Synthesis of a Cis-N2s2 Donor Macrocycle by Metal-Directed Condensation of Formaldehyde, Nitroethane and a Diaminodithiaalkane - Crystal-Structure of the (6-Methyl-6-Nitro-1,11-Dithia-4,8-Diazacyclotetradecane)-Copper(II) Perchlorate Product

1988 ◽  
Vol 41 (5) ◽  
pp. 773 ◽  
Author(s):  
P Comba ◽  
GA Lawrance ◽  
M Rossignoli ◽  
BW Skelton ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Structural Properties ◽  
Copper Ion ◽  
Macrocyclic Complex ◽  
High Yield ◽  
Monoclinic Space Group ◽  
Space Group ◽  
Complex Ion ◽  
Perchlorate Salt

Reaction of (3,7-dithianonane-1,9-diamine)copper(II) ion with nitroethane and formaldehyde in basic methanol gives the macrocyclic complex ion (6-methyl-6-nitro-1,II-dithia-4,8- diazacyclotetradecane )copper(II) in high yield. The complex as the perchlorate salt crystallizes in the monoclinic space group P21/n, a 15.008(5), b 8.606(3), c 17.967(4)Ǻ, β 113.79(2)�. The copper ion lies in a square plane of two nitrogen (average Cu-N 2.02 Ǻ) and two thioether (average Cu-S 2.295 Ǻ) donors, with perchlorate oxygens (Cu-O 2.46 and 2.70 Ǻ) in axial sites. Physical and structural properties of the CuIII complexes of the 14-membered cis-N2S2 macrocycle and the known analogous 14-membered N4-donor macrocycle 6-methyl-6-nitro-1,4,8,11- tetraazacyclotetradecane are compared.

Copper(II) and Cobalt(III) Complexes of a Mixed Secondary and Tertiary Nitrogen Donor Tetraaza Macrocycle. Crystal Structure of Aqua(7-methyl-7-nitro-1,5,9,13-tetraaza-bicyclo[11.2.2]heptadecane)copper(II) Perchlorate Hydrate

1989 ◽  
Vol 42 (11) ◽  
pp. 1859 ◽  
Author(s):  
LM Engelhardt ◽  
GA Lawrance ◽  
TM Manning ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Copper Ion ◽  
Chloride Ion ◽  
Macrocyclic Complex ◽  
High Yield ◽  
Tetraaza Macrocycle ◽  
Orthorhombic Space Group ◽  
Nitrogen Donor ◽  
Perchlorate Salt ◽  
Tertiary Nitrogen

Reaction of (bis(3-aminopropyl) piperazine )copper(11) ion with nitroethane and formaldehyde in basic methanol results in the ready formation of (7-methyl-7-nitro-1,5,9,13- tetraazabicyclo [11.2.2] heptadecane )copper(11) ion in high yield. The perchlorate salt of the macrocyclic complex crystallizes in the orthorhombic space group Pbca, a 19.144(8), b 17.499(5), c 14.635(5) �, Z=8, with the copper ion in a square-pyramidal environment of four nitrogen donors and a water molecule. The Cu-secondary N and Cu-tertiary N distances are 2.044(8), 2.056(8) and 2.053(8), 2.072(8) � respectively, with the Cu-O distance 2.259(8)�. Reduction of the complex with Zn/ HCl yields the 7-methyl-1,5,9,13-tetraazabicyclo [l1.2.2]heptadecane-7-amine analogue, characterized as copper(II) and cobalt(III) complexes. The cobalt(III) complex contains the latter macrocycle as a quinquedentate ligand with the pendant primary amine coordinated trans to a chloride ion, identified as the only isomer by chromatography, and characterized by electronic and n.m.r. spectroscopy. Consequences of 'reinforcement' of the macrocycle by the extra ethane bridge are discussed.

