The crystal and molecular structure of 1,1,2,4,4,5-hexaphenyl-1,4-diphosphoniacyclohexadiene-2,5 dibromide

The crystal and molecular structure of 1,1,2,4,4,5-hexaphenyl-1,4-diphosphoniacyclohexadiene-2,5 dibromide has been determined by a single crystal, x-ray diffraction study using diffractometer data. The compound crystallizes in the space group P2₁/_c with unit cell constants a = 8.813(1), b = 36.736(4), c = 12.478(1) Å, and β = 120.91°(1). The structure was solved by the heavy atom method and refined by block-diagonal least-squares to a final R = 0.04 for the 2761 statistically significant reflections. The structure determination shows that the central phosphonium ring is a diene and not a delocalized structure as anticipated. The ring is in the boat conformation with the axial phenyl rings aligned essentially parallel to each other and 3.55 Å apart.     

The crystal and molecular structure of 1,1,4,4-tetraethyl-2,5-dimethyl-1,4-diphosphoniacyclohexadiene-1,4-dibromide

The structure of the title compound has been determined by a single-crystal, x-ray diffraction study. The compound crystallizes in a monoclinic unit cell (P2₁/c) with two molecules per unit cell. Least-squared lattice parameters are: a = 7.164 ± 0.001Å, b = 14.770 ± 0.001Å, c = 10.562 ± 0.001Å, and β = 124.95 ± 0.01°. The structure parameters refined to a value of R=0.06₂, excluding hydrogens, for the 1475 statistically significant reflections. The structure determination confirmed that the compound is indeed a diene and not a delocalized structure. The ring is planar but the ethyl groups extend over the ring in an unusual crab-like fashion.     

The crystal and molecular structure of 1,1,4,4-tetraphenyl-1,4-diphosphoniacyclohexane dibromide

The crystal and molecular structure of 1,1,4,4-tetraphenyl-1,4-diphosphoniacyclohexane dibromide has been determined by a single-crystal, x-ray diffraction study using diffractometer data. The compound crystallizes in the monoclinic space group P2₁/c with unit cell constants of a = 12.777(1), b = 26.180 (2), c = 16.283 (1) Å, and β = 91.18(1)°. The structure was solved by the heavy atom method with the 4176 independent and statistically significant structure factors refining to a value of R = 0.07. The diphosphonium ring is in the chair conformation with each phosphorus ion having an axial and equatorial phenyl ring attached. P-C and C-C bond lengths of 1.78 ± .03 Å and 1.53 ± .03 Å respectively agree well with the literature value for these distances.     

Crystal and molecular structure of triphenyl 4,4,6-Trimetliyl-1-oxa-3-azaeyeiohex-2-enylcarbenyl phosphonium chloride

The structure of the title compound has been determined by a single crystal, x-ray diffraction study. The compound crystallizes in a monoclinic unit cell of P2₁/c symmetry and dimensions, a = 9.832 ± .001 Å, b = 15.398 ± .001 Å, c = 19.762 ± .002 Å, and β= 123.06 ± .01 ° with four molecules per unit cell. The 1633 statistically significant reflections (from a total of 2743 out to 20 = 100°) refined to a final value of R = 0.05₃. The molecule itself consists of a chloride ionically bonded to a cation containing a tetrahedral phosphorus bound to three phenyl rings and a fourth oxazine ring. It is the latter ring which displays extensive derealization as discussed in the paper.     

The crystal and molecular structure of an unusual49 heterocycle,62 2-thia-1,3,5-triaza-7-phosphaadamantane 2,2-dioxide51

The crystal and molecular structure of 2-thia-1,3,5-triaza-7-phosphaadamantane 2,2-dioxide (C₅H₁₀SPO₂N₃) has been determined by single crystal x-ray diffraction techniques. The compound crystallizes in the space group P2₁/c with four formula weights per unit cell of dimensions a = 6.129 (1) Å, b = 12.440 (2) Å, c = 14.028 (2) Å, β = 127.31 (1)°. The structure was solved by direct methods and refined to a final value of R = 0.079.     

Nitrosodicyanmethanid-Komplexe von Palladium(II) und Platin(II)

Crystal and Molecular Structure of 1,8-Dihydroxy-3,6-dithiaoctan-bis-mercury(II) Chloride The crystal structure of 1,8-dihydroxy-3,6-dithiaoctane-bis-mercury(II) chloride has been determined by X-ray crystal structure analysis. The compound crystallizes monoclinic, space group C2/c with a = 15.311(2), b = 5.870(2), c = 17.479(2) Å, β = 102.76° and 4 formula units per unit cell. The structure was solved by heavy atom technique and refined to a final R value of R = 0.050. Mercury is digonally coordinated by an S and a Cl ligator. In consequence of weak interactions to an oxygen atom of the ligand as well as to three further Cl ions the coordination number is increased to six and a strongly distorted octahedron is formed. The crystal structure is built up from polymeric complex molecules.     

