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The polymeric precursors 1 and 2 have been obtained as a non-crystalline, colorless powder-solid : 2 showed a wide spectrum of excellent antibacterial activities, but 1 did not. The antimicrobial activities of the complexes 1-4,evaluated by MIC (minimum inhibitory concentration), were compared and key factors affecting them were discussed. The crystal structures of the complexes 3 and 4 were determined by single-crystal X-ray diffraction. The complexes 3 and 4 in the solid-state were helical polymers consisting of AgN_2P_2 cores formed by bridging triazolate anions and two PPh_3 ligands. The complexes 3 and 4 were also fully characterized by elemental analyses, TG/DTA and FT-IR in the solid-state and by various solution NMR (^\u003c31\u003eP, ^\u003c109\u003eAg, ^1H and ^\u003c13\u003eC) spectroscopies and molecular weight measurements in solution. (2) Two novel gold (I)-triphenylphosphine complexes with nitrogen-containing heterocycles, [Au (1,2,3-L) (PPh_3)] 1 and [Au (1,2,4-L) (PPh_3)]_2・xH_2O (x=0.5-1.0) 2 (HL=triazole) were synthesized from stoichiometric reactions of a precursor complex [AuCl (PPh_3)] with HL in acetone in the presence of aqueous NaOH, and isolated as colorless needles and cubic crystals, respectively. The crystal structures of 1 and 2 were determined by single-crystal X-ray diffraction. 1 and 2 were also fully characterized by complete elemental analyses, TG/DTA and FT-IR in the solid-state and by solution NMR (^\u003c31\u003eP, ^1H and ^\u003c13\u003eC) spectroscopies and solution molecular-weight measurements. 1 consisted of a monomeric 2-coordinate AuNP core both in the solid-state and in solution, while, in contrast, 2 comprised a dimeric (AuNP)_2 core through an Au-Au bond in the solid-state, but a monomeric AuNP core in solution. Within the two gold (I) complexes composed of very closely related nitrogen-containing heterocycles and a common bulky PPh_3,ligand, it was found that the aggregation through the Au…Au interaction in 2 was overruled in 1. The molecular structures of 1 and 2 were also compared with those of the corresponding silver (I) analogs, [Ag (1,2,3-L) (PPh_3)_2]_n 3 and [Ag (1,2,4-L) (PPh_3)_2]_n 4,the molecular structures of both of which have been recently determined as helical polymers in the solid-state. (3) Polymeric silver (I) imidazolate [Ag (imd)]_n (1; Himd=imidazole, C_3H_4N_2) showing a wide spectrum of excellent antimicrobial activities against bacteria, yeast and mold, which has been obtained as non-crystalline, colorless powder, was successfully converted to molecular, crystalline complex [Ag (imd) (PPh_3)_3] 2 by a reaction of 1 with 3 equivalents of PPh_3 in CH_2Cl_2. This novel complex 2 was not obtained from reactions in solutions of the precursors [AgCl (PPh_3)_3] and/or [AgCl(PPh_3)_2]_2 with Himd in the presence of NaOH or with sodium salt of imd. On the contrary, the corresponding gold (I) complex [Au (imd) (PPh_3)] 3 was formed by a reaction of the precursor [AuCl (PPh_3)] and Himd in the presence of NaOH. From a synthetic viewpoint, these facts show the ordering of ligand replacement in these complexes to be Ag-P\u003e\u003eAg-Cl\u003eAg-N, while Au-P\u003e\u003eAu-N\u003eAu-Cl. This ordering also exhibits the different reactivity of silver (I) and gold (I) complexes with biological ligands such as proteins, enzymes, nucleic acids and amino acids. The complex 2 was fully characterized by complete elemental analyses, TG/DTA, FT-IR, solution molecular weight measurement and various solution NMR (^1H, ^\u003c13\u003eC, ^\u003c31\u003eP and ^\u003c109\u003eAg) spectroscopies. The complex 2 in solution was present in a rapid equilibrium with the dissociated species of two PPh_3 ligands, i. e., [Ag (imd) (PPh_3)]. The ^\u003c31\u003eP NMR measurements at low temperature showed that (i) all PPh_3 ligands in 2 in CHCl_3 solution migrated at room temperature between the two isotopes ^\u003c109\u003eAg and ^\u003c107\u003eAg, in addition to the dissociation of two PPh_3 ligands, and (ii) there were present the 4-coordinate tetrahedral