| | 2 | Author
| HeinzDieter Lutz, SalehM. El-Suradi, Christiane Mertins, Bernward Engelen | Requires cookie* | | | Title
| Zur Kenntnis der Hydrate des Mangan-und Zinksulfits. Röntgenographische, thermoanaly tische, Raman-und IR-spektroskopische Untersuchungen  | | | | Abstract
| X-ray, IR and Raman data as well as thermoanalytical measurements (DTA, TG, and DTG) of several new hydrates, viz. MnS03 • 2 1 /z H20, MnS03 • 2 H20, ZnS03 • 3 H20, /S-ZnS03 • 2 1 /2 H20, and y-ZnS03 • 2 x /2 H20, and of previously reported hydrates in the systems MnS03-H20, ZnS03-H20, and MnS03-ZnS03-H20 are presented. Furthermore, the formation of mixed crystals is studied in the system MnS03-ZnS03-H20. The following crystal data have been determined by single crystal measurements: MnS03 • 2 1 /2 H20 (P4i2i2):a = b = 968.4(1), c = 1040.9(1) pm, Z = 8, MnS03 • 2 H20 (P2i/w):a = 650.9(1), b = 873.8(1), c = 774.7(1) pm, ß = 99.80(1)°, Z = 4, ZnS03 • 3 H20 (Pnma): a = 953.6(1), b = 553.0(1), c = 941.9(1) pm, Z = 4, ß-ZnS03 • 21/2 H20 (P4i2!2): a = b = 952.1(1), c = 1025.4(1) pm, Z = 8, y-ZnS03 • 2 X \2 H20 (with small amount of Mn 2 +) (o-rh.): a = 1493(1), b = 1812(2), c = 753(1) pm, Z = 16, ZnS03 • 1/2 H20 (mon.): a = 1326.7(5), b = 706.3(2), c = 834.4(1) pm, ß = 117.41(3)°, Z = 8. The IR spectra show that, with the exception of y-ZnS03 • 2 x /2 H20, both weak and strong hydrogen bonds are present in the sulfite hydrates. Under an S02 atmosphere the sulfite hydrates can be dehydrated without simultaneous dissociation to the oxide and sulfur dioxide. The isotypic hydrates /?-MnS03 • 3 H20 and ZnS03 • 3 H20 (ß-MnSÖ3 • 3 H20 type), and MnS03 • 2 H20 and ZnS03 • 2 H20 (ZnSe03 • 2 H20 type) form complete mixed crystal series. Solid solutions are also formed from a-MnS03 • 3 H20 (a-FeS03 • 3 H20 type), y-ZnS03 • 2 l /2 H20, MnS03 • 1 H20, and ZnS03 • 1 /2 H20. No incorporation of Mn or Zn could be observed for a-ZnS03 • 2Va H20 and the isotype hydrates MnS03 • 2!/a H20 and ß-ZnS03 • 2 1 /2 H20 (CoS03 • 21/2 H20 type). | | | |
Reference
| Z. Naturforsch. 35b, 808—816 (1980); eingegangen am 17. Dezember 1979 | | | |
Published
| 1980 | | | |
Keywords
| Sulfite, Hydrates, Manganese, Zinc, X-ray | | | |
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| default:Reihe_B/35/ZNB-1980-35b-0808.pdf | | | | Identifier
| ZNB-1980-35b-0808 | | | | Volume
| 35 | |
| 3 | Author
| Christoph Kratky | Requires cookie* | | | Title
| | | | | Abstract
| The crystal structure of Rb2Ca(N3)4-4H20 has been determined by single crystal X-ray methods. The compound is isotypic with K2Ca(N3)4-4H20 and crystallizes in the orthorhombic space group Ccca, Z = 4, a = 1949.1(12) pm, b = 1099.5(3) pm, c — 622.2(1) pm. | | | |
Reference
| Z. Naturforsch. 43b, 497—498 (1988); eingegangen am 23. November 1987/14. Januar 1988 | | | |
Published
| 1988 | | | |
Keywords
| Azide, Calcium, Crystal Structure, Hydrate, Rubidium | | | |
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| default:Reihe_B/43/ZNB-1988-43b-0497_n.pdf | | | | Identifier
| ZNB-1988-43b-0497_n | | | | Volume
| 43 | |
| 4 | Author
| Gerhard Thiele, Dietmar Putzas | Requires cookie* | | | Title
