Showing papers in "Zeitschrift Fur Kristallographie-new Crystal Structures in 2004"
TL;DR: In this article, the authors measured the phase transition pressure of the mineral powellite, CaMoCU, in a 0.35 mm culet diamond-anvil cell with methanol/ethanol as pressure transmitting medium.
Abstract: CaMo04, monoclinic, I\\Ua\\ (no. 15), a = 5.034(1) A, b = 10.768(2) A, c = 5.108(1) A,/3 = 90.96(2)°, V= 276.9 A, Z= 4, Rgt(F) = 0.124, wRretfF) = 0.137, T= 298K ,P= 16GPa. Source of material The sample was prepared as a fine ground powder from a single crystal of powellite from Shiridi, India, and loaded into a0.35 mm culet diamond-anvil cell with methanol/ethanol as pressure transmitting medium. The pressure of the previously encountered transition is within the hydrostatic limits of this medium, our determination of the pressure of transition, however, is not. Pressure was measured by the shift of the R1 line of ruby [1,2]. Data were collected at approximately every 1 GPa to a maximum of 16 GPa. Discussion At ambient pressure and temperature conditions the mineral powellite, CaMoCU, is isostructural with the scheelite, CaWC>4 (/4i/a, Z = 4). The high pressure forms of the BaWC>4 [3] and CaWC>4 [4] scheelite-type phases has been determined to be the monoclinic fergusonite-type (/2/a, Z = 4) while other reversible transitions are also reported for the scheelite phases of SrWC>4, SrMo04 , PbW0 4 and PbMoC>4, occurring at 10.5 GPa, 12.5 GPa, 4.6 GPa and 6.5 GPa, respectively [5-7]. A high-pressure Raman spectroscopic study [8] found evidence for phase transitions in CaMoCU at 8.2 GPa and at 15 GPa. Though no structural evidence was available, it has been assumed that the first of these pressures was due to the post-scheelite transition. Christofilos et al. [8] were able, however, to rule out the possibility of the post-scheelite phase being that of either HgMo04-type or wolframite-type as both increase the coordination of Mo-O polyhedra and would involve bond lengthening, for which no evidence of abrupt mode-softening was observed. These authors [8] also indicated the behavior was most akin to that of YLiF4, which, it has more recently been shown, undergoes a high pressure scheelite-to-fergusonite phase transition with no or litde volume change [9]. Fitting of a Birch-Murnaghan equation of state to 10 pressure-volume data for the scheelite-type unit cell to 9.5 GPa results in equation of state described by V0 = 312.49(1) A, bulk modulus, K = 82.5(7) GPa and its first pressure derivative K' = 4.2(3) GPa. These results are in agreement with our measured ambient V0 = 312.49(1) A 3 and those of reference [10], where K= 81.5(7) GPa. We note a 9 % higher bulk modulus, compared to that of the denser isostructural CaWC>4 [4], which is also a feature in agreement with [10]. The variation in the da ratio is linear over the entire range studied and can be described as decreasing at a rate of0.0031 GPa . The high pressure phase is first clearly identified by the appearance of the 020 line at 4° (20) at 15 GPa. The pressure was increased one further step for data collection for refinement using GSAS [11], based on a pattern calculated using the atomic positions and cell parameters for CaWC>4-II fergusonite [4], The phase transition pressure of 15 GPa is in agreement with similar behavior seen for PbWC>4 and PbMoCU, and SrWC>4 and SrMoC>4, in that the molybdate has a higher phase transition pressure than that of the tungstate. * Correspondence author (e-mail: crichton@esrf.fr)
11 citations
TL;DR: In this paper, the title compound consists of imidazolato bridged polymeric chains in terms of C9H11CIC11N6, orthorhombic, Pmrili (no. 31), a = 13.733, b = 6.102(1) A, c = 7.252(2) A, V= 607.7 A 3, Z = 2, Rp{F) = 0.047, wRreffF ) =
Abstract: C9H11CIC11N6, orthorhombic, Pmrili (no. 31), a = 13.733(3) A , b = 6.102(1) A , c = 7.252(2) A , V= 607.7 A 3 , Z = 2, Rp{F) = 0.047, wRreffF ) = 0.101, T= 293 K. Source of material Addition of 2.0 ml 1 M K2CO3 solution to an aqueous solution of CuCl2 • 2H20 (0.257 g, 1.506 mmol) in 5.0 ml H 2 0 yielded blue precipitate, which was separated out and moved to an aqueous methanolic solution of imidazole (0.102 g, 1.500 mmol) in a mixture consisting of 10 ml H2O and 10 ml CH3OH. The insoluble solid was filtered out and the dark blue filtrate (pH = 8.45) was allowed to stand at room temperature. Slow evaporation for two weeks afforded prismatic blue crystals. Discussion The title compound consists of imidazolato bridged polymeric chains in terms of ¿[Cu(C3H4N2)2Cl(C3H3N2)2/2] extending infinitely along [010]. The Cu atoms are each square pyramidally coordinated by one CI atom and four N atoms of two imidazole ligands and two imidazolate anions with the CI atom at the apical Table 3. Atomic coordinates and displacement parameters (in A). Table 1. Data collection and handling.
