Latest documents http://publikationen.ub.uni-frankfurt.de/index/index/ Wed, 11 Jan 2012 14:54:22 +0100 Wed, 11 Jan 2012 14:54:22 +0100 http://publikationen.ub.uni-frankfurt.de/frontdoor/index/index/docId/27424 The crystal structure of the title compound, Na[(C6F5)BH3], is composed of discrete anions and cations. The sodium cations are surrounded by four anions with three short Na...B [2.848 (8), 2.842 (7) and 2.868 (8) Å] and two short Na...F contacts [2.348 (5) and 2.392 (5) Å], forming a three-dimensional network. The anion is the first structural example of a pentafluorophenyl ring carrying a BH3 group. Hannes Vitze; Hans-Wolfram Lerner; Michael Bolte article http://publikationen.ub.uni-frankfurt.de/frontdoor/index/index/docId/27424 Thu, 01 Nov 2012 14:54:22 +0100 http://publikationen.ub.uni-frankfurt.de/frontdoor/index/index/docId/25860 The crystal structure of the title compound, [Fe(C5H5)(CH3CN)(CO)2]BF4, of which only the coordinates of the non-H atoms of the cation have previously been reported [Fadel et al. (1979 [triangle]). Z. Anorg. Allg. Chem. 453, 98–106] has been redetermined. The FeII atom in the complex cation is coordinated by a cyclo­penta­dienyl ring, two carbonyl ligands and an acetonitrile mol­ecule displaying a three-legged piano stool structure. Three of the four F atoms of the BF4 − anion are disordered over two sets of sites, with a site-occupancy factor of 0.709 (10) for the major occupied site. Theresa Irene Kückmann; Hans-Wolfram Lerner; Michael Bolte article http://publikationen.ub.uni-frankfurt.de/frontdoor/index/index/docId/25860 Tue, 28 Aug 2012 09:00:44 +0200 http://publikationen.ub.uni-frankfurt.de/frontdoor/index/index/docId/25858 A new polymorph of the title compound, [Pd2(C8H18P)2(C8H19P)2], has been found. It belongs to the triclinic P-1 space group, whereas the known form [Leoni, Sommovigo, Pasquali, Sabatino & Braga (1992 [triangle]), J. Organo­met. Chem. 423, 263–270] crystallizes in the monoclinic C2/c space group. The title compound features a dinuclear palladium complex with a planar central Pd2(μ-P)2 core (r.m.s. deviation = 0.003 Å). The Pd—Pd distance of 2.5988 (5) Å is within the range of a PdI—PdI bond. The mol­ecules of both polymorphs are located on a crystallographic centre of inversion. The mol­ecular conformations of the two polymorphs are essentially identical. The crystal packing patterns, on the other hand, are slightly different. Jens Breunig; Hans-Wolfram Lerner; Michael Bolte article http://publikationen.ub.uni-frankfurt.de/frontdoor/index/index/docId/25858 Tue, 28 Aug 2012 08:26:52 +0200 http://publikationen.ub.uni-frankfurt.de/frontdoor/index/index/docId/25300 Mol-ecules of the title compound, [Zn(8)(C(6)F(5))(8)O(4)(C(4)H(10)O)(4)], are located on a special position of site symmetry [Formula: see text]. As a result, there is just one quarter-mol-ecule in the asymmetric unit. The title compound features a Zn(4)O(4) cube. Each Zn atom in the cube carries a pentafluorophenyl substituent. Each O atom is bonded to a further Zn atom, which is connected to a pentafluorophenyl substituent and the O atom of a diethyl ether mol-ecule. All ether C atoms are disordered over two sets of sites with a site occupation factor of 0.51 (2) for the major occupied site. Daniel Franz; Hans-Wolfram Lerner; Michael Bolte article http://publikationen.ub.uni-frankfurt.de/frontdoor/index/index/docId/25300 Wed, 27 Jun 2012 12:56:10 +0200 http://publikationen.ub.uni-frankfurt.de/frontdoor/index/index/docId/25298 The title compound, C25H20N4O2, is a ditopic ortho-hydro­quinone-based bis­(pyrazol-1-yl)methane ligand. The dihedral angles between the planes of the pyrazole rings and their attached phenyl rings are 17.4 (3) and 5.9 (4)°. The pyrazole rings make a dihedral angle of 87.84 (16)°. One of the two hy­droxy groups forms an intra­molecular hydrogen bond to the other hy­droxy group, whereas the second is involved in an inter­molecular O—H[cdots, three