complex 2 and the dissociated complex [Ag (imd) (PPh_3)] in solution.", "subitem_description_type": "Abstract"}]}, "item_3_publisher_33": {"attribute_name": "出版者", "attribute_value_mlt": [{"subitem_publisher": "神奈川大学"}]}, "item_3_source_id_10": {"attribute_name": "書誌レコードID", "attribute_value_mlt": [{"subitem_source_identifier": "AA11822302", "subitem_source_identifier_type": "NCID"}]}, "item_3_version_type_16": {"attribute_name": "著者版フラグ", "attribute_value_mlt": [{"subitem_version_resource": "http://purl.org/coar/version/c_970fb48d4fbd8a85", "subitem_version_type": "VoR"}]}, "item_creator": {"attribute_name": "著者", "attribute_type": "creator", "attribute_value_mlt": [{"creatorNames": [{"creatorName": "野宮, 健司"}], "nameIdentifiers": [{"nameIdentifier": "23036", "nameIdentifierScheme": "WEKO"}]}, {"creatorNames": [{"creatorName": "小田, 宗宏"}], "nameIdentifiers": [{"nameIdentifier": "23037", "nameIdentifierScheme": "WEKO"}]}, {"creatorNames": [{"creatorName": "Nomiya, Kenji"}], "nameIdentifiers": [{"nameIdentifier": "23038", "nameIdentifierScheme": "WEKO"}]}, {"creatorNames": [{"creatorName": "Oda, Munehiro"}], "nameIdentifiers": [{"nameIdentifier": "23039", "nameIdentifierScheme": "WEKO"}]}]}, "item_files": {"attribute_name": "ファイル情報", "attribute_type": "file", "attribute_value_mlt": [{"accessrole": "open_date", "date": [{"dateType": "Available", "dateValue": "2018-11-20"}], "displaytype": "detail", "download_preview_message": "", "file_order": 0, "filename": "kana-1-5-0030.pdf", "filesize": [{"value": "527.4 kB"}], "format": "application/pdf", "future_date_message": "", "is_thumbnail": false, "licensetype": "license_free", "mimetype": "application/pdf", "size": 527400.0, "url": {"label": "kana-1-5-0030.pdf", "url": "https://kanagawa-u.repo.nii.ac.jp/record/7370/files/kana-1-5-0030.pdf"}, "version_id": "576d10f0-5f08-43df-aec3-eece1676eb1f"}]}, "item_language": {"attribute_name": "言語", "attribute_value_mlt": [{"subitem_language": "eng"}]}, "item_resource_type": {"attribute_name": "資源タイプ", "attribute_value_mlt": [{"resourcetype": "departmental bulletin paper", "resourceuri": "http://purl.org/coar/resource_type/c_6501"}]}, "item_title": "I. \u003c種々の複素環窒素配位子による銀 (I) および金 (I) 錯体の合成と生理活性\u003e", "item_titles": {"attribute_name": "タイトル", "attribute_value_mlt": [{"subitem_title": "I. \u003c種々の複素環窒素配位子による銀 (I) および金 (I) 錯体の合成と生理活性\u003e"}]}, "item_type_id": "3", "owner": "1", "path": ["579"], "permalink_uri": "http://hdl.handle.net/10487/1258", "pubdate": {"attribute_name": "公開日", "attribute_value": "2009-02-23"}, "publish_date": "2009-02-23", "publish_status": "0", "recid": "7370", "relation": {}, "relation_version_is_last": true, "title": ["I. \u003c種々の複素環窒素配位子による銀 (I) および金 (I) 錯体の合成と生理活性\u003e"], "weko_shared_id": -1}
I. <種々の複素環窒素配位子による銀 (I) および金 (I) 錯体の合成と生理活性>
http://hdl.handle.net/10487/1258
http://hdl.handle.net/10487/12580a7856a7-2422-4c58-9d44-c5b742063222
名前 / ファイル | ライセンス | アクション |
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kana-1-5-0030.pdf (527.4 kB)
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Item type | 紀要論文 / Departmental Bulletin Paper(1) | |||||
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公開日 | 2009-02-23 | |||||
タイトル | ||||||
タイトル | I. <種々の複素環窒素配位子による銀 (I) および金 (I) 錯体の合成と生理活性> | |||||
言語 | ||||||
言語 | eng | |||||
資源タイプ | ||||||
資源タイプ識別子 | http://purl.org/coar/resource_type/c_6501 | |||||
資源タイプ | departmental bulletin paper | |||||
著者 |
野宮, 健司
× 野宮, 健司× 小田, 宗宏× Nomiya, Kenji× Oda, Munehiro |
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抄録 | ||||||
内容記述タイプ | Abstract | |||||
