Monomeric Titanium(IV) Azides as a New Route to Titanium Nitride

Monomeric Titanium(IV) Azides as a New Route to Titanium Nitride

The reaction of Ti(NMe2)4 with 2 equiv of Me3SiN3 in toluene solution affords a dark red polymeric material of composition [Ti(NMe2)2(N3)2] n (1). If the reaction is carried out in pyridine (py) solution, dark red, crystalline [Ti(NMe2)2(N3)2(py)2] (2) is formed. Analogous reactions of Ti(NMe2)4 wit...

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Veröffentlicht in:Inorganic chemistry 1997-07, Vol.36 (14), p.3108-3112
Hauptverfasser: Carmalt, Claire J, Cowley, Alan H, Culp, Robert D, Jones, Richard A, Sun, Yang-Ming, Fitts, Bill, Whaley, Sandra, Roesky, Herbert W
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container_end_page 3112
container_issue 14
container_start_page 3108
container_title Inorganic chemistry
container_volume 36
creator Carmalt, Claire J
Cowley, Alan H
Culp, Robert D
Jones, Richard A
Sun, Yang-Ming
Fitts, Bill
Whaley, Sandra
Roesky, Herbert W
description The reaction of Ti(NMe2)4 with 2 equiv of Me3SiN3 in toluene solution affords a dark red polymeric material of composition [Ti(NMe2)2(N3)2] n (1). If the reaction is carried out in pyridine (py) solution, dark red, crystalline [Ti(NMe2)2(N3)2(py)2] (2) is formed. Analogous reactions of Ti(NMe2)4 with 2 or 1 equiv of Me3SiN3 in the presence of 1 equiv of bipyridyl (bipy) in toluene solution afford brown crystals of [Ti(NMe2)2(N3)2(bipy)] (3) and dark red crystals of [Ti(NMe2)3(N3)(bipy)] (4), respectively. Crystallographic data for 2:  orthorhombic, C2221, a = 7.120(1) Å, b = 15.899(3) Å, c = 16.946(4) Å, V = 1918.3(6) Å3, ρ = 1.310 g/cm3, Z = 4. Crystallographic data for 3:  monoclinic, I2/a, a = 7.358(2) Å, b = 16.808(4) Å, c = 14.837(6) Å, β = 95.40(2)°, V = 1826.8(1) Å3, ρ = 1.368 g/cm3, Z = 4. Crystallographic data for 4:  monoclinic, P21/c, a = 15.682(2) Å, b = 8.814(1) Å, c = 15.128(1) Å, β = 108.39(1)°, V = 1984.2(4) Å3, ρ = 1.267 g/cm3, Z = 4. Compounds 1 and 2 deposit thin films of titanium nitride (TiN) on silica and/or nickel substrates in the temperature range 300−400 °C. The TiN films deposited from precursor 2 are superior to those deposited from 1.
doi_str_mv 10.1021/ic9614834
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If the reaction is carried out in pyridine (py) solution, dark red, crystalline [Ti(NMe2)2(N3)2(py)2] (2) is formed. Analogous reactions of Ti(NMe2)4 with 2 or 1 equiv of Me3SiN3 in the presence of 1 equiv of bipyridyl (bipy) in toluene solution afford brown crystals of [Ti(NMe2)2(N3)2(bipy)] (3) and dark red crystals of [Ti(NMe2)3(N3)(bipy)] (4), respectively. Crystallographic data for 2:  orthorhombic, C2221, a = 7.120(1) Å, b = 15.899(3) Å, c = 16.946(4) Å, V = 1918.3(6) Å3, ρ = 1.310 g/cm3, Z = 4. Crystallographic data for 3:  monoclinic, I2/a, a = 7.358(2) Å, b = 16.808(4) Å, c = 14.837(6) Å, β = 95.40(2)°, V = 1826.8(1) Å3, ρ = 1.368 g/cm3, Z = 4. Crystallographic data for 4:  monoclinic, P21/c, a = 15.682(2) Å, b = 8.814(1) Å, c = 15.128(1) Å, β = 108.39(1)°, V = 1984.2(4) Å3, ρ = 1.267 g/cm3, Z = 4. Compounds 1 and 2 deposit thin films of titanium nitride (TiN) on silica and/or nickel substrates in the temperature range 300−400 °C. 