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1.
(PPh4)2[(SN)ReCl3(μ‐N)(μ‐NSN)ReCl3(THF)] – a Nitrido‐Thionitrosyl‐Dinitridosulfato‐Complex of Rhenium The title compound has been prepared from PPh4[ReVIICl4(NSCl)2] with excess N(SiMe3)3 in dichloromethane solution to give red‐brown single crystals after recrystallisation from acetonitrile/THF solutions. As a by‐product PPh4[ReNCl4] is formed. (PPh4)2[(SN)ReCl3(μ‐N)(μ‐NSN)ReCl3(THF)] ( 1 ): Space group P21/n, Z = 4, lattice dimensions at –80 °C: a = 1024.1(1), b = 2350.2(1), c = 2315.4(2) pm, β = 94.09(1)°, R1 = 0.0403. In the complex anion of 1 the rhenium atoms are connected by an asymmetric Re≡N–Re bridge as well as by a (NSN)4–‐bridge to form a planar Re2N(NSN) six‐membered heterocycle. Both rhenium atoms are coordinated by three chlorine atoms, one of them by a thionitrosyl ligand, the other one by the oxygen atom of a thf molecule.  相似文献   

2.
S4N3[ReCl4(NSCl)2]?. Synthesis and Crystal Structure S4N3[ReCl4(NSCl)2]? is formed as a byproduct in the reaction of Re2(CO)10 with excess trithiazyl chloride. The compound is characterized by a crystal structure analysis by X-ray methods. S4N3[ReCl4(NSCl)2] crystallizes in the noncentrosymmetric space group P212121 with four formula units per unit cell and the lattice dimensions a = 980, b = 1205, c = 1362 pm (2376 observed, independent reflexions; R = 0.076). The compound consists of the well known cyclic planar S4N3-cations and anions [ReCl4(NSCl)2]?, in which the rhenium atom is coordinated octahedral by four Cl atoms and two cis-positioned NSCl ligands. The mean Re? N and N? S bond lengths (177 pm and 158 pm) correspond to double bonds. The bond lengths and angles are much like in the structure of AsPh4[ReCl4(NSCl)2]; however the chlorine atoms of the NSCl ligands are turned to each other.  相似文献   

3.
(PPh4)2[Cl2Re(N3S2)(μ‐NSN)(μ‐N≡ReCl3)]2 – a Rhenium(VII) Complex with a Nitrido, a Dinitridosulfato(II), and a Rhena‐3,5‐dithia‐2,4,6‐triazino Function The title compound has been prepared from PPh4[ReVIICl4(NSCl)2] with N(SiMe3)3 in dichloromethane solution to give red‐brown single crystals, which were suitable for a crystal structure determination. As a by‐product PPh4[ReNCl4] is formed. (PPh4)2[Cl2ReVII(N3S2)(μ‐NSN)(μ‐N≡ReVIICl3)]2 ( 1 ): Space group P21/c, Z = 2, lattice dimensions at –80 °C: a = 1280.8(2), b = 1017.5(1), c = 2467.8(3) pm, β = 95.04(1)°, R = 0.049. The complex anion of 1 consists of a planar ReN3S2‐heterocycle which is connected with the second rhenium atom by a μ‐nitrido bridge as well as by a μ‐dinitridosulfato(II) ligand to form a planar Re2(N)(NSN) six‐membered heterocycle. This [Cl2Re(N3S2)(μ‐NSN)(μ‐N≡ReCl3)] unit dimerizes via one of the N‐atoms of the (NSN)4– ligand to give a centrosymmetric Re2N2 four‐membered ring.  相似文献   