dots, centered]N hydrogen bond. As a result of these inter­molecular hydrogen bonds, helical chains running along the b axis are formed. Florian Blasberg; Hans-Wolfram Lerner; Michael Bolte article http://publikationen.ub.uni-frankfurt.de/frontdoor/index/index/docId/25298 Wed, 27 Jun 2012 10:04:29 +0200 http://publikationen.ub.uni-frankfurt.de/frontdoor/index/index/docId/25286 The title compound, [Li4O4(C12H8BO)4(C4H10O)4], features a Li4O4 cube. Each Li atom in the cube is additionally coordinated by a diethyl ether mol­ecule and each O atom in the cube carries a 9-oxa-10-boraanthracene residue. The crystal studied was a non-merohedral twin [twin law (-1 0 0 / 0 0 1 / 0 1 0); the contribution of the major twin component refined to 0.553 (3)] emulating apparent tetra­gonal symmetry, whereas the actual crystal system is just ortho­rhom­bic. Daniel Franz; Hans-Wolfram Lerner; Dominik Büttner; Michael Bolte article http://publikationen.ub.uni-frankfurt.de/frontdoor/index/index/docId/25286 Mon, 25 Jun 2012 14:29:53 +0200 http://publikationen.ub.uni-frankfurt.de/frontdoor/index/index/docId/25285 The crystal structure of the title compound, hexa-μ2-bromido-μ4-oxido-tetra­kis­[(diethyl ether)magnesium], [Mg4Br6O(C4H10O)4], determined from data measured at 173 K, differs from the previously known structure of diethyl ether magnesium oxybromide, which was determined from room-temperature data [Stucky & Rundle (1964 [triangle]). J. Am. Chem. Soc. 86, 4821–4825]. The title compound crystallizes in the tetra­gonal space group I An external file that holds a picture, illustration, etc. Object name is e-67-m1614-efi7.jpg, whereas the previously known structure crystallizes in a different tetra­gonal space group, namely P An external file that holds a picture, illustration, etc. Object name is e-67-m1614-efi7.jpg21 c. Both molecules have crystallographic An external file that holds a picture, illustration, etc. Object name is e-67-m1614-efi7.jpg symmetry and show almost identical geometric parameters for the Mg, Br and O atoms. The crystal of the title compound turned out to be a merohedral twin emulating a structure with apparent Laue symmetry 4/mmm, whereas the correct Laue group is just 4/m. The fractional contribution of the minor twin component converged to 0.462 (1). Hannes Vitze; Hans-Wolfram Lerner; Michael Bolte article http://publikationen.ub.uni-frankfurt.de/frontdoor/index/index/docId/25285 Mon, 25 Jun 2012 14:21:18 +0200 http://publikationen.ub.uni-frankfurt.de/frontdoor/index/index/docId/25277 Mol­ecules of the title compound, [HgBr(C9H11)], are located on a crystallographic twofold rotation axis. Due to the mol­ecular symmetry, the HgII atom is linearly coordinated by the ipso-C of the mesityl group and the Br atom. In the crystal, mol­ecules lie in planes parallel to (001). Frank Meyer-Wegner; Tanja Sinke; Hans-Wolfram Lerner; Michael Bolte article http://publikationen.ub.uni-frankfurt.de/frontdoor/index/index/docId/25277 Mon, 25 Jun 2012 13:06:15 +0200 http://publikationen.ub.uni-frankfurt.de/frontdoor/index/index/docId/25214 The AuI atom of the title compound, [AuI(C12H27P)], shows an almost linear coordination, with a P—Au—I angle of 178.52 (3)° [Au—P = 2.2723 (14) Å and Au—I = 2.5626 (6) Å]. Inge Sänger; Hans-Wolfram Lerner; Tanja Sinke; Michael Bolte article http://publikationen.ub.uni-frankfurt.de/frontdoor/index/index/docId/25214 Fri, 22 Jun 2012 16:55:40 +0200 http://publikationen.ub.uni-frankfurt.de/frontdoor/index/index/docId/25232 The title complex, [PdCl2(C18H15P)2]·0.5C6H6, has the PdII ion in a square-planar coordination mode (r.m.s. deviation for Pd, P and Cl atoms = 0.024 Å) with the PPh3 and Cl ligands mutually trans. The benzene solvent mol­ecule is located about a crystallographic inversion centre. The title complex is isostructural with trans-dichloridobis(triphenyl­phosphane)­palladium(II) 1,4-dichloro­benzene sesquisolvate [Kitano et al. (1983 [triangle]). Acta Cryst. C39, 1015–1017]. Frank Meyer-Wegner; Hans-Wolfram Lerner; Tanja Sinke; Michael Bolte article http://publikationen.ub.uni-frankfurt.de/frontdoor/index/index/docId/25232 Sun, 17 Jun 2012 17:41:00 +0200 http://publikationen.ub.uni-frankfurt.de/frontdoor/index/index/docId/21915 In the title molecular salt, C16H36N+·C12H20BS3-, three of the four n-butyl chains show a trans conformation, whereas the fourth has the C—C—C—C torsion angle in a gauche conformation [-77.8 (5)°]. In the crystal, mol­ecules are packed in layers parallel to the (101) plane. Jan Tillmann; Hans-Wolfram Lerner; Michael Bolte article http://publikationen.ub.uni-frankfurt.de/frontdoor/index/index/docId/21915 Mon, 20 Jun 2011 10:57:46 +0200 http://publikationen.ub.uni-frankfurt.de/frontdoor/index/index/docId/21908 In contrast to the previous structure determinations of the title structure, (NH4)2[MoS4], the present determination at 173 K localized the positions of the H atoms. The title structure belongs to the beta-K2SO4 family and all the ions are located on crystallographic mirror planes. The ions are held together by N—H ... S hydrogen bonds (some of which are bifurcated), forming a three-dimensional network. One of the N atoms has nine contacts to the S atoms shorter than 4 Å, and the other has ten. Björn Hill; Hans-Wolfram Lerner; Michael Bolte article http://publikationen.ub.uni-frankfurt.de/frontdoor/index/index/docId/21908 Mon, 20 Jun 2011 10:16:23 +0200 http://publikationen.ub.uni-frankfurt.de/frontdoor/index/index/docId/21904 The title compound, C12H8BBr, crystallizes with three essentially planar mol­ecules (r.m.s. deviations = 0.018, 0.020 and 0.021Å) in the asymmetric unit: since the title compound is rigid, there are no conformational differences between these three mol­ecules. The crystal packing resembles a herringbone pattern. Alexander Hübner; Hans-Wolfram Lerner; Matthias Wagner; Michael Bolte article http://publikationen.ub.uni-frankfurt.de/frontdoor/index/index/docId/21904 Mon, 20 Jun 2011 10:02:38 +0200 http://publikationen.ub.uni-frankfurt.de/frontdoor/index/index/docId/21892 The title compound, [Na(CF3O3S)(C12H24O6)], features a sodium cation that is coordinated by eight O atoms in an irregular hexa­gonal bipyramidal environment. The equatorial positions are occupied by the six O atoms of an 18-crown-6 ether ring. In the axial positions, there is one O atom of a trifluoro­methane­sulfonate anion and an ether O atom of a symmetry-equivalent crown ether ring. In this way, centrosymmetric dimers are formed. Hien Ngoc Phan; Hans-Wolfram Lerner; Michael Bolte article http://publikationen.ub.uni-frankfurt.de/frontdoor/index/index/docId/21892 Fri, 17 Jun 2011 17:07:58 +0200 http://publikationen.ub.uni-frankfurt.de/frontdoor/index/index/docId/21891 The asymmetric unit of the title compound, [K(C5HF6N2)(H2O)2]n, is composed of two 3,5-bis­(trifluoro­meth­yl)pyrazol­ide anions, two potassium cations and four water mol­ecules. The water mol­ecules and 3,5-bis­(trifluoro­meth­yl)pyrazolide anions act as bridges between the potassium cations. Each potassium cation is surrounded by four O atoms [K—O = 2.705 (3)–2.767 (3) Å] and four F atoms [K—F = 2.870 (7)–3.215 (13) Å]. The water mol­ecules and the 3,5-bis­(trifluoro­meth­yl)pyrazolide anions are connected by O—H ... N hydrogen bonds, forming layers in the ab plane. All –CF3 groups show rotational disorder between two orientations each. Hien Ngoc Phan; Hans-Wolfram Lerner; Michael Bolte article http://publikationen.ub.uni-frankfurt.de/frontdoor/index/index/docId/21891 Fri, 17 Jun 2011 17:02:17 +0200 http://publikationen.ub.uni-frankfurt.de/frontdoor/index/index/docId/21884 The title compound, [Li3(C4F9O)3(C3H6O)3], features an open Li/O cube with an Li ion missing at one corner. Three of the four bridging O atoms of the cube carry a fluorinated tert-butyl residue, whereas the fourth is part of an acetone mol­ecule. Two of the Li atoms