9 citations
TL;DR: In this article, the authors proposed a monoclinic approach to the problem of monoclonality in monocular microscopy and showed that β = 104.774(7)°, V = 2900.5 A 3.
Abstract: C 12 H 14 Br 2 Cl 4 N 2 Pb, monoclinic, P12 1 /c1 (no. 14), a = 17.373(2) A, b = 7.763(1) A, c = 22.242(2) A, β = 104.774(7)°, V = 2900.5 A 3 , Z= 6, R gt (F) = 0.057, WR ref (F 2 ) = 0.145, T= 293 K.
9 citations
TL;DR: In this paper, the triclinic trichotomy is defined as a triclastic triconyclic model where a = 6.5126 A, b = 10.499 A, c = 12.635 A, β = 79.141(2)°, y = 86.737°, V = 846.818°.
Abstract: C 40 H 30 N 4 S 4 , triclinic, P1 (no. 2), a = 6.5126(7) A, b = 10.499(1) A, c = 12.635(1) A, a = 87.818(2)°, β = 79.141(2)°, y = 86.737(2)°, V = 846.7 A 3 , Z = 1, 1, R gt (F) = 0.057, wR ref (F 2 ) = 0.150, T= 100 K.
8 citations
TL;DR: In this article, the authors synthesize 4-chloroaniline (Pbfc) using a mixture of concentrated aqueous hydroiodic acid (30.0 ml) and anhydrous ethanol (20 ml) under argon at 60 °C.
Abstract: Ci2Hi4Cl2LtN2Pb, monoclinic, P\\2\\lc\\ (no. 14), a = 15.444(1) A, b = 8.1786(7) A, c = 9.0478(7) A, P = 100.002(6)°, V = 1125.5 A3, Z = 2, Re,(F) = 0.052, wRrerfF) = 0.134, J = 293 K. Source of material The title compound was synthesized according to the method of literature [1]. Solid 4-chloroaniline (1.283 g, 0.01 mol) was dissolved in the mixture of concentrated (45 %) aqueous hydroiodic acid (30.0 ml) and anhydrous ethanol (20.0 ml) under argon at 60 °C. The solution of Pbfc (2.308 g, 5.0 mmol) in 20.0 ml of concentrated (45 %) aqueous HI was then added to the above solution gradually with stirring. The resulting solution was allowed to sit at 60 °C for 4 hours and then slowly (5 K/h) cooled to room temperature without stirring. The precipitation was filtered off. After drying in vacuo, yellow plate-like crystals (2.087 g, yield 43 %) suitable for X-ray single-crystal analysis were harvested. C, H and N elemental analyses were performed on a Vario EL m elemental analyzer: found C, 15.00 %; H, 1.30 %; N, 3.08 %; calc. for Ci2Hi4Cl2l4N2Pb C, 14.83 %; H, 1.45 %; N, 2.82%. Discussion Compared with the 4-bromoanilinium salt [1], the asymmetric unit of the tide structure contains only one 4-chloroanilinium cation and half a PbL» anion (figure, top). Furthermore, the structure is characterized by alternate well-ordered inorganic layers and organic layers stacked along a-axis (figure, bottom). The lead atoms lie in special positions on inversion centers. Each Pb atom is surrounded by six I atoms forming a distorted Pbl6 octahedron with Pb—I distances from 3.1711(10) A to 3.2191(8) A. Among six coordination atoms, four of them are bridging iodine atoms. A Pbl6 octahedron shares four 12 corners with four neighboring Pbl6 octahedra to form a two-dimensional network. The two shortest Pb—I distances correspond to bonds Pb—II with an angle of 180°. The other four distances correspond to the coordination bonds Pb—12 with angles of 86.46(1)° and 93.54(1)°, respectively, as well as 180°. Angles between Pb—II and Pb—12 edges range from 87.00(3)° and 93.54(1)°. Organic bilayers are formed by two kinds of parallel p-chloroanilinium ions. The interfacial angle between them is 43.9°. Values of C—C bonds range from 1.33(2) A to 1.40(2) A, while C—N and C—CI distances are 1.47(2) A and 1.75(1) A, respectively. Angles except for those containing hydrogen atoms in phenyl ring are between 118(1)° and 122(1)°. These values are similar to those of (p-BiC6H4NH3)2PbCl4 [1]. The cohesion of the atomic arrangement is enhanced by hydrogen bonding contacts: N1-H1A-I1, N1-H1B-I2 and N1-H1C-I1, which provided a linkage between NH3 cationic entities of organic bilayers and Pbl6 octahedra of inorganic perovskite layers. Table 1. Data collection and handling. Crystal: Wavelength: fiDiffractometer, scan mode: 2BmaxNfhkllmasimd, W(7lW)umque: Criterion for /obs, N(hkl)gi, N(param)nfined: Programs: yellow plate, size 0.02 x 0.20 x 0.24 mm Mo Ka radiation (0.71073 Â) 132.15 cm Broker P4, m 53.96° 3332,2464 /obs > 2 CTf/obs), 1641 98 SHELXTL-97 [2], WinGX [3] Table 2. Atomic coordinates and displacement parameters (in Â). Correspondence author (e-mail: namezhi@hotmail.com) Atom Site X y z c/iso H(2A) 4e 0.6095 0.4924 0.1225 0.070 H(3A) 4e 0.7532 0.5358 0.2492 0.067 H(5A) 4e 0.6814 0.3747 0.6286 0.075 H(6A) 4e 0.5415 0.3262 0.4% 1 0.079 H(1A) 4e 0.8314 0.6008 0.5098 0.108 H(1B) 4e 0.8554 0.4292 0.5059 0.108 H(1C) 4e 0.8171 0.4920 0.6303 0.108
8 citations
TL;DR: In this paper, the authors proposed a monoclinic approach to the problem of monoclonality and showed that the approach is more effective than the traditional monocline approach.