The crystal and molecular structure of 3,5-Di-(t-butyl)-1-phenylphosphoryl-4-aza-2,5-cyclohexadiene

The crystal and molecular structure of the title compound (C₁₈H₂₆NOP) has been determined by a single crystal, x-ray diffraction study using Cu-Kα. radiation. The compound was found to crystallize in the orthorhombic space group Pnma with unit cell constants a = 12.686 ± .001 Å, b = 14.776 ± .001 Å, and c = 9.540 ± .001 Å. The structure was solved by the heavy atom method and refined by block-diagonal least-squares to a final R = 0.09₉ for the 696 statistically significant reflections. The compound exhibits orientational disorder in the crystalline state. Nevertheless, the planarity of this ring; the lengthening of the diene carbon-carbon bond to 1.41 Å the resultant shortening of both the carbon-nitrogen bond (1.43 Å) and the carbon-phosphorus bond (1.74 Å), and the CNC bond angle of 121° all strongly support the assumption of delocalization of the diene π-electrons within the heterocyclic ring system.     

Über Chalkogenolate. 131. Untersuchungen über Rhodanine 2. Kristall- und Molekülstruktur von 5-Methylrhodanin

On Chalcogenolates. 131. Studies on Rhodanines 2. Crystal and Molecular Structure of 5-Methyl Rhodanine The title compound crystallizes with Z = 4 in the monoclinic space group P2₁/c with cell dimensions a = 6.087(1), b = 6.846(4), c = 15.336(2) Å, β = 99.85(1)°. The crystal and molecular structure has been determined from single crystal X-ray data at ?25°C and refined to a conventional R of 0.044. The structure consists of discrete 5-methyl-2-thio-4-oxo-thiazolidine molecules, which are linked together by N? H…?O hydrogen bridges. The thiazolidine ring is plane. The compound contains no located double-bonds.     

Kristall- und Molekülstruktur von Bis[N-(diethylaminothiocarbonyl)-benzamidin]silber(l)-nitrat

Crystal and Molecular Structure of Bis[N-(diethylaminothiocarbonyl)-benzamidine]-silver(I) Nitrate The crystal structure of bis[N-(diethylaminothiocarbonyl)-benzamidine]silver(I) nitrate has been determined by X-ray structure analysis on a single crystal. The compound is monoclinic, space group P2₁/n with a = 12.541, b = 43.470, c = 11.096 Å, β = 106.27° and 8 formula units per unit cell. The structure was solved by application of direct methods to difference structure factors (DIRDIF) and refined for 5242 observed reflections to a final R value of R = 0.070. There are two symmetrically independent molecules of the title compound in the asymmetric unit. The central Ag ion is coordinated by the S atoms of two ligands. The nitrate ions do not coordinate. The coordination geometry is slightly bent.     

The crystal and molecular structure of |2-keto-|7-deoxo-8-azacstrone methyl ether hydrohromide

The crystal and molecular structure of 12-keto-17-deoxo-8-azaeslrone methyl ether hydro-bromide (C₁₈H₂₄BrNO₂) has been determined by a single crystal, x-ray diffraction study. The compound crystallizes in the monoclinie space group P2₁/n with unit cell constants a = 12.024 (2), b = 10.340 (1), c = 14.269 Å (2), β = 104.12° (1). The structure was solved by the heavy atom method and refined by block-diagonal least-squares to a final R-value = 0.03₆ for the 8.35 independently measured, statistically significant reflections. All hydrogen atoms, including methyl hydrogens, were located.     

