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13320-71-3

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13320-71-3 Usage

Chemical Properties

black crystal(s); sensitive to both air and moisture [STR93]

Check Digit Verification of cas no

The CAS Registry Mumber 13320-71-3 includes 8 digits separated into 3 groups by hyphens. The first part of the number,starting from the left, has 5 digits, 1,3,3,2 and 0 respectively; the second part has 2 digits, 7 and 1 respectively.
Calculate Digit Verification of CAS Registry Number 13320-71:
(7*1)+(6*3)+(5*3)+(4*2)+(3*0)+(2*7)+(1*1)=63
63 % 10 = 3
So 13320-71-3 is a valid CAS Registry Number.
InChI:InChI=1/4ClH.Mo/h4*1H;/q;;;;+4/p-4/rCl4Mo/c1-5(2,3)4

13320-71-3SDS

SAFETY DATA SHEETS

According to Globally Harmonized System of Classification and Labelling of Chemicals (GHS) - Sixth revised edition

Version: 1.0

Creation Date: Aug 16, 2017

Revision Date: Aug 16, 2017

1.Identification

1.1 GHS Product identifier

Product name molybdenum tetrachloride

1.2 Other means of identification

Product number -
Other names Molybdenum chloride

1.3 Recommended use of the chemical and restrictions on use

Identified uses For industry use only.
Uses advised against no data available

1.4 Supplier's details

1.5 Emergency phone number

Emergency phone number -
Service hours Monday to Friday, 9am-5pm (Standard time zone: UTC/GMT +8 hours).

More Details:13320-71-3 SDS

13320-71-3Synthetic route

trans-(Et2O)2MoCl4
30411-56-4

trans-(Et2O)2MoCl4

molybdenum(IV) chloride
13320-71-3

molybdenum(IV) chloride

Conditions
ConditionsYield
In neat (no solvent, solid phase) MoCl4(Et2O)2 heated under vac. in oil bath at 120°C (5 h) or 130°C (2 h); elem. anal.;99%
tetrachloromethane
56-23-5

tetrachloromethane

molybdenum(IV) oxide

molybdenum(IV) oxide

κ-oxide

κ-oxide

molybdenum suboxide

molybdenum suboxide

A

molybdenum(VI) oxychloride

molybdenum(VI) oxychloride

B

carbon dioxide
124-38-9

carbon dioxide

C

carbon monoxide
201230-82-2

carbon monoxide

D

molybdenum(IV) chloride
13320-71-3

molybdenum(IV) chloride

Conditions
ConditionsYield
In neat (no solvent) Kinetics; byproducts: C2Cl4; heating of Mo oxides in stream of N2 with CCl4 (560 - 800 K); reaction followed by X-ray diffraction;
tetrachloromethane
56-23-5

tetrachloromethane

molybdenum
7439-98-7

molybdenum

A

phosgene
75-44-5

phosgene

B

molybdenum(VI) oxide chloride

molybdenum(VI) oxide chloride

C

molybdenum(IV) chloride
13320-71-3

molybdenum(IV) chloride

Conditions
ConditionsYield
With oxygen at 310°C;
molybdenum(V) chloride
10241-05-1

molybdenum(V) chloride

molybdenum
7439-98-7

molybdenum

A

molybdenum(VI) oxide chloride

molybdenum(VI) oxide chloride

B

molybdenum(IV) chloride
13320-71-3

molybdenum(IV) chloride

Conditions
ConditionsYield
In neat (no solvent) 300°C 2d, 250°C 5 d; sublimation (100°C, vac.), extraction (dry C2Cl4);
hydrogenchloride
7647-01-0

hydrogenchloride

molybdenum
7439-98-7

molybdenum

molybdenum(IV) chloride
13320-71-3

molybdenum(IV) chloride

Conditions
ConditionsYield
With water In neat (no solvent) byproducts: H2, MoCl4; at 1200°C by presence of H2O;;
In neat (no solvent) byproducts: H2; at 1200°C;;
In neat (no solvent) byproducts: H2; at 1200°C;;
With H2O In neat (no solvent) byproducts: H2, MoCl4; at 1200°C by presence of H2O;;
chlorine
7782-50-5

chlorine

molybdenum
7439-98-7

molybdenum

A

molybdenum(V) chloride
10241-05-1

molybdenum(V) chloride

B

molybdenum(IV) chloride
13320-71-3

molybdenum(IV) chloride

Conditions
ConditionsYield
In neat (no solvent) introduction of Cl2-gas (8-9 Torr/20 min/1.8 l/h) through purified (90min/H2 stream/1000°C) Mo powder (860 - 1160°C);; extraction of MoCl5 (CCl4); extraction MoCl4 (diethylether or water); further extraction (ethanol or water);;A n/a
B 0-10
molybdenum(IV) oxide

