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1.
Sangeeta Sharma Suresh Magotra Sushil K. Pandey 《Phosphorus, sulfur, and silicon and the related elements》2013,188(8):2140-2151
Reactions of (m- and p-ClC 6 H 4 NH 2 ), (p-BrC 6 H 4 NO 2 ), and (p-ClCOC 6 H 4 NO 2 ) with sodium O,O′-ditolyl/dibenzylphosphorodithionates, (ArO) 2 PS 2 Na, (Ar = o?, m?, and p?CH 3 C 6 H 4 or –C 6 H 5 CH 2 ) in 1:1 molar ratio in refluxing toluene under anhydrous conditions resulted in the formation of the compounds (ArO) 2 PS 2 C 6 H 4 L and (ArO) 2 PS 2 COC 6 H 4 L (L = NH 2 or NO 2 ) in 87–94% yield. These viscous compounds were characterized by elemental analyses, molecular weight determination, and IR and NMR ( 1 H, 13 C, and 31 P) spectroscopic studies, which revealed a monodentate mode of bonding of the dithiophosphate moiety with the carbon of the phenyl ring of the organic moiety leading to a P–S–C linkage. 相似文献
2.
3.
《Journal of Coordination Chemistry》2012,65(2):236-248
We report the reaction of a sterically congested NHC–Zn(CH2CH3)2 Lewis adduct (1) prepared through reaction of an equimolar ratio of 1,3-di-tert-butylimidazol-2-ylidene and diethyl zinc, with various substituted phenols (4-tert-butyl-phenol, 2,6-di-tert-butyl-4-methyl phenol, and 1-bromo-4,6-di-tert-butyl phenol). The NHC–Zn dative bond was cleaved in each of the reactions with the substituted phenols to afford the corresponding ionic complexes of imidazolium cation and aryloxo-zincate, [{(4-CMe3C6H4O)2Zn(μ-OC6H4-4-CMe3)}2{(1,3-(CMe3)2-ImCH}2] (2), [{(2,6-(CMe3)2-4-Me-C6H3O)2}Zn{(1,3-(CMe3)2-ImCH}] (3), and [{(1-Br-3,5-(CMe3)2C6H2O)2}2-Zn{(1,3-(CMe3)2-ImCH}] (4), where 1,3-(CMe3)2-ImCH) is imidazolium carbocation. The molecular structures of 1–4 were established by X-ray diffraction analyses and from the solid-state structures of 2–4, it was confirmed that, in all the compounds, zinc ions are coordinated through substituted phenolate groups. 相似文献
4.
Sudhakar Padmanabhan Wei Wang Shohei Katao Kotohiro Nomura 《Macromolecular Symposia》2007,260(1):133-139
Syntheses of titanatranes containing [(O-2,4-Me2C6H2-6-CH2)2-{O(CH2)nCH2}]N3− (n = 1,2) have been explored. Catalytic activity for ethylene polymerization by Ti2(OiPr)2{[(O-2,4-Me2C6H2-6-CH2)2(µ2-OCH2-CH2)]N}2 ( 1a ) - MAO catalyst increased at high temperature; the activity also increased upon addition of AlMe3. Ti(O- 2,6-iPr2C6H3){[(O-2,4-Me2C6H2-6-CH2)2(OCH2CH2)]N} ( 1c ) showed higher activity than 1a under the same conditions. Ti{[(O-2,4-Me2C6H2-6-CH2)2(HOCH2CH2CH2)]N}2 was isolated from the reaction of Ti(OiPr)4 with bis(2-hydroxy-3,5-dimethylbenzyl)-propanolamine; the structure was determined by X-ray crystallography. 相似文献
5.