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Chem</addtitle><description>The reaction of Ti(NMe2)4 with 2 equiv of Me3SiN3 in toluene solution affords a dark red polymeric material of composition [Ti(NMe2)2(N3)2] n (1). If the reaction is carried out in pyridine (py) solution, dark red, crystalline [Ti(NMe2)2(N3)2(py)2] (2) is formed. Analogous reactions of Ti(NMe2)4 with 2 or 1 equiv of Me3SiN3 in the presence of 1 equiv of bipyridyl (bipy) in toluene solution afford brown crystals of [Ti(NMe2)2(N3)2(bipy)] (3) and dark red crystals of [Ti(NMe2)3(N3)(bipy)] (4), respectively. Crystallographic data for 2:  orthorhombic, C2221, a = 7.120(1) Å, b = 15.899(3) Å, c = 16.946(4) Å, V = 1918.3(6) Å3, ρ = 1.310 g/cm3, Z = 4. Crystallographic data for 3:  monoclinic, I2/a, a = 7.358(2) Å, b = 16.808(4) Å, c = 14.837(6) Å, β = 95.40(2)°, V = 1826.8(1) Å3, ρ = 1.368 g/cm3, Z = 4. Crystallographic data for 4:  monoclinic, P21/c, a = 15.682(2) Å, b = 8.814(1) Å, c = 15.128(1) Å, β = 108.39(1)°, V = 1984.2(4) Å3, ρ = 1.267 g/cm3, Z = 4. Compounds 1 and 2 deposit thin films of titanium nitride (TiN) on silica and/or nickel substrates in the temperature range 300−400 °C. 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Chem</addtitle><date>1997-07-02</date><risdate>1997</risdate><volume>36</volume><issue>14</issue><spage>3108</spage><epage>3112</epage><pages>3108-3112</pages><issn>0020-1669</issn><eissn>1520-510X</eissn><abstract>The reaction of Ti(NMe2)4 with 2 equiv of Me3SiN3 in toluene solution affords a dark red polymeric material of composition [Ti(NMe2)2(N3)2] n (1). If the reaction is carried out in pyridine (py) solution, dark red, crystalline [Ti(NMe2)2(N3)2(py)2] (2) is formed. Analogous reactions of Ti(NMe2)4 with 2 or 1 equiv of Me3SiN3 in the presence of 1 equiv of bipyridyl (bipy) in toluene solution afford brown crystals of [Ti(NMe2)2(N3)2(bipy)] (3) and dark red crystals of [Ti(NMe2)3(N3)(bipy)] (4), respectively. Crystallographic data for 2:  orthorhombic, C2221, a = 7.120(1) Å, b = 15.899(3) Å, c = 16.946(4) Å, V = 1918.3(6) Å3, ρ = 1.310 g/cm3, Z = 4. Crystallographic data for 3:  monoclinic, I2/a, a = 7.358(2) Å, b = 16.808(4) Å, c = 14.837(6) Å, β = 95.40(2)°, V = 1826.8(1) Å3, ρ = 1.368 g/cm3, Z = 4. Crystallographic data for 4:  monoclinic, P21/c, a = 15.682(2) Å, b = 8.814(1) Å, c = 15.128(1) Å, β = 108.39(1)°, V = 1984.2(4) Å3, ρ = 1.267 g/cm3, Z = 4. Compounds 1 and 2 deposit thin films of titanium nitride (TiN) on silica and/or nickel substrates in the temperature range 300−400 °C. The TiN films deposited from precursor 2 are superior to those deposited from 1.</abstract><cop>United States</cop><pub>American Chemical Society</pub><pmid>11669964</pmid><doi>10.1021/ic9614834</doi><tpages>5</tpages></addata></record>
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