5-溴化铌 98 | 13478-45-0

• 物质功能分类: 有机原料 - 有机金属盐
• 分子结构分类: 无机化合物 - 混合金属/非金属化合物 - 过渡金属盐
• 中文名称: 5-溴化铌 98
• 中文别名: 5-溴化铌98；5-溴化铌；溴化铌
• 英文名称: niobium pentabromide
• 英文别名: Niobium(5+);pentabromide
• CAS: 13478-45-0
• 化学式: Br₅Nb
• 分子量: 492.426
• InChiKey: DSYRJFDOOSKABR-UHFFFAOYSA-I

物化性质

• 熔点：
  150°C
• 沸点：
  361,6°C
• 密度：
  4.360
• 溶解度：
  溶于水、乙醇
• 稳定性/保质期：
  遵照规定使用和储存则不会分解，但在水中会分解。

计算性质

• 辛醇/水分配系数(LogP)：
  4.23
• 重原子数：
  6
• 可旋转键数：
  0
• 环数：
  0.0
• sp3杂化的碳原子比例：
  0.0
• 拓扑面积：
  0
• 氢给体数：
  0
• 氢受体数：
  0

ADMET

毒理性

• 副作用

Dermatotoxin - 皮肤烧伤。

Dermatotoxin - Skin burns.

来源:Haz-Map, Information on Hazardous Chemicals and Occupational Diseases

安全信息

• 危险等级：
  8
• 危险品标志：
  C
• 危险类别码：
  R20/21/22
• 危险品运输编号：
  UN 3260 8/PG 2
• WGK Germany：
  3
• 包装等级：
  III
• 危险类别：
  8
• 安全说明：
  S26,S27,S28,S36/37/39,S45
• 储存条件：
  存于阴凉干燥处

SDS

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Section 1: Product Identification
Chemical Name: Niobium (V) bromide (99.9%-Nb)
CAS Registry Number: 13478-45-0
Formula: NbBr5
EINECS Number: 236-778-5
Chemical Family: metal halide
Synonym: Niobium pentabromide, Columbium pentabromide

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Section 2: Composition and Information on Ingredients
Ingredient CAS Number Percent ACGIH (TWA) OSHA (PEL)
Title Compound 13478-45-0 100% no data no data

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Section 3: Hazards Identification
With moisture, this material becomes a strong, corrosive acid. The liquid and its vapor are extremely corrosive
Emergency Overview:
to skin, eyes, mucous membranes and respiratory tract.
Primary Routes of Exposure: Ingestion, inhalation, eyes and skin
Eye Contact: Severe corrosive to the eyes. Exposure can lead to permanent eye damage.
Skin Contact: Corrosive to skin. Contact can lead to redness, pain, blistering, ulceration, and scar formation.
Material releases corrosive fumes. Severe burning of the mucous membranes and lungs. Pulmonary edema
Inhalation:
may occur.
Product is a highly corrosive acid. Ingestion may cause pain, vomiting, burns of mouth and throat, and
Ingestion:
ulceration of gastrointestinal tract.
Acute Health Affects: Severe corrosive to eyes, skin, mucous membranes and respiratory tract. Ingestion may be fatal.
Repeated or prolonged exposure to bromides by any route may cause skin rashes (bromaderma) and central
Chronic Health Affects:
nervous system depression, including ataxia, psychoses, memory loss, irritability, and headache.
NTP: No
IARC: No
OSHA: No

---

SECTION 4: First Aid Measures
Immediately flush the eyes with copious amounts of water for at least 10-15 minutes. A victim may need
Eye Exposure:
assistance in keeping their eye lids open. Get immediate medical attention.
Wash the affected area with water. Remove contaminated clothes if necessary. Seek medical assistance if
Skin Exposure:
irritation persists.
Remove the victim to fresh air. Closely monitor the victim for signs of respiratory problems, such as difficulty
Inhalation:
in breathing, coughing, wheezing, or pain. In such cases seek immediate medical assistance.
Seek medical attention immediately. Keep the victim calm. Give the victim water (only if conscious). Induce
Ingestion:
vomiting only if directed by medical personnel.

