Polysulfonylamine, LVIII [1] Erhaltung der Konformation des unkomplexierten Koronanden in einem supramolekularen 18-Krone-6-Komplex: Darstellung und Kristallstrukturen von 18-Krone-6-Dimesylamin (3/2) und von zwei Modifikationen des freien Dimesylamins / Polysulfonylamines, LVIII [1] Conservation of the Conformation of the Uncomplexed Coronand in a Supramolecular 18-Crown-6 Complex: Formation and Crystal Structures of 18-Crown-6-Dimesylamine (3/2) and of Two Modifications of Free Dimesylamine

1994 ◽  
Vol 49 (8) ◽  
pp. 999-1011 ◽  
Author(s):  
Armand Blaschette ◽  
Peter G. Jones ◽  
Karin Linoh ◽  
Ilona Lange ◽  
Martina Näveke ◽  
...  
Keyword(s):  
Hydrogen Bond ◽  
Guest Molecule ◽  
Three Dimensional ◽  
Molar Ratio ◽  
Monoclinic Space Group ◽  
Monoclinic System ◽  
Space Group ◽  
Guest Species ◽  
Dimensional Network ◽  
Oxygen Atoms

The title compound 1 is an unprecedented example of an 18-crown-6 complex in which coronand rings preserve the conformation of the uncomplexed crystalline polyether. 1 is precipitated, independently of the molar ratio employed, by mixing methanolic solutions of its components at room temperature. The complex crystallizes in the monoclinic system, space group P21/n, with (at -130°C) a = 1771.9(7). b = 833.3(3), c = 2024.2(6) pm, β = 107.13(3)°, V = 2.856(2) nm3, Z = 4. Dϰ = 1.325 Mg m-3. The structure contains infinite chains of alternating host and guest species, in which every HN(SO2CH3)2 guest is linked via C-H ··· O(crown) and C-H ··· O(sulfonyl) interactions with two D3d-pseudosymmetric crown rings. Within the chain, each D3d ring acts as an acceptor in six C-H ··· O(crown) and as a donor in four C-H -O(sulfonyl) interactions. Equivalent molecules in the chain are related by v-translation. Pairs of antiparallel chains are connected into ladder-like strands by a sec­ond type of 18-crown-6 molecule that crystallographically preserves the centrosymmetric C′i conformation of the uncomplexed polyether. These rings accept, via their two symmetry- related pseudocorner oxygen atoms, an N-H ··· O hydrogen bond (H ··· O 210 pm) from one guest molecule in each chain and are also connected to the same guests by a C-H ··· O(sulfonyl) interaction. Parallel strands are linked through C-H- (crown) ··· O(sulfonyl) and C-H(crown) ··· O(crown) interactions to form a three-dimensional network. The H ··· O distances of the strand-building and the strand-connecting C-H ··· O interactions lie in the range 230-260 pm. For comparison, two modifications of the pure guest compound, crystallized from CCl4 (modification 2a) or CH2Cl2 (modification 2b), were structurally characterized. The crystallographic data (at -95 °C) are for 2a: monoclinic, space group P21/c, a = 767.5(2), b = 974.5(2), c = 915.0(3) pm, β = 105.80(2)°, V = 0.6585(3) nm3, Z = 4, Dϰ = 1.747 Mg m-3; for 2b: monoclinic, space group P21/c, a = 776.2(3), b = 997.1(3), c = 923.0(4) pm, β = 111.10(3)°, V = 0.6665(4) nm3. Z = 4, Dϰ = 1.726 Mg m 3. In both modifications, the molecules are connected by an N-H ··· O hydrogen bond (H ··· O 234 pm in 2a, 220 pm in 2b) into chains in the z-direction, the principal difference between 2a and 2b arising from the differing conformational character of the acceptor oxygen atoms. Corresponding bond lengths and bond angles in 2a and 2b and in the guest molecule of 1 are essentially identical, as are the torsion angles around the S-N bonds in 2a and 2b. The local C1 symmetry of the CO2SNSO2C framework in 2a and 2b changes to an approximate C2 symmetry upon complexation with 18-crown-6. thus optimizing the host-guest comple­mentarity.