| Antiprismatische und dodekaedrische Oktaaquokationen von Calcium und Strontium in den Kristallstrukturen von Tetrahalogenocadmaten und -mercuraten Antiprismatic and Dodecahedral Oktaaquo Cations of Calcium and Strontium in the Crystal Structures of Tetrahalogeno Cadmates and Mercurates | | | | Abstract
| The tetrahalogenometallates CaHgBr 4 -8H 2 0, CaCdI 4 -8H 2 0 and SrCdI 4 -8H 2 0 which have been obtained by crystallization from aqueous solutions form different structures. The orthorhombic compounds CaHgBr 4 -8H^O (Cmca, a — 1720.1(6) pm, b = 1329.2(4) pm. c = 1369.5(7) pm, Z — 8, R -0.041) and SrCdI 4 -8H 2 0 (Pnma, a = 1404.6(2) pm, b = 1841.1(5) pm. c = 1420.6(3) pm, Z = 8, R = 0.037) are built up from dodecahedral [A(H 2 0) 8 ] cations (A = Ca, Sr) and tetrahedral MX 4 anions (M = Hg, Cd) which are cubic closed packed in a CuAu type structure. The tetragonal structure of CaCdI 4 -8H 2 0 (P4/nbm, a = 1268.14(13) pm, c = 536.96(35) pm. Z = 2, R = 0.034) contains antiprismatic [Ca(H 2 0) x ] 2+ cations and tetrahedral Cdl 4 anions, which form together a tetragonal primitive rod package. | | | |
Reference
| Z. Naturforsch. 43b, 1224—1234 (1988); eingegangen am 9. Juni 1988 | | | |
Published
| 1988 | | | |
Keywords
| Crystal Structure, Hydrates, Cadmium Complexes, Mercury Complexes | | | |
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| default:Reihe_B/43/ZNB-1988-43b-1224.pdf | | | | Identifier
| ZNB-1988-43b-1224 | | | | Volume
| 43 | |
| 5 | Author
| Rolf-Rüdiger Krüger, W. Alter, Abriel | Requires cookie* | | | Title
| Über das Hochdruckverhalten von Gips On the Behaviour of Gypsum under High Pressure | | | | Abstract
| The decom position o f gypsum (dehydration) was studied in the pressure range 7 .5 -6 0 kbar and the temperature range 7 5 -4 0 0 °C using a belt type apparatus. Surprisingly, gypsum is rather stable even at pressures greater than 20 kbar contradicting the results o f a calculation o f the space requirement o f the competing phases (A I I -C a S 0 4 + H-,0; Hemihydrate + H20). Only when rising the temperature, as the most important thermodynamic variable for this reaction, the kinetically controlled decomposition starts. N o acceleration o f the dehydration process under shear stress (simple squeezer device) could be detected due to the limited (not geological) time. | | | |
Reference
| Z. Naturforsch. 45b, 1221—1226 (1990); eingegangen am 27. Februar 1990 | | | |
Published
| 1990 | | | |
Keywords
| Gypsum, Hydrates, High-Pressure, D ecom position | | | |
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| default:Reihe_B/45/ZNB-1990-45b-1221.pdf | | | | Identifier
| ZNB-1990-45b-1221 | | | | Volume
| 45 | |
| 6 | Author
| Crystal, FrankH. Artm Anna, D. Ietrich, M. Ootz, Reinhard Schwesinger | Requires cookie* | | | Title
| Zur Kristallchemie ungeladener Phosphazen-Basen, I [1] Strukturen zweier Hydrate und eines Acetats von Tris(dimethylamino)methyliminophosphoran | | | | Abstract
| C hem istry o f U ncharged Phosphazene Bases, I [ 1 ] Structures o f Two H ydrates and an A cetate o f T ris(dim ethylam ino)m ethylim inophosphorane Two hydrates and an acetate of the uncharged, very strong phosphazene base tris(dimethylamino)methyliminophosphorane, (Me2N)3P=NMe (for short Me-P]), have been characterized by their crystal structures. A monohydrate, Me-P, • H:0 , mp. 3°C, is monoclinic | | | |