内容記述 | (1) Two novel polymeric silver (I)-triphenylphosphine complexes with nitrogen-containing heterocycles, [Ag (1,2,3-triz) (PPh_3)_2]_n 3 and [Ag (1,2,4-triz) (PPh_3)_2]_n 4 (Htriz=triazole) were synthesized from reactions of polymeric precursors [Ag (1,2,3-triz)]_n 1 and [Ag (1,2,4-triz)]_n 2 with 3 equiv of PPh_3 in CH_2Cl_2,respectively. The polymeric precursors 1 and 2 have been obtained as a non-crystalline, colorless powder-solid : 2 showed a wide spectrum of excellent antibacterial activities, but 1 did not. The antimicrobial activities of the complexes 1-4,evaluated by MIC (minimum inhibitory concentration), were compared and key factors affecting them were discussed. The crystal structures of the complexes 3 and 4 were determined by single-crystal X-ray diffraction. The complexes 3 and 4 in the solid-state were helical polymers consisting of AgN_2P_2 cores formed by bridging triazolate anions and two PPh_3 ligands. The complexes 3 and 4 were also fully characterized by elemental analyses, TG/DTA and FT-IR in the solid-state and by various solution NMR (^<31>P, ^<109>Ag, ^1H and ^<13>C) spectroscopies and molecular weight measurements in solution. (2) Two novel gold (I)-triphenylphosphine complexes with nitrogen-containing heterocycles, [Au (1,2,3-L) (PPh_3)] 1 and [Au (1,2,4-L) (PPh_3)]_2・xH_2O (x=0.5-1.0) 2 (HL=triazole) were synthesized from stoichiometric reactions of a precursor complex [AuCl (PPh_3)] with HL in acetone in the presence of aqueous NaOH, and isolated as colorless needles and cubic crystals, respectively. The crystal structures of 1 and 2 were determined by single-crystal X-ray diffraction. 1 and 2 were also fully characterized by complete elemental analyses, TG/DTA and FT-IR in the solid-state and by solution NMR (^<31>P, ^1H and ^<13>C) spectroscopies and solution molecular-weight measurements. 1 consisted of a monomeric 2-coordinate AuNP core both in the solid-state and in solution, while, in contrast, 2 comprised a dimeric (AuNP)_2 core through an Au-Au bond in the solid-state, but a monomeric AuNP core in solution. Within the two gold (I) complexes composed of very closely related nitrogen-containing heterocycles and a common bulky PPh_3,ligand, it was found that the aggregation through the Au…Au interaction in 2 was overruled in 1. The molecular structures of 1 and 2 were also compared with those of the corresponding silver (I) analogs, [Ag (1,2,3-L) (PPh_3)_2]_n 3 and [Ag (1,2,4-L) (PPh_3)_2]_n 4,the molecular structures of both of which have been recently determined as helical polymers in the solid-state. (3) Polymeric silver (I) imidazolate [Ag (imd)]_n (1; Himd=imidazole, C_3H_4N_2) showing a wide spectrum of excellent antimicrobial activities against bacteria, yeast and mold, which has been obtained as non-crystalline, colorless powder, was successfully converted to molecular, crystalline complex [Ag (imd) (PPh_3)_3] 2 by a reaction of 1 with 3 equivalents of PPh_3 in CH_2Cl_2. This novel complex 2 was not obtained from reactions in solutions of the precursors [AgCl (PPh_3)_3] and/or [AgCl(PPh_3)_2]_2 with Himd in the presence of NaOH or with sodium salt of imd. On the contrary, the corresponding gold (I) complex [Au (imd) (PPh_3)] 3 was formed by a reaction of the precursor [AuCl (PPh_3)] and Himd in the presence of NaOH. From a synthetic viewpoint, these facts show the ordering of ligand replacement in these complexes to be Ag-P>>Ag-Cl>Ag-N, while Au-P>>Au-N>Au-Cl. This ordering also exhibits the different reactivity of silver (I) and gold (I) complexes with biological ligands such as proteins, enzymes, nucleic acids and amino acids. The complex 2 was fully characterized by complete elemental analyses, TG/DTA, FT-IR, solution molecular weight measurement and various solution NMR (^1H, ^<13>C, ^<31>P and ^<109>Ag) spectroscopies. The complex 2 in solution was present in a rapid equilibrium with the dissociated species of two PPh_3 ligands, i. e., [Ag (imd) (PPh_3)]. The ^<31>P NMR measurements at low temperature showed that (i) all PPh_3 ligands in 2 in CHCl_3 solution migrated at room temperature between the two isotopes ^<109>Ag and ^<107>Ag, in addition to the dissociation of two PPh_3 ligands, and (ii) there were present the 4-coordinate tetrahedral complex 2 and the dissociated complex [Ag (imd) (PPh_3)] in solution. | |||||
書誌情報 |
年報 巻 '98, p. 161-162, 発行日 1999-03 |
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書誌レコードID | ||||||
収録物識別子タイプ | NCID | |||||
収録物識別子 | AA11822302 | |||||
著者版フラグ | ||||||
出版タイプ | VoR | |||||
出版タイプResource | http://purl.org/coar/version/c_970fb48d4fbd8a85 | |||||
出版者 | ||||||
出版者 | 神奈川大学 |