4.
Chlorothionitrene Complexes of Rhenium. Crystal Structure of AsPh4[ReCl4(NSCl)2] · CH2Cl2 Rhenium pentachloride reacts in POCl3 solution with (NSCl)3 forming the chlorothionitrene complexes [(Cl3PO)ReCl4(NSCl)] ( I ) and [(Cl3PO)ReCl3(NSCl)2] ( II ). I reacts with AsPh4Cl in CH2Cl2 solution under abstraction of SCl2 and POCl3, yielding AsPh4[ReNCl4], while II forms the complex AsPh4[ReCl4(NSCl)2] · CH2Cl2. The i.r. spectra of the compounds are discussed and assigned. The crystal structure of AsPh4[ReCl4(NSCl)2] · CH2Cl2 was determined and refined with X-ray diffraction data (R = 0.031 for 2785 reflexions). It crystallizes in the space group Pī with two formula units per unit cell; the lattice constants are a = 1119, b = 1144, c = 1473 pm, α = 77.6, β = 70.8 and γ = 71.2°. The two NSCl ligands have cis arrangement with nearly linear Re?N?S groups, with interatomic distances corresponding to double bonds. The Re? Cl bonds are somewhat longer than usual and show no trans-effect; this is possibly due to Cl…?H? C bridges.  相似文献   

5.
Crystal Structures of [ReCl4(PhC?CPh)]2 · 2 CH2Cl2 and PPh4[ReOCl4] Single crystals of [ReCl4(PhC?CPh)]2 · 2 CH2Cl2 were obtained by chilling dilute solutions of the solvate [ReCl4(PhC?CPh)POCl3] in CH2Cl2. PPh4[ReOCl4] was formed by the reaction of the diphenyl acetylene complex [ReCl5(PhC?CPh)] with PPh4Cl · H2O in CH2Cl2 solution. [ReCl4(PhC?CPh)]2 · 2 CH2Cl2: space group P21/c, Z = 2, 2244 observed independent reflexions, R = 0.038. Lattice parameters (19°C): a = 987.2 pm; b = 1533.9 pm; c = 1193.8 pm; β = 90.17° The compound forms centrosymmetrical dimeric molecules with ReCl2Re bridges with Re? Cl distances of 241.2 and 267.6 pm. The longer Re? Cl bond is situated in trans-position to the equatorial, side-on coordinated diphenyl acetylene ligand with mean Re? C distances of 200 pm. PPh4[ReOCl4]: space group P4/n, Z = 2, 1487 observed, independent reflexions, R = 0.047. Lattice parameters (19°C): a = b = 1272.0 pm; c = 771.3 pm. The compound crystallizes in the AsPh4[RuNCl4] type; it consists of [ReOCl4]? anions and PPh4+ cations. The anions are tetragonal with C4v symmetry and bond lengths Re? O = 165.4 pm and Re? Cl = 232.6 pm; the bond angle OReCl is 106.7°.  相似文献   

6.
[ReCl2(NS)(NSCl)(Pyridine)2], a Thionitrosyl-chlorothionitrene Complex of Rhenium The title compound was obtained by the reaction of pyridine with either [ReCl3(NSCl)2POCl3] or [ReCl3(NSCl)2]2 · (μ-N2S2) under the reducing action of dichloromethane. It is slightly soluble in CH2Cl2, from which it can be obtained in form of black crystals. The IR spectrum is reported. The crystal structure of [ReCl2(NS)(NSCl)(Pyridine)2] was determined by X-ray diffraction (R = 0.027 for 2105 observed reflexions). Crystal data: a = 1551.6, b = 694.9, c = 1513.2 pm, β = 96.50°, space group P21/c, Z = 4. In the monomer molecules, each rhenium atom has a distorted octahedral coordination of two cis-chlorine atoms, two cis-nitrogen atoms of the pyridine ligands and two cis-nitrogen atoms of the thionitrosyl and chloro thionitrene ligands. One of the pyridine groups is in trans position to the nearly linear thionitrosyl group (angle ReNS 176°) with distances ReN of 177 pm and NS of 152 pm. However, in the trans position of the chlorothionitrene group (angle ReNS 159°, distances ReN 189 pm, NS 149 pm) a chlorine atom is found.  相似文献   