---

SECTION 5: Fire Fighting Measures
Flash Point: not applicable
Autoignition Temperature: none
Explosion Limits: none
Extinguishing Medium: None. Material is non-flammable.
If this product is involved in a fire, fire fighters should be equipped with a NIOSH approved positive pressure
Special Fire Fighting Procedures:
self-contained breathing apparatus and full protective clothing.
Hazardous Combustion and none
Decomposion Products:
Unusual Fire or Explosion Hazards: No unusual fire or explosion hazards.

---

SECTION 6: Accidental Release Measures
Small spills can be mixed with powdered sodium bicarbonate, lime, or calcium carbonate and swept up. Avoid
Spill and Leak Procedures:
raising dust.

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SECTION 7: Handling and Storage
Store solid in a tightly sealed container away from moisture. Handle in a fume hood under a dry atmosphere of
Handling and Storage:
air or nitrogen. Prolonged exposure to the atmosphere may degrade the product.

---

SECTION 8: Exposure Controls and Personal Protection
Eye Protection: Always wear approved safety glasses when handling a chemical substance in the laboratory.
Skin Protection: Wear protective clothing and gloves. Consult with glove manufacturer to determine the proper type of glove.
Ventilation: The solid may form corrosive vapors. It should be handled in an efficient fume hood.
If in form of fine dust and ventilation is not available a respirator should be worn. The use of respirators
Respirator:
requires a Respirator Protection Program to be in compliance with 29 CFR 1910.134.
Ventilation: The solid may form corrosive vapors. It should be handled in an efficient fume hood.
Additional Protection: No additional protection required.

---

SECTION 9: Physical and Chemical Properties
Color and Form: -100 mesh reddish-brown pwdr.
Molecular Weight: 492.49
Melting Point: 150°
Boiling Point: 361.6°C
Vapor Pressure: no data
Specific Gravity: no data
Odor: pungent odor
Solubility in Water: reacts with water

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SECTION 10: Stability and Reactivity
Stability: moisture sensitive
Hazardous Polymerization: no hazardous polymerization
Conditions to Avoid: contact with moisture
Incompatibility: water, mineral acids and active metals
Decomposition Products: none

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SECTION 11: Toxicological Information
RTECS Data: No information available in the RTECS files.
Carcinogenic Effects: no data
Mutagenic Effects: no data
Tetratogenic Effects: no data

---

SECTION 12: Ecological Information
Ecological Information: No information available

---

SECTION 13: Disposal Considerations
Disposal: Dispose of according to local, state and federal regulations.

---

SECTION 14: Transportation
Shipping Name (CFR): Corrosive solids, N.O.S.
Hazard Class (CFR): 8
Additional Hazard Class (CFR): NA
Packaging Group (CFR): I
UN ID Number (CFR): UN# 1759
Shipping Name (IATA): Corrosive solid, N.O.S.
Hazard Class (IATA): 8
Additional Hazard Class (IATA): NA
Packaging Group (IATA): I
UN ID Number (IATA): UN# 1759

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SECTION 15: Regulatory Information
TSCA: Listed in the TSCA inventory.
SARA (Title 313): Title compound not listed.
Second Ingredient: none

---

SECTION 16 - ADDITIONAL INFORMATION
N/A

制备方法与用途

合成制备方法

先装配成如图V-3所示的装置。

1. 辅助接受管；
2. 产物；
3. 外热器；
4. Br₂；
5. N₂

其中，高温加热部分可采用高硼硅酸耐热玻璃或石英玻璃。而硼硅酸玻璃部分则用磨口连接。如不处于反应产物沸点以上的温度，则会堵塞系统，故其通路可用卷成螺旋形的加热器或将镍铬丝缠在石棉上进行加热。另外，可使用一个倒立的1L锥形烧瓶作为旋风分离器，并将上述加热器的端部与该烧瓶熔接起来；而在旋风分离器的下端，则与用作接受器的磨口圆底烧瓶相连接。为了减少摩擦，接受器的磨口最好不涂润滑脂，因此建议使用未涂润滑油的磨口或采用聚四氟乙烯套管。