η6-o-Chlorotoluene-η5-cyclopentadienyliron hexafluorophosphate undergoes nucleophilic substitution of the chlorine atom with anions generated (K2CO3/DMF) from methyl thioglycolate, diethyl malonate, dimethyl malonate, methyl acetoacetate and 2,4-pentanedione. The compounds prepared were o-CH3C6H4SCH2CO2CH3FeCp+PF6−, o-CH3C6H4CH(CO2C2H5)2FeCp+PF6−, o-CH3C6H4CH(CO2CH3)2FeCp+PF6−, o-CH3C6H4CH(COCH3)CO2CH3FeCp+PF6− and o-CH3C6H4CH2COCH3FeCp+PF6
. Similarly, the reaction of diethyl malonate, dimethyl malonate, methyl acetoacetate anions and methylamine with η6-2,6-dichlorotoluene-η5-cyclopentadienyliron hexafluorophosphate yielded monosubstitution of one of the chloro groups. The complexes prepared in this study were η6-diethyl(3-chloro-2-methyl) phenylmalonate- η5-cyclopentadienyliron hexafluorophosphate, η6-dimethyl(3-chloro-2-methyl)phenylmalonate-η5-cyclopentadienyliron hexafluorophosphate, η6-methyl(3-chloro-2-methyl)phenylacetoacetate-η5-cyclopentadienyliron hexafluorophosphate and η6-3-chloro(2-methyl-N-methyl)aniline-η5-cyclopentadienyliron hexafluorophosphate. Reaction of η6-2,6-dichlorotoluene-η5-cyclopentadienyliron hexafluorophosphate with excess methanol as well as methyl thioglycolate in the presence of K2CO3 resulted in disubstitution of both chloro groups to yield new complexes, η6-2,6-dimethoxytoluene-η5-cyclopentadienyliron hexafluorophosphate and η6-methyl[(2-methylphenyl)1,3-dithio] diacetate-η55-cyclopentadienyliron hexafluorophosphate, respectively. Complexes o-CH3C6H4CH(CO2C2H5)2FeCp+PF6−, o-CH3C6H4CH(CO2CH3)2FeCp+PF6− and o-CH3C6H4CH2 COCH3FeCp+ PF6− react with excess K2CO3 and benzyl bromide in refluxing methylene chloride to give 80–90% yields of complexes o-CH3C6H4C(CH2C6H5)(CO2C2H5)2FeCp+PF6−, o-CH3C6H4C(CH2C6H5)(CO2CH3)2FeCp+PF6− and o-CH3C6H4CH(CH2C6H5)COCH3FeCp+PF6−, respectively. Reaction of complex, o-CH3C6H4C(CH2C6H5)(CO2C2H5)2FeCp+PF6− with one molar equivalent of t-BuOK followed by acidic work-up gives o-(C2H5CO2CH2)C6H4CH(CO2C2H5)CH2C6H5FeCp+PF6−. Similarly, reactions of complexes o-CH3C6H4C(CH2C6H5)(CO2C2H5)2FeCp+PF6− and o-CH3C6H4C(CH2C6H5)(CO2CH3)2FeCp+PF6− with t-BuOK in THF followed by alkylation with methyl iodide gave the new complexes, o-(C2H5O2C(CH3)CH)C6H4CH(CH2C6H5)CO2C2H5FeCp+PF6− and o-(CH3O2C(CH3)CH)C6H4CH(CH2C6H5)CO2CH3FeCp+PF6−, respectively. Vacuum sublimation of the new complexes, o-CH3C6H4C(CH2C6H5)(CO2C2H5)2FeCp+PF6− and o-(C2H5O2CCH2)C6H4CH(CH2C6H5)CO2C2H5FeCp+PF6− gives o-CH3C6H4C(CH2C6H5)(CO2C2H5)2 and O-(C2H5O2CCH2)C6H4CH(CH2C6H5)CO2C2H5, respectively. 相似文献
6.
Gregory B. Kharas Youya Gao Jihad Aburas Christina Chintanaphol Mallory L. Davis Hubert Dolubizno 《高分子科学杂志,A辑:纯化学与应用化学》2013,50(8):593-598
Novel trisubstituted ethylenes, ring-substituted butyl 2-cyano-3-phenyl-2-propenoates, RPhCH=C(CN)CO2C4H9 (where R is 2-C6H5CH2O, 3-C6H5CH2O, 4-C6H5CH2O, 4-CH3COO, 3-CH3CO, 4-CH3CO, 4-CH3CONH, 2-CN, 3-CN, 4-CN, 4-(CH3)2N, 4-(C2H5)2N) were prepared and copolymerized with styrene. The monomers were synthesized by the piperidine catalyzed Knoevenagel condensation of ring-substituted benzaldehydes and butyl cyanoacetate, and characterized by CHN analysis, IR, 1H and 13C-NMR. All the ethylenes were copolymerized with styrene (M1) in solution with radical initiation (ABCN) at 70°C. The compositions of the copolymers were calculated from nitrogen analysis and the structures were analyzed by IR, 1H and 13C-NMR. The order of relative reactivity (1/r1) for the monomers is 4-C6H5CH2O (6.39) > 2-C6H5CH2O (2.06) > 3-CH3CO (1.86) > 3-C6H5CH2O (1.78) > 4-CH3COO (1.58) > 3-CN (1.47) > 4-CN (1.21) > 4-(C2H5)2N (1.19) > 4-(CH3)2N (1.18) > 2-CN (1.04) > 4-CH3CO (0.71) > 4-CH3CONH (0.63). Decomposition of the copolymers in nitrogen occurred in two steps, first in the 200–500°C range with residue (3.6–9.5% wt), which then decomposed in the 500–800°C range. 相似文献
7.