微波辐照下4-苯基-7,7-二甲基-2,5-二氧代-1,2,3,4,5,6,7,8八氢喹啉的合成和晶体结构

标题化合物C1 7H1 9NO2 是由苯甲醛、5,5 二甲基 1 ,3 环己二酮、丙二酸亚异丙酯及醋酸铵在微波辐照下干反应而得。结构通过单晶X 射线衍射法确定 ,其晶体属于单斜晶系 ,空间群P2 1 /a ,a =7.52 4 (2 ) ,b =2 2 .483(3) ,c =9.2 73(2 ) ,β =1 1 3 0 4 (2 )°,V =1 44 3.7(5) 3,Mr=2 69.34,Dc=1 .2 39g/cm3,Z =4,μ(MoKα) =0 81cm- 1 ,F(0 0 0 ) =576,在 6 <2θ <51 0°范围内收集 2 994个独立衍射点 ,其中可观测衍射点 2 0 91个 [I >2 .50σ(I) ]。晶体结构用直接法解出 ,经用全矩阵最小二乘法对原子参数进行修正 ,最后的偏离因子为R =0 .0 4 4 ,Rw=0 .0 58。在晶体结构中 ,O(3) -C(9) -C(4) -C(5) -N(1 )构成一个平面 ,该平面与苯环的二面角为 84.2 5°     

Über Chalkogenolate. 143 [1]. Untersuchungen über Guanidinodithioformiate 5. Kristall- und Molekülstruktur vom S-Methylester der Guanidinodithioameisensäure [2]

On Chalcogenolates. 143. Studies on Guanidinodithioformates. 5. Crystal and Molecular Structure of the S-Methyl Ester of Guanidinodithio Formic Acid The title compound crystallizes with Z = 4 in the monoclinic space group P2₁/c with cell dimensions a = 8.701(5), b = 11.426(8), c = 8.221(4) Å, ß = 125.7(1)°. The crystal and molecular structure has been determined from single crystal X-ray data at 20°C and refined to a conventional R of 0.032 (R_w = 0.039). The structure consists of isolated molecules, which exist as E conformers. The molecules have delocated double-bonds and are linked together by S…?H? N hydrogen bridges.     

Electrochemical synthesis of metal complexes of schiff bases: The crystal structure of bis{2-[(4-methylphenyl)iminomethyl]pyrrolato}copper(II)

The electrochemical oxidation of anodic nickel, copper, zinc or cadmium in acetonitrile solutions of Schiff bases (HL) derived from H-pyrrole-2-carbaldehyde and substituted anilines gives compounds of general formula ML₂. The crystal structure of bis{2-[(4-methylphenyl)iminomethyl]pyrrolato}copper(II) has been determined by X-ray diffraction. The compound crystallizes in the monoclinic space group P2₁/n with a = 9.356(2), b = 16.697(2), c = 14.145(2) Å and β = 108.47(2)°. The crystal structure consists of monomeric molecules in which the central CuN₄ unit has distorted square-planar geometry with a dihedral angle of 25.8(3)° between the coordination planes. The IR, ¹H NMR and UV-visible spectra of the complexes are discussed and related to the structure.     

The crystal and molecular structure of 6-oxadihydrouracil

The crystal and molecular structure of 6-oxadihydrouracil (C₃H₄N₂O₃) has been determined by single crystal x-ray diffraction techniques. The compound crystallizes in the space group P2₁ 2₁ 2₁ with four molecules in a unit cell of dimensions: a = 5.106(1)Å, b = 12.461(2)Å and c = 7.112(1)Å. The structure was solved by direct methods and refined to a final value of R = 0.052. The oxauracil ring is non-planar with the C5 atom assuming tetrahedral geometry and the ring oxygen having oxazinal distances and angle (C-O = 1.43₂Å, N-O = 1.40₈Å, and CON angle of 109.0°). The usual hydrogen bonding patterns associated with the uracil ring are absent in this compound.     

1－苯基－3－甲基－4－（6－氢－4－氨基－5－硫杂－2，3－吡嗪）－吡唑啉酮光致变色超分子化合物的合成、结构与性能

通过1－苯基－3－甲基－4－氯乙酰基－吡唑啉酮－5（PMCP）和氨基硫脲（ TSC）缩合，形成了一种含NNS六元杂环的光致变色化合物（PMCP－TSC）。利用元 素分析，MS，”1H NMR，IR和UV光谱进行了表征。通过紫外可见光谱对它的光致 变色性质进行了研究，测出了光致变色反应的动力学常数。并用X线单晶衍射仪测 定了PMCP－TSC变色后的晶体结构，该晶体属单斜晶系，具有P2_1/c空间群，a = 0.105 10(2) nm, b = 0.150 61(3) nm, c = 0.993 70(10) nm, β = 107.890 (10)°, V = 1.496 9(4) nm~3, Z - 4, D_c = 1.417 Mg/m~3, μ = 0.232 mm~(- 1), F(000) = 672, R = 0.033 4, wR = 0.089 6。结构分析表明：其光致变色现 象是由于它在溶剂与光的共同作用下发生了从醇式到酮式的异构化。同时该化合物 经分子间氢键形成二聚体，又通过甲醇与本体分子之间的氢键使化合物形成具有三 维网络结构的超分子化合物。     

