2 · 6H2O (0.048 g, 0.4 mmol) and disodium naphthalene-1,5-disulfonate (1.5-Na2NDS) ligands.
Abstract: C16H24CoN2O13S2, triclinic, P1 (no. 2), a = 9.954(1) Å, b = 10.278(1) Å, c = 11.675(1) Å, + = 95.579(2)°, * = 106.855(2)°, ( = 94.513(2)°, V = 1130.5 Å, Z = 2, Rgt(F) = 0.029, wRref(F) = 0.082, T = 298 K. Source of material Nicotinamide (NA, 0.048 g, 0.4 mmol) was added with constant stirring to an aqueous solution (20 ml) of CoCl2 · 6H2O (0.048 g, 0.2 mmol). The solution was then treated with disodium naphthalene-1,5-disulfonate (1,5-Na2NDS, 0.58 g, 0.2 mmol). Yellow crystals of the title complex were collected after a few days (46 % yield based on Co). Experimental details The C-bound H atoms were geometrically placed (d(C—H) = 0.93 Å) and refined as riding with Uiso(H) = 1.2 Ueq(C). The Obound H atoms were located in difference Fourier maps and refined as riding in their as-found relative positions with Uiso(H) = 1.2 Ueq(O). Discussion Recently, assembling metal complexes through hydrogen bonds to create inorganic-organic hybrid materials has attracted considerable attention [1-8]. However, rationally control of molecular self-assembly into ordered solid state networks with a desired arrangement and dimensionality is a challenge to chemists. In this paper, we chose the appropriate transition metal such as Co with well-defined geometries and organic ligands with the inherent coordination and hydrogen bonding donor/acceptor functionalities, nicotinamides as the strategy to construct extended frameworks to evaluate the effect of intermolecular hydrogen bonds upon the assembly process of complex cations. In the title crystal structure, the Co centre is hexa-coordinated with five aqua ligands and one nicotinamide ligand through the pyridine nitrogen atom, of which one aqua ligand and the nicotinamide ligand are bound to apical positions [d(Co—O) = 2.113(2) Å, d(Co—N) = 2.133(2) Å], other aqua ligands at equatorial positions [d(Co—O) = 2.071(2) 2.113(2) Å], which is similar to those observed in [9]. The 1,5-NDS anion does not participate in the coordination of the Co(II), and has an inversion centre at the midpoint of the central C—C bond. The hexacoordinated Co(II) complexes are connected by hydrogen bonds between amides and the coordinated water molecules [d(O1–H···O7) = 2.686(2) Å, d(O3–H···O7) = 2.849(2) Å] to form infinite chains along [100]. The hydrogen bond motif results in the formations of two unique rings in each chain, C2(16) and C4(12), respectively. In the larger ring, the distance between pyridine rings is 3.35 Å, indicating significant aromatic interactions. Adjacent chains are interlinked by 1,5-NDS ligands via hydrogen bonds between the sulfonate oxygen atoms and the remaining N–H protons on the nicotinamide ligands and the coordinated water molecules, respectively, to generate 2D hydrogen bonded sheets. One kind of the 1,5-NDS ligands behave as pillar to sustain the layers through hydrogen bonds formed between the sulfonate oxygen atoms and the coordinated water molecules and between the sulfonate oxygen atoms and the N–H protons on the nicotinamide ligands to form 3D channel structures. Another kind of 1,5-NDS ligands and the lattice water molecules are located in the channels and make contact with host channels through hydrogen bonding interactions between the sulfonate oxygen atoms and the coordinated water molecules, between the sulfonate oxygen atoms and the lattice water molecules, and between the lattice water molecules and the coordinated water molecules. Z. Kristallogr. NCS 225 (2010) 371-373 / DOI 10.1524/ncrs.2010.0163 371 © by Oldenbourg Wissenschaftsverlag, München
5 citations
TL;DR: In this article, the title complex was prepared by dissolving aquabis(acetylacetonato-\"O,O')-(diacetylmethanido-C)iridium(III) in dimethylsulfoxide to form saturated solution at 189 °C, and then the insoluble substance was filtered off.
Abstract: C17H27IrO7S, triclinic, P1 (no. 2), a = 7.9964(7) Å, b = 9.0166(7) Å, c = 15.940(1) Å, * = 94.203(1)°, ) = 101.801(1)°, & = 111.274(1)°, V = 1034.5 Å, Z = 2, Rgt(F) = 0.023, wRref(F) = 0.078, T = 293 K. Source of material The title complex was prepared by dissolving aquabis(acetylacetonato-\"O,O')-(diacetylmethanido-C)iridium(III) in dimethylsulfoxide to form saturated solution at 189 °C, and then the insoluble substance was filtered off. The filtrate was slowly cooled to room temperature, a yelleow product precipitated. Several single crystals were selected from the precipitate. Experimental details All the hydrogen atoms were positioned geometrically with d(C—H) = 0.93 0.98 Å, and refined as riding with Uiso(H) = 1.2 Ueq(C). Discussion The Ir atom is six-coordinated and situated in a slightly distorted octahedral environment, formed by four oxygen atoms of two acetylacetone ligands, one carbon atom of one acetylacetone ligand and one S atom of dimethylsulfoxide. The average Ir—O bond length of two acetylacetone ligands is 2.022 Å. The Ir—C bond length is found to be 2.174 Å, which agree with the literature data for Ir(C5H7O2)3 and Ir(C5H7O2)3(H2O) [1-3]. The Ir—S bond length is found to be 2.3078 Å. Z. Kristallogr. NCS 225 (2010) 575-576 / DOI 10.1524/ncrs.2010.0252 575 © by Oldenbourg Wissenschaftsverlag, München Crystal: yellow block, size 0.19 × 0.23 × 0.27 mm Wavelength: Mo K* radiation (0.71073 Å) -: 65.87 cm−1 Diffractometer, scan mode: Bruker SMART CCD, #/% 2+max: 50° N(hkl)measured, N(hkl)unique: 6086, 3379 Criterion for Iobs, N(hkl)gt: Iobs > 2 ((Iobs), 3166 N(param)refined: 235 Programs: SHELXS-97, SHELXL-97, SHELXTL [4] Table 1. Data collection and handling. H(2A) 2i −0.0010 0.3568 0.0013 0.067 H(2B) 2i 0.1176 0.2831 −0.0091 0.067 H(2C) 2i −0.0006 0.2185 0.0598 0.067 H(3) 2i 0.4138 0.3493 0.0566 0.043 H(5A) 2i 0.7812 0.4313 0.1830 0.060 H(5B) 2i 0.7345 0.4381 0.0835 0.060 H(5C) 2i 0.8419 0.6009 0.1372 0.060 H(7A) 2i 0.7907 1.2214 0.4464 0.073 H(7B) 2i 0.8015 1.0799 0.4904 0.073 H(7C) 2i 0.8797 1.1215 0.4136 0.073 H(8) 2i 0.4396 1.1021 0.4008 0.052 H(10A) 2i −0.0148 0.8856 0.2753 0.072 H(10B) 2i 0.1094 0.9914 0.3775 0.072 H(10C) 2i 0.1118 1.0484 0.2866 0.072 H(11) 2i 0.4205 0.4623 0.2958 0.042 H(13A) 2i −0.0385 0.4464 0.3688 0.079 H(13B) 2i 0.1421 0.5659 0.4251 0.079 H(13C) 2i 0.0511 0.6104 0.3434 0.079 H(15A) 2i 0.7509 0.6629 0.3750 0.091 H(15B) 2i 0.7565 0.6599 0.4811 0.091 H(15C) 2i 0.6875 0.5155 0.4231 0.091 H(16A) 2i 0.2278 0.9841 0.1266 0.084 H(16B) 2i 0.4350 1.0964 0.1714 0.084 H(16C) 2i 0.3823 1.0875 0.0786 0.084 H(17A) 2i 0.7275 1.0949 0.1103 0.105 H(17C) 2i 0.7710 0.9565 0.1518 0.105 H(17B) 2i 0.7503 1.0933 0.2102 0.105 Table 2. Atomic coordinates and displacement parameters (in Å). Atom Site x y z Uiso
5 citations
TL;DR: In this article, a mixture of CaCl2 (0.5 mmol, 0.95 g) in 15 ml of H2O solution was sealed in an autoclave equipped with a Teflonlined stainless steel vessel (25 ml) and then heated at 373 K for 3 days.
Abstract: C14H18CaN4O10, monoclinic, C12/c1 (no. 15), a = 12.248(1) Å, b = 13.345(2) Å, c = 11.315(1) Å, * = 99.191(1)°, V = 1825.7 Å, Z = 4, Rgt(F) = 0.034, wRref(F ) = 0.091, T = 298 K. Source of material A mixture of CaCl2 (0.5 mmol, 0.05 g) and 2-ethyl-1Himidazole-4,5-dicarboxylic acid (0.5 mmol, 0.95 g) in 15 ml of H2O solution was sealed in an autoclave equipped with a Teflonlined stainless steel vessel (25 ml) and then heated at 373 K for 3 days. Crystals of the title compound were obtained by slow evaporation of the solvent at room temperature. Experimental details Carbon and nitrogen bound hydrogen atoms were placed at calculated positions and treated as riding on the parent atoms with d(C—H) = 0.93 Å, d(N—H) = 0.86 Å, and with Uiso(H) = 1.2 Ueq(C,N). The water H atoms were located in a difference Fourier map, and refined with a distance restraint of d(O—H) = 0.84 Å. Discussion 4,5-imidazoledicarboxylic acid, known as a rigid N-heterocyclic carboxylic acid, owns great potential for coordination interactions and hydrogen bonding, it can genrate huge diversity of supramolecular architectures due to its quality of being deprotonated into different species with different proton numbers. Up to date, it has been found that imidazoledicarboxylate complexes exhibit useful properties [1,2]. In the title complex, the Ca cation is eight-coordinated (N2O6), with two chelating rings from N,O-bidentate 2-ethyl-1Himidazole-4,5-dicarboxylate anions, two carboxylate O atoms from another two 2-ethyl-1H-imidazole-4,5-dicarboxylate anions, and two coordinated water molecules, generating a slightly distorted square-antiprismatic coordination. The Ca—N bond distances are both 2.584(2) Å, and the Ca—O bond lengths vary from 2.412(2) Å to 2.539(1) Å. The Ca centres are interconnected by the ligands, whereby the ligand is functioning as tridentate and bridges Ca atoms into an infinite two-dimensional layer constructed of Ca4 squares, the edge distances of the quasisquare are of 9.0568(9) Å and the angles are 85.090(1)° and 94.910(5)°, respectively. The layers are further linked into a three-dimensional network by an extensive number of hydrogen bonds involving the coordinated water molecules and the 2-ethyl1H-imidazole-4,5-dicarboxylate ligands. Z. Kristallogr. NCS 225 (2010) 403-404 / DOI 10.1524/ncrs.2010.0177 403 © by Oldenbourg Wissenschaftsverlag, München Crystal: colorless block, size 0.22 × 0.23 × 0.45 mm Wavelength: Mo K+ radiation (0.71073 Å) .: 4.09 cm−1 Diffractometer, scan mode: SMART 1000 CCD, #/' 2,max: 49.98° N(hkl)measured, N(hkl)unique: 4509, 1613 Criterion for Iobs, N(hkl)gt: Iobs > 2 )(Iobs), 1293 N(param)refined: 133 Programs: SHELXS-97, SHELXL-97, SHELXTL [3] Table 1. Data collection and handling.