合成了2个苯甲羟肟酸有机锡配合物:[(o-Cl-C6H4CH2)2Sn (C6H5CONO)2](1)和[(o-CH3-C6H4CH2)2Sn (C6H5CONO)(C6H5COO)](2)。通过元素分析、红外光谱、核磁共振氢谱、热重分析、单晶X射线衍射等方法对配合物进行了结构表征,对其结构进行量子化学从头计算和体外抗癌活性研究。结果显示:配合物均为单锡核结构,配合物1为六配位的畸变八面体构型,配合物2为五配位的畸变三角双锥构型;配合物1对人宫颈癌细胞(HeLa)、肝癌细胞(HuH-7)和肺腺癌细胞(H1975)显示出比临床使用的顺铂强的抑制活性,而配合物2的抑制活性要弱得多。 相似文献
8.
Some new bimetallic carboxylates of tin and germanium with general formula where R1 = m-CH3C6H4, p-CH3C6H4, C6H5, R2 = o-CH3C6H4, p-CH3C6H4, o-CH3OC6H4, C6H5, CH3, have been prepared by the condensation reaction of diethyltin oxide and triarygermyl(substituted)propanoic acid in 1:2 mole ratio, respectively, and characterized by multinuclear (1H, 13C, 119Sn) NMR, 119mSn Mössbauer and IR spectroscopy. The X-ray crystal structure of the ligand I4 [(C6H5)3GeCH(o-CH3OC6H4)CH2COOH] delineate four coordinated germanium atom with a peculiarity of having a molecule of solvent (CHCl3). The chiral center in the synthesized compounds was identified on the basis of 1H NMR data and measurements of angle of rotations. 相似文献
9.
Abstract The reaction of primary amine hydrochlorides with phosphorus oxychloride in the presence of 1/4 mole of H20 yields the title compounds I (R = C6H5-, 4-CH3CH6H4 ?′ 4-CH3CH6H4 ?, 3-CH3CH6H4 ? CF3CH2-). Hydrochlorides Of more basic amines do not yield any cyclic material. The compound I (R = C6H5) was isolated as one isomer. An X-ray crystallographic study has shown an open ring structure in which the two chlorine atoms are positioned on the same face of the P4N4 ring as the P-O-P bridge. 相似文献
10.
Pascale Tavares Philippe Meunier Bernard Gautheron Gabriel Dousse Helene Lavayssiere 《Phosphorus, sulfur, and silicon and the related elements》2013,188(1-4):249-253
Abstract The first examples of compounds R1R2GeSe2C6H4R3 (R1,R2=CH3 C2H5, C3H2, n-C4H9, i-C5H11, Ph, p-CH3Ph. R3=H, CH3, OCH3) were easily obtained (40–80% yield) from electrophilic cleavage of diselenophenylene zirconocenes by dialkyl or diaryl dichlorogermanes. The synthesis of a spirodi-selenagermole was achieved in the same way using germanium tetrachloride. Analytical data, 1H and 77Se NMR. mass spectra are perfectly consistent with the expected structures. 相似文献
11.