Two- and three-dimensional coordination polymers based on zinc(II) and furan-2,5-dicarboxylic acid: structure variation due to metal-to-linker ratio

2018 ◽  
Vol 74 (12) ◽  
pp. 1719-1724 ◽  
Author(s):  
Yimin Mao ◽  
Peter Y. Zavalij
Keyword(s):  
Dicarboxylic Acid ◽  
Coordination Polymers ◽  
Three Dimensional ◽  
Molar Ratio ◽  
Monoclinic Space Group ◽  
Structure Variation ◽  
Space Group ◽  
Hydrogen Bonding Pattern ◽  
Solvent Molecules ◽  
A Chain

Two ZnII-based coordination polymers (CPs) were synthesized by the hydrothermal method, using Zn(NO3)2·6H2O and furan-2,5-dicarboxylic acid (FDCA) in dimethylformamide (DMF) solvent, at 95 °C. Poly[tetrakis(dimethylazanium) [tetrakis(μ2-furan-2,5-dicarboxylato-κ2 O 2:O 5)dizinc(II)]], {(C2H8N)4[Zn2(C6H2O5)4]} n or {[DMA]4[ZnII 2(FDC)4]} n (DMA = dimethylazanium and FDC = furan-2,5-dicarboxylate), (1), was obtained with a 1:1 molar ratio of ZnII and FDCA. It crystallized in the monoclinic space group C2/c. Coordinated by ZnII ions, FDC2− ligands form 21 double-stranded helices propagating along the b axis. The helices are interconnected and extend laterally in the a direction, forming a two-dimensional (2D) sheet-like network. The 2D sheets are stacked along the c direction without interconnections. DMA cations are cocrystallized in (1) and are hydrogen bonded with carboxylate O atoms of the FDC2− ligands. The hydrogen-bonding pattern consists of R 2 2(4) and R 2 2(10) motifs alternating in a chain. Poly[bis(dimethylazanium) [bis(μ4-furan-2,5-dicarboxylato-κO 2:κO 2′:κO 5:κO 5)bis(μ3-furan-2,5-dicarboxylato-κO 2:κO 2′:κO 5)dizinc(II)] dimethylformamide 3.08-solvate], {(C2H8N)2[Zn2(C6H2O5)4]·3.08C3H7NO} n or {[DMA]2[ZnII 3(FDC)4]·3.08DMF} n , (2), was obtained with a 1:2 molar ratio of ZnII and FDCA. It crystallized in the monoclinic space group P21/c, forming a three-dimensional network. The pores are filled with DMA cations and DMF solvent molecules.

Polysulfonylamine, LXIII [1] / Polysulfonylamines, LXIII [1]

1995 ◽  
Vol 50 (1) ◽  
pp. 128-138 ◽  
Author(s):  
Dagmar Henschel ◽  
Armand Blaschette ◽  
Peter G. Jones
Keyword(s):  
Hydrogen Bond ◽  
Phenyl Group ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
Amine Molecule ◽  
Chain Sequence ◽  
O 193 ◽  
Oxygen Atoms

Complexes of Uncharged Molecules, Crystal StructureThe thermally labile ternary complexes 18C6 · 2MeOH · 2 HN(SO2Ph)2 (2a), 18C6 · 2MeOH · 2HN(SO2–C6H4-4-Cl)2 (2b) and 18C6 · 3 MeOH · HN(SO2Me)(SO2Ph) (3) were obtained by co-crystallization of 18-crown-6 (18C6) and the appropriate di(organosulfonyl)amine from methanolic solutions and characterized by low-temperature X-ray diffraction. The crystal structures of 2a (monoclinic, space group P21/n) and 2b (triclinic, space group P1̄) consist of monomeric, centrosymmetric formula units. Each di(arenesulfonyl)-amine molecule is connected to a methanol molecule by an N-Η ··· O hydrogen bond (H ··· O 203 pm in 2a, 190 pm in 2b). The methanol molecules are linked to three alternate crown oxygen atoms via one O-Η ··· O(crown) hydrogen-bond and two weaker C-Η ··· O(crown) interactions (OH ··· O 201 pm in 2a, 186 pm in 2b; CH ··· O 236 and 247 pm in 2a, 240 and 254 pm in 2b); two symmetry-related oxygen atoms of the crown are involved in O-Η ··· O and the other four in C-Η ··· O interactions. The structure of complex 3 (monoclinic, space group P21) is built of infinite chains parallel to [101]. The methyl group of the di(organosulfonyl)amine is bonded by C-Η ··· O(crown) interactions to a set of three alternate oxygen atoms of the cyclic polyether (H ··· O 228, 245 and 247 pm). Starting from the acidic NH function, a sequence of three methanol molecules catenated by hydrogen bonds curves around the bulky phenyl group and links with its terminal MeOH through one O-H ··· O(crown) and two C-Η ··· O(crown) bonds to the second set of alternate oxygen atoms in the adjacent symmetry-equivalent crown (OH ··· O 193 pm, CH ··· O 248 and 250 pm). Within the chain sequence N-H ··· O′(Me)H′ ··· O″(Me)H″ ··· O‴(Me)H, the H ··· O distances are H ··· O′ 184, H′ ··· O″ 189 and H″··· O‴ 183 pm. In the structures of 2a, 2b and 3, the crown rings adopt the frequently observed D3d pseudosymmetry.