Reference
| Z. Naturforsch. 51b, 1369—1374 (1996); eingegangen am 11. März 1996 | | | |
Published
| 1996 | | | |
Keywords
| Crystal Structure, Hydrate, Hydrogen Bonding, Phosphazene, Uncharged Base | | | |
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| default:Reihe_B/51/ZNB-1996-51b-1369.pdf | | | | Identifier
| ZNB-1996-51b-1369 | | | | Volume
| 51 | |
| 7 | Author
| Z. Naturforsch | Requires cookie* | | | Title
| Kristallstruktur von MgS03*H20 | | | | Abstract
| The crystal structure of M g S 0 3 H20 , space group P 2 \ln, Z = 4, Dx = 2.415 g em -3 , a = 4.699(1), b = 12.751(3), c = 5.618(1) Ä, ß = 90.49(3)°, was determined by single crystal X-ray diffraction. M g S 0 3 H20 crystallizes in the M n S 0 3 H20 type. The structure consists of buckled trans layers ^ [M gS03 H20 ], which are built up from strongly distorted M g 0 5(H20) octahedra sharing four equatorial vertices, and of trigonal pyramidal S 0 32-ions. It is close ly related to the structures of orthorhombic M nSe0s3 D 20 and monoclinic Z n S e 0 3 H20 . The M g -0 distances range from 2.051(3) to 2.175(4) A. The S-O distances (1.543(3), 1.547(3) and 1.493(3) Ä) and the O-S-O angles (98.4(2) and 2x 106.0(2)°) correspond to those in M n S 0 3 H20 . The distortion of the M 0 5(H20) octahedra (M = Mg, Mn) and of the S 0 32-ions is smaller in M g S 0 3 H20 , but with greater deviations from m symmetry. The distances between the H-connected ^ [M S 03 H20 ] layers are greater in M g S 0 3 H 20 , indicating weaker inter-layer hydrogen bonds. The lateral arrangement of the 2 [M S 0 3 H20 ] layers is nearly the same in both sulfite monohydrates. E in le itu n g | | | |
Reference
| Z. Naturforsch. 53b, 131—134 (1998); eingegangen am 10. November 1997 | | | |
Published
| 1998 | | | |
Keywords
| X-Ray, Sulfites, Hydrates, Magnesium, Pseudosymmetry | | | |
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| default:Reihe_B/53/ZNB-1998-53b-0131.pdf | | | | Identifier
| ZNB-1998-53b-0131 | | | | Volume
| 53 | |
| 8 | Author
| Dietrich Mootz, D. Agm Ar Boenigk | Requires cookie* | | | Title
| Fluoride und Fluorosäuren, VII [1] Kristallstrukturen von Säurehydraten und Oxoniumsalzen, XXII [2] Hydratbildung der Trifluoressigsäure sowie Strukturen eines Monohydrats und eines Tetrahydrats [3] Fluorides and Fluoro Acids, VII [1] Crystal Structures of Acid H ydrates and Oxonium Salts, XXII [2] H ydrate Form ation of Trifluoroacetic Acid and Structures of a M onohydrate and a Tetrahydrate [3] | | | | Abstract
| The liquidus and solidus lines of the quasi binary system CF3C O O H —H20 were determined by low temperature difference thermal analysis and the resulting phase relations controlled by X-ray powder diffraction. Formation of a monohydrate and a tetrahydrate, melting congruently at —43 and —16 °C, respectively, is confirmed. In addition a metastable form of the monohydrate and a low temperature form of the tetrahydrate, stable below —47 °C, are indicated. The crystal struc tures of the stable high temperature forms were determined. From these the monohydrate (tetra gonal, space group I42d, Z = 16) is a true acid hydrate, C F ,C 0 0 H H 20 . and the tetrahydrate (triclinic, P I, Z -2) a hydrated oxonium salt, (H 50 2) + [H(CF3COO)2]~ • 6 H:0 . | | | |