7.
[PPh3Cl][ReCl4(N2S2)]?; Synthese, IR-Spektrum und Kristall Strukture The title compound is prepared by the reaction of [ReCl3(NSCl)2(POCl3)] with triphenylphosphane; it formes black crystals. The crystal structure determination was solved with X-ray methods (2861 observed independent reflexions, R = 0.038). The compound crystallizes monoclinic in the space group P21/n with four formula units per unit cell. The structure consists of [PPh3Cl] cations and [ReCl4(N2S2)]? anions, in which the rhenium atom is surrounded octahedrally by four chlorine ligands and the N atoms of a ReN2S2-five-membered ring in cis-position (symmetry C2v). The Re? N bond lengths (181 pm) and the NS bond lengths (152 pm) are in the range of double bonds; the S? S distance is very long (253 pm). The i.r. spectrum is reported.  相似文献   

8.
Complexes of Rhenium with Planar ReN2S2 Rings. Syntheses and Crystal Structures of AsPh4[ReCl4(N2S2)] and PPh4[ReBr4(N2S2)] The complex [ReCl4(N2S2)]? can be obtained as PPh4 or AsPh4 salt by the action of S(NSiMe3)2 and of diphenylacetylene, respectively, on the chlorothionitrene complex [ReCl4(NSCl)2]?. Another method of synthesis is the reaction of [ReCl3(NSCl)2(POCl3)] with SbPh3. [ReBr3(N2S2)]2 is obtained from excess Me3SiBr and [ReCl3(NSCl)2(POCl3)]. The anionic complex [ReBr4(N2S2)]? forms from either [ReCl4(NSCl)2]? or [ReCl4(N2S2)]? with Me3SiBr. All compounds are black, diamagnetic, and sensitive to moisture; the PPh4 and AsPh4 salts are soluble in CH2Cl2 and CH2Br2. The IR spectra are reported. The crystal structures of AsPh,4[ReCl4(N2S2)] and PPh4[ReBr4(N2S2)] were determined by X-ray diffraction. AsPh4[ReCl4(N2S2)]: space group P2/n, Z = 2, a = 1244.5, b = 1429.3, c = 791.1 pm, γ = 96.89° (1715 observed reflexions, R = 0.082). PPh4[ReBr4[ReBr4(N2S2)]: space group P21/n, Z = 4, a = 961.7, b = 1397.4, c = 2205.7 pm, β = 102.10° (1787 observed reflexions, R = 0.073). In both compounds the [ReX4(N2S2)]? anions have the same type of structure, the Re atoms forming part of planar ReN2S2 rings; the bond lengths are ReN 177 pm, NS 152 pm, and SS 259 for the chloro compound and ReN 184 pm, NS 153 pm, and SS 264 pm for the bromo compound. In AsPh4[ReCl4(N2S2)] the cations are stacked to form columns in the c-direction; in PPh4[ReBr4(N2S2)], there is considerable distortion form this packing principle.  相似文献   

9.
Preparation and Vibrational Spectra of Dichloro and Dibromodithiophosphate. Crystal Structures of [PPh3Me][PS2Cl2] and [PPh4][PS2Br2] Dichloro and dibromodithiophosphates [Cat+][PS2X2?] with a large organic cation can be obtained from P4S10, CatX and HX in CH2Cl2 (Cat+ = PPh4+, PPh3Me+; X = Cl, Br). The vibrational spectra (i.r. and Raman) of the [PS2X2]? ions are reported and discussed; force constants were calculated. The crystal structures of [PPh3Me][PS2Cl2] and [PPh4][PS2Br2] were determined and refined with X-ray diffraction data. In both cases, simple anions [PS2X2]? are present. [PPh3Me][PS2Cl2]: orthorhombic, space group P212121, a = 1089, b = 1334, c = 1476 pm, Z = 4, refinement to a residual index R = 0.046 for 1116 reflexions; the structure is isotopic with [PPh3Me][VO2Cl2]. [PPh4][PS2Br2]: tetragonal space group I4 , a = 1301, c = 721 pm, Z = 2, refinement to R = 0.065 for 357 reflexions; the structure is isotypic with [AsPh4][FeCl4] with [PS2Br2]? ions occupying positions of 4 -symmetry with statistical orientation (statistical superposition of Br and S positions).  相似文献   