scholarly journals Synthesis and Crystal Structure of the New Telluric Acid Adduct (RbCl)3·Te(OH)6

2012 ◽  
Vol 67 (1) ◽  
pp. 1-4
Author(s):  
Dirk Mahlmeister ◽  
Elisabeth Irran
Keyword(s):  
Crystal Structure ◽  
Three Dimensional ◽  
Molar Ratio ◽  
X Ray Diffraction ◽  
Tellurium Atom ◽  
Synthesis And Crystal Structure ◽  
Dimensional Network ◽  
Tricapped Trigonal Prism ◽  
Acid Adduct ◽  
Oxygen Atoms

The new telluric acid adduct (RbCl)3 ・ Te(OH)6 was prepared by dissolving RbCl and Te(OH)6 in the molar ratio of 3 : 1 in deionized water at r. t. and slow evaporation of the solvent in air. The crystal structure of the colorless crystals was determined with single-crystal X-ray diffraction (trigonal space group: R3̄c (no. 167), a = 14.4392(8), c = 10.4301(16) Å , Z = 6). In (RbCl)3 ・ Te(OH)6, the rubidium atom is surrounded by five chlorine and four oxygen atoms in form of an irregular tricapped trigonal prism. Each tellurium atom is octahedrally surrounded by six oxygen atoms. The Te(OH)6 octahedra and the RbCl5O4 polyhedra are linked to a dense three-dimensional network which is additionally strengthened by hydrogen bonds.

Synthesis and Characterization of the Manganese Borate α-MnB2O4

2011 ◽  
Vol 66 (9) ◽  
pp. 882-888
Author(s):  
Stephanie C. Neumair ◽  
Lukas Perfler ◽  
Hubert Huppertz
Keyword(s):  
High Pressure ◽  
Three Dimensional ◽  
Lattice Parameters ◽  
Synthesis And Characterization ◽  
Manganese Ions ◽  
Space Group ◽  
Dimensional Network ◽  
Oxygen Atoms

The high-pressure manganese borate α-MnB2O4 was synthesized under high-pressure/hightemperature conditions of 6.5 GPa and 1100 ◦C in a modified Walker-type multianvil apparatus. The monoclinic compound is isotypic to α-FeB2O4, CaAl2O4-II, CaGa2O4, andβ -SrGa2O4 crystallizing with eight formula units in the space group P21/c (Z = 8) with the lattice parameters a = 712.1(2), b = 747.1(2), c = 878.8(2) pm, β = 94.1(1)◦, V = 0.466(1) nm3, R1 = 0.0326, and wR2 = 0.0652 (all data). The compound is built up from layers of “sechser” rings of corner-sharing BO4 tetrahedra that are interconnected to a three-dimensional network. The manganese ions are coordinated by seven oxygen atoms and situated in channels along the a axis.

Die Kristallstruktur von Zinkformiat-Dihydrat

1977 ◽  
Vol 145 (5-6) ◽  
Author(s):  
N. Burger ◽  
H. Fuess
Keyword(s):  
Hydrogen Bonding ◽  
Three Dimensional ◽  
Dimensional Structure ◽  
Water Molecules ◽  
Monoclinic Space Group ◽  
Space Group ◽  
Three Dimensional Structure ◽  
Oxygen Atoms

AbstractZinc formate cristallizes isomorphous to the formates of Mg, Sr, Cd, Mn and Ni in the monoclinic space groupThe structure has been refined including an isotropic extinction correction toThe octahedra of the two nonequivalent zinc atoms are slightly distorted. Zn(l) in (000) is surrounded by six oxygen atoms of the formate groups [distances Zn(l)–O = 2.071 Å–2.145 Å]; the octahedron of Zn(2) in (½½0) consists of the oxygen atoms of the two formate groups and two water molecules [distances Zn(2)–O = 2.053 Å–2.165 Å].The three-dimensional structure is stabilized by hydrogen bonding between formate groups and water molecules.