5 citations
TL;DR: In this article, a mixture of ZnO (0.5 mmol), 3-animo-4-chlorobenzenesulphonic acid (1.0 mmol) in H2O (20 ml) was sealed into a 25 ml Teflon-lined stainless steel reactor and heated at 443 K for 1 d. The reactor was then cooled slowly to room temperature and the solution was filtered.
Abstract: C36H34Cl2N6O10S2Zn, triclinic, P1 (no. 2), a = 10.8271(9) Å, b = 12.480(1) Å, c = 16.427(1) Å, + = 75.019(1)°, * = 86.335(1)°, ( = 68.937(1)°, V = 2000.0 Å, Z = 2, Rgt(F) = 0.042, wRref(F) = 0.112, T = 296 K. Source of material A mixture of ZnO (0.5 mmol), 1,10-phenanthroline (phen, 0.5 mmol), 3-animo-4-chlorobenzenesulphonic acid (1.0 mmol) in H2O (20 ml) was sealed into a 25 ml Teflon-lined stainless steel reactor and heated at 443 K for 1 d. The reactor was then cooled slowly to room temperature and the solution was filtered. Red block-shaped crystals were obtained from the filtrate after several days at room temperature. Discussion The design and construction of metal-organic coordination polymers is of current interest in the fields of supramolecular chemistry and crystal engineering. Major reasons for this interest stem from their intriguing variety of topologies and structural diversity, such as helixes and diamondoid nets, and from their potential applications as functional materials. So far, most of these materials are constructed by various rigid organic bidentate ligands containing pyridine rings, dicarboxylate, phosphonate, and sulfonate as spacers and metal cores as connectors [1-6]. 3-amino-4chlorobenzenesulphonic acid is versatile coordinating ligands and it can act not only as hydrogen-bond aceptor but also as hydrogen-bond donor. In the title crystal structure, there are two 3-amino-4-chlorobenzenesulphonate anions, one Zn(II) ion, two phen, two coordinated water and two lattice water molecules in the asymmetric unit. Zn ion is six-cooridnated by two water oxygen atoms and four N atoms from two phen, forming a distorted octahedron. The bond angles around central Zn ion range from 77.38(8)° to 169.35(9)°. The bond lengths of Zn—O are 2.091(2) and 2.108(2) Å. The bond lengths of Zn—N are 2.153(2) Å, 2.160(2) Å, 2.156(2) Å, 2.163(2) Å. In the title complex, there are four kinds of hydrogen bonds: (a) hydrogen bonding between the lattice water molecules with d(O···O) = 2.733(6) Å; (b) hydrogen bonding between 3-amino-4-chlorobenzenesulphonate oxygen atoms or sulfur atoms and lattice water molecules with d(O···O) = 2.784(4) Å, 2.802(4) Å and d(S···O) = 3.767(3) Å, 3.657(4) Å, respectively; (c) hydrogen bonding between coordinating water molecules and lattice water molecules with d(O···O) = 2.644(3) Å; (d) hydrogen bonding between the 3-amino-4-chlorobenzenesulphonate either by oxygen atoms/oxygen atoms with d(O···O) = 2.729(3) Å, 2.767(3) Å, 2.761(3) Å, or by oxygen and sulfur atoms with d(O···S) = 3.666(2) Å and 3.710(2) Å, or by oxygen and nitrogen atoms with d(O···N) = 3.128(4) Å, 3.364(5) Å, respectively. An extended two-dimensional network of hydrogen bonds contributes to the stability of the structure. 410 Z. Kristallogr. NCS 225 (2010) 410-412 / DOI 10.1524/ncrs.2010.0180 © by Oldenbourg Wissenschaftsverlag, München
TL;DR: In this paper, a methanol solution (20 mL) of 3-thiosemicarbazide (0.073 g, 8.0 mmol) was added gradually to the solution (10 mL) with stirring, and the resulting mixture was diffused with diethyl ether vapor at room temperature for two weeks to obtaine blue block-shaped crystals of the title complex.
Abstract: C16H18N8NiO8S2, monoclinic, C12/c1 (no. 15), a = 17.964(2) A, b = 9.834(1) A, c = 14.122(2) A, ) = 110.582(1)°, V = 2335.7 A, Z = 4, Rgt(F) = 0.028, wRref(F ) = 0.070, T = 296 K. Source of material A methanol solution (20 mL) of 3-thiosemicarbazide (0.073 g, 8.0 mmol) was added gradually to the methanol solution (10 mL) of salicylaldelyde (0.197 g, 16 mmol) with stirring. The reaction mixture was heated at 60 °C for 2 h. Then an ethanol solution of Ni(NO3)2.·.6H2O (1.16 g, 4.0 mmol) was added dropwise to the above solution, the resultant mixture was stirred 2 h, then cooled, and filtrated. The resulting clear solution was diffused with diethyl ether vapor at room temperature for two weeks to obtaine blue block-shaped crystals of the title complex suitable for X-ray crystal determination (yield 0.822 g, 36%).Chemical analysis— found: C, 34. 02 %; H, 3.09 %; N, 19.51 %; calculated for C16H18NiN8O8S2: C, 33.53%;H, 3.17%;N, 19.55%. IR data are available in the CIF. Discussion During past decades, the design and syntheses of Schiff base complexes has been extensively investigated due to their inherent coordination functionalities, spectroscopic characteristics, optical properties as well as biological and catalytic activities [1-4]. These complexes can serve as potent antitumor, antiviral and antibacterial agents [5]. Among these Schiff-base complexes, nickel(II) representatives have attracted great attention since nickel has been recognized as a considerably important biological agent forming the active site of a variety of metalloproteins, such as hygrogenase(H2-ase), carbon monoxide dehydrogenase (CODH), S-methyl-coenzyme-M methylreductase (MCR) and urease [6-8]. In addition, their adducts with nitrogen have potential applications in area of organic conductors andmagneticmaterials [9]. The asymmetric unit in the title complex contains a discrete mononuclear cation [Ni(HBTC)2] and two nitrate groups (figure, top). Each salicylaldehyde thiosemicarbazide Schiff base provides O, N, S as donor atoms, acting as a tridentate ligand. Two HBTC ligands chelate the central Ni(II) ion. The coordination polyhedron around Ni(II) ion can be considered as a slightly distored octahedron (NiO2N2S2). The equatorial plane is comprised of two oxygen atoms and two sulfur atomswhile two nitrogen atoms occupy the axial positions with N1–Ni1–N1A bond angle of 176.72(9)°. The chelation of each HBTC ligand with nickle ion form a five-membered ring Ni1–C8–N1–N2–S1 and one six-membered ring Ni1–C1–C6–C7–N1–O1 with dihedral angle of 21.27°. The bond lengths Ni—N, Ni—O, and Ni—S are 2.030(2) A, 2.118(1) A, and 2.3779(6) A, respectively, being comparable to those observed in Ni(II) complexes containing a S–C–N–N unit [10]. Every nitrate ion is planar, and the plane is nearly perpendicular to the adjacent benzene ring of HBTC with dihedral angle of 89.779(3)°. All atoms of nitrate ions participate in the formation of hydrogen bonds. Five kinds of intermolecular hydrogen bonds are formed between phenol oxygen atoms and nitrate ions [O1–H1···N4, O1–H1···O4, O1–H1···O2; symmetry code i: –x,y,–z+1/2] or between HBTC N atoms and nitrate O atoms [N3–H3A···O2, N2–H2D···O3; symmetry code ii: –x+1/2,y+1/2,–z+1/2]. These hydrogen bonds interconnect [Ni(HBTC)2] units to a layered supramolecular network (figure, bottom).Along [001], such layers are parallel stacked and Z. Kristallogr. NCS 225 (2010) 79-80 / DOI 10.1524/ncrs.2010.0032 79 © by Oldenbourg Wissenschaftsverlag, Munchen
TL;DR: In this article, a solution of 2-ethoxy-2-oxoethyl 2-(4-fluorophenyl)acetate (0.96 g, 4 mmol) was added dropwise to a suspension of NaH in dry THF in an ice cold bath.
Abstract: C10H7FO3, monoclinic, P121/c1 (no. 14), a = 7.584(2) Å, b = 8.863(2) Å, c = 12.707(3) Å, * = 90.64(1)°, V = 854.1 Å, Z = 4, Rgt(F) = 0.041, wRref(F) = 0.107, T = 296 K. Source of material A solution of 2-ethoxy-2-oxoethyl 2-(4-fluorophenyl)acetate (0.96 g, 4 mmol) in dry THF was added dropwise to a suspension of NaH in dry THF in an ice cold bath. The stirring was maintained at room temperature for 5 h. Water was added and the solution was extracted twice with ethyl ether. The aqueous phase was cooled to 0 °C and then acidified with concentrated hydrochloric acid to give a solid precipitate. The title compound was crystallized from ethanol-water (2:1, v/v) to give the colorless blockshaped crystals suitable for single-crystal structure determination. Discussion Compounds with &-butyrolactone-core (furanone) show diverse biological activities such as antitumor and anti-inflammatory activity [1-3]. It is reported that butalactin exhibits moderate antibacterial activity against Gram-positive bacteria [4]. Based on this findings, some derivatives of &-butyrolactone (5-alkoxy-4aminofuran-2(5H)-one) showing good antibacterial activity against multiresistant Staphylococcus aureus were reported [5]. Recently, we focused our efforts to synthesize enamines with &butyrolactone-core for antibacterial activity screening. In the title crystal structure, the bond length d(C7—C10) = 1.346(2) Å is in the range of a typical double bond (1.32 1.38 Å), and the title compound was therefore identified as a furan-2(5H)one not a furan-2(3H)-one. Because C9 attaches to a double bond, )-hyperconjugation occurring between C9—H9A (H9B) and C7—C10 slightly shortens C9—C10 bond from about 1.53 to 1.490(2) Å. C10—O3 (1.316(2) Å) bond length is shorter than the standard C—O single bond (1.41 1.44 Å), but longer than C—O double bond (1.19 1.23 Å). This clearly indicated that an sp orbital of O3 is conjugated with the molecular orbital of C7=C10 double bond, which was supported by the small torsion angle (–1.5(2)°) of C1–C7–C10–O3. The stereochemistry of the double bond in lactone ring was assigned as (E)-configuration (figure, top). The butyrolactone moiety makes a dihedral angle of 17.86(6)° with the 4-fluorophenyl group. In the title compound, the two independent hydrogen bonds generate a two-dimensional layer of edge-fused centrosymmetric rings running parallel to (100), with R2(8) rings built from pairs of C–H···F hydrogen bonds centred at (0,3n/2 + 1,–1n/2), where n represents an integer, and with the R6(44) rings built from pairs of C–H···F and O–H···O hydrogen bonds centred at (0,3n/2+1, 1n/2), where n again represents an integer (figure, bottom). The resulted layer has a zigzag pattern in the cross section, running along the [010] direction. In a layer, each R6(44) ring runs through by other two R6(44) rings which are from other two layers, respectively, and these layers (three) therefore interweave each other to form a layered tablet. The title ompound extends further to its final three-dimensional network through intermolecular C9–H9A···(benzene ring) contacts. Z. Kristallogr. NCS 225 (2010) 797-798 / DOI 10.1524/ncrs.2010.0351 797 © by Oldenbourg Wissenschaftsverlag, München
TL;DR: In this article, the authors used a riding model to calculate the positions of the bridate bridates of the 2,2'-bipyridine (2.2') and 2.3'-carboxylate (1,3-dicarboxylates) ligands.