10.
NH4[Re3Cl10(OH2)2] · 2 H2O: Synthesis and Structure. An Example for “Strong” N? H …? O and O? H …? Cl Hydrogen Bonding The red NH4[Re3Cl10(OH2)2] · 2 H2O crystallizes from hydrochloric-acid solutions of ReCl3 with NH4Cl. It is tetragonal, P41212, No. 92, a = 1157.6, c = 1614.5 pm, Z = 4. The crystal structure contains “isolated” clusters [Re3Cl10(OH2)2]?. These contain Cl…?H? O? H…?Cl units with “very strong” hydrogen bonds: distances Cl? O are only 286 pm. NH4+ has seven Cl? as nearest neighbours and, additionally, one H2O which belongs to a cluster [d(N? O1) = 271 pm] and one crystal water [d(N? O2) = 286 pm].  相似文献   

11.
Synthesis and Structure of [(Me2PhP)3Cl2ReN]2ReCl4, [(Me2PhP)3Cl2ReN]2ReCl4 · 2 SbCl3 and [Re(NH)Cl2(PMe2Ph)3][SbCl6] The reaction of ReNCl2(PMePh)3 with SbCl5 in toluene yields the trinuclear complex [(Me2PhP)3Cl2Re≡N]2ReCl4 · 2 SbCl3 ( 1 · 2 SbCl3). It forms triclinic crystals with the composition 1 · 2 SbCl3, as well as monoclinic crystals 1 · 2 SbCl3 · 4 C7H8. The monoclinic crystals with the space group P21/c, and a = 1212.3(2), b = 2098.5(4), c = 1827.7(3) pm, β = 95.51(1)°, Z = 2, have been used for a crystal structure determination. In the centrosymmetric complex 1 two complexes ReNCl2(PMe2Ph)3 coordinate with their nitrido ligands a square planar, central unit ReCl4. The SbCl3 molecules are coordinated by chlorine bridges to Cl atoms of 1 , and, in addition, connect the complexes 1 with each other. The SbCl3 free compound 1 is obtained in good yield by the reaction of ReNCl2(PMePh)3 with ReCl4(NCEt)2. It crystallizes in the triclinic space group P1 with a = 1037.7(3), b = 1153.0(2), c = 1393.8(3) pm, α = 72.31(2)°, β = 74.06(2)°, γ = 67.94(2)°, and Z = 1. The bond lengths of the Re–N triple bonds are 172 pm in 1 and 170 pm in 1 · 2 SbCl3. By the reaction of ReNCl2(PMePh)3 with SbCl5 in CH2Cl2 the solvent is decomposed forming HCl which protonates the nitrido ligand to afford the imido complex [Re(NH)Cl2(PMe2Ph)3][SbCl6] ( 2 ) crystallizing in the monoclinic space group P21/n with a = 1221.4(2), b = 1358.6(2), c = 2177.3(1) pm, β = 92,72(1)° and Z = 4. The Re–N distance in the almost linear unit Re≡N–H is 169,1 pm.  相似文献   

12.
MoCl4, ReCl4, and ReCl5 react with PCl5 in sealed glass ampoules at temperatures between 220° and 320° to [PCl4]2[Mo2Cl10] ( 1 ) [PCl4]2[Re2Cl10] ( 2 ), and [PCl4]3[ReCl6]2 ( 3 ). 2 crystallizes isotypically to the previously reported 1 and the respective titanium and tin containing analogues. The structure (triclinic, P1, Z = 1, a = 897.3(2), b = 946.0(2), c = 687.13(9) pm, α = 95.59(2)°, β = 95.80(2)°, γ = 101.07(2)°, V = 565.4(2) 106 pm3) is built of tetrahedral [PCl4]+ and edge sharing double octahedral [Re2Cl10]2– ions and can be derived from a hexagonal closest packing of Cl ions with tetrahedral and octahedral holes partially filled by P(V) and Re(IV), respectively. 3 crystallizes isotypically to [PCl4]3[PCl6][MCl6] (M = Ti, Sn) (tetragonal, P 42/mbc, Z = 4, a = 1496.2(1), c = 1363.2(2) pm). Because no evidence was found for the presence of [PCl6] ions, Re in 3 has to be of mixed valency with ReIV and ReV sharing the same crystallographic site. The structure can be derived from a cubic closest packing or alternatively from an only sparsely distorted body centered cubic arrangement of Cl ions which is rarely found for anion arrays. The tetrahedral and octahedral holes are partially filled by PV and MIV/V, respectively. Magnetic measurements show all three compounds to be paramagnetic and confirm the oxidation state IV for Mo and Re in 1 and 2 and the mixed valence (IV/V) for Re in 3 .  相似文献   