《Journal of Coordination Chemistry》2012,65(2):131-136
The dimeric complex [{(η6-p-cymene)Ru(μ-Cl)Cl}2] (1) reacts with S,N-donor Schiff base ligands, para-substituted S-(thiophen-2-ylmethylene)phenylamines in methanol to give mononuclear amine complexes of the type [(η6-p-cymene)RuCl2(NH2–C6H4–p-X)] {X?=?H (2a); X?=?CH3 (2b); X?=?OCH3 (2c); X?=?Cl (2d); Br (2e) X?=?NO2 (2f), respectively} by hydrolysis of the imine group of the ligand after coordination to the metal. The complexes were characterized by analysis and IR and NMR spectroscopy. The molecular structure of [(η6-C10H14)RuCl2(H2N–C6H4–p-Cl)] (2d) was established by a single-crystal X-ray diffraction study. 相似文献
12.
《Journal of Coordination Chemistry》2012,65(15):1739-1747
Two new bifunctionalized arylimido derivatives of hexamolybdate, [n-Bu4N]2[Mo6O17(C6H3N-2-C2H5-6-CH3)2] (1) and [n-Bu4N]2[Mo6O17(C6H3N-2-CH(CH3)2-6-CH3)2]?·?H2O (2), in which the two organoimido groups are covalently bonded to hexamolybdate at the cis positions, were synthesized by self-assembled metathesis of α-octamolybdate and organoimido ligands with N,N′-dicyclohexylcarbodiimide as dehydration agent, and characterized by elemental analysis, 1H NMR, IR and electronic spectroscopy, and X-ray diffraction analysis. Both derivatives have short Mo–N bond distances [Mo(1)–N(1), 1.740(3)?Å; Mo(2)–N(2), 1.739(3)?Å for 1 and Mo(1)–N(1), 1.734(3)?Å; Mo(2)–N(2), 1.741(3)?Å for 2] and form dimers via π–π stacking in the crystalline state. 相似文献
13.
《Journal of Coordination Chemistry》2012,65(3):121-126
Abstract Thirty compounds of the type (ZC6H4)3PM(CO)5 where Z is 3-CH3, 4-CH3, 3-CH3O, 4-CH3O, 3-CF3, 4-CF3, 4-Cl, 4-F, 4-CH3S, or 4-(CH3) C and M is Cr, Mo, or W are reported, in addition to [4-(CH3)3SiC6H4]3 PW(CO)5 and [(2-CH3C6H4)n(C6H5)3–n P] M(CO)5 where n is 1 or 2 and M is Cr, Mo, or W. Phosphorus-31 NMR and infrared data are presented. In general, the compounds containing the more effective electron withdrawing substituents on the tertiary arylphosphines exhibit the larger 31P coordination chemical shifts, the higher carbonyl stretching frequencies, and the larger phosphorus-31-tungsten-183 coupling constants. 相似文献
14.
Hydrothermal reactions of cadmium(II) chloride with three amino-diphosphonic acids, C6H5CH2N(CH2PO3H2)2 (H4L1), C6H5CH2CH2N(CH2PO3H2)2 (H4L2) and 4-CH3-C6H4CH2N (CH2PO3H2)2) (H4L3) resulted in three new metal amino-diphosphonates, namely, Cd(H3L1)2, 1 Cd(H3L2)2·2H2O 2 and Cd(H3L3)23. In all three complexes, the Cd(II) ion is octahedrally coordinated by six phosphonate oxygen atoms from six ligands. Complexes 1 and 3 have a similar structure in which the CdO6 octahedra are cross-linked by bridging ligands into a double chain along the c-axis, such double chains are further interlinked via hydrogen bonds between non-coordinated phosphonate oxygen atoms to form 〈100〉 and 〈200〉 layers with the phenyl groups of the ligands orientated toward the interlayer space. The structure of complex 2 features a 〈100〉 cadmium(II) diphosphonate layer. The effects of the substitute groups attached to the amine groups on the structures of the metal phosphonates are also discussed. 相似文献
15.
Benedikt Suchland Astrid Malassa Helmar Görls Sven Krieck Matthias Westerhausen 《无机化学与普通化学杂志》2020,646(3):125-132
A series of thiolate ligands were used to synthesize diiron(I) hexacarbonyl bis(thiolates) for structural studies. Conversion of the corresponding thiols with triiron(0) dodecacarbonyl yields complexes of the type [{(CO)3Fe(μ-SR)}2] [R = C6H5 ( 1 ), C6H4-4-CH3 ( 2 ), C6H4-4-F ( 3 ), C6F5 ( 4 ), C6H4-4-CF3 ( 5 ), C6H2-2,4,6-(CH3)3 ( 6 ), CH2–C6H4-4-Cl ( 7 )]. These complexes were isolated and fully characterized, including X-ray crystal structures of complexes 2 – 7 . The bridging thiolate ligands mainly influence the Fe–CO bond which is trans-positioned to the second iron(I) center. In solution, the anti-isomer with one axially and one equatorially oriented thiolate is the major species; severe steric strain induced by mesityl groups only allows the formation of syn-endo-isomeric molecules of 7 . Furthermore, light-induced CO release at solid material at the three representative complexes 1 , 3 , and 6 verify suitability as photoCORMs. 相似文献
16.