按图所示方式组装后，将金属铌粉放入反应管中并使其位于加热部位，如有需要也可用试料舟。接着，反应管应先用氮气或氩气充满，并在通风柜中将溴充入分液漏斗里。此时，升温出口的加热器至产物沸点以上，然后装上分液漏斗。再用氮气(或氩气)预先清洗系统内部，从分液漏斗滴入少量溴至捕集器约一半的位置。

启动后，使氮气流量为500～600mL/min，并将溴导入金属铌粉上。由于溴的气化热会使捕集器冷却，在此过程中可以在敞口烧杯中用温水加热以保持温度。如果捕集器中的溴量减少，则可再次从分液漏斗中加入溴，重复进行此操作直至溴完全使用完毕后，再用氮气逐出剩余的溴，并迅速卸下接受器并加塞密封。

反应信息

• 作为反应物：
  描述：

  5-溴化铌 98 在 Nb 作用下， 以 neat (no solvent) 为溶剂， 生成 niobium(IV) chloride
  参考文献：
  名称：

  The Preparation and Properties of Niobium(IV) Compounds. I. Some Niobium(IV) Halides and their Pyridine Adducts

  摘要：

  DOI：

  10.1021/ic50007a029
• 作为产物：
  描述：

  tribromooxide niobium(V) 以 neat (no solvent) 为溶剂， 生成 5-溴化铌 98
  参考文献：
  名称：

  A STUDY OF THE SPECTRUM AND THE BROMIDES OF COLUMBIUM.¹

  摘要：

  DOI：

  10.1021/ja01953a002
• 作为试剂：
  描述：

  乙二醇二甲醚 在 5-溴化铌 98 、 水 作用下， 以 二氯甲烷 、 chloroform-d8 为溶剂， 反应 360.0h， 生成 1,4-二氧六环 、 2-溴乙基甲基醚
  参考文献：
  名称：

  Further insights into the chemistry of niobium and tantalum pentahalides with 1,2-dialkoxyalkanes: Synthesis of bromo- and iodoalkoxides, spectroscopic and computational studies

  摘要：

  The room temperature reactions of a series of 1,2-dialkoxyalkanes ROCH2CH(R')OR" with MX5 (M = Nb, Ta; X = Br, I) in 1:1 ratio result in single C-O bond cleavage and high-yield formation of the halo-alkoxides MBr4[K-2-OCH2CH(R')OR"] or [Nbl(4){K-1-OCH2CH(R')OR")](2), and equimolar amounts of the corresponding alkyl halides RX. The reaction of NbBr5 with 1,2-climethoxyethane, dme, proceeds with preliminary formation of the ionic species (NbBr4(K-2-dme)(K-1-dme)][NbBr6], 3b, which has been identified by solution NMR at low temperature and conductivity analyses. The gas-phase structure of 3b has been optimized by DFT calculations, confirming that the dme ligands adopt bidentate and monodentate coordination, respectively. Although the formation of NbOBr3(dme), 4b, 1,4-dioxane and MeBr from NbBr5/dme (ratio 1:2) is an exoergonic process (calculated Delta G(r)(degrees) = -115.96 kcal mol(-1)), it is inhibited at room temperature. High temperature conditions enhance the production of 1,4-dioxane at the expense of selectivity. The dinuclear species NbOBr3(dme)NbBr5 (Nb-O-Nb), 5b, (X-ray) has been isolated in modest yield as byproduct of the room temperature reaction of NbBr5 with dme. In general, the 1:2 molar reactions of NbX5 (X = Br. I) with ROCH2CH(R')OR" occur with the exclusion of nearly one equivalent of organic reactant. (C) 2011 Elsevier Ltd. All rights reserved.