Abstract: C22H24MnN2O5, triclinic, P1 (no. 2), a = 9.597(2) Å, b = 10.825(2) Å, c = 11.445(3) Å, * = 63.137(3)°, ) = 70.425(4)°, & = 77.851(3)°, V = 996.9 Å, Z = 2, Rgt(F) = 0.037, wRref(F) = 0.101, T = 298 K. Source of material An ethanolic solution of 2,2'-bipyridine (0.1 mmol) and Mn(OAc)2.·.2H2O (0.1 mmol) was slowly added to a 20 ml ethanolic solution of sodium adamantane-1,3-dicarboxylate (Na2ADC, 0.1 mmol), with stirring for 5 h at room temperature, colorless crystals of the title compound were obtained by slow evaporation of the solvent after three weeks. Experimental details The hydrogen atoms of were placed in calculated positions (d(C—H) = 0.93 Å) refined using a riding model, with Uiso(H) = 1.2 Ueq(C). Hydrogen atoms of water molecules were located in a difference Fourier map and refined with restraints of d(O—H) = 0.83(1) Å, and Uiso(H) = 1.5 Ueq(O). Discussion The design and construction of polymeric metal-organic frameworks (MOFs) with intriguing structural motifs, unique chemical and physical properties leading to potential applications in catalysis, luminescence, magnetism, sorption, ion exchange, nonlinear optics, electricity has been attracting enormous interest in supramolecular chemistry and material chemistry [1-5]. It is well known that multicarboxylate ligands play an important role in coordination chemistry, which can adopt diverse binding modes and geometrical configuration to provide unique MOFs [6-8]. Among them, the rigid organic aromatic multicarboxylate species such as benzenedicarboxylate isomers, have been widely used in constructing novel metal-organic hybrid complexes [9,10]. Adamantane-1,3-dicarboxylate (ADC), is a typical dicarboxylic acid and one of the most stable hydrocarbons. As a consequence of its stability, it can be produced catalytically from a wide various precursor organic substances [11]. On the other hand, in the past decades, kinds of supramolecular self-assemblies were directed by non-covalent intermolecular interactions such a hydrogen bonding and ,-, stacking interactions have been fixed by carefully employed building blocks and linkers [12]. Therefore, to avoid inter-penetration the heterocyclic aromatic lignad 2,2'bipyridine was introduced into the Mn-ADC system based on the following considerations: (a) the steric hindrance at the metal centers will be increased when the bulky aromatic ligand bonds to the metal ions, this reduce the dimensions of the net shaped; (b) chelating bipyridyl-like ligands may provide recognition sites for ,-, stacking interactions to form interesting supramolecular motifs [13]. In the title crystal structure, Mn(II) ion has a slightly distorted octahedral coordination, where the equatorial plane comprise one N2 atom three O atoms of three different ADC ligands. The apical postions are occupied by the N atom of bipy ligand and one O atom from a chelating-bidentate carboxylate group. The Mn—O and Mn—N bond lengths fall in the ranges of 2.163(2) 2.448(2) and 2.267(2) 2.325(2) Å, respectively, and the transand cisoid bond angles fall in the regions of 71.58(8)° 102.88(8)° and 144.43(8)° 164.63(7)°, respectively, showing considerable deviation from the corresponding vaules for an ideal octahedron. The distorted octahedron of Mn(II) ions can be explained by Jahn-Teller effect. The Mn—O/N bond lengths are well agree with related Mn complex [14]. The Mn(II) ions are bridged by ADC into a dimeric metal unit with the separation of 3.8 Å for Mn···Mn. Additionally, a eight-membered ring is also shaped due to the connection. The bidentate O3–C21–O4 carboxylate groups chelate one Mn(II) ion while bridging bidentate O1–C11–O2 ends binds to the second Mn(II) cation. Thus, the adjacent Mn(II) are linked by ADC ligands into 1D polyermic chains extending along [001]. A similar 1D chain structure of a Co complex with ADC is also observed recently [15]. The 2,2'-bipy ligand is nealy perfect planar with the maximal deviation of 0.062(3)°. The chains are further held together by aromatic interactions with distance of 3.61(2) Å, shaping a double-stranded chain. Furtheremore, the lattice water molecule provides a hydrogen-acceptor to O3, forming a strong hydrogen-bonding interaction. The interchain hydrogen bond is reponsible for supramolecular assembly of the 2D sheet and the lattice water molecule are sandwiched between sheets. This is related to the fact that chelating ligands such as 2,2'-bipy take a Z. Kristallogr. NCS 225 (2010) 483-485 / DOI 10.1524/ncrs.2010.0212 483 © by Oldenbourg Wissenschaftsverlag, München
TL;DR: In this article, the structure of AgCH3COO (silver acetate), PPh3 (triphenylphosphine) and C4H5N3 (2-AMP = 2-aminopyrimidine) was analyzed using a single crystal X-ray diffraction.
Abstract: C77H72Ag2O6P4, monoclinic, C12/c1 (no. 15), a = 44.268(2) Å, b = 13.2848(5) Å, c = 24.9524(9) Å, * = 105.449(2)°, V = 14144.1 Å, Z = 8, Rgt(F) = 0.067, wRref(F) = 0.143, T = 296 K. Source of material A mixture of AgCH3COO (silver acetate), PPh3 (triphenylphosphine) and C4H5N3 (2-AMP = 2-aminopyrimidine) in molar ratio of 1:1:2 in CH2Cl2/CH3OH (10 ml, v/v = 1/1) was stirred for 2 hours at room temperature, then filtered. Subsequent slow evaporation of the filtrate resulted in the formation of colorless crystals of the title complex. Crystals suitable for single crystal X-ray diffraction were selected directly from the sample as prepared. Discussion For extending study on systematic structural chemistry of silver complexes of ligands containing P and N atoms, such as [Ag(.X)(2-Apy)(PPh3)]2 (X = Cl, Br) [1], [Ag2(.-dppm)2(.-SO4)(2AMP)2] · CH3OH [2], [Ag2Cl2(PPh3)2(2-AMP)]∞ [3] [Ag2Br2(PPh3)2(2-AMP)]∞ [4], we synthesized a new complex with the formula [Ag(PPh3)2(CH3COO)]2 · H2O · CH3OH in the presence of 2-aminopyridine by the similar reaction as the two similar complexes [Ag(PPh3)2(CH3OH)(ClO4)] and [Ag(PPh3)3(ClO4)] [5]. The title complex consists of two [Ag(PPh3)2(CH3COO)] units, a water molecule and a methanol molecule. Both the two silver atoms are four-coordinated with a AgP2O2 environment, where two phosphorus atoms are from PPh3 with d(Ag—P) ranging from 2.398(2) Å to 2.453(2) Å, two oxygen atoms are from CH3COO with the d(Ag—O) in the range of 2.395(5) Å 2.450(5) Å. The bond angles ∠P–Ag–O are in the range of 102.32(1) 121.2(2)°, the bond angles ∠P–Ag–P are in the range of 128.13° 128.27(6)°, the bond angles ∠O–Ag–O are 52.8(2)° and 53.6(2)°, which comfirm the distorted tetrahedral environment around the silver atom. Two [Ag(PPh3)2(CH3COO)] units are linked via hydrogen bond O6–H6A···O1 (with d(O6···O1) = 2.873 Å and ∠O6–H6A–O1 of 173.27°) and hydrogen bond O6–H6B···O3 (with d(O6···O3) = 2.841 Å and ∠O6–H6–O1 = 171.28°). The compound is further stablized by hydrogen bond O5–H5A···O2 formed between O–H donor of methanol and O atom of acetate anion with d(O5···O2) = 2.795 Å and ∠O5–H5A–O2 = 170.69°. The similar complex AgCH3COO · PPh3 · dmp · MeOH [6] has d(Ag—P) = 2.3792(3) Å, and d(Ag—O) = 2.3993(9) Å and 2.875(1) Å, but the silver atom is five-coordinated. Z. Kristallogr. NCS 225 (2010) 645-648 / DOI 10.1524/ncrs.2010.0282 645 © by Oldenbourg Wissenschaftsverlag, München Crystal: colorless block, size 0.10 × 0.15 × 0.20 mm Wavelength: Mo K+ radiation (0.71073 Å) .: 6.95 cm−1 Diffractometer, scan mode: Bruker SMART CCD, #/% 2,max: 55.78° N(hkl)measured, N(hkl)unique: 52160, 16529 Criterion for Iobs, N(hkl)gt: Iobs > 2 )(Iobs), 8979 N(param)refined: 812 Programs: SHELXS-97, SHELXL-97, SHELXTL [7] Table 1. Data collection and handling.
TL;DR: In this article, the authors describe the structure of the monoclinic compound Mn(CH3COO)3 · 2H2O (0.93 g), which consists of a neutral complex and an acetonitrile solvent molecule.