Abstract: Na07P2Yb, monoclinic, P12,/nl (no. 14), a = 9.0211(3) Â, b = 5.3571(4) Â, c = 12.7802(6) Â,/? = 103.176(5)°, I p , 0 7 | V = 601.4 A, Z = 4, RgtfF) = 0.040, wR^F) = 0.110,
8 citations
TL;DR: Amino nitrogen, N7, has a nearly planar environment (the sum of angles is 355.02°) where the N(1)···H(7) distance is fairly long 2.13°.
Abstract: C13H14N2, monoclinic, P121/n1 (no. 14), a = 11.304(8) A, b = 7.775(8) A, c = 13.451(9) A, = 113.98(5)°, V = 1080.2 A, Z = 4, Rgt(F) = 0.050, wRref(F) = 0.112, T = 193 K. Source of material The title compound was obtained in one-step procedure. 2chloropyridine and corresponding amine hydrochloride were heated at 180 °C for 90minutes. The hydrochlorous raw product was suspended to aqueous sodium carbonate and then extracted with dichloromethane. Drying over anhydrous sodium sulfate, filtering and evaporation yielded the desired product. The white solid was crystallized from diethyl ether/heptane solution to afford a white crystalline solid. Discussion The structure obtained is highly similar to those reported for 2phenylaminopyridines [1]. The title compound crystallizes as centrosymmetric dimer with two identical linear N7 H7···N1 interactions. The N7 H7···N1 angle is 173.9(2)° where the N(1)···H(7) distance is fairly long 2.16(2) A. This leads to long donor acceptor distance of 3.057(2)A.Amino nitrogen, N7, has a nearly planar environment (the sum of angles is 355.02°). Z. Kristallogr. NCS 219 (2004) 67-68 67 © by OldenbourgWissenschaftsverlag, Munchen Crystal: colorless, prismatic, size 0.20 × 0.35 × 0.35 mm Wavelength: Mo K radiation (0.71073 A) : 0.73 cm−1 Diffractometer, scan mode: Rigaku AFC7S, /2 2 max: 50.06° N(hkl)measured, N(hkl)unique: 3618, 1863 Criterion for Iobs, N(hkl)gt: Iobs > 2 (Iobs), 1625 N(param)refined: 193 Programs: SHELXS-86 [2], SHELXL-97 [3], SHELXTL-NT [4], teXsan [5] Table 1. Data collection and handling. H(3) 4e 0.466(2) −0.197(2) 0.207(1) 0.041(4) H(4) 4e 0.523(2) −0.495(3) 0.238(1) 0.049(5) H(5) 4e 0.626(2) −0.595(3) 0.424(1) 0.045(5) H(6) 4e 0.652(2) −0.394(3) 0.565(1) 0.043(4) H(7) 4e 0.483(2) 0.089(3) 0.409(2) 0.062(6) H(101) 4e 0.696(2) 0.037(3) 0.308(2) 0.051(5) H(102) 4e 0.661(2) −0.028(3) 0.186(2) 0.072(6) H(103) 4e 0.719(2) 0.158(3) 0.224(2) 0.075(7) H(121) 4e 0.493(2) 0.311(3) −0.046(2) 0.063(6) H(122) 4e 0.634(2) 0.312(3) 0.065(2) 0.064(6) H(123) 4e 0.574(2) 0.136(4) 0.008(2) 0.065(6) H(13) 4e 0.309(2) 0.366(3) −0.007(2) 0.055(5) H(14) 4e 0.195(2) 0.348(3) 0.100(1) 0.055(5) H(15) 4e 0.280(2) 0.184(3) 0.266(1) 0.049(5) Table 2. Atomic coordinates and displacement parameters (in A). Atom Site x y z Uiso
7 citations
TL;DR: In this article, the authors proposed a monoclinic approach to the problem of monoclonality and showed that it is possible to obtain monoclanic results in the case of β = 105.522 degrees.
Abstract: C 20 H 28 O 3 , monoclinic, P2 1 (no. 4), a = 10.0279(2) A, b = 11.1076(3) A, c = 17.0856(4) A, β = 105.522(1)°, V= 1833.7 A 3 , Z = 4, R gt (F) = 0.058, wR ref (F 2 ) = 0.159, T= 293 K.