are further bonded to a non-bridging acetone mol­ecule. Two of the lithium ion coordination geometries are very distorted LiO4 tetra­hedra; the third could be described as a very distorted LiO3 T-shape with two distant F-atom neighbours. The Li[cdots, three dots, centered]Li contact distances for the three-coordinate Li+ ion [2.608 (14) and 2.631 (12) Å] are much shorter that the contact distance [2.940 (13) Å] between the tetra­hedrally coordinated species. Hannes Vitze; Hans-Wolfram Lerner; Michael Bolte article http://publikationen.ub.uni-frankfurt.de/frontdoor/index/index/docId/21884 Fri, 17 Jun 2011 16:13:38 +0200 http://publikationen.ub.uni-frankfurt.de/frontdoor/index/index/docId/21883 The title compound, [Tl4(C4H9O)4], featuring a (Tl—O)4 cube, crystallizes with a quarter-mol­ecule (located on a special position of site symmetry An external file that holds a picture, illustration, etc. Object name is e-66-m1621-efi1.jpg..) and a half-mol­ecule (located on a special position of site symmetry 23.) in the asymmetric unit. The Tl—O bond distances range from 2.463 (12) to 2.506 (12) Å. All O—Tl—O bond angles are smaller than 90° whereas the Tl—O—Tl angles are wider than a recta­ngular angle. Florian Blasberg; Hans-Wolfram Lerner; Michael Bolte article http://publikationen.ub.uni-frankfurt.de/frontdoor/index/index/docId/21883 Fri, 17 Jun 2011 16:09:49 +0200 http://publikationen.ub.uni-frankfurt.de/frontdoor/index/index/docId/6982 The title compound, [Fe2(C5H5)2(C24H22BP2)(CO)4][FeCl4]·CHCl3, is an oxidation product of CpFe(CO)2PPh2BH3. One pair of phenyl rings attached to the two different P atoms are almost parallel, as are the other pair [dihedral angles = 8.7 (5) and 8.9 (5)°]. The planes of the two cyclopentadienyl rings are inclined by 26.8 (7)° with respect to each other. The carbonyl groups at each Fe atom are almost perpendicular [C-Fe-C = 92.6 (6) and 94.3 (5)°]. Key indicators: single-crystal X-ray study; T = 173 K; mean σ(C–C) = 0.019 Å; R factor = 0.112; wR factor = 0.177; data-to-parameter ratio = 16.8. Franz Dornhaus; Hans-Wolfram Lerner; Michael Bolte article http://publikationen.ub.uni-frankfurt.de/frontdoor/index/index/docId/6982 Tue, 15 Sep 2009 09:05:17 +0200 http://publikationen.ub.uni-frankfurt.de/frontdoor/index/index/docId/6980 The title compound, [Re2(OH)(C10H8N2)2(CO)6][ReO4], is a mixed-valence rhenium compound containing discrete anions and cations. The ReI atoms are in a slightly distorted octahedral environment, whereas the ReVII atoms show the typical tetrahedral coordination mode. The dihedral angle between the two bipyridine groups is 34.3 (7)°. Key indicators: single-crystal X-ray study; T = 173 K; mean σ(C–C) = 0.044 Å; R factor = 0.093; wR factor = 0.262; data-to-parameter ratio = 13.9. Kai Ruth; Thorsten Morawitz; Hans-Wolfram Lerner; Michael Bolte article http://publikationen.ub.uni-frankfurt.de/frontdoor/index/index/docId/6980 Tue, 15 Sep 2009 08:53:56 +0200 http://publikationen.ub.uni-frankfurt.de/frontdoor/index/index/docId/6970 The title compound, C18H15BrSi, crystallizes with two almost identical molecules (r.m.s. deviation for all non-H atoms = 0.074 Å) in the asymmetric unit. It is isomorphous with chlorotriphenylsilane. Key indicators: single-crystal X-ray study; T = 173 K; mean σ(C–C) = 0.010 Å; R factor = 0.095; wR factor = 0.288; data-to-parameter ratio = 17.0. Hannah Steinert; Hans-Wolfram Lerner; Michael Bolte article http://publikationen.ub.uni-frankfurt.de/frontdoor/index/index/docId/6970 Mon, 14 Sep 2009 09:19:23 +0200 http://publikationen.ub.uni-frankfurt.de/frontdoor/index/index/docId/6969 The complete molecule of the title compound, [Sn(C6H5)2Cl2(C9H21OP)2], is generated by crystallographic inversion symmetry, the Sn atom is located on a special position of site symmetry \overline{1}. The Sn atom adopts an all-trans SnC2O2Cl2 octahedral geometry. As a consequence of the bulky substituents at the O atom, the P-O-Sn bond angle