Abstract: C25H30MnN3O6, monoclinic, P21/n (no. 14), a = 9.8702(6) Å, b = 12.0550(7) Å, c = 22.083(1) Å, * = 102.628(1)°, V = 2564.0 Å, Z = 4, Rgt(F) = 0.050, wRref(F) = 0.140, T = 200 K. Source of material Mn(CH3COO)3 · 2H2O (0.50 g, 1.86 mmol), NaCl (0.11 g, 1.88 mmol) and N,N'-bis(3-ethoxysalicylidene)-1,3-diiminopropane (0.70 g, 1.89 mmol) in EtOH (70 ml) and H2O (5 ml) were stirred for 3 h at room temparature and then filtered. The solvent was evaporated in vacuo, the residue washed with acetone/H2O and dried, to give a dark brown powder (0.93 g). Crystals suitable for X-ray diffraction analysis were obtained by slow evaporation from a CH3CN solution. Experimental details Hydrogen atoms were positioned geometrically and allowed to ride on their respective carrier atoms [d(C—H) = 0.95 Å (CH), 0.99 Å (CH2) or 0.98 Å (CH3) and Uiso(H) = 1.2 Ueq(CH, CH2) or 1.5 Ueq(CH3)]. Discussion The crystal structure of the title compound consists of a neutral complex [Mn(C21H24N2O4)(CH3COO)] and an acetonitrile solvent molecule. Mn(III) ion is six-coordinated by two N and two O atoms from the N,N'-bis(3-ethoxysalicylidene)-1,3-diiminopropane dianionic ligand and two O atoms of the acetate anion in a considerably distorted octahedral environment. In the octahedral structures of metal complexes of salen or salen-like ligands (where salen is dianion of N,N'-bis(salicylidene)ethylenediimine), the equatorial planes were generally defined by the two N and two O atoms of the dianion [1,2]. However, in this complex, the four atoms (N1, N2, O2 and O3) are not coplanar, with the torsion angle ∠N1–N2–O3–O2 = 40.80(8)°. The N2, O2, O5 and O6 atoms lie on the equatorial plane (∠O5–O6–O2–N2 = 0.70(9)°). Within the plane, the ∠O5–Mn1–O6 chelate angle is 58.21(8)°, which results in the distortion of the octahedral structure. The apical bond angle ∠N1–Mn1–O3 is 176.09(9)°. While the Mn—N and Mn—Ophenoxo bond lengths are nearly equivalent, respectively (d(Mn—N) = 1.998(2) Å and 2.160(2) Å; d(Mn—O) = 1.891(2) Å and 1.889(2) Å), the two Mn—Oacetato bond lengths are somewhat different (2.043(2) Å and 2.402(2) Å). The compound displays the intermolecular C–H···O hydrogen bonds with d(C···O) = 3.266(4) Å 3.411(3) Å. Moreover, there are weak intermolecular --interactions between the adjacent benzene rings. For Cg1 (the centroid of 6-membered ring C14-C19) and Cg1 (symmetry code i: –x,1–y,–z), the centroid-centroid distance is 5.254(2) Å and the ring planes are parallel and shifted for 3.902 Å. Z. Kristallogr. NCS 225 (2010) 257-258 / DOI 10.1524/ncrs.2010.0112 257 © by Oldenbourg Wissenschaftsverlag, München Crystal: brown rod, size 0.17 × 0.25 × 0.26 mm Wavelength: Mo K+ radiation (0.71073 Å) .: 5.59 cm−1 Diffractometer, scan mode: Bruker SMART 1000 CCD, #/' 2,max: 56.64° N(hkl)measured, N(hkl)unique: 18767, 6349 Criterion for Iobs, N(hkl)gt: Iobs > 2 )(Iobs), 3746 N(param)refined: 320 Programs: SHELXS-97 [3], SHELXL-97 [4], ORTEP [5], PLATON [6] Table 1. Data collection and handling.
TL;DR: In this article, the authors describe the structure of a monoclinic ZnO4N2 complex, which consists of four aqua ligands in the equatorial positions, and two nicotinamide ligands through the pyridine nitrogen atom.
Abstract: C24H28N4O12S2Zn, monoclinic, P12/c1 (no. 13), a = 14.6271(3) Å, b = 6.8558(1) Å, c = 15.0743(3) Å, * = 111.185(2)°, V = 1409.5 Å, Z = 2, Rgt(F) = 0.044, wRref(F ) = 0.123, T = 298 K. Source of material Nicotinamide (0.048 g, 0.4 mmol) was added with constant stirring to an aqueous solution (20 ml) of Zn(NO3)3 · 6H2O (0.060 g, 0.2 mmol). The solution was then treated with disodium 4,4'biphenyldisulfonate (0.72 g, 0.2 mmol). Colourless crystals of the title complex were collected after 10 d (63 % yield based on Zn). Experimental details The hydrogen atoms bound to carbon and nitrogen atoms were geometrically placed (d(C—H) = 0.93 Å, d(N—H) = 0.86 Å) and refined as riding with Uiso(H) = 1.2 Ueq(C,N). The hydrogen atoms bound to oxygen atoms were located in difference Fourier maps and refined as riding in their as-found relative positions with d(O—H) = 0.85 0.86 Å and Uiso(H) = 1.2 Ueq(O). Discussion The sulfonate group shows interesting functional properties owing to a flexible coordination mode and weak interactions between the metal centres and sulfonate groups [1-6]. Furthermore, the sulfonate group is an excellent candidate for a hydrogen acceptor. The three O atoms of a SO3 group can form up to six hydrogen bonds leading to extended networks [7-12]. In the title crystal structure, the Zn(II) atom occupies an inversion centre, and is coordinated by four aqua ligands in the equatorial positions, and two nicotinamide ligands through the pyridine nitrogen atom in trans positions. The Zn—O distances range from 2.1360(2) to 2.1659(2) Å, which is consistent with those found in comparable structure of trans-Diaquabis(N,N'-dimethylethylenediamine)zinc(II) naphthalene-2,6-disulfonate [13]. Zn—N bond length is 2.080(2) Å. The angles subtended at Zn(II) atom by cis pairs of ligating atoms cover the range 87.99(6)° 92.01(6)°, and the angles subtended by the trans pairs are 180°, indicating that the [ZnO4N2] unit is only slightly deviating from regular octahedral arrangement. The 4,4'-biphenyldisulfonate (BPDS) anion does not participate in the coordination of zinc(II) atom, and has an inversion centre at the midpoint of the central C—C bond. The hexacoordinated zinc(II) complexes ions are connected into a one-dimensional zigzag chain running parallel to [100] via two symmetry related N–H···O hydrogen bonds with d(N···O) = 2.963(2) Å. The chains are arranged in a parallel manner, forming the complex cationic layers. The 4,4'-biphenyldisulfonate anions are located between the layers, which is made possible by the well matched ionic size. The Zn···Zn separation within chains is 14.627 Å. The shortest through space inter-chain distance between Zn···Zn ions is 7.537 Å. These chains are held together via the hydrogen bonds between the remaining N–H proton on the nicotinamide ligands and an oxygen atom of BPDS anions, the coordinated water moleculses and the sulfonate O atoms of the BPDS anions, forming a 3D hydrogen-bonded networks, which is different to [Zn(N,N'-Dmda)2(H2O)2](2,6-NDS) [13]. In the latter compound, the hexa-coordinated complex cations are held together via N–H···O and O–H···O hydrogen bonds, resulting in infinite chains, which are connected by centerosymmetric naphthalene-2,6-disulfonate (2,6-NDS) ligands as linkers, generating a two-dimensional hydrogenbonded network. Z. Kristallogr. NCS 225 (2010) 379-380 / DOI 10.1524/ncrs.2010.0166 379 © by Oldenbourg Wissenschaftsverlag, München Crystal: colorless block, size 0.33 × 0.35 × 0.40 mm Wavelength: Cu K+ radiation (1.54178 Å) .: 32.28 cm−1 Diffractometer, scan mode: Bruker SMART CCD, ' 2,max: 134.86° N(hkl)measured, N(hkl)unique: 6185, 2462 Criterion for Iobs, N(hkl)gt: Iobs > 2 )(Iobs), 2077 N(param)refined: 197 Programs: SHELXS-97, SHELXL-97, SHELXTL [14] Table 1. Data collection and handling.
TL;DR: In this paper, the 2,2'-bipyridine-2,6,-disulfonate (Na22,6-ADS) was obtained as yellow block-shaped crystals, recovered by vacuum filtration and dried in air (78 % yield based on Cd).
Abstract: C34H26CdN4O10S2, triclinic, P1 (no. 2), a = 9.897(3) Å, b = 12.856(6) Å, c = 14.076(4) Å, * = 88.31(3)°, ) = 80.54(2)°, & = 69.54(4)°, V = 1654.4 Å, Z = 2, Rgt(F) = 0.045, wRref(F) = 0.151, T = 298 K. Source of material A mixture of disodium 9,10-dioxoanthracene-2,6,-disulfonate (Na22,6-ADS, 0.1 mmol, 0.042 g), Cd(NO3)2 · 4H2O (0.1 mmol, 0.031 g), 2,2'-bipyridine (2,2'-bipy, 0.1 mmol, 0.016 g) and water 10 mL was stirred for about 30 min, and then sealed in a Teflonlined stainless steel autoclave and heated at 393 K for 3 days. The autoclave was then allowed to cool to amibent temperature. The title compound was obtained as yellow block-shaped crystals, recovered by vacuum filtration and dried in air (78 % yield based on Cd). Experimental details The hydrogen atoms bound to carbon atoms were geometrically placed and refined as riding with d(C—H) = 0.93 Å) and Uiso(H) = 1.2 Ueq(C). The hydrogen atoms of water molecules were located in difference Fourier maps and refined as riding in their as-found relative positions with Uiso(H) = 1.2 Ueq(O). Discussion The sulfonate group, being a structural analogue of phosphonate, can also be utilized as a synthon to build inorganic-organic lamellar structures. Consequently, a wide variety of transition metal sulfonates with interesting structures and desired properties have been prepared, in which the sulfonate group exhibits flexible coordination modes [1-3]. In this contribution, 2,6-ADS will serve as a probe to examine the coordination polymer chemistry of the late transiton metal. In the title crystal structure, the Cd(II) is hexa-coordinated by four pyridine N atoms of two 2,2'-bipyridine molecules, one oxygen atom from the SO3 group of the 2,6-ADS ligand and one oxygen atom of the aqua ligand. The bond lengths Cd—N and Cd—O are in the ranges 2.321(3) 2.349(4) Å and 2.278(3) 2.291(3) Å, respectively, which are in agreement with the values observed previously [4,5]. The angles subtended at Cd by cis pairs of ligands cover the range 70.6(1)° to 105.5(1)° and the angles subtended by the trans pairs are in the range 150.01(1)° to 164.61(2)°, indicating that the CdN4O2 unit is a distorted octahedron. The bond lengths S—O fall within the typical range of bond lengths in a sulfonate ion, and the distance C—S is also as expected for a 2,6ADS ligand. The 2,2'-bipy ligand binds in a chelate fashion to the metal ion. The whole 2,6-ADS adopts an O-monodentate mode, while in the comparable structure of Yb(H2O)(OH)(2,6-ADS) [6], 2,6-ADS adopts -4-mode binding four metal centres. In the 454 Z. Kristallogr. NCS 225 (2010) 454-456 / DOI 10.1524/ncrs.2010.0199 © by Oldenbourg Wissenschaftsverlag, München
TL;DR: In this article, a sample with nominal composition Yb21Au43Sn36 was prepared in a closed, degassed molybdenum crucible for differential thermal analysis (DTA).