Reference
| Z. Naturforsch. 39b, 298—3 (1984); eingegangen am 8. November 1983 | | | |
Published
| 1984 | | | |
Keywords
| Trifluoroacetic Acid, Hydrates, Phase Diagram, Crystal Structure, Hydrogen Bonding | | | |
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| default:Reihe_B/39/ZNB-1984-39b-0298.pdf | | | | Identifier
| ZNB-1984-39b-0298 | | | | Volume
| 39 | |
| 9 | Author
| Antje Albert, D. Ietrich, M. Ootz | Requires cookie* | | | Title
| Formation and Crystal Structures of the Hydrates of 18-Crown-6 [1] | | | | Abstract
| The melting diagram of the system 18-crown-6/water has been set up and the existence of four binary hydrates confirmed. Crystal structures have been determined for three of these, in addition to that for the hexahydrate already published. The hydrates are monoclinic, a tetrahydrate (previously reported as a 4.5-hydrate) with space group P2|/c and Z = 2 formula units per unit cell, an octahydrate with I2/a and Z = 4, and a dodecahydrate with P2i/n and Z= 2. In each structure the crown ether molecule has the (pseudo) D.^ conformation common for many of its complexes, and is immediately hydrogen-bonded by a group of four water molecules in a similar, characteristic pattern. In the tetrahydrate, with one of the waters disordered, the total connectivity is that of a 1D chain, while the overall structures of the octa-and dodecahydrate are 3D networks. Four of the six independent water molecules in the dodecahydrate are linked with each other into a rare 2D ice-like layer. | | | |
Reference
| Z. Naturforsch. 52b, 615—619 (1997); received January 15 1997 | | | |
Published
| 1997 | | | |
Keywords
| Crown Ether, Crystal Structure, Hydrate, Hydrogen Bonding, Melting Diagram | | | |
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| default:Reihe_B/52/ZNB-1997-52b-0615.pdf | | | | Identifier
| ZNB-1997-52b-0615 | | | | Volume
| 52 | |
| 10 | Author
| Antje Albert, Dietrich Mootz | Requires cookie* | | | Title
| 8-Krone-6 und kleine Carbonsäuren. Bildung und Struktur binärer Addukte mit Ameisen-und Essigsäure sowie ternärer mit Essigsäure und Wasser 18-Crown-6 and Small Carboxylic Acids. Formation and Structure of Binary Adducts with Formic and Acetic Acid, as well as Ternary Ones with Acetic Acid and Water | | | | Abstract
| The melting diagrams of the binary systems 18-crown-6/formic acid and 18-crown-6/acetic acid have been set up and the crystal structures of the adducts 18C6 • 2 HCOOH (1, space group P 2 !/c with Z = 2 formula units per unit cell) and 18C6 • 2 CH 3COOH (2, C2/m, Z = 2) determined. Furthermore three ternary phases, 18C6 • CH3COOH • H20 (3, P2!/c, Z = 4) and dimorphic 18C6 • 2 C H 3COOH • 4 H 20 (high temperature form 4, P2,/n, Z = 2; low temperature form 5, P2|/n, Z = 2) have been characterized in the same way. In each structure the crown ether molecule has the (pseudo) D3d conformation common for many of its complexes. Various aspects of the intermolecular hydrogen bonding are described. | | | |
Reference
| Z. Naturforsch. 53b, 242—248 (1998); eingegangen am 29. Oktober 1997 | | | |
Published
| 1998 | | | |
Keywords
| Acetic Acid, Crown Ether, Formic Acid, Hydrate, Melting Diagram | | | |