  DOI：

  10.1016/j.poly.2011.03.005

文献信息

• Scanning tunneling and atomic force microscopy study of layered transition metal halides Nb3X8 (X = Cl, Br, I)
  作者：S. N. Magonov、P. Zoennchen、H. Rotter、H. J. Cantow、G. Thiele、J. Ren、M. H. Whangbo

  DOI：10.1021/ja00059a053

  日期：1993.3

  Niobium halides Nb[sub c]X[sub 8] (X = Cl, Br, I) are made up of layers of composition Nb[sub 3]X[sub 8], and the two surfaces (A and B) of their individual Nb[sub 3]X[sub 8] layers are not equivalent in atomic corrugations. The surfaces of these halides were examined by atomic force microscopy (AFM) and scanning tunneling microscopy (STM) to obtain atomic resolution images. For a given surface, AFM

  铌卤化物 Nb[sub c]X[sub 8] (X = Cl, Br, I) 由 Nb[sub 3]X[sub 8] 组成的层组成，它们的两个表面（A 和 B）单个 Nb[sub 3]X[sub 8] 层在原子波纹中是不等价的。通过原子力显微镜 (AFM) 和扫描隧道显微镜 (STM) 检查这些卤化物的表面以获得原子分辨率图像。对于给定的表面，AFM 图像与 STM 图像显着不同，并且 STM 图像的分辨率取决于隧道条件。通过计算总电子密度分布[rho](r[sub 0])和部分电子密度分布[rho](r[sub 0],e[sub f])来分析观察到的AFM和STM图像，对于单个 Nb[sub 3]X[sub 8] (X = Cl, Br, I) 层的两个表面。工作表明，AFM 和 STM 图像分别由 [rho](r[sub 0]) 和 [rho](r[sub 0], e[sub f]) 图很好地描述。AFM
• Reactivity of Niobium and Tantalum Pentahalides with Cyclic Ethers and the Isolation and Characterization of Intermediates in the Polymerization of Tetrahydrofuran
  作者：Fabio Marchetti、Guido Pampaloni、Stefano Zacchini

  DOI：10.1021/ic7012254

  日期：2008.1.1

  3f) result from reactions of MX5 with 0.5 and 1.5 equiv of THF, respectively. Compounds 3 contain the unprecedented 4-(tetrahydrofuran-1-ium)-butan-1-oxo ligand and are likely to play a role in the course of THF polymerization catalyzed by MX5. The addition of L (L = 2,5-dimethyltetrahydrofuran, tetrahydropyran, 1,4-dioxane) to MX5 results in the formation of the hexacoordinated complexes MX5(L). The

  配合物MX5（THF）（M = Nb，X = Cl，2a; M = Ta，X = F，2c，X = Cl，2d）和[MX4（THF）O（CH2）4O（CH2）3CH2） }] [MX6]（M = Nb，X = Cl，3a； M = Ta，X = Cl，3d，X = Br，3e，X = I，3f）是MX5与0.5和1.5当量的THF反应生成的， 分别。化合物3包含空前的4-（四氢呋喃-1-基）-丁-1-氧化配体，并可能在MX5催化的THF聚合过程中发挥作用。向MX5中添加L（L ＝ 2，5-二甲基四氢呋喃，四氢吡喃，1，4-二恶烷）导致六配位配合物MX5（L）的形成。X射线衍射研究确定了2d，3d和NbCl5（二恶烷）6a的分子结构。
• Fragmentation of oxygen-containing molecules via C–O bond cleavage promoted by coordination to niobium and tantalum pentahalides
  作者：Fabio Marchetti、Guido Pampaloni、Stefano Zacchini

  DOI：10.1039/b905023j

  日期：——

  Cl, ; X = Y = Br, ; X = I, Y = Br, ) slowly convert into the corresponding alkoxides [NbX(4)(OCH(2)CH(2)Y)](2) (X = Br, Y = Cl, ; X = Y = Br, ; X = I, Y = Br, ) in CDCl(3). The further conversion of to NbOBr(3), MeBr and Br(CH(2))(2)Br takes place at 60 degrees C. N(2)CHCO(2)Et behaves as a ligand with respect to NbF(5), whereas it undergoes fragmentation and halogenation when contacted with NbCl(5)