Abstract: Au3Sn2Yb2, trigonal, R3m (no. 166), a = 4.7684(2) Å, c = 46.898(3) Å, V = 923.5 Å, Z = 6, Rgt(F) = 0.042, wRref(F ) = 0.101, T = 294 K. Source of material A sample with nominal composition Yb21Au43Sn36 was prepared in a closed, degassed molybdenum crucible for differential thermal analysis (DTA). Stoichiometric amounts of high purity commercial metals (99.9 wt.% for Yb; 99.999 wt.% for both Au and Sn) with a total mass of about 2 g were directly set and slightly pressed together into the crucible, which was sealed by arc welding under a flow of pure argon. The sample was melted by heating up to 1473 K in a high-frequency induction furnace with shaking to ensure homogenization. The crucible, after being subjected to two DTA runs, was then sealed under vacuum in a quartz tube and annealed in a resistance furnace at 973 K for 13 days. No contamination of the alloy due to reactivity towards the Mo container was noticed: the alloy was brittle and stable in air. Experimental details Lattice parameters of the Yb2Au3Sn2 compound were obtained from a Guinier powder pattern using Cu K+ radiation and Si as an internal standard (a = 5.4308 Å). Discussion In the course of an investigation on the R-Au-Sn compounds with R = rare earth, a small number of exploratory samples was prepared in the Yb-Au-Sn system. In one of these samples a phase could be identified by DTA, likely forming by peritectic reaction at 1043 K, while its composition was determined by electron probe microanalysis as Yb28.6(2)Au42.6(2)Sn28.8(2) and confirmed by X-ray crystal structure analysis. In the crystal structure of Yb2Au3Sn2 the atoms are arranged in triangular nets normal to [001]. The compound is a new representative of a structural family with formula Rm+nT2m+nXm+n, where m and n indicate the number of slabs taken from the GdPt2Sn [1,2] and SrPtSb [3] types, respectively. Two other members of this family had been already found in the Yb-Cu-Sn system [4]. In the present case m = 2 and n = 2, namely two segments of the GdPt2Sn type and two cells of the SrPtSb type (ternary ordered AlB2 type) alternate along [001]. In the figure, a bit more than one third of cell is drawn. In the GdPt2Sn slab trigonal antiprisms are formed by the Au1 and Au3 atoms around Sn2, as highlighted in the figure. In the SrPtSb segment the Au2 and Sn1 atoms, located in layers separated by 0.23 Å, form slightly puckered hexagons (planar in the figure) and are surrounded by ytterbium trigonal prisms. The Yb1 atoms are at the boundary between the two kinds of slabs, while Yb2 and Yb3 belong to the SrPtSb and GdPt2Sn segment, respectively. The shortest distances d(Au2—Sn1) = 2.763(1) Å, d(Yb1—Sn1) = 3.228(2) Å and d(Yb1—Yb2) = 3.610(2) Å are found in the SrPtSb segment, while d(Yb3—Au3) = 2.954(1) Å is found between atoms in the GdPt2Sn segment. No Au—Au bonds occur. Z. Kristallogr. NCS 225 (2010) 221-222 / DOI 10.1524/ncrs.2010.0095 221 © by Oldenbourg Wissenschaftsverlag, München Crystal: metallic irregular prism, size 0.04 × 0.08 × 0.12 mm Wavelength: Mo K+ radiation (0.71069 Å) .: 1091.00 cm−1 Diffractometer, scan mode: Bruker-Nonius MACH3, '/, 2,max: 59.58° N(hkl)measured, N(hkl)unique: 1979, 403 Criterion for Iobs, N(hkl)gt: Iobs > 2 )(Iobs), 291 N(param)refined: 24 Programs: SIR97 [5], SHELXL-97 [6], ATOMS [7] Table 1. Data collection and handling.
TL;DR: In this article, a solution of Bi(NO3)3 was dropped slowly into a solution containing 5-bromo-1hydroxy-2(1H)-pyridinethione (5-Br-HPT, 618 mg, 3 mmol) in EtOH (25 mL), which was then cooled to room temperature to give yellow polycrystals, which were collected by filtration, washed successively with H2O and EtOH, and dried in vacuo.
Abstract: C33H25Bi2Br6N7O7S6, P1 (no. 2), a = 13.484(1) Å, b = 13.631(1) Å, c = 15.249(1) Å, + = 94.434(1)°, * = 114.215(2)°, ( = 107.841(2)°, V = 2365.9 Å, Z = 2, Rgt(F) = 0.066, wRref(F) = 0.194, T = 298 K. Source of material A solution of Bi(NO3)3.·.5H2O (475 mg, 1 mmol) in water (15 mL) was dropped slowly into a solution of 5-bromo-1hydroxy-2(1H)-pyridinethione (5-Br-HPT, 618 mg, 3 mmol) in EtOH (25 mL). The mixed solution was stirred for 3 h at 40 °C and was then cooled to room temperature to give yellow polycrystals, which were collected by filtration, washed successively with H2O and EtOH, and dried in vacuo. Yellow square-shaped crystals suitable for X-ray analysis were obtained by recrystallization of the precipitate from N,N-dimethylformamid (m.p. 247 249 °C). Discussion Bismuth compounds have been used to treat a variety of medical disorders for over 200 years [1]. Current interest in bismuth thiolates derives in part from their ability as fungicides, antitumor agents, nanoparticle synthesis and mechanism research of bioactivity [2-5]. Although Bi(III) compounds of the Bi(mpo)3 and Bi(ph)(mpo)2 (Hmpo = 2-mercaptopyridine-N-oxide) have been prepared previously [6,7], X-ray structural data are available only for not-substituted base on the pyridine ring. The crystal structure of the title compound is a dimer with heptacoordination for each bismuth imposed by three sulfur and four oxygen atoms. Except for bridging oxygen atom O2, the coordination polyhedron around Bi1 can be described as a distorted trigonal prism with O1, S1, S4 and O3, O4, S3 at the triangular bases (dihedral angle between their mean planes 29.3(4)°, which is larger than 9.5(2)° in Bi(mpo)3) [7], different from Fe(mpo)3 [8]. In Fe(mpo)3, the arrangement of the ligands gives the complex with meridional octahedral geometry. Because of the short distances (av. 2.939 Å) of the ligands, the coordination of the bismuth atoms is distorted from regular trigonal prism with angles within chelate rings of average 68°. The present complex exhibits Bi—S bond lengths within the range from 2.646 to 2.749 Å with a mean value of 2.685 Å, shorter than in Bi(mpo)3 (2.808 Å), and Bi—O distances within the range from 2.395 to 2.783 Å with a mean value of 2.622 Å, longer than in Bi(mpo)3 (2.480 Å), but close to those in [Bi(mpo)2Ph] [6], in which the Bi—S and Bi—O bond distances are 2.674 and 2.525 Å, respectively. The relatively short C—S distances (av. 1.720 Å) as observed in [Bi(mpo)2Ph] (1.700 Å) and Bi(mpo)3 (1.707 Å) reveals partial double bond character, and nearly 0.1 Å shorter than the distance (1.81 Å) for a single bond [9]. The distances (O···S) of average 2.939 Å are similar to that in Bi(mpo)3 (2.934 Å). The three O–Bi–S angles are nearly equivalent and close to 68.00°, similar [Bi(mpo)3] (70.0°). In the surrounding of Bi1 atom, there are three five-membered ring planes Bi1/O1/N1/C1/S1 (I), Bi1/O3/ N3/C11/S3 (II) and Bi1/O4/N4/C16/S4 (III) with RMS deviation of fitted atoms of 0.276, 0.107 and 0.080 Å, respectively. The dihedral angles between planes I/II, II/III, and I/III are 69.57°, 88.80° and 31.67°, respectively. The Bi–S–C angles of average 102.2° and Bi–O–N angles of average 118.2° show that the bonding orbitals of the sulfur atoms are mainly of sp, and that of oxygen atom are of sp character, similar to H2mp complexes [10]. In the molecular packing N6, O2, O4, O6, O7, S2 and S6 form hydrogen bonds with d(C15–H···N6 ) = 3.31 Å, d(C5–H · · ·O2 ) = 3.35 Å , d(C25–H · · ·O4 ) = 3.02 Å , d(C15–H···O6 ) = 3.18 Å, d(C32–H···O7 i ) = 2.54 Å, d(C7–H···S2) = 3.63 Å, and d(C12–H···S6) = 3.65 Å, respectively, giving rise to a chain along [010] (symmetry code i: 1–x,1–y,1–z; ii: x,y,z; iii: x,1–y, 1–z; iv: x,y–1,z). The distance Bi1···Bi2 is 4.556 Å, being shorter than that in [Bi(mpo)2Ph] (4.89 Å) and longer than that in [Bi(mpo)3] (3.803 Å). Z. Kristallogr. NCS 225 (2010) 277-279 / DOI 10.1524/ncrs.2010.0120 277 © by Oldenbourg Wissenschaftsverlag, München
TL;DR: In this paper, a mixture of 2-bromopyrene (2 mmol), 4-(diphenylamino)phenyl boronic acid (2.2 mmol) and tetrakis(triphenylphosphine)palladium (30 mg) was added to 20 mL tetrahydrofuran.
Abstract: C34H23N, monoclinic, P121/c1 (no. 14), a = 18.236(2) Å, b = 10.724(1) Å, c = 12.255(1) Å, ) = 95.883(1)°, V = 2384.1 Å, Z = 4, Rgt(F) = 0.040, wRref(F) = 0.106, T = 296 K. Source of material The title compound was synthesized by Suzuki coupling reaction. A mixture of 2-bromopyrene (2 mmol), 4-(diphenylamino)phenyl boronic acid (2.2 mmol) and tetrakis(triphenylphosphine)palladium (30 mg) was added to 20 mL tetrahydrofuran. After 5 mL of aqueous potassium carbonate (2 M) was added to the mixture, the reaction mixture was purged with nitrogen for 30 min. After refluxing overnight, the reaction mixture was poured into 100 mL water. The crude product was purified by column chromatography, then recrystallized from ethanol to crystals suitable for X-ray diffraction investigation. The palladium complex was used as catalyst in the synthesis, it was reduced to palladium black after the reaction. Discussion As a large conjugate aromatic ring, pyrene not only has the advantage of high photo-luminescence efficiency, high carrier mobility, but also has the much improved hole-injection ability than oligofluorenes or polyfluorenes [1]. In recent years, some pyrene derivatives have been used in organic light-emitting diodes (OLEDs) [1,2]. Pyrene and its derivatives show a large propensity to aggregate and to form excimers. The high tendency towards ,, stacking of the pyrene moieties generally leads to a substantial red-shift and a decrease of the fluorescence quantum yields [3-7]. The intermolecular interactions can be limited by introducing bulky substituents in pyrene backbone [8]. The crystal structure of the title compound revealed that pyrene ring and benzene rings are not coplanar (dihedral angles are 131.5°, 73.6° and 78.8°, respectively). All the bond lengths and angles are within normal ranges. In the crystal there exist CH-, interactions, which form the one-dimensional chains in the crystal structure. Z. Kristallogr. NCS 225 (2010) 573-574 / DOI 10.1524/ncrs.2010.0251 573 © by Oldenbourg Wissenschaftsverlag, München Crystal: colorless block, size 0.18 × 0.37 × 0.45 mm Wavelength: Mo K* radiation (0.71073 Å) -: 0.71 cm−1 Diffractometer, scan mode: Bruker SMART CCD, #/% 2+max: 51° N(hkl)measured, N(hkl)unique: 14297, 4407 Criterion for Iobs, N(hkl)gt: Iobs > 2 ((Iobs), 2879 N(param)refined: 316 Programs: SHELXS-97, SHELXL-97, SHELXTL [9] Table 1. Data collection and handling. H(2) 4e 0.7185 0.3878 0.1027 0.060 H(3) 4e 0.5996 0.3694 0.1441 0.057 H(5) 4e 0.5997 0.7270 0.2346 0.056 H(6) 4e 0.7197 0.7460 0.1960 0.060 H(8) 4e 0.7549 0.7197 −0.0409 0.080 H(9) 4e 0.8031 0.8978 −0.1098 0.093 H(10) 4e 0.9108 0.9810 −0.0265 0.095 H(11) 4e 0.9687 0.8887 0.1273 0.100 H(12) 4e 0.9213 0.7095 0.1969 0.086 H(14) 4e 0.9006 0.5079 −0.0102 0.096 H(15) 4e 0.9759 0.3350 −0.0021 0.119 H(16) 4e 0.9752 0.1952 0.1398 0.119 H(17) 4e 0.8995 0.2292 0.2766 0.105 H(18) 4e 0.8251 0.4046 0.2713 0.083 H(20) 4e 0.4791 0.4390 0.0740 0.057 H(21) 4e 0.3555 0.4228 0.0862 0.058 H(23) 4e 0.2451 0.4683 0.1842 0.065 H(24) 4e 0.1961 0.5458 0.3322 0.070 H(26) 4e 0.2129 0.6503 0.5155 0.077 H(27) 4e 0.2884 0.7340 0.6578 0.080 H(28) 4e 0.4137 0.7410 0.6511 0.072 H(30) 4e 0.5241 0.6998 0.5513 0.059 H(31) 4e 0.5737 0.6315 0.4014 0.056 Table 2. Atomic coordinates and displacement parameters (in Å). Atom Site x y z Uiso
TL;DR: In this paper, a 3,6-bis(imidazol-1-yl)pyridazine (21 mg, 0.10 mmol) was synthesized according to the published procedure, and the solution was then filtered into a test tube and left standing at room temperature.