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| default:Reihe_B/53/ZNB-1998-53b-0242.pdf | | | | Identifier
| ZNB-1998-53b-0242 | | | | Volume
| 53 | |
| 11 | Author
| Stephanie Janeda, Dietrich Mootz, Herrn | Requires cookie* | | | Title
| Niedere Hydrate aliphatischer primärer Amine. Neue Untersuchungen zu Bildung und Struktur [1] Lower Hydrates of Aliphatic Primary Amines. New Studies of Formation and Structure [1] | | | | Abstract
| After earlier work in this laboratory on lower hydrates of amines, the melting diagram of the system 1 ,8-diaminooctane/water and six new crystal structures of hemi-and monohydrates of terminal primary n-alkylamines and diamines have been determined. In the hydrates 1 -PrNH2 • 0.5 H20 (space group C 2/m with Z = 4 formula units per unit cell), l-HexNH2 • 0.5 H20 (PI, Z = 2) and H2N(CH2)nNH2 • H20 with n = 4, 6, 8 (P 2x/c, Z = 4), the O and N atoms are hydrogen-bonded into a two-dimensional array analogous to the mutual coordination of cations and anions in the Cdl2 structure type: [ON6/3] ~ [CdI6/3]. In the hydrate H2N(CH2)2NH2 • H20 (C 2/c, Z = 4), the H20/N H 2 partial structure is three-dimensional but can be reduced, by neglecting the longest H bond, to an array which is again just two-dimensional and related now to the red Hgl2 structure type: [ON4y2] ~ [HgI4/2], In all the monohydrates, the arrays as defined are crosslinked by the alkylene cnains of the bifunctional amine molecules. | | | |
Reference
| Z. Naturforsch. 53b, 1197—1202 (1998); eingegangen am 22. Mai 1998 | | | |
Published
| 1998 | | | |
Keywords
| Amine Hydrates, Hydrates, Melting Diagram, Crystal Structure, Hydrogen Bonding | | | |
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| default:Reihe_B/53/ZNB-1998-53b-1197.pdf | | | | Identifier
| ZNB-1998-53b-1197 | | | | Volume
| 53 | |
| 12 | Author
| Di, Stephanie Janeda, Dietrich Mootz | Requires cookie* | | | Title
| Di-bis Pentahydrate von fünf Alkylendiaminen. Eine Fallstudie zu ein-und zweidimensionalen Wasserpolymeren in Festkörpern [1]-to Pentahydrates of Five Alkylenediamines. A Case Study of One-and Two-Dimensional Water Polymers in Solids [1] | | | | Abstract
| The crystal structures of five low-melting hydrates of »-alkane-a,u;-diamines, H2N(CH2)"NH2 • x H20 , for short C" ■ x W, have been determined. As a common feature, the water molecules are mutually linked by hydrogen bonds O-H -O to form low-dimensional polymers. These are a meandering chain in C2 • 2 W (space group I 2la, Z -4 formula units per unit cell), a zig zag chain in C6 • 2 W (P 2,/c, Z = 2), a ribbon of consecutively condensed five-membered rings in C3 • 3 W (P 2,/c, Z = 4) and a layer of condensed and spiro-linked rings of varying size each in C7 • 3 W (P i, Z = 4) and C4 • 5 W (C 21c, Z = 4). Further hydrogen bonding, between the water polymers and the bifunctional amine molecules, leads to overall connectivities which are three-dimensional in each structure. | | | |
Reference
| (Z. Naturforsch. 54b, 103—108 [1999]; eingegangen am 7. September 1998) | | | |
Published
| 1999 | | | |
Keywords
| Amine Hydrates, Hydrates, Melting Diagram, Water Polymers, Hydrogen Bonding | | | |
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| default:Reihe_B/54/ZNB-1999-54b-0103.pdf | | | | Identifier
| ZNB-1999-54b-0103 | | | | Volume