  新型mu-oxo配合物NbOX（3）[kappa（2）-O（Me）CH（2）CO（2）Me] NbX（5）（X = Cl，; X = Br，），NbOCl（3） [kappa（2）-（MeO（2）C）CH [双键，长度为m-破折号] CH（CO（2）Me）] NbCl（5）（）和NbOCl（3）[kappa（2）- CH（2）（CO（2）Me）（2）] NbCl（5）（）已通过卤化物NbX（5）（X = Cl，Br）与甲氧基甲基的摩尔比为1：1的反应以高收率制备乙酸盐[MeOCH（2）CO（2）Me]，马来酸二甲酯[（MeO（2）C）CH [双键，长度为m-dash] CH（CO（2）Me）]和丙二酸二甲酯[CH（2 ）（CO（2）Me）（2）]，分别在不同的实验条件下进行。NMR研究表明，和的氧代单元通过选择性断裂（CO键断裂）形成一半当量的有机材料。离子络合物[NbX（4）OO}（2）]
• Crystal Structure and Physical Properties of RbNb₄Br₁₁
  作者：Katja Habermehl、Holger Kleinke、Gerd Meyer

  DOI：10.1002/zaac.200900427

  日期：2010.1

  (Nb2–Nb2), respectively. The structure consists of [Nb4}Br6iBr10/2a–a]–cluster complex anions that are interconnected by two common edges and two faces to the next cluster complexes, thus forming a 2D undulated layer structure. The Rb+ ion is coordinated by 12 Br– ions in the shape of an anticuboctahedron. Electronic structure calculations indicate the presence of a band gap of approximately 0.33 eV

  RbNb4Br11 是通过铌粉、NbBr5 和 RbBr 在密封的铌管中在 500 °C 下固态反应获得的。它在正交空间群 Pmma 中结晶，a = 1699.5(1), b = 726.7(1), c = 694.5(1) pm, V = 857.6(1)·106 pm3, Z = 2，与 CsNb4Br11 同型。四个铌原子形成一个菱形簇，键距分别为 295 pm (Nb1–Nb2) 和 304 pm (Nb2–Nb2)。该结构由[Nb4}Br6iBr10/2a-a]-簇复合阴离子组成，这些阴离子通过两个公共边缘和两个面与下一个簇复合物互连，从而形成二维波浪状层结构。Rb+ 离子与 12 Br- 离子配位成反立方八面体。电子结构计算表明存在大约 0.33 eV 的带隙。
• Heavier halides of early transition elements by halide-exchange reactions. Crystal and molecular structure of [Ph3C]2[Hf2Cl10]
  作者：Fausto Calderazzo、Piersandro Pallavicini、Guido Pampaloni、Pier Francesco Zanazzi

  DOI：10.1039/dt9900002743

  日期：——

  The decahalogenodimetalates of zirconium(IV) and hafnium(IV) as their triphenylmethyl derivatives [Ph3C]2[M2Cl10] have been obtained by the reaction of M(BH4)4 with the appropriate Ph3CX or by addition of Ph3CX to MX4. The crystal and molecular structure of [Ph3C]2[Hf2Cl10] has been studied by X-ray diffraction methods: triclinic, space group P, a= 15.965(3), b= 12.907(3), c= 10.526(3)Å, α= 99.75(2)

  锆（的decahalogenodimetalates IV）和铪（IV）作为它们的三苯甲基衍生物[PH 3 C] 2 [M 2氯10 ]已经由M（BH反应得到4）4与适宜的pH 3 CX或通过加入Ph 3 CX转换为MX 4的过程。[ X 3 C] 2 [Hf 2 Cl 10 ]的晶体和分子结构已通过X射线衍射方法研究：三斜晶系，空间群P，a = 15.965（3），b= 12.907（3），c = 10.526（3）Å，α= 99.75（2），β= 84.84（2），γ= 102.64（2）°，Z =2。该结构由[Ph 3 C]组成+阳离子和[Hf 2 Cl 10 ] 2-阴离子，后者具有晶体对称性。氯化物桥接的二聚体具有扭曲的八面体配位，而[Ph 3 C] +阳离子在中心碳周围具有三角平面的几何形状。铌（V）和钽（V）的卤化物较重，是通过与Pr i Br进行交换反应从氯化物制备的（对于NbBr