Abstract: C10H8N6, monoclinic, P121/c1 (no. 14), a = 3.7908(5) Å, b = 15.359(1) Å, c = 16.242(2) Å, ) = 96.642(1)°, V = 939.3 Å, Z = 4, Rgt(F) = 0.042, wRref(F) = 0.113, T = 298 K. Source of material The title compound was synthesized according to the published procedure [1]. 3,6-bis(imidazol-1-yl)pyridazine (21 mg, 0.10 mmol) was then dissolved in 8 mL of 85 % formic acid, The solution was then filtered into a test tube and left standing at room temperature. After about one month colorless needle-like crystals were obtained. X-ray diffraction analysis indicated that the title compound crystallizes without solvent molecules. Experimental details Hydrogen atoms attached to the C atoms were placed in calculated positions with d(C—H) = 0.93 Å. All Uiso values were restrained on Ueq values of the parent atoms. Discussion Imidazole (Im), and their derivatives are ubiquitous in biological and biochemical structure and function [2,3]. Im derivatives have also found wide applications in drug design in the forms of antitumor and anticancer agents [4,5]. In addition to the above mentioned fields, imidazole derivatives can also be used in building coordination polymeric frameworks [6,7]. In the title crystal structure all of the bond distances and angles are in the normal range. The two imidazole rings are situated at trans configuration (figure, top). The imidazole rings and the pyridazine ring are planar with the largest deviation from the least square plane of 0.0061 Å. The dihedral angle between the imidazole ring and the pyridazine rings are 7.4° and 1.5°, respectively, the dihedral angle between the two imidazole rings in the same molecule is 6.4°, which is different to the published results [8]. Each two molecules are connected through two C–H···N hydrogen bonds to form a dimer. The adjacent dimers are connected by two 3,6-bis(imidazol-1-yl)pyridazines along [001] through eight C–H···N hydrogen bonds (figure, bottom). Every terminal N atom of the imidazole group form two C–H···N hydrogen bonds with the dimers in bifurcate mode with the C—N distances of 3.460 Å and 3.482 Å, respectively. Caused by such weak interactions, the compound displayed corrugated layer structure. These layers were further stacked along [100] through C–H···N hydrogen bonds and ,-, interactions (with centroid-centroid distance of 3.374 Å) to form 3D network structure. Z. Kristallogr. NCS 225 (2010) 467-468 / DOI 10.1524/ncrs.2010.0205 467 © by Oldenbourg Wissenschaftsverlag, München Crystal: colorless block, size 0.30 × 0.42 × 0.49 mm Wavelength: Mo K* radiation (0.71073 Å) -: 1.01 cm−1 Diffractometer, scan mode: Bruker SMART CCD, #/% 2+max: 50.04° N(hkl)measured, N(hkl)unique: 4638, 1665 Criterion for Iobs, N(hkl)gt: Iobs > 2 ((Iobs), 1103 N(param)refined: 145 Programs: SHELXS-97, SHELXL-97, SHELXTL [9] Table 1. Data collection and handling.
TL;DR: In this paper, the isonicotinamide (INA) ligand has been employed to construct metal-containing hydrogen-bonded networks owing to the inherent coordination and hydrogen bonding donor/acceptor functionalities, which is exemplified by a few analogous compounds based on transition metal ions Cu(II), Co-II), Ni(II, Ag(I) and INA ligand observed in the literatures.
Abstract: C34H46N8O18S2Zn, triclinic, P1 (no. 2), a = 10.366(6) Å, b = 10.920(6) Å, c = 10.941(5) Å, * = 70.83(5)°, ) = 74.81(5)°, & = 78.29(5)°, V = 1119.6 Å, Z = 1, Rgt(F) = 0.042, wRref(F) = 0.120, T = 298 K. Source of material Isonicotinamide (INA, 0.048 g, 0.4 mmol) was added with constant stirring to an aqueous solution of Zn(NO3)3 · 6H2O (0.060 g, 20 ml, 0.2 mmol). The solution was then treated with disodium naphthalene-1,5-disulfonate (0.66 g, 0.2 mmol). Colourless crystals of the title complex were collected after 10 d (61 % yield based on Zn). Experimental details The O-bound H atoms were located in difference Fourier maps and refined as riding in their as-found relative positions with Uiso(H) = 1.2 Ueq(O). The other hydrogen atoms were geometrically placed and refined as riding with d(C—H) = 0.93 Å, d(N—H) = 0.86 Å, Uiso(H) = 1.2 Ueq(C,N). Discussion The isonicotinamide (INA) ligand has been employed to construct metal-containing hydrogen-bonded networks owing to the inherent coordination and hydrogen-bonding donor/acceptor functionalities, which is exemplified by a few analogous compounds based on transition metal ions Cu(II), Co(II), Ni(II), Ag(I) and INA ligand observed in the literatures [1-3]. On the other hand, the sulfonate group is also a flexible hydrogen bond acceptor, and has been employed successfully by Ward and coworkers in their guanidinium sulfonate inclusion family [4,5]. In the title crystal structure, the Zn atom is located on a inversion center and surrounded by four oxygen donors from four water ligands in the basal plane and two pyridyl nitrogen atoms from a pair of isonicotinamide ligands in trans arrangement at the apical sites. The Zn—O bond lengths range from 2.103(2) to 2.120(2) Å, and the Zn—N distance is 2.1403(2) Å, which is close to those for reported complexes [6]. The angles subtended at Zn by cis pairs of ligating atoms cover the range 87.45° to 92.55°, indicating that the Zn[N2O4] unit is a slightly distorted octahedron. The amide substituents are twisted away from the pyridine ring plane with the torsion angle of 5.30°. The naphthalene-1,5-disulfonate (1,5-NDS) anion does not participate in the coordination of the Zn(II) centre, and has an inversion centre at the midpoint of the central C—C bond. The most interesting structural feature of the title compound is the intermolecular self-complementary hydrogen bonding pattern. The complex cations are bridged by 1,5NDS anions through intermolecular N–H···O hydogen bonds formed by the amide groups and the sulfonate O atoms, resulting in infinite chains. Adjacent chains are further linked by hydrogen bonds formed between the coordinated water molecules and the sulfonate O atoms, to form an extended grid structure containing two kinds of cavities. Two INA solvent molecules and two lattice water molecules are anchored to the cavity, and interact with host frameworks via N–H···O and O–H···N hydrogen bonds. Z. Kristallogr. NCS 225 (2010) 461-462 / DOI 10.1524/ncrs.2010.0202 461 © by Oldenbourg Wissenschaftsverlag, München Crystal: colorless block, size 0.30 × 0.33 × 0.38 mm Wavelength: Cu K* radiation (1.54178 Å) -: 23.38 cm−1 Diffractometer, scan mode: Oxford CrysAlis CCD, \" geometry 2+max: 135° N(hkl)measured, N(hkl)unique: 8855, 3956 Criterion for Iobs, N(hkl)gt: Iobs > 2 ((Iobs), 3590 N(param)refined: 287 Programs: SHELXS-97, SHELXL-97, SHELXTL [7] Table 1. Data collection and handling.
TL;DR: In this paper, the stock solutions were prepared by dissolving 0.5 mmol (Z)-1(2,4-dinitrophenyl)-2-(3-methylcyclohex-2-enylidene)hydrazine in 100 ml dry CH2Cl2.
Abstract: C13H13N5O6, monoclinic, P121/c1 (no. 14), a = 14.501(2) Å, b = 6.362(1) Å, c = 17.166(2) Å, * = 110.913(9)°, V = 1479.3 Å, Z = 4, Rgt(F) = 0.034, wRref(F) = 0.093, T = 293 K. Source of material The stock solutions was prepared by dissolving 0.5 mmol (Z)-1(2,4-dinitrophenyl)-2-(3-methylcyclohex-2-enylidene)hydrazine in 100 ml dry CH2Cl2. NO was produced by the reaction of 1 mol H2SO4 solution with saturated NaNO2 aqueous solution. The former was added to the latter, which was stirred under argon atmosphere. NO was carried by argon and purified by passing it through a series of scrubbing bottles containing 4 M KOH, distilled water, and CaCl2 in turn. The bottles were under an argon atmosphere. The purified NO was bubbled through a degassed stirred stock solution at room temperature for an appropriate time. After completing of the reaction, as indicated by TLC, the reaction mixture was dried with unhydrous MgSO4, concentrated in vacuum, then recrystallized from hexane/ethyl acetate. Experimental details Hydrogen atoms were positioned geometrically, with d(C—H) = 0.93 (aromatic) and 0.96 Å (methyl), and constrained to ride on their parent atoms with Uiso(H) = x Ueq(C), where x = 1.2 (aromatic) and x = 1.5 (methyl), respectively. Discussion In recent years, nitric oxide (NO) has attracted again much attention bacause of its novel physiological function and chemical reactivity. The research concerning the reactivity of NO with some bioactive compounds has increased rapidly, e.g., its reactions with PAH [1], chiral epoxide [2], chalcone [3], coumarin [4], flavanone [5], contributed to understanding more deep the reactive characteristics of NO. Hydrazone group are the important unit in many pharmaceutical and pesticide compounds. Some of compounds containing hydrazone unit were found to have antibacterial, antitumor and other activities [6]. In addition hydrazones have been used to build chiral centers and special skeletons in organic synthesis [7]. The crystal structure of the title compoud is built up by only the C13H13N5O6 molecules. All bond lengths and bond angles are in normal ranges. The six-membered phenyl ring A (C7/C8/C9/ C10/C11/C12) is nearly planar, while another six-membered ring B (C1/C2/C3/ C4/C5/C6) is envelope-shaped and the distance of C2 to the plane (C1/C3/C4/C5/C6) is 0.54 Å. The double bond N1=N2 connects the two rings together, which make them nearly planar with the dihedral angle of 21.7(2)°. The bond lengths of N1—C6 and N3—C5 are 1.29(2) Å and 1.48(2) Å, respectively, is due to the electronegative effects in the O1/N3/O2 nitryl group. The bond lengths of C7—N2, C10—N5 and C12—N4 are 1.353(2) Å, 1.460(2) Å and 1.447(2) Å, which are similar to that of the conventional single C—N bond length (1.450 Å). The C7—N2 bond is much shorter than those of the C10—N5 and C12—N4 bonds, indicating that the C7—N2 is more conjugated with the ring B than the other two bonds. There are some intermolecular hydrogen bonds C1–H1···O exit in the compound. These hydrogen bonds play very important roles in the formation, stability and crystallization of the title compound. Z. Kristallogr. NCS 225 (2010) 359-360 / DOI 10.1524/ncrs.2010.0157 359 © by Oldenbourg Wissenschaftsverlag, München Crystal: colorless block, size 0.32 × 0.32 × 0.58 mm Wavelength: Mo K+ radiation (0.71073 Å) .: 1.22 cm−1 Diffractometer, scan mode: Siemens P4, ' 2,max: 50.5° N(hkl)measured, N(hkl)unique: 3177, 2681 Criterion for Iobs, N(hkl)gt: Iobs > 2 )(Iobs), 1893 N(param)refined: 219 Programs: SHELXS-97, SHELXL-97, SHELXTL [8] Table 1. Data collection and handling.
