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211.
Simon G. Bott Alan P. Marchand Sulejman Alihodzic 《Journal of chemical crystallography》1998,28(4):259-266
Crystal structures of four dibromomethylene-functionalized hexa- and heptacyclotetradecane cages are reported. 7-(Dibromomethylene)heptacyclo[6.6.0.02,6.03,13.04,11.05,9.010,14]tetradecane (3): orthorhombic, Pnma, a = 14.744(1), b = 11.237(1), c = 7.4625(7) Å Z = 4; R = 0.0531 for 504 observed reflections. 7,12-Bis(dibromomethylene)heptacyclo[6.6.0.02,6.03,13-04,11 .05,9.010,14]tetradecane (4): monoclinic, I2/a, a = 11.257(1), b = 9.5844(8), c = 13.884(2) Å, = 92.254(8)° Z = 4; R = 0.0413 for 663 observed reflections. 10,14-bis(dibromomethylene)hexacyclo[6.6.0.02,6.03,13.04,11.05,9]tetradecane (6): monoclinic, P21/n, a = 8.118(1), b = 15.273(4), c = 12.826(3) Å, = 104.20(1)° Z = 4; R = 0.0384 for 1392 observed reflections. 14-(dibromomethylene)hexacyclo[6.6.0.02,6.03,13.04,11.05,9]tetradecan-10-one (7): monoclinic, P21/n, a = 8.2879(7), b = 15.273(1), c = 10.0565(9) Å, = 92.271(8)° Z = 4; R = 0.0320 for 1402 observed reflections. The functional groups lead to slight shortening of bond lengths. 相似文献
212.
Simon G. Bott Huafeng Shen Michael G. Richmond 《Journal of chemical crystallography》1998,28(5):385-399
Thermal and Me3NO-assisted activation of the donor–acceptor complex Ru2(CO)6(bpcd) (1) [where bpcd = 4,5-bis(diphenylphosphino)-4-cyclopenten-1,3-dione] with PMe3 or tBuNC affords the mono-substituted complexes Ru2(CO)5L(bpcd), as a result of regiospecific ligand attack at the diphosphine-substituted ruthenium center. Solution NMR measurements (1H and 31P) reveal that the PMe3 derivative exists as a noninterconverting mixture of axial (3a) and equatorial (3e) isomers, with the only the equatorial isomer being observed for Ru2(CO)5(tBuNC)(bpcd) (5). Near-UV irradiation of 1 in the presence of added ligand yields Ru2(CO)5L(bpcd), in addition to the known 2-phosphido complex Ru2(CO)6 [-C=C(PPh2)C(O)CH2C(O)](2-PPh2) (2) and the corresponding phosphido-substituted complexes Ru2(CO)5L[-{C =C(PPh2)C(O)CH2C}(O)]2-PPh2)[4 (L = PMe3); 6 (L = tBuNC)]. As with compounds 3a, 3e, and 5, both 4 and 6 exhibit ligand attachment at the diphosphine-substituted ruthenium center. The molecular structures of 3e, 4, 5, and 6 were determined by X-ray crystallography. 3e, as the 1/2 C6H6 solvate, crystallizes in the monoclinic space group C2/c: a = 40.573(3) Å, b = 10.2663(9) Å, c = 18.347(1) Å, = 95.371(6)°, V = 7609(1) Å3 and Z = 8; 4, crystallizes in the monoclinic space group P21/n: a = 10.8241(8) Å, b = 18.074(1) Å, c = 19.194(1) Å, = 96.968(6)°, V = 3727.3(5) Å3, and Z = 4; 5, as the 1/2CH2Cl2 solvate, crystallizes in the monoclinic space group C2/c: a = 40.955(3) Å, b = 9.7230(6) Å, c = 20.542(1) Å, = 106.596(5)°, V = 7839.2(9) Å3, and Z = 8; 6, as the 1/2C5H12 solvate, crystallizes in the monoclinic space group P21/c: a = 21.773(2) Å, b = 10.907(3) Å, c = 18.744(4) Å, = 114.68(1)°, V = 4045(1) Å3, and Z = 4. The site occupied by the PMe3 and tBuNC ligands in these compounds is discussed relative to the steric size/electronic properties of the ancillary ligand and its interaction with the bpcd ligand. 相似文献
213.
The molecular structures of (tBu)Ga(S2CNnPr2)2 (1) and (iPrO)Ga(S2CNEt2)2 (2) have been determined. The variation in the geometries observed for bis-dithiocarbamate compounds of gallium, (X)Ga(S2CNMe2)2 (X=Cl, iPrO, tBu) do not lie along the Berry pseudorotation pathway for the square-based pyramid to trigonal bipyramid geometrical transition. Instead, the structures appear to lie on an unusual ligand two-step, Texas, pseudorotation mechanism which results in a highly distorted trigonal bipyramidal geometry. Crystal data: (1) monoclinic, P21,/c, a = 9.786(1), b = 29.218(3), c = 9.452(1) Å, = 108.379(9)°, V = 2564.7(5) Å3, and Z = 4. (2) Monoclinic, P21
/c, a = 10.980(3), b = 15.673(4), c = 12.461(3) Å, = 97.47(2)°, V = 2126.2(9) Å3 and Z = 4. 相似文献
214.
Simon G. Bott D. Rajagopal Alan P. Marchand Kaipenchery A. Kumar 《Journal of chemical crystallography》1996,26(6):425-428
The compound crystallizes in the triclinic space group,
, witha=6.7702(4),b=7.0180(4),c=9.1960(7) Å, =92.457(6), =96.150(6), =93.444(5)°, andZ=2. The structure contains a rather short intramolecular H...H contact of 2.26(4) Å. 相似文献
215.
Simon G. Bott Alan P. Marchand Dongxia Xing Rajesh Shukla Stephen James Obrey K. Venkatesan J. Narasimha Moorthy 《Journal of chemical crystallography》1994,27(11):661-665
NaBH4 reduction of a cage dione proceeds in a stereospecific fashion to give theendo,endo-diol. This reactivity is related to the crystal structure. 相似文献
216.
217.
Alan H. Cowley Richard A. Jones Miguel A. Mardones Jerry L. Atwood Simon G. Bott 《Heteroatom Chemistry》1991,2(1):11-15
The reaction of (t-BuGaCl2)2 with Ar′P(H)Li (AR′ = 2,4,6-t-Bu3C6H2) affords the chloride-bridged dimer [t-BuGa(Cl)P(H)Ar′]2 ( 1 ). The structure of 1 has been established by X-ray crystallography. Compound 1 , C44H78Cl2Ga2P2, crystallizes in the monoclinic space group P21/n with Z = 2, a = 10.468(1), b = 14.967(1), c = 16.182(2) Å, and Å = 94.48(1)β. The reaction of 1 with t-BuLi is described. 相似文献