13.
The decahydrate of [Re3Cl9(H2O)3] is obtained from aqueous solutions of ReCl3 at zero to -5°C. The crystal structure (orthorhombic, Pnma, Z = 4; a = 1125.16(3), b = 1 630.30(5), c = 1 378.84(5) pm) has been determined from single-crystal X-ray diffractometer data. The [Re3Cl9(H2O)3] molecules are stacked in the [0 1 0] direction and the rows of such molecules are separated by the crystal water molecules. Together with the water ligands, these form a rather strong hydrogen bonding system judging from O? O distances (d = 277 pm) alone.  相似文献   

14.
[ReCl3(NSCl)2(CH3CN)]. Synthesis, I. R. Spectrum, and Crystal Structure Black, moisture sensitive crystals of the title compound are obtained from [ReCl3(NSCl)2]2 and acetonitrile in dichloromethane. The complex is characterized by its i.r. spectrum and an X-ray crystal structure determination (2483 observed independent reflexions, R = 0.035). Crystal data: triclinic, space group P1 , Z = 2, a = 681.8, b = 899.9, c = 1104.0 pm, α = 110.50, β = 97.90 and γ = 101.34°. In the monomeric [ReCl3(NSCl)2(CH3CN)] molecule the Re atom has a distorted octahedral coordination with meridional arrangement of the Cl atoms. The chlorothionitrene ligands have nearly linear ReNS groups with bond lengths that correspond to double bonds (ReN 178 and 179 pm); this agrees with the NReN bond angle of 100°.  相似文献   

15.
Synthesis and Crystal Structure of Hydronium-tris-ethylenediamine-cobalt(rhodium)-μ-trichloro-nonachlorotrirhenate(III)-chloride, H3O[MEn3][Re3Cl12]Cl (M=Co, Rh) The chlorides H3O[MEn3][Re3Cl12]CI (M = Co, 1 ; Rh, 2 ) crystallize from hydrochloric acid solutions of ReCl3 and MEn3 · 3H2O as deep red hexagonal columns. They are isotypic and crystallize with the hexagonal system (P6 , Z = 1; 1: a = 1010.87(3); c = 794.30(4) pm, R = 0.023, Rw = 0.016; 2: a = 1018.58(3); c = 794.74(4) pm, R = 0.026, Rw = 0.018). The anions [Re3Cl12]3? are connected via H3O+ cation (C.N. 3). The large channels that run in the [001] direction contain, alternatively, the cations [MEn3]3+ and the lonesome Cl?-anions  相似文献   

16.
N(SCl)2 [MoCl5(NSCl)]?, a Chlorothionitrene Complex of Molybdenum (VI) . The title compound is formed together with MoCl3(N3S2) by the reaction of MoCl4 or MoCl5 with (NSCl)3 in CH2Cl2. The black, crystalline compound was characterized by its i.r. spectrum and an X-ray crystal structure determination. N(SCl)2[MoCl5(NSCl)]? crystallizes in the monoclinic space group P21/n with four formula units per unit cell. The lattice constants are a = 716.3, b = 1627.4, c = 1178.9 pm and β = 100.90°. The [MoCl5(NSCl)]? ion posseses an almost linear Mo = N = S grouping with bond lengths that can be interpreted as double bonds. Crystal data for AsPh4[MoCl5(NSCl)] are reported.  相似文献   