Facile Metal-Directed Synthesis and Crystal Structure of a New Amino Acid Ester, Methyl 3-[(2-Aminoethyl)amino]-2-[(2-aminoethyl)aminomethyl]propionate, as the Copper(II) Complex

1990 ◽  
Vol 43 (2) ◽  
pp. 399 ◽  
Author(s):  
PV Bernhardt ◽  
GA Lawrance ◽  
BW Skelton ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Amino Acid ◽  
Acid Ester ◽  
Copper Ion ◽  
Diethyl Malonate ◽  
Amino Acid Ester ◽  
Monoclinic Space Group ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
Directed Synthesis

Condensation of bis (ethane-1,2-diamine) copper(II) perchlorate with formaldehyde and diethyl malonate in basic methanol generates the new amino acid ester complex (ethyl hydrogen bis [(2-aminoethyl ) aminomethyl ] malonate )copper(II) perchlorate, [Cu(1)] (ClO4)2. Base- catalysed ester hydrolysis and decarboxylation in methanol of[Cu(1)]2+ yields, with reesterification, (methyl 3-[(2-aminoethy )amino]-2-[(2-aminoethyl) aminomethyl ]propionate)copper(II) perchlorate, [Cu(2)](ClO4)2. This complex crystallizes in the monoclinic space group P21/c, a 12.763(6), b 9.176(2), c 16.32(2)Ǻ, β 112.49 (6)°, Z 4, R 0.054 for 2626 independent 'observed' reflections. The copper ion lies in a near plane of four nitrogens with perchlorates occupying axial sites.

The Crystal Structure of Tris(2,2'-bipyridine)ruthenium(II) Perchlorate

1994 ◽  
Vol 47 (4) ◽  
pp. 763 ◽  
Author(s):  
JM Harrowfield ◽  
AN Sobolev
Keyword(s):  
Crystal Structure ◽  
Aqueous Solution ◽  
Single Crystal ◽  
Bond Length ◽  
Monoclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Perchlorate Salt

[Ru ( bpy )3] (ClO4)2 ( bpy = 2,2′-bipyridine) crystallizes from aqueous solution in an anhydrous form as deep red tablets. A single-crystal X-ray study at 293(2) K has shown the material to be monoclinic, space group C 2/c, a 17.633(4), b 10.761(2), c 15.924(4) Ǻ, β 90.77(2)°, V 3021(1) Ǻ3, Z 4; R was 0.034 for 2405 'observed' [I > 3σ(I)] reflections. The [ Ru ( bpy )3]2+ cation in the perchlorate salt shows very closely similar bond length [ Ru -N, 2.056(3)- 2.060(3)Ǻ], angle and torsion characteristics to those of the known hexafluorophosphate salt, though the two salts are not isomorphous.

A New Host Lattice Built of the Werner-Type Copper(I,II) Cyanide Complex Involving a Macrocyclic Ligand

1998 ◽  
Vol 63 (5) ◽  
pp. 622-627 ◽  
Author(s):  
Hidetaka Yuge ◽  
Takayoshi Soma ◽  
Takeshi Ken Miyamoto
Keyword(s):  
Macrocyclic Ligand ◽  
Host Lattice ◽  
Macrocyclic Complex ◽  
Monoclinic Space Group ◽  
Cyanide Complex ◽  
New Host ◽  
Space Group

Crystals of a new clathrate [CuII(hmtd)CuI(CN)3]·CH2Cl2 were afforded from a Me2CO-EtOH-CH2Cl2 solution of a macrocyclic complex CuII(hmtd)CuI(CN)3·2 H2O (hmtd = 5,7,7,12,14,14-hexamethyl- 1,4,8,11-tetraazacyclotetradeca- 4,11-diene). It crystallizes in the monoclinic space group P21/n, a = 7.936(5), b = 18.717(4), c = 17.783(6) Å, β = 98.55(4)°, Z = 4, R = 0.0558 for 1 870 reflections. Unprecedentedly, only one of the three nitrogen-ends of a CuI(CN)3 moiety is coordinated to the square-pyramidal Cu(II) center. The guest CH2Cl2 molecules are captured in the channel between the potlid-shaped [CuII(hmtd)CuI(CN)3] molecules.