| 54 | |
| 13 | Author
| Thom As Kellersohn, Konrad Beckenkamp, HeinzDieter Lutz | Requires cookie* | | | Title
| Extrem asymmetrisch gebundene Wassermoleküle - Kristallstrukturen von Sr(OH)Cl * 4 H zO, Sr(OH)Br * 4 H 20 und Ba(O H )I * 4 H 20 Extremely Asymmetrically Bound W ater Molecules - Crystal Structures of Sr(OH)Cl * 4 H 70 , Sr(OH)Br * 4 H 20 , and Ba(OH)I -4 H 20 | | | | Abstract
| The crystal structures o f isotypic Sr(OH)Cl 4 H 20 , Sr(OH)Br ■ 4 H zO, and Ba(OH)I ■ 4 H 20 are repojted. The title compounds crystallize in a hitherto unknown structure type, space group P i, Z = 2. The final R values obtained are 0.0261, 0.069, and 0.062, respectively. The coordination o f the metal ions is monocapped square antiprismatic with 7 H2Ö, 1 OH~ and 1 halide ion. The halide ions separate metal/water/hydroxide layers. Each o f the four crystallo-graphically different water molecules serves as donor for one very strong and one very weak hydrogen bond and, hence, is extremely asymmetrically bound. Owing to this strong distor tion, the largest one known so far, the OH stretching vibrations o f the H 20 m olecules are intramolecularly decoupled as shown from vibrational spectra. The enthalpies o f dehydration obtained from differential scanning calorimetry are reported. | | | |
Reference
| Z. Naturforsch. 46b, 1279—1286 (1991); eingegangen am 22. April 1991 | | | |
Published
| 1991 | | | |
Keywords
| Strontium Hydroxide Halides, Barium Hydroxide Halides, Crystal Structure, Hydrates, Asymmetrically Bound H 20 | | | |
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| default:Reihe_B/46/ZNB-1991-46b-1279.pdf | | | | Identifier
| ZNB-1991-46b-1279 | | | | Volume
| 46 | |
| 14 | Author
| Michael Born, Dietrich Mootz, Sigrid Schaefgen | Requires cookie* | | | Title
| Tautomere Wasserschichten. Bildung und Struktur tiefschmelzender Trihydrate von Triethylamin und 4-Methylpyridin [1] Tautomeric Water Layers. Formation and Structure of Low-Melting Trihydrates of Triethylamine and 4-Methylpyridine [1] | | | | Abstract
| Low-melting trihydrates of triethylamine (E t3N) and 4-methylpyridine (4-M ePy) have been confirmed and detected by phase analysis and the crystal structures determined. Both are monoclinic with space group P 2!/c and Z = 4 formula units per unit cell. The lattice parameters are a = 13.606, b = 6.291, c = 12.412 A , and ß = 99.47° at -1 0 0 °C for Et3N -3 H 20 , and a = 9.982, b = 6.877, c = 12.958 Ä , and ß = 103.50° at -9 0 °C for 4-M eP y-3 H20 . The water m olecules in the two structures are hydrogen-bonded in condensed four-, five-, and six-membered rings with 1:2:1 ratio, thus forming characteristic layers parallel (1 0 0) of identical topology and tautomeric to each other. The amine m olecules are linked to both sides of the layers by O -H — N bonds from different O atoms. | | | |
Reference
| (Z. Naturforsch. 50b, 101—105 [1995]; eingegangen am 11. August 1994) | | | |
Published
| 1995 | | | |
Keywords
| Am ine Hydrates, Crystal Structure, Hydrates, Hydrogen Bonding, M elting Diagram, Water Layers | | | |
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| | | | | TEI-XML for
| default:Reihe_B/50/ZNB-1995-50b-0101.pdf | | | | Identifier
| ZNB-1995-50b-0101 | | | | Volume
| 50 | |
|