6 citations
TL;DR: In this paper, the orthorhombic Cmcm (no. 63), a = 4.0948(6), b = 15.582(3), c = 6.610(1) A, V = 421.8 A 3, Z = 4, R gt (F) = 0.028, wR obs (F 2 ).
Abstract: Ak 4 NiSm, orthorhombic, Cmcm (no. 63), a = 4.0948(6) A, b = 15.582(3) A, c = 6.610(1) A, V = 421.8 A 3 , Z = 4, R gt (F) = 0.028, wR obs (F 2 ) = 0.074, T= 293 K.
6 citations
TL;DR: In this paper, the authors present the results of a monoclinic analysis of P12 1 /n1 (no. 14), a = 6.8939(4) A, b = 17.7781(7) A and c = 12.396(1) A.
Abstract: BO 17 P 2 Pr 7 , monoclinic, P12 1 /n1 (no. 14), a = 6.8939(4) A, b = 17.662(1) A, c = 12.442(1) A, β=97.24(1)°, V= 1502.9 A 3 , Z=4, R gt (F) = 0.029, WR ref (F 2 ) = 0.052, T = 293 K. BO 17 P 2 Sm 7 , monoclinic, P12 1 /n1 (no. 14), a = 6.7781(7) A, b = 17.396(1) A, c = 12.218(1) A, β=96.96(1)°, V= 1430.0 A 3 , Z=4, R gt (F) = 0.022, WR ref (F 2 ) = 0.044, T = 293 K.
6 citations
TL;DR: In this article, the authors proposed a monoclinic approach to the problem and showed that β = 90.13(1)°, V = 1966.7 A 3, Z = 4, R gt (F) = 0.041, wR ref (F 2 )= 0.117, T = 293 K.
Abstract: C 22 H 20 BrNO 3 , monoclinic, P12 1 /c1 (no. 14), a = 17.643(1) A, b = 5.935(1) A, c = 18.782(1) A, β = 90.13(1)°, V = 1966.7 A 3 , Z = 4, R gt (F) = 0.041, wR ref (F 2 ) = 0.117, T = 293 K.
TL;DR: In this article, the triclinic PI (no. 2), a = 10.405(4), b = 11.787(5), c = 14.217(6) A, β = 103.479(6), y = 93.895(6)-°, V= 1631.5 A 3, Z = 1, R gt (F) = 0.027, wR ref (F 2 ) =0.071, T= 293 K.
Abstract: C 70 H 50 N 8 O 18 Tb 2 , triclinic, PI (no. 2), a = 10.405(4) A, b = 11.787(5) A, c = 14.217(6) A, a = 103.479(6)°, β = 103.925(6)°, y = 93.895(6)°, V= 1631.5 A 3 , Z = 1, R gt (F) = 0.027, wR ref (F 2 ) = 0.071, T= 293 K.
TL;DR: Zhang et al. as mentioned in this paper derived the crystal structure of the pyrrolo-[2,3-£]pyridine via X-ray single-crystal diffraction, and the purpose of their investigation is to gain better insight into the structure of this molecule.
Abstract: C10H12N2, triclinic, PI (No. 2), a = 5.5503(7) A , b = 7.926(1) A , c = 9.992(1) A , a = 76.891(2)°, P = 89.395(2)°, y = 82.459(2)°, V = 424.3 A 3 , Z = 2, Rgl(F) = 0.038, wRrerfF) = 0.099, T= 100 K. Source of material The title compound was synthesized from li/-pyrrolo-[2,3¿]pyridine via 1-substituted Grignard derivative [1], Light yellow crystals were grown by slow evaporation from a 95 % ethanol solution at 4 °C. Discussion The l//-pyrrolo-[2,3-fc]pyridine derivatives have attracted the attention of chemists in recent years because of their extensive use as gastrointestinal inflammatory disease inhibitor [2] and angiotensin II antagonists [3]. In our synthesis of the substituted 1Hpyrrolo-[2,3-£]pyridines for the bioactive drugs, 2-propyl-l//pyrrolo-[2,3-fr]pyridine may be prepared with large scale in high yield. To understand the relationship between the structurally endogenous hormone and overall biological property [4], the crystal structure of the title compound was determined by X-ray singlecrystal diffraction. The purpose of our investigation is to gain better insight into the structure of this molecule. * Correspondence author (e-mail: zhangqf@ahut.edu.cn) In the title structure, the overall conformation of the molecule can be described by two torsion angles: C6-C7-C8-C9 [-0.8( 1)°] defines the relative orientation of the side chain towards the aromatic plane, whereas the orientation of propyl group is given by the angle C7-C8-C2-C10 [-177.9(2)°]. The aromatic 7-azaindole nucleus is planar with average deviation of 0.007(1) A from the best least-square plane. The molecular geometry of 7azaindole moiety is characterized by shortening of CI—N1 [1.338(1) A ] and C5—N1 [1.334(1) A ] bonds, and shrinkage of the C1-N1-C5 angle [114.69(9)°]. The same character of bond distortion has been observed in a similar compound, l//-pyrrolo[2,3-6]pyridine-3-acetic acid [5]. The crystal packing of the title