4-(2'-羟基苯甲酰肼)苯亚甲基／亚乙基－5－甲基－2－苯基－2，4－二氢－吡唑啉酮－3超分子化合物的合成与晶体结构

报道了4-(2'－羟基苯甲酰肼)苯亚甲基－5－甲基－2－苯基－2，4－二氢－吡 唑啉酮－3（B_1）和4-(2'－羟基苯甲酰肼)亚乙基－5－甲基－2－苯基－2，4－二 氢－吡唑啉酮－3（B_2）的合成、表征及晶体结构分析，B_1晶体属单斜晶系， C2/c空间群，所得晶胞参数为：a = 1.4201(2) nm, b = 1.65542(2) nm, c = 1. 8455(3) nm, β = 101.32(1)°，V = 4.2541(10) nm~3, Z = 8, D_c = 1.344 g/cm~3, μ = 0.094 mm~(-1), F(000) = 1808, R = 0.0442, wR = 0.1037。该 化合物由水分子通过氢键连接成沿ac面无限延伸的二维网络结构的超分子。B_2晶 体属三斜晶系，P1空间群，a = 1.2120(2) nm, b = 1.2223 (2) nm, c = 1.4159 (3) nm, α = 70.38 (1)°, β = 74.91 (1)°, γ = 63.64(1)°, V = 1.7549 (5)° nm~3, Z = 4, D_c = 1.326 g/cm~3, μ = 0.092 mm~(-1), F(000) = 736, R = 0.0436, wR = 0.1076。此化合物通过分子间氢键形成沿α轴无限延伸的一维 链状结构的超分子，由于分子间的作用力使其分子又沿b轴呈层状堆积。     

(QuinH)_3〔Mo(i-mnt)_4〕的晶体和分子结构

(QuinH)_3 [Mo(i-mnt)_4]为黑色柱状晶体(式中Qui=喹啉 难溶于水,在空气中很稳定。晶体属单斜晶系,空间群Cc,晶胞参数:a=10.688(16),b=31.545(5),c=14.682(26),B=109.28(14)°;ρobs=1.50克/厘米~3,Z=4(ρcalc=1.489克/厘米~3)。晶体在CAD-4衍射仪上,用Mo-Kα射线,θ-2θ扫描方式,在1°<θ<23°范围内收集了4275个独立衍射点。晶体结构用Patterson函数法和Fourier合数法解出,经全矩阵最小二乘方修正,偏离因子R=0.075。结构分析结果说明Mo原子与四个双齿螯合配位基的八个硫原子形成近似于D_(2d)对称性的十二面体结构。     

Die Kristallstruktur von CuBr · (C2H5)4P2

The crystal structure of CuBr · (C₂H₅)₄P₂ has been determined by single crystal X-ray methods. The crystals are triclinic (space group P 1 ) with two formula units per unit cell (a) = 9,29, b = 9,92, c = 7,57 Å, α = 85,3°, β = 106,6°, γ = 109,1°. The copper atoms are tetrahedrally coordinated by two bromine and two phosphorus atoms (of different biphosphine molecules). The structure has continuous chains running parallel c, in which the copper atoms are linked together by alternating double bridges consisting of two biphosphine molecules and two bromine atoms, respectively.     

The molecular structure of 1,1-dimethyl-3-phenylpyrazolium-5-oxide

The molecular structure of 1,1-dimethyl-3-phenylpyrazolium-5-oxide has been determined by a single crystal x-ray diffraction study. The crystals are monoclinic, space group P2₁/a, with unit cell dimensions a = 12.630 (5) Å, b = 6.644 (1) Å, c = 12.486 (5) Å, β = 99.17 (2)°. The final R value was 0.049 for 2930 reflections. The bond lengths and angles suggest that a significant contribution to the structure is made by a resonance form in which one of the ring bonds does not exist. No close intermolecular approaches were found.     

The crystal structure and conformation of 15-phenyl-bicyclo[10.3.0]pentadec-1(12)-en-13-one

The title compound has been synthesized and its crystal structure determined by X-ray crystallographic method. The crystal is monoclinic, space group C2/c, with unit cell dimensions a=19.260 (3), b=11.217 (1), c=15.997 (1) Å; β=92.08 (2)° and Z=8. This is the first crystal structure determined in the series of bicyclo[10.3.0]pentadec-1(12)-en-13-one derivatives. The structure and the conformation of the cis-cyclododecene moiety in this compound is demonstrated to be closely similar to the lowest energy conformer [lene 2333].