scholarly journals Molekül- und Kristallstruktur von 1.1-Dimethylsilylentitanocendichlorid, (CH3)2Si(C5H4)2TiCl2 / Molecular and Crystal Structure of l,r-Dimethylsilylene Titanocene Dichloride, (CH3)2Si(C5H4)2TiCl2

1981 ◽  
Vol 36 (10) ◽  
pp. 1208-1210 ◽  
Author(s):  
Hartmut Köpf ◽  
Joachim Pickardt
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Structure Determination ◽  
Titanocene Dichloride ◽  
Molecular And Crystal Structure ◽  
Monoclinic Space Group ◽  
Crystal Data ◽  
Space Group ◽  
X Ray ◽  
Structural Dimensions

Abstract The molecular structure of the bridged [1]-titanocenophane 1,1'-dimethylsilylene titanocene dichloride, (CH3)2Si(C5H4)2TiCl2, has been investigated by an X-ray structure determination. Crystal data: monoclinic, space group C2/c, Z = 4, a = 1332.9(3), 6 = 988.7(3), c = 1068.9(3) pm, β = 113.43(2)°. The results are compared with the structural dimensions of similar compounds: 1,1'-methylene titanocene dichloride, CH2(C5H4)TiCl2, with the unbridged titanocene dichloride, (C5H5)2TiCl2 and the ethylene-bridged compound (CH2)2(C5H4)2TiCl2

Two lithium tricyanomethanide compounds: syntheses and single-crystal structure determination of LiK[C(CN)3]2 and Li[C(CN)3]·½ (H3C)2CO

2015 ◽  
Vol 70 (3) ◽  
pp. 191-196 ◽  
Author(s):  
Olaf Reckeweg ◽  
Francis J. DiSalvo
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Single Crystals ◽  
Structure Determination ◽  
Monoclinic Space Group ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
Cell Parameters ◽  
New Compounds

AbstractThe new compounds LiK[C(CN)3]2 and Li[C(CN)3]·½ (H3C)2CO were synthesized and their crystal structures were determined. Li[C(CN)3]·½ (H3C)2CO crystallizes in the orthorhombic space group Ima2 (no. 46) with the cell parameters a=794.97(14), b=1165.1(2) and c=1485.4(3) pm, while LiK[C(CN)3]2 adopts the monoclinic space group P21/c (no. 14) with the cell parameters a=1265.7(2), b=1068.0(2) and c=778.36(12) pm and the angle β=95.775(7)°. Single crystals of K[C(CN)3] were also acquired, and the crystal structure was refined more precisely than before corroborating earlier results.

Structure of 3α,4α:5β,6β-Diepoxyandrostan-17-one

1983 ◽  
Vol 36 (11) ◽  
pp. 2333 ◽  
Author(s):  
B Kamenar ◽  
RA Pauptit ◽  
JM Waters
Keyword(s):  
Crystal Structure ◽  
Title Compound ◽  
Direct Methods ◽  
Monoclinic Space Group ◽  
Space Group ◽  
X Ray

The X-ray crystal structure of 3α,4α:5β,6β-diepoxyandrostan-17-one has been determined. Crystals of the title compound (C19H26O3)are monoclinic, space group P21, with a 9.208(2), b 9.620(4), c 9.312(3) �, β 99.14(2)�, V 814.5 Ǻ3 and Z 2. The structure was solved by direct methods and refined to R 0.039 for 887 observed reflexions. The 3α,4α:5β,6β configuration of the epoxide rings confirms the assignment based on proton n.m.r. studies.