compound is determined by two N-H—N hydrogen bonds, accordingly, two formula units form a consecutive dimer across a crystallographic center of symmetry via near-linear hydrogen bonds. The angle at the hydrogen [N2-H2A-N1A, 0.88 A , 2.059(2) A , 2.923(2) A , 167.0(2)°] is also consistent with this character. These hydrogen bonds form an eight-membered ring in the dimeric conformation. Table 1. Data collection and handling. pale yellow plate, size 0.10 x 0.30 x 0.40 mm Mo Ka radiation (0.71073 Â) 0.76 cm\" Broker SMART CCD, 2 O(lobs), 1713 109 SHELXTL-Plus [6], SHELXTL-97 [7] Table 2. Atomic coordinates and displacement parameters (in Â). Atom Site X y z {/is0 H(2A) 2i 0.1642 0.9029 0.4369 0.023 H(1B) li -0.0095 0.9582 0.8808 0.027 H(2B) 2i 0.3371 0.8108 1.0022 0.028 H(3A) li 0.6604 0.6845 0.8881 0.027 H(6A) li 0.7871 0.6345 0.6033 0.025 H(8A) li 0.5468 0.8552 0.2688 0.024 H(8B) li 0.4248 0.6788 0.3006 0.024 H(9A) li 0.9275 0.6905 0.3551 0.026 H(9B) li 0.8036 0.5148 0.3808 0.026 H(10A) li 1.0156 0.5500 0.1732 0.039 H(10B) li 0.8553 0.7353 0.1159 0.039 H(10C) li 0.7315 0.5597 0.1415 0.039 Crystal:
TL;DR: In this article, the triclinic trichotomy is defined as a triconnective trichlinic, and β = 82.988(4)°, y = 83.742°, V = 1467.7 A 3, Z = 4, R gt (F) = 0.072, wR ref (F 2 ) = 0., T = 293 K.
Abstract: C 9 H 18 S 6 , triclinic, P1 (no. 2), a = 5.637(1) A, b = 14.748(4) A, c = 17.913(4) A, a = 86.663(5)°, β = 82.988(4)°, y = 83.742(4)°, V = 1467.7 A 3 , Z = 4, R gt (F) = 0.072, wR ref (F 2 ) = 0.166, T = 293 K.
TL;DR: In this article, the authors obtained a monoclinic Amino nitrogen N7 with a centrosymmetric dimer with two identical linear N7-H7-N1' interactions.
Abstract: C13H14N2, monoclinic, f 12i/cl (no. 14), a = 11.892(6) A , b = 7.570(7) A , c = 13.309(7) A, P = 112.65(3)°, V = 1105.7 A 3 , Z = 4, RgJF) = 0.055, wRntfF) = 0.151, T = 193 K. Source of material The title compound was obtained in one-step synthesis. 2chloropyridine and 2-ethylaniline hydrochloride were heated at 450 K for two hours. The resulting hydrochlorous raw product was suspended to sodium carbonate. The product was crystallized from diethyl ether/heptane. Experimental details The H7 atom found in the fourier map was refined freely to comment the hydrogen bonding pattern. Some other H atoms were not found from fourier map and, therefore, all H atoms except H7 were introduced in the refinements as calculated positions. Table 2. Atomic coordinates and displacement parameters (in Â). Atom Site X y z f/iso H(3A) 4e 0.2862 -0.1294 0.2915 0.049 H(4A) 4e 0.2654 0.0534 0.4236 0.054 H(5A) 4c 0.1011 0.2528 0.3751 0.060 H(6A) 4c -0.0299 0.2686 0.1954 0.058 H(7) 4e 0.080(2) -0.128(4) 0.018(2) 0.056(8) H(10A) 4c 0.5017 -0.3633 0.1233 0.060 H(11A) 4c 0.4545 -0.6425 0.1646 0.063 H(12A) 4c 0.2635 -0.6988 0.1679 0.066 H(13A) 4c 0.1218 -0.4726 0.1317 0.060 H(14A) 4e 0.4611 -0.0470 0.1095 0.065 H(14B) 4c 0.3326 0.0252 0.1048 0.065 H(15A) 4c 0.3521 0.0808 -0.0610 0.101 H(15B) 4c 0.2419 -0.0537 -0.0806 0.101 H(15C) 4c 0.3703 -0.1256 -0.0759 0.101 Discussion The outline of the structure obtained is similar to 2-(2,3dimethylphenylamino)pyridine [1], The title compound crystallizes as centrosymmetric dimer with two identical linear N7-H7-N1' interactions. N7-H7-N1' angle is 175(2)° where the distance N1—H7' is fairly long 2.05(3) A and donor acceptor distance is 2.965(3) A. Amino nitrogen N7 has a planar environment (the sum of angles 359.89°) and its plane is almost coplanar with pyridine ring deviating 3.4° from optimal coplanarity. The bond length of N7—C2 is considerably shorter than the bond * Correspondence author (e-mail: markku.talja@helsinki.fi)
TL;DR: ' Mersin University, Faculty of Arts and Sciences, Department of Chemistry, 33343Mersin, Turkey II Georgia Institute of Technology, School of Chemistry and Biochemistry, 770 State Street Atlanta, Georgia 30332-0400 as mentioned in this paper.