CsPr2(CH3COO)7, ein caesiumarmes wasserfreies ternäres Caesium-Praseodym-Acetat / CsPr2(CH3COO)7, a Cesium Poor Anhydrous Ternary Cesium Praseodymium(III) Acetate

1993 ◽  
Vol 48 (7) ◽  
pp. 886-892 ◽  
Author(s):  
Adalbert Lossin ◽  
Gerd Meyer
Keyword(s):  
Crystal Structure ◽  
Acetic Acid ◽  
Acid Solution ◽  
Single Crystals ◽  
Acetic Acid Solution ◽  
Three Dimensional ◽  
Molar Ratio ◽  
Triclinic System ◽  
Dimensional Network ◽  
Oxygen Atoms

Single crystals of CsPr2(CH3COO)7 were obtained from an acetic acid solution of Pr(CH3COO)3 • H2O and Cs2CO3 in a molar ratio of 4:1 at 120°C. It crystallizes in the triclinic system, PĪ (no. 2), Z = 2, a = 1028.1(5), b = 1034.6(5), c = 1199.4(6) pm, α = 84.82(2), β = 67.07(3), γ = 76.01(2)°, Vm = 343.3(3) cm3/mol, R = 0.031, Rw = 0.027. The crystal structure contains infinite chains, 1∞[Pr2(CH3COO)6], running along the [110] direction. The chains are built up by bridging acetate ions coordinated to two crystallographically different Pr3+ ions which are both surrounded by 9 oxygen ligands. These chains are linked by “intercalated” Cs(CH3COO) to layers parallel (100). Cs+ has contacts to oxygen atoms of neighbouring layers, such that a three-dimensional network is formed.

Crystal Structures of mer-Cr(pyridine)3(N3)3 and Polymeric NaCr(pyridine)4(N3)4. A Structure Containing μ(1,3) Bridging Azido Ligands between Chromium-and Sodium-Centered Polyhedra

1992 ◽  
Vol 47 (1) ◽  
pp. 139-143 ◽  
Author(s):  
Mohamed A. S. Goher ◽  
Morsy A. M. Abu-Youssef ◽  
Franz A. Mautner
Keyword(s):  
Three Dimensional ◽  
Sodium Cation ◽  
Monoclinic Space Group ◽  
Bridging Ligands ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray Crystallography ◽  
Pyridine Ligands ◽  
Sodium Cations ◽  
Dimensional Network

The structures of mer-Cr(py)3(N3)3 (1) and polymeric NaCr(py)4(N3)4 (2) were determined by X-ray crystallography. Crystal data; 1, C15H15N12Cr, triclinic, space group P1̄, a = 895.3(2), b = 999.1(3), c = 1269.9(5) pm , α = 106.76(3), β = 96.69(3), γ = 116.30(2)°, V = 943.8(6) · 106 pm3, Z = 2 and Rw = 0.038 for 1736 observed MoKα diffractometer data; 2, C20H20N16CrNa, monoclinic, space group C2/c, a = 1561.2(3), b = 1028.8(2), c = 1573.6(4) pm, β = 90.70(2)°, V = 2 527.3(9) · 106 pm3, Z = 4 and = 0.033 for 1272 MoKα diffractometer data.The coordination around the chromium (III) ion in the discrete molecules of 1 is six-coordinate with mean distances Cr-N(py) of 210.2(4) pm and Cr-N(N3) of 200.8(4) pm. The terminal azido ligands are almost linear and asymmetric, the N-N bonds nearer to the metal (118.8(6) to 120.5(7) pm) being significantly longer than the terminal ones (114.7(7) to 115.5(7) pm). In compound 2, each chromium or sodium cation is six-coordinated by four azido groups and two pyridine molecules. The azido groups act as μ(1,3) bridging ligands between chromium and sodium octahedra to form a three-dimensional network structure. The chromium atoms are trans-coordinated by the pyridine ligands whereas the sodium cations are cis-coordinated.

The crystal and molecular structure of scandium formate

1990 ◽  
Vol 55 (2) ◽  
pp. 426-434 ◽  
Author(s):  
Jindřich Hašek ◽  
Jan Ondráček ◽  
Pavel Karen ◽  
Jaroslav Bauer
Keyword(s):  
Molecular Structure ◽  
Hydrogen Bond ◽  
Raman Spectra ◽  
Crystal And Molecular Structure ◽  
Three Dimensional ◽  
Ir And Raman Spectra ◽  
Octahedral Coordination ◽  
Monoclinic System ◽  
Space Group ◽  
Ir And Raman

The structure of Sc(HCOO)3 was refined up to R = 0.046. The substance crystallizes in the monoclinic system, space group P21/c, a = 10.340(2), b = 6.631(1), c = 9.027(2) Å, β = 98.11(2)°, Z = 4. Scandium atoms are placed in the two symmetrically non-equivalent centres of symmetry thus forming alternating layers parallel to the plane of b,c. All formate oxygens are coordinated to Sc atoms thus forming a three-dimensional net with octahedral coordination of both independent Sc atoms. C-H bonds are oriented in between the nearest oxygens of neighbouring formate groups, but only one contact is sufficiently short to be denoted as the C-H···O hydrogen bond. IR and Raman spectra seem to confirm the differences between formate anions.