17.
Synthesis and Structures of the Multinuclear Rhenium Nitrido Complexes [Re2N2Cl4(PMe2Ph)4(MeCN)] and [Re4N3Cl9(PMe2Ph)6] The binuclear rhenium complex [Re2N2Cl4(PMe2Ph)4(MeCN)] ( 1 ) is obtained as a byproduct of the synthesis of [(Me2PhP)3(MeCN)ClReNZrCl5] from [ReNCl2(PMe2Ph)3] and [ZrCl4(MeCN)2] in toluene. It crystallizes as 1 · 2 toluene in the monoclinic space group P21/n with a = 1517.0(3); b = 1847.7(2); c = 1952.4(6) pm; β = 106.44(1)° and Z = 4. The two Re atoms are connected by an asymmetric nitrido bridge Re≡N–Re with distances Re–N of 169.9(5) and 208.7(5) pm. In course of the reaction of [ReNCl2(PMe2Ph)3] with [ZrCl4(THF)2] in CH2Cl2 hydrochloric acid is formed by acting of the Lewis acid on the solvent. HCl protonates and eliminates phosphine ligands of the educt [ReNCl2(PMe2Ph)3] to form the phosphonium salt [PMe2PhH]2[ZrCl6] ( 2 ). It crystallizes in the monoclinic space group C2/c with a = 1536.9(3); b = 1148.8(1); c = 1402.2(3) pm, β = 100.70(2)° and Z = 4. The remaining fragments of the rhenium complex combine to yield the tetranuclear mixed valent complex [Re4N3Cl9(PMe2Ph)6] ( 3 ), crystallizing as 3 · CH2Cl2 in the triclinic space group P 1 with a = 1312.9(19); b = 1661.4(2); 1897.1(2) pm; α = 78.62(1)°; β = 86.77(1)°; γ = 68.28(1)° and Z = 2. The four Re atoms occupy the corners of a tetrahedron. Its edges are formed by three nitrido and three chloro bridges. The asymmetric nitrido bridges Re≡N–Re are characterized by short distances in the range of 172(2) to 176(3) pm and long distances of 194(3) to 204(2) pm. The angles Re–N–Re are between 154(1) and 160(1)°.  相似文献   

18.
Synthesis and Crystal Structure of (PPh4)3[Re2NCl10] The rhenium(V) nitrido complex (PPh4)3[Re2NCl10] ( 1 ) is obtained from the reaction of (PPh4)[ReNCl4] with 1, 3‐dioxan‐(2‐ylmethyl)diphenyl phosphine in CH2Cl2/CH3CN in form of orange red crystals with the composition 1 ·2CH2Cl2 crystallizing in the triclinic space group P1¯ with a = 1210.7(2), b = 1232.5(1), c = 2756.3(5) pm, α = 99.68(1)°, β = 100.24(1)°, γ = 98.59(1)° and Z = 2. The crystal structure contains two symmetry independent, centrosymmetrical complex anions [Re2NCl10]3‐ with a symmetrical nitrido bridge Re=N=Re and distances Re(1) ‐ N(1) = 181.34(5) and Re(2) ‐ N(2) = 181.51(4) pm.  相似文献   