Abstract: ' Mersin University, Faculty of Arts and Sciences, Department of Chemistry, 33343 Mersin, Turkey II Georgia Institute of Technology, School of Chemistry and Biochemistry, 770 State Street Atlanta, Georgia 30332-0400, USA III Clemson University, Department of Chemistry, Clemson, SC 29634-0973, USA [ v Inönii University, Faculty of Science and Arts, Department of Chemistry, 44069 Malatya, Turkey v Ege University, Department of Chemistry, 35100 Bornova Izmir, Turkey
TL;DR: In this article, the triclinic compound of the chemical formula Ca2(Mg,Co) has been found to contain more Co than Mg (0.532H4Mgo.
Abstract: As2Ca2Coo.532H4Mgo.4680io, triclinic, P\\ (no. 2), a = 5.884(1) A , b = 6.981(1) A , c = 5.564(1) A , a = 97.33(2)°, fl = 108.93(2)°,y = 108.18(2)°, V= 198.6 A 3 , Z = 1, Rgl(F) = 0.017, wR^F) = 0.047, T= 293 K. Source of material The crystals were taken from a mine near Bou-Azzer, Morocco. In contrast to the crystals investigated by Dunn, Sturman and Nelen, which had much more Mg than Co [1], our samples contain according to electron microprobe analyses in the average more Co than Mg (0.579:0.473). Experimental details The average Ha of the measured X-ray intensities is 76.6. The hydrogen atoms could be refined isotropically, nevertheless the measurements were carried out at room temperature. The largest peak and hole in the difference density map were 0.778 and -0.854 e/A, respectively. Despite die average If II equals 0.808, the adequate space group isPl . The refinement in PI with racemic twinning resulted in the same structure with slightly higher ^-values {RgiF) = 0.020, wR^F 2 ) = 0.055). Discussion According to Catti et al. [2] and Hawthorne & Ferguson [3] the triclinic compound of the chemical formula Ca2(Mg,Co)(AsC>4)2 2H2O is called talmessite, the monoclinic one roselite [3]; the name/7-roselite [4] will not be used by us. The top figure shows the krOhnkite-type chains. According to M. Fleck the structure should be assigned to the structural type A [5], roselite to structural type D. The high significance of the hydrogen positions allows an unambiguous identification of the water molecules and the hydrogen bonding [2]. 04 is the acceptor of two hydrogen bonds originating from the two hydrogens of the water molecule. The hydrogen bond 0W1-H2 0 4 (2.616 A ) connects twochains within the layers parallel (101), whereas OW1-H1— 0 4 (2.579A) connects the layers. There are, however, no hydrogen bonds within the chains [5]. The bottom figure shows a least squares fit between krohnkite-type chains of talmessite (bold lines) and roselite (dashed lines) [3]. The chains are very similar indeed. There seems to exist a solid solution seria between Mg and Co [ 1 ], whose relative content has apparently no influence on the crystal structure. There is an analysis of the miscibility in minerals, but not in crystals grown in the laboratory [1]. The average e.s.d. for metal-metal distances is 0.001 A , for metal-oxygen and oxygenoxygen distances 0.002 A and for the oxygen-hydrogen distances 0.04 A . The average e.s.d. of angles between metals with no oxygens in is 0.02°, with one oxygen 0.04° and with 2 oxygens 0.1°, in the water molecule it is 3°. Table 1. Data collection and handling. Crystal: Wavelength: PDiffractometer, scan mode: /V(MJ>roeasured, WltyJuniqi*: Criterion for labs, N(hkl) N(param)rcfmcd: Programs: pink plate, size 0.05 x 0.175 x 0.25 mm Mo K„ radiation (0.71073 A) 107.92 cm\" Nonius CAD4,0-20-scan 59.92° 2318,1159 / „ b s > 2 a ( W , 1141 80 SHELXS-97 [6], SHELXL-97 [9], SHELXTL-PLUS [8] * Correspondence author (e-mail: e.paulus@kristall.uni-frankfurt.de) 342 Ca2(Coo.532Mgo.468)[As04]2 • 2H20 Table 2. Atomic coordinates and displacement parameters (in À).
TL;DR: In this paper, the authors proposed a monoclinic approach to the problem of monoclonality and showed that it is possible to construct monoclanic structures from monoclastic structures.
Abstract: C 18 H 18 N 4 Ni 2 O 12 , monoclinic, P12 1 /c1 (no. 14), a = 7.558(2) A, b = 20.004(3) A, c = 7.135(2) A, β = 92.02(3)°, V = 1078.1 A 3 , Z = 2, R gt (F) = 0.023, wR ref (F 2 ) = 0.061, T = 293 K.
TL;DR: In this paper, the orthorhombic orthorehombics were used to obtain orthoregressive orthorehodo-nomenclature of the ortho-homomorphic P2 1 2 1 2 2 1 (no. 19), a = 10.5617(5), b = 19.1580(9) A, c = 21.5366(9), V = 4357.