Inclusion of 4,4'-Bipyridine (γbpy) in Its Copper(II) Aqua Perchlorato Complex. Crystal Structure of [Cu( γbpy )(H2O)2(ClO4)2]n.( γbpy )n

1996 ◽  
Vol 49 (7) ◽  
pp. 835 ◽  
Author(s):  
XM Chen ◽  
ML Tong ◽  
YJ Luo ◽  
ZN Chen
Keyword(s):  
Crystal Structure ◽  
Three Dimensional ◽  
Water Molecules ◽  
Monoclinic Space Group ◽  
Two Dimensional ◽  
Octahedral Environment ◽  
Dimensional Network ◽  
Complex Crystal Structure ◽  
Complex Crystal ◽  
Oxygen Atoms

An example of a 4,4'-bipyridine ( γbpy ) clathrate in its copper(II) complex has been established. The compound, [Cu( γbpy )(H2O)2(ClO4)2]n.( γbpy )n, crystallizes in the monoclinic space group C2/c with a 16.651(3), b 11.089(2), c 14.360(3) Ǻ, β 116.45(3)°, V 2373.9(8)Ǻ3. The crystal structure comprises γbpy -bridged linear polymeric [Cu( γbpy )(H2O)2(ClO4)2]n chains, where the copper atom, located on a crystallographic twofold axis, is coordinated in an elongated octahedral environment by two nitrogen atoms of the bridging γbpy ligands (Cu-N 1.998(4)Ǻ) and two water molecules (Cu-O 1.968(3)Ǻ) at the equatorial positions, and two perchlorate oxygen atoms at the axial positions (Cu-O 2.414(4)Ǻ). The chains are interconnected by hydrogen bonds between the aqua ligands and the uncoordinated perchlorate oxygen atoms to form two-dimensional layers with cavities each enclosing a γbpy molecule. Hydrogen bonding between the aqua ligands and the nitrogen atoms of the solvate γbpy molecules further extends the structure into a three-dimensional network in the solid.

scholarly journals Crystal Structure Investigation of Two Polymeric Chromium(III) Azide Complexes; KCr(pyridine)4(N3)4 and RbCr(pyridine)3(N3)4. A Structure Containing μ(l,3) and μ(1,1,3) Bridging Azido Ligands between Chromium and Rubidium Centered Polyhedra

1992 ◽  
Vol 47 (12) ◽  
pp. 1754-1758 ◽  
Author(s):  
M. A. S. Goher ◽  
M. A. M. Abu-Youssef ◽  
F. A. Mautner ◽  
H. P. Fritzer
Keyword(s):  
Crystal Structure ◽  
Three Dimensional ◽  
Monoclinic Space Group ◽  
Coordination Geometry ◽  
Space Group ◽  
X Ray ◽  
X Ray Crystallography ◽  
Pyridine Ligands ◽  
Dimensional Network ◽  
Distorted Octahedral

The structures of two polymeric complexes of chromium(III) azide with pyridine, KCr(py)4(N3)4 (1), and RbCr(py)3(N3)4 (2), were determined by X-ray crystallography. Crystal data: 1, C20H20N16CrK, monoclinic, space group C2/c, a = 1611.2(5), b = 1050.6(3), c = 1609.0(5) pm, β = 91.69(3)°, Ζ = 4 and Rw = 0.037 for 923 diffractometer data; 2, C15H15N15CrRb, monoclinic, space group P21/n, a = 1311.9(3), b = 1139.0(4), c = 1523.3(4) pm, β = 109.39(2)°, Ζ = 4 and Rw = 0.046 for 2336 data.The crystal structure of 1 contains six-coordinated chromium and potassium cations with two pyridine ligands and four µ(1,3) bridging azido groups forming a three-dimensional network structure. The chromium atoms are trans-coordinated by the pyridine ligands, whereas the potassium cations are cis-coordinated. The polymeric complex 2 features di-µ(l,1,3) azido bridged CrRbN2 rings, distorted octahedral chromium(III) coordination geometry, sevencoordinated rubidium, and di-μ(1,3) azido bridges which link the binuclear RbCr(pyridine)3(N3)2 moieties into infinite chains parallel to the b axis.

Sign in / Sign up

Export Citation Format

Share Document