Gregory B. Kharas Benjamin L. Hill Vida M. Gaizutis Irma T. Garcia Lara Gutierrez Michelle E. Huddle 《高分子科学杂志,A辑:纯化学与应用化学》2013,50(6):575-580
Novel electrophilic trisubstituted ethylene monomers, oxy ring-disubstituted 2-cyano-3-phenyl-2-propenamides, RC6H3CH? C(CN)CONH2 (where R is 2,3-(CH3O)2, 2,4-(CH3O)2, 2,5-(CH3O)2, 2,6-(CH3O)2, 3,4-(CH3O)2, 3,5-(CH3O)2, 3-CH3?4-CH3O, 3-C2H5O-4-CH3O, 3,4-(C6H5CH2O)2, 2-C6H5CH2O-3-CH3O, 3-C6H5CH2O-4-CH3O, 4-C6H5CH2O-3-CH3O) were synthesized by potassium hydroxide catalyzed Knoevenagel condensation of ring-disubstituted benzaldehydes and cyanoacetamide, and characterized by CHN analysis, IR, 1H- and 13C-NMR. Novel copolymers of the ethylenes and styrene were prepared at equimolar monomer feed composition by solution copolymerization in the presence of a radical initiator, AIBN at 70°C. The composition of the copolymers was calculated from nitrogen analysis, and the structures were analyzed by IR, 1H- and 13C-NMR. High Tg of the copolymers in comparison with that of polystyrene indicates a decrease in chain mobility of the copolymer due to the high dipolar character of the trisubstituted ethylene monomer unit. Decomposition of the copolymers in nitrogen occurred in two steps, first in the 300–500°C range with residue (2–9% wt), which then decomposed in the 500–800°C range. 相似文献
17.
《Journal of Coordination Chemistry》2012,65(10):1111-1118
Lanthanum(III) tris(dithiophosphates), [La{S2P(OR)2}3] (where R=-CH2CH2CH3 or -C6H5) and [La{S2PO2G}3] [where G=-C(CH3)2CH2CH(CH3)-, -CH2C(CH3)2CH2-, -C(CH3)2C(CH3)2- and -CH2CH2CH(CH3)-] were prepared in methanolic solutions of anhydrous LaCl3 and ammonium dithiophosphates. Addition complexes of the type [La{S2P(OR)2}3·nL] and [La{S2PO2G}3·nL] [where n = 1, L = N2C10H8 or N2C12H8 and n = 2, L = P(C6H5)3] were prepared by reaction of lanthanum(III) tris(dithiophosphates) and nitrogen or phosphorus donor bases in benzene. These newly synthesized derivatives have been characterized by elemental analyses, molecular weights, IR, 1H and 31P NMR spectral measurements. Coordination numbers of six and eight are suggested for lanthanum(III) in these derivatives. 相似文献
18.
Anahid Saneei Jerry P. Jasinski Titus A. Jenny Aurelien Crochet Katharina M. Fromm 《Phosphorus, sulfur, and silicon and the related elements》2018,193(4):257-266
The supramolecular assemblies of three new phosphoric triamides, {(C6H5CH2)(CH3)N}2(4-CH3-C6H4C(O)NH)P(O) (1), {(C6H11)(CH3)N}2(4-CH3-C6H4C(O)NH)P(O) (2) and {(C2H5)2N}2(4-CH3-C6H4C(O)NH)P(O) (3) were studied by single crystal X-ray diffraction as well as by Hirshfeld surface analysis. It was found that a synergistic cooperation of NH?O and CH?O hydrogen bonds occurs in all three structures, but forming unique supramolecular architectures individually. Along with the presence of centrosymmetric dimers in 1, 2 and 3, based on a classical NH?O hydrogen bond, the presence of weak CH?O interactions play an additional and vital role in crystal architecture and construction of the final assemblies, collectively identified as a centrosymmetric dimer (0D), a 1-D array and a 3-D network, respectively. These differences in superstructures are related to the effect of aromatic, bulk and flexible groups used in the molecules designed, with a similar C(O)NHP(O) backbone. The NH?O contacts in 1, 2 and 3 are of the “resonance-assisted hydrogen bond” types and also the anti-cooperativity effect can be considered in the multi-acceptor sites P═O in 1 and 2 and C═O in 3. All three compounds were further studied by 1D NMR experiments, 2D NMR techniques (HMQC and HMBC (H–C correlation)), high resolution ESI–MS, EI–MS spectrometry and IR spectroscopy methods. 相似文献
19.