Abstract: C 42 H 67 NaO 11 , orthorhombic, P2 1 2 1 2 1 (no. 19), a = 10.5617(5) A, b = 19.1580(9) A, c = 21.5366(9) A, V = 4357.7 A 3 , Z = 4, R gt (F) = 0.035, wR ref (F 2 ) = 0.082, T = 293 K.
TL;DR: In this article, the authors proposed a monoclinic approach to the problem and showed that β = 91.021(5)°, V = 920.8 A 3, Z = 2, R gt (F) = 0.048, WR ref (F 2 )= 0.183, T= 295 K.
Abstract: C 23 H 15 ClN 2 O 3 , monoclinic, P12 1 1 (no. 4), a = 12.417(2) A, b = 4.4910(6) A, c = 16.514(2) A, β = 91.021(5)°, V = 920.8 A 3 , Z = 2, R gt (F) = 0.048, WR ref (F 2 ) = 0.183, T= 295 K.
TL;DR: In this paper, Jansen et al. presented the KAg2AsK04, tetragonal, /42m (no. 121), a = 5.9033(8) Â, c = 7.082 Â and V = 246.8 Â.
Abstract: Ag2AsK04, tetragonal, /42m (no. 121), a = 5.9033(8) Â, c = 7.082(1) Â, V= 246.8 Â, Z= 2, R^F) = 0.030, wRref(F) = 0.068, T= 293 K. Table 1. Data collection and handling. Crystal: Wavelength: HDiffractoraeter, scan mode: Nfhkllmnsumi, N(hkl)unique'. Criterion for /ot», N(hkl)gc. N(param)nfùKà: Programs: yellow cube, size 0.2 x 0.2 x 0.2 mm Mo Ka radiation (0.71073 A) 153.33 cm\" Broker AXS SMART APEX CCD, m 69.66° 1892,293 /obs > 2 O(Iotx), 292 14 SHELXL-97 [5], DIAMOND [6] Table 2. Atomic coordinates and displacement parameters (in A). References 1. Linke, C.; Jansen, M.: Über Ag2Sn03, das erste Silberstannat. Z. Anorg. Allg. Chem. 623 (1997) 1441-1446. 2. Curda, J.; Peters, E.-M.; Jansen, M.: Ein Metaarsenat(V)-Anion neuartiger Konstitution in AgAsÛ3. Z. Anorg. Allg. Chem. 630(2004) 49 M94. 3. Helmholtz, L.; Levine, R.: A Determination of Parameters in Potassium Dihydrogen Arsenate and Silver Arsenate. J. Am. Chem. Soc. 64(1942) 354-358. 4. Schimek, G. L.; Kolis, J. W.: KAg2AsS4. Acta Crystallogr. C53 (1997) 991-992. 5. Sheldrick, G. M.: SHELXL-97. Program for the Refinement of Crystal Structures. University of Göttingen, Germany 1997. 6. Brandenburg, K.: DIAMOND. Visual Crystal Structure Information System. Version 2. Id. Crystal Impact GbR, Bonn, Germany 2000. * Correspondence author (e-mail: m.jansen@fkf.mpg.de)
Journal Article•
TL;DR: In this article, the orthorhombic Pnma (no. 62), a = 12.265, b = 16.707, c = 10.044, V = 2058.1 A 3, Z = 4, R gt (F) = 0.057, wR obs (F 2 )= 0.158, T = 293 K
Abstract: C 18 H 33 ISn, orthorhombic, Pnma (no. 62), a = 12.265(1) A, b = 16.707(2) A, c = 10.044(2) A, V = 2058.1 A 3 , Z = 4, R gt (F) = 0.057, wR obs (F 2 ) = 0.158, T = 293 K.
TL;DR: In this article, the orthorhombic Pbca (no. 61), a = 14.922(2), b = 8.605(9), c = 15.308(9) A, V = 1965.6 A 3, Z = 8, R gt (F) = 0.071, wR ref (F 2 ) = 0.112, T= 173 K.
Abstract: C 11 H 8 F 2 N 2 , orthorhombic, Pbca (no. 61), a = 14.922(2) A, b = 8.605(9) A, c = 15.308(9) A, V = 1965.6 A 3 , Z = 8, R gt (F) = 0.071, wR ref (F 2 ) = 0.112, T= 173 K.
TL;DR: In this article, the Au atom in Ph3PAu(S2COBu) exists in a linear geometry defined by S, d(Au-SI) = 2.3179(7) A, and P, ¿ (Au -Au) = 3.2531(3) A; symmetry operation -x, y, Yi-z.