is 163.9 (3)°. Key indicators: single-crystal X-ray study; T = 173 K; mean σ(C–C) = 0.012 Å; R factor = 0.058; wR factor = 0.099; data-to-parameter ratio = 18.6. Manuela Müller; Hans-Wolfram Lerner; Michael Bolte article http://publikationen.ub.uni-frankfurt.de/frontdoor/index/index/docId/6969 Mon, 14 Sep 2009 08:45:09 +0200 http://publikationen.ub.uni-frankfurt.de/frontdoor/index/index/docId/6965 In the title compound, C12H14N22+·2Cl-, the 4,4'-dimethyl-2,2'-bipyridinium cation is essentially planar (r.m.s. deviation for all non-H atoms = 0.004 Å) and is located on a crystallographic inversion centre. The cations and chloride anions lie in planes parallel to (111) and are connected by N-H...Cl and C-H...Cl hydrogen bonds. Key indicators: single-crystal X-ray study; T = 173 K; mean σ(C–C) = 0.003 Å; R factor = 0.036; wR factor = 0.080; data-to-parameter ratio = 14.7. Urs David Eckensberger; Hans-Wolfram Lerner; Michael Bolte article http://publikationen.ub.uni-frankfurt.de/frontdoor/index/index/docId/6965 Fri, 11 Sep 2009 09:15:19 +0200 http://publikationen.ub.uni-frankfurt.de/frontdoor/index/index/docId/6960 The geometric parameters of the molecule of the title compound, C14H16O2P2, are in the usual ranges. It is a meso compound with the two chiral P atoms having opposite configurations. The P-CH2-CH2-P chain adopts a trans conformation [torsion angle -178.59 (17)°]. The P=O bonds are almost coplanar with the adjacent phenyl ring [torsion angles = 3.8 (3) and 0.3 (3)°]. Whereas one of them is synclinal [torsion angle = -59.0 (2)°] to the central C-C bond, the other is anticlinal [torsion angle = 56.6 (2)°] to the central C-C bond. The dihedral angle between the two phenyl rings is 5.2 (3)°. The molecules are linked by weak C-H...O hydrogen bonds. They crystallize in rows running along the c axis. Key indicators: single-crystal X-ray study; T = 173 K; mean σ(C–C) = 0.005 Å; R factor = 0.038; wR factor = 0.093; data-to-parameter ratio = 15.2. Franz Dornhaus; Hans-Wolfram Lerner; Michael Bolte article http://publikationen.ub.uni-frankfurt.de/frontdoor/index/index/docId/6960 Fri, 11 Sep 2009 08:34:01 +0200 http://publikationen.ub.uni-frankfurt.de/frontdoor/index/index/docId/6897 The asymmetric unit of the title compound, [K(C3H3N2)(C12H24O6)], is composed of a potassium cation bonded to the six O atoms of a crown ether molecule and the two N atoms of a pyrazolate anion. The K...O distances range from 2.8416 (8) to 3.0025 (8) Å, and the two K...N distances are 2.7441 (11) and 2.7654 (11) Å. The K cation is displaced by 0.8437 (4) Å from the best plane through the six O atoms. The latter plane is almost perpendicular to the plane of the pyrazolate ring [dihedral angle 83.93 (3)°]. Key indicators: single-crystal X-ray study; T = 173 K; mean σ(C–C) = 0.002 A°; R factor = 0.026; wR factor = 0.066; data-to-parameter ratio = 16.5. Kerstin Kunz; Hans-Wolfram Lerner; Michael Bolte article http://publikationen.ub.uni-frankfurt.de/frontdoor/index/index/docId/6897 Fri, 04 Sep 2009 14:05:55 +0200 http://publikationen.ub.uni-frankfurt.de/frontdoor/index/index/docId/6871 The title compound, C14H14Si, crystallizes with two almost identical molecules (r.m.s. deviation = 0.080 Å for all non-H atoms) in the asymmetric unit. All atoms of the silafluorene moiety lie in a common plane (r.m.s. deviations = 0.049 and 0.035 Å for the two molecules in the asymmetric unit). The Si-Cmethyl bonds are significantly shorter [1.865 (4)-1.868 (4) Å] than the Si-Caromatic bonds [1.882 (3)-1.892 (3) Å]. Owing to strain in the five-membered ring, the endocyclic C-Si-C angles are reduced to 91.05 (14) and 91.21 (14)°. Key indicators: single-crystal X-ray study; T = 173 K; mean σ(C–C) = 0.005 A°; R factor = 0.061; wR factor = 0.157; data-to-parameter ratio = 16.3. Jan Mewes; Hans-Wolfram Lerner; Michael Bolte article http://publikationen.ub.uni-frankfurt.de/frontdoor/index/index/docId/6871 Wed, 02 Sep 2009 13:44:31 +0200