Darstellung von Mononitropentahydrohexaborat(2-) und Kristallstruktur von M2[B6H5(NO2)], M = K, Cs / Preparation of Mononitropentahydrohexaborate(2—) and Crystal Structure of M2[B6H5(NO2)], M = K, Cs

1993 ◽  
Vol 48 (12) ◽  
pp. 1727-1731 ◽  
Author(s):  
A. Franken ◽  
W. Preetz ◽  
M. Rath ◽  
K.-F. Hesse
Keyword(s):  
Crystal Structure ◽  
Ion Exchange ◽  
Ion Exchange Chromatography ◽  
Exchange Chromatography ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Dichloromethane Solution ◽  
Space Group ◽  
X Ray ◽  
Diethylaminoethyl Cellulose

By electrochemical oxidation of [B6H6]2- in the presence of nitrite ions and the base DBU in dichloromethane solution mononitropentahydrohexaborate [B6H5(NO2)]2- ions are formed and can be isolated by ion exchange chromatography on diethylaminoethyl cellulose. The crystal structures of the K and Cs salt were determined from single crystal X-ray diffraction analyses. K2[B6H5(NO2)] is monoclinic, space group P21/m with a = 5.953(1), b = 8.059(4), c = 8.906(1) Å, β = 109.553(9)°; Cs2[B6H5(NO2)] is monoclinic, space group P21/a with a = 9.438(6), b = 9.644(7), c = 11.138(9) Å, β = 101.44(9)°. The B6 octahedron is compressed in the direction of the B—NO2 bond by about 5%, with bond lengths between 1.67 and 1.77 A.

Primäre und sekundäre Ethyl-und i-Propylsulfoniumsalze sowie Kristallstruktur von i-C3H7SH2+SbF6- [1]

1996 ◽  
Vol 51 (2) ◽  
pp. 277-285
Author(s):  
Rolf Minkwitz ◽  
Ulrike Lohmann ◽  
Hans Preut
Keyword(s):  
Crystal Structure ◽  
Structure Analysis ◽  
Bond Distance ◽  
Crystal Structure Analysis ◽  
Unit Cell ◽  
Monoclinic Space Group ◽  
Spectroscopic Methods ◽  
Sulfonium Salt ◽  
Space Group

Abstract The synthesis of salts of the type RnSH3-n+MF6- (R = C2H5, i-C3H7; n = 1, 2; M = As, Sb) by protonation of the corresponding thiols and sulfides in the superacid systems HF/MF5 is reported. The salts have been characterized by vibrational and NMR spectroscopic methods. Isopropylsulfonium hexafluoroantimonate is the first known example of a sulfonium salt, for which a SH bond distance has been determined by a crystal structure analysis, i-C3H7SH2+SbF6- crystallizes in the monoclinic space group P21/m with a = 568.0(4), b = 801.1(6), c = 1019.7(8) pm, β = 82.63(6) °, with two formula units per unit cell.

scholarly journals CRYSTAL STRUCTURE OF TRIPHENYLTIN (IV) FORMATE POLYMER, (HCO2SnPh3)n

2020 ◽  
Vol 26 (3) ◽  
pp. 212-217
Author(s):  
MODOU SARR ◽  
MOUHAMADOU BIRAME DIOP ◽  
AMINATA DIASSE-SARR ◽  
AI WANG ◽  
ULLRICH ENGLERT
Keyword(s):  
Crystal Structure ◽  
Infinite Chain ◽  
Monoclinic Space Group ◽  
Space Group ◽  
Axis Direction ◽  
Trigonal Bipyramidal ◽  
Triphenyltin Chloride

The title polymer [HCO2Sn(C6H5)3]n was isolated by serendipitous from reaction in ethanol 96 % between bis-(monocyclohexyl ammonium) 2-carboxyethyl hydrogen phosphonate, {(CyNH3)2[CO2CH2CH2PO2(OH)]} and triphenyltin chloride, SnPh3Cl. The polymer crystallizes in the monoclinic space group P21/n with Z = 4, a = 14.7091 (18) Å, b = 15.4133 (19) Å, c = 14.7639 (18) Å, β = 94.242 (2)° and V = 3338.0 (7) Å3. The structure consists of an infinite chain propagating along the crystallographic a-axis direction with bidentate formate anions. The O2SnC3 core is organized into a trans-trigonal bipyramidal like-arrangement.

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