Abstract: C23H24AUOPS2, monoclinic, C12/cl (no. 15), a = 23.581(1) A, b = 13.7153(8) A, c = 17.182(1) A, 0 = 125.554(1)°, V = 4521.2 A, Z= 8, Rgt(F) = 0.026, wRreffF) = 0.062, T= 183 K. Source of material The title compound was prepared as documented in the context of the putative anti-tumour activity of this class of compound [1]. Crystals were obtained from the slow evaporation of dichloromethane into an ethanol solution of the compound. Discussion The Au atom in Ph3PAu(S2COBu) exists in a linear geometry defined by S, d(Au—SI) = 2.3179(7) A, and P, ¿(Au—PI) = 2.2627(7) A, atoms. The xanthate ligand is orientated so as to place the O atom in close proximity to Au so that d(Au—0) = 3.078(2) A. The distortion from a linear geometry, ZSl-Au-Pl is 170.92(3)°, is, in part, ascribed to the Au—O intramolecular interaction. The most significant intermolecular contact in the crystal structure is an aurophilic interaction, as indicated in the figure. These Au—Au contacts occur between molecules that are related to each other by a two-fold axis of symmetry so that ¿(Au -Au) = 3.2531(3) A; symmetry operation -x, y, Yi-z. Similar Au—Au interactions are found in only two other R3PAu(S2COR') structures, namely R = Ph and R' = nPr [2] and R = Et and R' = Cy [3]. The orientation of the xanthate ligand in the title structure is as originally reported for Ph3PAu(S2COMe) [4], Table 2. Atomic coordinates and displacement parameters (in Â).
TL;DR: Li et al. as discussed by the authors proposed orthorhombic Pnnm (no. 58), a = 10.968 A, b = 11.687 A, c = 4.5482 A, V = 583.0 A 3, Z = 4, R gt (F) = 0.023, WR ref (F 2 ),
Abstract: Eu 2 Ge 3 Li, orthorhombic, Pnnm (no. 58), a = 10.968(2) A, b = 11.687(2) A, c = 4.5482(7) A, V = 583.0 A 3 , Z = 4, R gt (F) = 0.023, WR ref (F 2 ) = 0.048, T = 293 K.
TL;DR: In this article, a methanol solution of benzene-1,4-dioxyacetic acid (23 mg, 0.1 mmol), acting as the oxidizing agent in this reaction, was added into a solution of Co(C104)2 • 6H2O in H2O (10 mL) with vigorous stirring.
Abstract: C30H28CI3C0N6O14, trigonal, R3c (no. 161), a = 30.391(4) À, c = 20.748(5) À, V= 16596(5) À, Z = 18, RgrfF) = 0.060, wRreffF) = 0.185, T= 293 K. Source of material A methanol solution (10 mL) of benzene-1,4-dioxyacetic acid (23 mg, 0.1 mmol), acting as the oxidizing agent in this reaction, was added into a solution of Co(C104)2 • 6H2O (40 mg, 0.1 mmol) in H2O (10 mL) with vigorous stirring, and then a methanol solution (5 mL) of 2,2'-bipyridine (32 mg, 0.2 mmol) was added into the above light-pink solution under stirring for ca. 30 min. The resultant yellow solution was Altered and left to stand at room temperature. Yellow prism-like single crystals suitable for X-ray diffraction were obtained after several days by slow evaporation of the solvent in 70 % yield. * Correspondence author (e-mail: dumiao@public.tpt.tj.cn) Experimental details Except hydrogen atoms of lattice water molecules, which could not be located definitely, all hydrogen atoms of the ligands were placed in geometrically calculated positions and included in the final refinement in riding model approximation, with displacement parameters derived from the atoms to which they were bonded [Uiso(H) = 1.2t/eq(C)].
TL;DR: In this article, Diethyl 2-(dibenzoylmethyl)-3-(triphenylphosphoranylidene)-succinate was synthesized in accordance with the published procedure.
Abstract: C 41 H 37 O 6 P, triclinic, P 1 (no. 2), a = 11.128(5) A, b = 12.548(5) A, c = 13.420(5) A, = 87.523(5)°, = 84.819(5)°, = 64.188(5)°, V = 1680.0 A 3 , Z =2, R gt (F) = 0.058, wR ref (F 2 ) = 0.148, T = 173 K. Source of material Diethyl 2-(dibenzoylmethyl)-3-(triphenylphosphoranylidene)-succinate was synthesized in accordance with the publishedprocedure [1]. Single crystals of the title compound were pre-pared from a mixture of ethyl acetate/light petroleum ether (1:5)at 322 K during six weeks using branch tube method. The color-less crystals were filtered off, washed with cold mixture of ethylacetate/lightpetroleumether(1:5,6ml)anddriedinvacuumoverP 4 O 10 (m.p. 478 K). Elemental analysis: found – C, 75.06 %;H, 5.61 %; calc. for C 41 H 37 O 6 P – C, 74.99 %; H, 5.68 %.MeltingpointwasmeasuredonanElectrothermal9100apparatusand is uncorrected. Elemental analysis was performed using aHeraeus CHN-O-Rapid analyzer. Discussion Phosphorus ylides are important reagents in synthetic organicchemistry,especiallyinthesynthesisofnaturallyoccurringcom-pounds with biological and pharmacological activity [1]. Thecrystal structure of the title compound is only built up by theC
TL;DR: In this article, the authors proposed a monoclinic approach to the problem of monoclonality in the context of monocular vision. But their approach is limited to monocular images and requires the use of a monocular camera.
Abstract: C 15 H 15 N 6 OP, monoclinic, P12 1 /n1 (no. 14), a = 10.558(2) A, b = 13.448(2) A, c = 21.814(4) A, β = 92.314(4)°, V = 3094.6 A 3 , Z = 8, R gt (F) = 0.051, wR ref (F 2 ) = 0.101, T = 120 K.