TL;DR: In this article, the authors used the difference Fourier map (DFM) to find the hydrogen atoms bound to carbon atoms and refined them freely, and then added water to precipitate a colorless product that was purified by recrystallization from ethanol (yield 62 %, m.p.
Abstract: C11H15NO4S, monoclinic, P121/c1 (no. 14), a = 8.1325(6) Å, b = 13.770(1) Å, c = 11.4871(9) Å, * = 100.629(2)°, V = 1264.3 Å, Z = 4, Rgt(F) = 0.035, wRref(F) = 0.118, T = 293 K. Source of material Ethyl acetoacetate (1.30 g, 10 mmol), ethyl cyanoacetate (1.13 g, 10 mmol), diethylamine (5 mL) and sulfur (0.32 g, 10 mmol ) in absolute ethanol (20 ml) were refluxed for 5 h. Water (200 mL) was added to precipitate a colorless product that was purified by recrystallization from ethanol (yield 62 %, m.p. 366 368 K). Experimental details The hydrogen atoms bound to N were found in the difference Fourier map and refined freely. All the H atoms bound to carbon atoms were positioned geometrically (d(C—H) = 0.96 0.97 Å) and refined as riding with Uiso(H) = 1.2 or 1.5 Ueq(C). Discussion 2-Aminothiophene derivatives are important intermediates in the synthesis of a variety of agrochemicals, dyes and pharmacologically active compounds [1]. The most convergent and well established classical approach for the preparation of 2-aminothiophenes is Gewald’s method [2,3], which involves the multicomponent condensation of a ketone with an activated nitrile and elemental sulfur in the presence of diethylamine as a catalyst. The crystal structure of 5-acetyl has been reported [4]. Each molecule of the title compound consists of a five-membered thiophene ring and amino group, methyl and dicarboxylate groups (figure, top). The thiophene ring is almost planar. The sulphur contacts were clearly indentified as S—C5 and S—C6 with distance of 1.726(2) Å and 1.749(1) Å, respectively. The molecular conformation of the title compound is additionally stabilized by an intramolecular N–H···O with d(N–H···O2) = 2.054 Å, and ∠N–H···O2 = 156° (figure, top). The packing is consolidated by further N–H···O links (figure, bottom). Z. Kristallogr. NCS 225 (2010) 283-284 / DOI 10.1524/ncrs.2010.0122 283 © by Oldenbourg Wissenschaftsverlag, München Crystal: colorless block, size 0.23 × 0.44 × 0.58 mm Wavelength: Mo K+ radiation (0.71073 Å) .: 2.59 cm−1 Diffractometer, scan mode: multiwire proportional, #/' 2,max: 54.94° N(hkl)measured, N(hkl)unique: 12054, 2867 Criterion for Iobs, N(hkl)gt: Iobs > 2 )(Iobs), 2325 N(param)refined: 163 Programs: SHELXS-97 [5], SHELXL-97 [6], SHELXTL [7] Table 1. Data collection and handling. H(1A) 4e 1.0246 0.9694 1.8206 0.124 H(1B) 4e 0.8444 0.9828 1.7456 0.124 H(1C) 4e 1.0001 0.9823 1.6829 0.124 H(2A) 4e 1.0462 0.8190 1.7316 0.063 H(2B) 4e 0.8900 0.8194 1.7947 0.063 H(8A) 4e 0.5635 0.9319 1.3367 0.089 H(8B) 4e 0.7439 0.9164 1.4106 0.089 H(8C) 4e 0.5899 0.9215 1.4748 0.089 H(10A) 4e 0.2846 0.7918 0.9620 0.060 H(10B) 4e 0.1290 0.7940 1.0259 0.060 H(11A) 4e 0.0849 0.6795 0.8729 0.093 H(11B) 4e 0.0931 0.6271 0.9950 0.093 H(11C) 4e 0.2482 0.6247 0.9317 0.093 H(0A) 4e 0.673(2) 0.486(2) 1.463(2) 0.067(6) H(0B) 4e 0.759(3) 0.553(1) 1.558(2) 0.068(6) Table 2. Atomic coordinates and displacement parameters (in Å). Atom Site x y z Uiso
TL;DR: In this paper, a triclinic triconyclic compound (C24H18Br6N4Pt) was obtained by slow evaporation from a CH3CN solution.
Abstract: C24H18Br6N4Pt, triclinic, P1 (no. 2), a = 7.604(1) A, b = 8.100(1) A, c = 11.110(2) A, + = 84.351(3)°, ) = 81.358(3)°, & = 88.421(3)°, V = 673.1 A, Z = 1, Rgt(F) = 0.054, wRref(F) = 0.171, T = 223 K. Source of material A suspension of K2PtCl6 (0.261 g, 0.537 mmol), 1,10-phenanthroline (0.100.g, 0.555.mmol) and NaBr (0.884.g, 8.591.mmol) in H2O (10 ml) was refluxed for 4 h at 100 °C. After cooling, the formed precipitate was separated by filtration, washedwithwater and dried under vacuum, to give an orange powder (0.277 g). Crystals suitable for X-ray structure analysis were obtained by slow evaporation from a CH3CN solution. Experimental details H atoms were positioned geometrically and allowed to ride on their respective parent atoms [d(C—H) = 0.94 A, d(N—H) = 0.87.A and Uiso(H) = 1.2Ueq(C,N)]. Some large residue electron densities were found close to Pt and Br atoms. Owing to the poor quality of the crystal the H atoms on C and N atoms could not be located from Fourier difference maps. However, one of the N atoms of the 1,10-phenanthroline molecule had to be protonated for charge balancing. For the refinement of the structure H atoms were added geometrically on bothN atomswith an occupancy ratio of 0.5/0.5, because it was not distinct which N atom was protonated. The large R-values are connected with the poor quality of the crystal. Discussion The title compound with a crystallization water molecule, (C12H9N2)2[PtBr6].·.H2O, was previously prepared by the reaction of H2[PtBr6].·.6H2O with 1,10-phenanthroline and HBr, and its thermal decomposition was studied by means of derivatography and differential scanning calorimetry [1]. The crystal structure of the title compound consists of twomonoprotonated 1,10-phenanthroline cations and an anionic Pt(IV) complex. The asymmetric unit contains one half of the formula unit; a center of inversion is located at the Pt atom in the special position (1⁄2,0,1⁄2). In the complex, the Pt(IV) ion is sixcoordinated in an almost perfect octahedral environment by six Br atoms: the Pt—Br bond lengths are nearly equivalent with the range of 2.467(2) 2.477(2) A, and the cis ∠Br−Pt−Br bond angles lie in the range of 88.22(5) 91.78(5)°. These values are similar to those found in the complexes K2[PtBr6] [2], [Rh(NH3)5Cl][PtBr6] [3] and (C21H19N2)2[PtBr6] [4]. The compound displays numerous intermolecular --interactions between six-membered rings of the phenanthrolinium cation. The distance between Cg1 (the centroid of six-membered ring N2C11) and Cg1 (symmetry code i: 1−x,1−y,−z) is 3.53(1) A, and the dihedral angle between the ring planes is 0°. Moreover, there are interand intramolecular N−H···Br and N−H···N hydrogen bonds with d(N···Br) = 3.39(1) A and d(N···N) = 2.72(2) A. Z. Kristallogr. NCS 225 (2010) 37-38 / DOI 10.1524/ncrs.2010.0014 37 © by Oldenbourg Wissenschaftsverlag, Munchen Crystal: orange block, size 0.05 × 0.07 × 0.20 mm Wavelength: Mo K+ radiation (0.71073 A) .: 141.38 cm−1 Diffractometer, scan mode: Bruker SMART 1000 CCD, #/% 2,max: 56.6° N(hkl)measured, N(hkl)unique: 4959, 3232 Criterion for Iobs, N(hkl)gt: Iobs > 2 ((Iobs), 2478 N(param)refined: 160 Programs: SHELXS-97 [5], SHELXL-97 [6], ORTEP-III [7], PLATON [8] Table 1. Data collection and handling. H(1A) 2i 0.50 0.1757 0.1994 0.2352 0.038 H(2A) 2i 0.50 0.3002 0.1676 0.0861 0.048 H(1) 2i −0.0024 0.2032 0.4154 0.038 H(2) 2i −0.1608 0.4472 0.4565 0.043 H(3) 2i −0.1040 0.6811 0.3265 0.044 H(5) 2i 0.0404 0.8226 0.1204 0.048 H(6) 2i 0.2152 0.7936 −0.0638 0.044 H(8) 2i 0.3985 0.6084 −0.2127 0.051 H(9) 2i 0.5004 0.3410 −0.2505 0.059 H(10) 2i 0.4528 0.1315 −0.0943 0.054 Table 2. Atomic coordinates and displacement parameters (in A). Atom Site Occ. x y z Uiso
TL;DR: In this article, a mixture of Cu(OAc)2 · H2O (40 mg, 0.2 mmol) was stirred in dimethylformamide (20 mL) at room temperature in air for about one day.