Patricia Lara Margarita Paneque Prof. Dr. Manuel L. Poveda Prof. Dr. Laura L. Santos Dr. José E. V. Valpuesta Verónica Salazar Dr. Ernesto Carmona Prof. Dr. Salvador Moncho Gregori Ujaque Dr. Agustí Lledós Prof. Dr. Celia Maya Dr. Kurt Mereiter Prof. Dr. 《Chemistry (Weinheim an der Bergstrasse, Germany)》2009,15(36):9046-9057
Experimental and theoretical studies on equilibria between iridium hydride alkylidene structures, [(TpMe2)Ir(H){?C(CH2R)ArO }] (TpMe2=hydrotris(3,5‐dimethylpyrazolyl)borate; R=H, Me; Ar=substituted C6H4 group), and their corresponding hydride olefin isomers, [(TpMe2)Ir(H){R(H)C? C(H)OAr}], have been carried out. Compounds of these types are obtained either by reaction of the unsaturated fragment [(TpMe2)Ir(C6H5)2] with o‐C6H4(OH)CH2R, or with the substituted anisoles 2,6‐Me2C6H3OMe, 2,4,6‐Me3C6H2OMe, and 4‐Br‐2,6‐Me2C6H2OMe. The reactions with the substituted anisoles require not only multiple C? H bond activation but also cleavage of the Me? OAr bond and the reversible formation of a C? C bond (as revealed by 13C labeling studies). Equilibria between the two tautomeric structures of these complexes were achieved by prolonged heating at temperatures between 100 and 140 °C, with interconversion of isomeric complexes requiring inversion of the metal configuration, as well as the expected migratory insertion and hydrogen‐elimination reactions. This proposal is supported by a detailed computational exploration of the mechanism at the quantum mechanics (QM) level in the real system. For all compounds investigated, the equilibria favor the alkylidene structure over the olefinic isomer by a factor of between approximately 1 and 25. Calculations demonstrate that the main reason for this preference is the strong Ir–carbene interactions in the carbene isomers, rather than steric destabilization of the olefinic tautomers. 相似文献
20.
Yuxing Tan Zhijian Zhang Yuhuan Tan Daizhi Kuang Jiangxi Yu Xiaoming Zhu 《Journal of Coordination Chemistry》2017,70(15):2606-2624
Three new dialkytin complexes, {[o-OH–C6H4(O)C=N–N=C(CH2Ph)COO](n-Bu2Sn)}n (1), {[o-OH–C6H4(O)C=N–N=C(CH2Ph)COO](MeOH)(p-MeC6H5CH2)2Sn}2 (2), and {[o-OH–C6H4(O)C=N–N=C(CH2Ph)COO](EtOH)(C6H5CH2)2Sn}2 (3), were synthesized by reactions of 2-oxo-3-phenylpropionic acid salicyloylhydrazone with the corresponding diorganotin(IV) complex, respectively. All the complexes were characterized by IR, 1H, 13C, 119Sn NMR spectra, elemental analysis, X-ray single crystal diffraction and TGA. For in vitro antitumor activities, complexes were evaluated by the MTT assay against three human cancer cell lines (NCI-H460, HepG2 and MCF7) and human cell line (HL7702). The results showed that 1 may be a better potential candidate for further chemical optimization and cancer therapy than 2 and 3. The interactions between the complexes and calf thymus DNA were studied; the interaction of 1 with calf thymus DNA was intercalation, 2 and 3 were intercalation and electrostatic binding. 相似文献