19.
Synthesis and Crystal Structures of the Complexes [(Me2PhP)3Cl2Re≡N‐IrCl2(C5Me5)], [(Me2PhP)3Cl2Re≡N‐IrCl(COD)], [PPh4][O3Os≡N‐IrCl2(C5Me5)], and [PPh4][O3Os≡N‐IrCl(COD)] with Nitrido bridges Re≡N‐Ir and Os≡N‐Ir The heteronuclear complexes [(Me2PhP)3Cl2Re≡N‐IrCl2(C5Me5)] ( 1 ), [(Me2PhP)3Cl2Re≡N‐IrCl(COD)] ( 2 ), [PPh4][O3Os≡N‐IrCl2(C5Me5)] ( 3 ) and [PPh4][O3Os≡N‐IrCl(COD)] ( 4 ) were obtained by the reaction of the nitrido complexes [ReNCl2(PMe2Ph)3] and [OsO3N] with the iridium compounds [IrCl2(C5Me5)]2 and [IrCl(COD)]2 in benzonitrile. 1 forms red crystals with the composition 1 ·C6H5CN in the monoclinic space group P21/c and a = 1264.7(2); b = 1945.3(2); c = 1835.4(1) pm, β = 90.35(1)°, Z = 4. The complex fragment [IrCl2(C5Me5)] in the dinuclear complex is connected by an asymmetric nitrido bridge Re≡N‐Ir to the nitrido complex [ReNCl2(PMe2Ph)3]. The nitrido bridge is characterized by a Re‐N‐Ir bond angle of 179.4(2)° and distances Re‐N = 170.9(4) pm and Ir‐N = 203.3(4) pm. 2 forms brownish red, triclinic crystals with the space group P1¯ and a = 1076.6(2), b = 1373.2(2), c = 1452.4(1) pm, α = 107.513(8), β = 101.843(9), γ = 110.04(1)°, Z = 2. The nitrido bridge to the complex fragment [IrCl(COD)] has a Re‐N‐Ir bond angle of 173, 8(4)° and distances Re‐N = 170, 4(8) pm and Ir‐N = 196, 2(8) pm. 3 crystallizes as monoclinic red crystals in the space group P21/n and a = 1449.9(2), b = 906.74(4), c = 2628.9(5) pm, β = 103.50(1)°, Z = 4. The nitrido bridge Os≡N‐Ir is slightly bent (Os‐N‐Ir = 165.0(3)°). The distances are Os‐N = 168.3(5) pm and Ir‐N = 201.9(5) pm. 4 forms dark brown, orthorhombic crystals with the space group P212121 and a = 704.35(2), b = 1228.17(6), c = 3442.0(4) pm, Z = 4. The distances in the slightly bent nitrido bridge (Os‐N‐Ir = 161.8(4)°) are Os‐N = 169.3(7) pm und Ir‐N = 197.8(7) pm.  相似文献   

20.
The Crystal Structures of (NH4)2[ReCl6], [ReCl2(CH3CN)4]2[ReCl6] · 2CH3CN and [ReCl4(18)(Crown-6)] Brown single crystals of (NH4)2[ReCl6] are formed by the reaction of NH4Cl with ReCl5 in a suspension of diethylether. [ReCl2(CH3CN)4]2[ReCl6] · 2CH3CN crystallizes as brown crystal plates from a solution of ReCl5 in acetonitrile. Lustrous green single crystals of [ReCl4(18-crown-6)] are obtained by the reaction of 18-crown-6 with ReCl5 in a dichloromethane suspension. All rhenium compounds are characterized by IR spectroscopy and by crystal structure determinations. (NH4)2[ReCl6]: Space group Fm3 m, Z = 4, 75 observed unique reflections, R = 0.01. Lattice constant at ?70°C: a = 989.0(1) pm. The compound crystallizes in the (NH4)2[PtCl6] type, the Re? Cl distance is 235.5(1) pm. [ReCl2(CH3CN)4]2[ReCl6] · 2CH3CN: Space group P1, Z = 1, 2459 observed unique reflections, R = 0.12. Lattice dimensions at ?60°C: a = 859.0(1), b = 974.2(7), c = 1287.3(7) pm, α = 102.69(5)°, b? = 105.24(7)°, γ = 102.25(8)°. The structure consists of two symmetry-independent [ReCl2(CH3CN)4]+ ions with trans chlorine atoms, [ReCl6]2? ions, and included acetonitrile molecules. In the cations the Re? Cl bond lengths are 233 pm in average, in the anion they are 235 pm in average. [ReCl4(18-crown-6)]: Space group P21/n, Z = 4, 3 633 observed unique reflections, R = 0.06. Lattice dimensions at ?70°C: a = 1040.2(4), b = 1794.7(5), c = 1090.0(5) pm, b? = 108.91(4)°. The compound forms a molecular structure, in which the rhenium atom is octahedrally coordinated by the four chlorine atoms and by two oxygen atoms of the crown ether molecule.  相似文献   

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