Abstract: C13H14CuIn3S2, triclinic, P1 (no. 2), a = 8.8080(1) Å, b = 10.1039(5) Å, c = 11.2436(2) Å, + = 66.70(2)°, * = 76.20(2)°, ( = 66.36(2)°, V = 838.0 Å, Z = 2, Rgt(F) = 0.038, wRref(F) = 0.108, T = 293 K. Source of material A mixture of Cu(OAc)2 · H2O (40 mg, 0.2 mmol), NaS2CNMe2 · 2H2O (45 mg, 0.2 mmol), 2,2'-bipyridine (31 mg, 0.2.mmol) and NaI.·.2H2O (37 mg, 0.2 mmol) was stirred in dimethylformamide (20 mL) at room temperature in air for about one day. The vapor of i-PrOH was diffused slowly into the resulting solution, and after about one month gray block-shaped crystals (32.mg) were obtained. Experimental details The H atoms were positioned geometrically and refined as riding atoms with d(C—H) = 0.93 (aromatic) or 0.96 Å (methyl) and Uiso(H) = 1.2 Ueq(Caromatic) or 1.5 Ueq(Cmethyl). Discussion Organonitrogen ligands, such as 2,2'-bipyridine (bipy), 1,10phenanthroline, 4,4'-bipyridine and their derivatives as suitable spacers have been extensively used in the construction of coordination complexes [1-3]. They not only are versatile ligands for coordination bonding but also can form aromatic --stacking interactions, C–H···interactions and hydrogen bonding which are important supramolecular force enhancing the stability of the complexes in both solution and solid states [4,5]. In the title crystal structure, the Cu(II) atom is five-coordinated in a distorted square pyramidal manner by one I atom in the apical position with d(Cu—I) = 2.9485(9) Å, two S atoms from a S2CNMe2 ligand [d(Cu—S1) = 2.296(1) Å and d(Cu—S2) = 2.323(1) Å] and two N atoms from a bipy ligand in the basal plane [d(Cu—N2) = 2.004(4) Å and d(Cu—N3) = 2.015(4) Å]. Two adjacent s t ructural uni ts are l inked to a dimer [CuI(bipy)(S2CNMe2)]2 by face-to-face --interactions between bipy ring R1 (N2/C4-C8) to adjacent symmetry-related ring R2 (N3/C9-C13) with dihedral angle of 3.68°, centroid-tocentroid distance of 4.470(4) Å, and plane-to-plane distance of 3.372 Å [6]. The dimers are further connected through C2–H2C···(R2) interactions (∠C–H···R = 125.00° and d(C···R) = 3.559(7) Å) and C2–H2B···I hydrogen bonds (∠C–H···I = 164.00° and d(C···I) = 3.963(6) Å) to form 2D structure in the (001) plane [6]. Z. Kristallogr. NCS 225 (2010) 347-348 / DOI 10.1524/ncrs.2010.0151 347 © by Oldenbourg Wissenschaftsverlag, München Crystal: gray block, size 0.20 × 0.20 × 0.20 mm Wavelength: Mo K+ radiation (0.71073 Å) .: 33.87 cm−1 Diffractometer, scan mode: Rigaku Mercury CCD, ' 2,max: 55° N(hkl)measured, N(hkl)unique: 6208, 3630 Criterion for Iobs, N(hkl)gt: Iobs > 2 )(Iobs), 2629 N(param)refined: 181 Programs: PLATON [6], SHELXS-97, SHELXL-97, SHELXTL [7] Table 1. Data collection and handling. H(2A) 2i 0.0220 0.0026 0.3699 0.098 H(2B) 2i 0.0638 −0.1127 0.2961 0.098 H(2C) 2i −0.0750 0.0490 0.2513 0.098 H(3A) 2i 0.2669 0.0973 0.0173 0.117 H(3B) 2i 0.0815 0.1104 0.0254 0.117 H(3C) 2i 0.2202 −0.0515 0.0696 0.117 H(4A) 2i 0.2266 0.2015 0.5966 0.086 H(5A) 2i 0.2799 0.2047 0.7853 0.095 H(6A) 2i 0.5078 0.2650 0.7841 0.094 H(7A) 2i 0.6743 0.3250 0.5909 0.079 H(10A) 2i 0.8203 0.3801 0.3994 0.084 H(11A) 2i 0.9495 0.4448 0.1900 0.089 H(12A) 2i 0.8502 0.4302 0.0251 0.088 H(13A) 2i 0.6290 0.3466 0.0720 0.074 Table 2. Atomic coordinates and displacement parameters (in Å). Atom Site x y z Uiso
TL;DR: In this paper, the asymmetric unit of the title crystal structure consists of two 2aminopyridinium cations, one 2,2'-dithiobis(benzoate) anion and two discrete water molecules.
Abstract: C24H26N4O6S2, monoclinic, C12/c1 (no. 15), a = 13.429(1) Å, b = 9.7934(9) Å, c = 20.331(2) Å, * = 105.808(2)°, V = 2572.7 Å, Z = 4, Rgt(F) = 0.039, wRref(F ) = 0.098, T = 296 K. Source of material All reagents were commercially available and of analytical grade. The 5 ml ethanol soloution of 2-aminopyridine (1.0 mmol, 0.094 g) was slowly added to an aqueous solution (25 ml) of 2,2'dithiodibenzoic acid (1.0 mmol, 0.301 g). The mixture was stirred for 10 minutes at 100 °C. The solution was filtered, and the filtrate was kept at the room temperature. After 6 d, crystals suitable for single crystal X-ray diffraction were obtained. Experimental details Hydrogen atoms bonded to N and O were located in difference Fourier maps and refined isotropically with distance restraints d(N—H) = 0.89(2), d(O—H) = 0.82(2) and d(H—H) = 1.34(2) Å, respectively. All the remaining H atoms were positioned geometrically and treated as riding with d(C—H) = 0.93 Å and Uiso(H) = 1.2 Ueq(C). Discussion Rational design and assembly of novel supramolecular aducts through hydrogen bonding interaction are still an important research area due to their striking structures [1,2]. This work continues our previously investigations of supra-molecular interactions between aromatic molecular salts and adducts [3]. The asymmetric unit of the title crystal structure consists of two 2aminopyridinium cations, one 2,2'-dithiobis(benzoate) anion and two discrete water molecules. 2,2'-Dithiobis(benzoate) anion has an inversion centre at the midpoint of the S1—S1 (–x,y,–z+1⁄2) bond. Two benzene rings of 2,2'-dithiobis(benzoate) anion are nearly perpendicular to each other with the dihedral angles of 103.4° and C6–S1–S1A angle of 105°. 3-Aminopyridinium cation and 2,2'-dithiobis(benzoate) anion are linked together through a pair of N–H···O hydrogen bonds forming a R2(6) motif, in which 3-aminopyridinium cation uses another N–H donor contacting to one water molecule via N–H···O hydrogen bonds. In addition, each R2(6) motif interacts with neighbor two water molecule through O···H–O hydrogen bonds. In contrast, each water molecule links adjacent three R2(6) motifs leading to an infinite three-dimensional hydrogen-bonded framework. Z. Kristallogr. NCS 225 (2010) 367-368 / DOI 10.1524/ncrs.2010.0161 367 © by Oldenbourg Wissenschaftsverlag, München Crystal: colorless block, size 0.13 × 0.18 × 0.20 mm Wavelength: Mo K+ radiation (0.71073 Å) .: 2.53 cm−1 Diffractometer, scan mode: Bruker SMART Apex CCD, ' 2,max: 52° N(hkl)measured, N(hkl)unique: 6999, 2520 Criterion for Iobs, N(hkl)gt: Iobs > 2 )(Iobs), 1851 N(param)refined: 183 Programs: SHELXS-97, SHELXL-97, SHELXTL [4] Table 1. Data collection and handling.
TL;DR: In this article, the authors describe the structure of the 2-Biphenylboronic acid (2-BBA) using a single crystal X-ray diffraction.
Abstract: C12H11BO2, triclinic, P1 (no. 2), a = 8.313(2) Å, b = 9.420(2) Å, c = 14.687(3) Å, + = 99.255(2)°, * = 104.533(2)°, ( = 100.311(2)°, V = 1069.5 Å, Z = 4, Rgt(F) = 0.043, wRref(F) = 0.113, T = 296 K. Source of material 2-Biphenylboronic acid was purchased from Aldrich, and recrystallized from water/ethanol solution at room temperature to give the desired crystals suitable for single crystal X-ray diffraction investigation. Discussion Arylboronic acids ArB(OH)2 are important starting materials in organic synthesis [1]. They are predominantly applied for the Suzuki cross-coupling reaction [2]. Recently arylboronic acids have also been employed as promising building blocks in crystal engineering and various types of novel supramoolecular assemblies have been generated [3,4]. Analogous to carboxylic acids, they are capable of forming dimeric units, this is the most basic and frequent structural motif found in the solid state [5]. The title crystal structure has two crystallographically independent molecules in the asymmetric unit. The benzene rings are not coplanar, with dihedral angles between the two benzene rings of 132.7° and 129.1° in the two molecules. The B(OH)2 group is twisted by 125.5° and 127.2° from the palne of the benzene ring in the two independent molecules. In the crystal structure of the title compound, the B(OH)2 moiety adopted the most preferred synanti conformation [6,7], there exist O–H···O hydrogen bonds between the adjacent molecules, which enforce the chain structure of the title compound. Z. Kristallogr. NCS 225 (2010) 295-296 / DOI 10.1524/ncrs.2010.0127 295 © by Oldenbourg Wissenschaftsverlag, München Crystal: colorless block, size 0.16 × 0.18 × 0.38 mm Wavelength: Mo K+ radiation (0.71073 Å) .: 0.81 cm−1 Diffractometer, scan mode: Bruker SMART APEXII CCD, #/' 2,max: 51° N(hkl)measured, N(hkl)unique: 8212, 3954 Criterion for Iobs, N(hkl)gt: Iobs > 2 )(Iobs), 2575 N(param)refined: 275 Programs: SHELXS-97 [8], SHELXL-97 [9], SHELXTL [10] Table 1. Data collection and handling. H(1) 2i 0.1217 0.7310 0.1263 0.074 H(2) 2i 0.1181 0.4250 0.0125 0.082 H(3) 2i 0.0060 −0.0772 0.0632 0.076 H(4) 2i 0.2198 0.2348 0.0831 0.072 H(2A) 2i 0.6379 0.8616 0.3866 0.093 H(3A) 2i 0.8507 0.8839 0.3135 0.113 H(4A) 2i 0.7983 0.7693 0.1549 0.104 H(5) 2i 0.5272 0.6364 0.0683 0.079 H(8) 2i 0.3585 0.9321 0.3905 0.090 H(9) 2i 0.1612 0.8978 0.4751 0.114 H(10) 2i −0.0006 0.6664 0.4601 0.110 H(11) 2i 0.0338 0.4661 0.3608 0.087 H(12) 2i 0.2299 0.4979 0.2758 0.068 H(14) 2i 0.6138 0.3550 0.4016 0.074 H(15) 2i 0.4478 0.3490 0.5041 0.086 H(16) 2i 0.1660 0.2236 0.4489 0.083 H(17) 2i 0.0500 0.1054 0.2896 0.069 H(20) 2i 0.6462 0.4534 0.2499 0.077 H(21) 2i 0.8250 0.4523 0.1535 0.098 H(22) 2i 0.8385 0.2339 0.0636 0.097 H(23) 2i 0.6707 0.0146 0.0690 0.085 H(24) 2i 0.4899 0.0138 0.1650 0.068 Table 2. Atomic coordinates and displacement parameters (in Å). Atom Site x y z Uiso