molybdenum(IV) oxide

boron trichloride
10294-34-5

boron trichloride

molybdenum(IV) chloride
13320-71-3

molybdenum(IV) chloride

Conditions
ConditionsYield
below 500 K;
tetrachloromethane
56-23-5

tetrachloromethane

molybdenum(IV) oxide

molybdenum(IV) oxide

A

molybdenum(VI) oxychloride

molybdenum(VI) oxychloride

B

carbon dioxide
124-38-9

carbon dioxide

C

carbon monoxide
201230-82-2

carbon monoxide

D

molybdenum(IV) chloride
13320-71-3

molybdenum(IV) chloride

Conditions
ConditionsYield
In neat (no solvent) Kinetics; byproducts: C2Cl4; heating of Mo oxide in stream of N2 with CCl4 (560 - 800 K); reaction followed by X-ray diffraction;
tetrachloromethane
56-23-5

tetrachloromethane

molybdenum(IV) oxide

molybdenum(IV) oxide

molybdenum(IV) chloride
13320-71-3

molybdenum(IV) chloride

Conditions
ConditionsYield
In neat (no solvent) reaction on heating pulverized MoO2 with CCl4 to 250°C in a closed tube for 8h;;90-92
High Pressure; at 250°C in an autoclave, 8 h;90-92
In neat (no solvent) react. of MoO2 with CCl4 at 250°C;;
In neat (no solvent) react. of MoO2 with CCl4 at 250°C;;
In neat (no solvent) reaction on heating pulverized MoO2 with CCl4 to 250°C in a closed tube for 8h;;90-92
tetrachloromethane
56-23-5

tetrachloromethane

molybdenum(IV) oxide

molybdenum(IV) oxide

A

molybdenum(V) chloride
10241-05-1

molybdenum(V) chloride

B

molybdenum(IV) chloride
13320-71-3

molybdenum(IV) chloride

Conditions
ConditionsYield
With pyrographite mass ratio MoO2:C = 5:1; mixt. heated at 300°C in a flow of N2 loaded with CCl4; absence of moisture and oxygen; further by-product: Mo oxide chloride; removal of MoCl5 and Mo oxide chloride by vac. distn.;A <1
B n/a
molybdenum(IV) oxide

molybdenum(IV) oxide

chlorine
7782-50-5

chlorine

molybdenum(IV) chloride
13320-71-3

molybdenum(IV) chloride

Conditions
ConditionsYield
In Hexachlorobutadiene MoO2 refluxed in hexachloro-1,3-butadiene satd. with chlorine for 24 h; MoCl4 crystals obtained on cooling;
With tetrachloromethane In neat (no solvent) heating of powdered MoO2 with a dry mixt. of Cl2 and CCl4 at 250°C in a closed tube for several hours;; washing with CCl4; drying in vac.;;
With CCl4 In neat (no solvent) heating of powdered MoO2 with a dry mixt. of Cl2 and CCl4 at 250°C in a closed tube for several hours;; washing with CCl4; drying in vac.;;
molybdenum(VI) fluoride
7783-77-9

molybdenum(VI) fluoride

phosphorus trichloride
7719-12-2, 52843-90-0

phosphorus trichloride

A

molybdenum(V) fluoride
13819-84-6, 194303-41-8

molybdenum(V) fluoride

phosphorus pentafluoride
7647-19-0, 874483-74-6

phosphorus pentafluoride

C

chlorine
7782-50-5

chlorine

D

trifluorophosphane
7783-55-3

trifluorophosphane

E

molybdenum(IV) chloride
13320-71-3

molybdenum(IV) chloride

Conditions
ConditionsYield
In not given react. with an excess of MoF6 forming PF3, MoCl5 and Cl2; react. of MoCl5 forming MoCl4 and Cl2; further react. of MoF6 with PF3 forming PF5 and MoF5;;
In not given react. with an excess of MoF6 forming PF3, MoCl5 and Cl2; react. of MoCl5 forming MoCl4 and Cl2; further react. of MoF6 with PF3 forming PF5 and MoF5;;
tetramethylstannane
594-27-4

tetramethylstannane

molybdenum(V) chloride
10241-05-1

molybdenum(V) chloride

A

trimethyltin(IV)chloride
1066-45-1

trimethyltin(IV)chloride

B

molybdenum(IV) chloride
13320-71-3

molybdenum(IV) chloride

Conditions
ConditionsYield
byproducts: CH3Cl; 2-fold excess of MoCl5;
byproducts: CH3Cl; 2-fold excess of MoCl5;
tungsten(V) chloride
13470-14-9

tungsten(V) chloride

molybdenum(V) chloride
10241-05-1

molybdenum(V) chloride

A

tungsten(VI) chloride
13283-01-7

tungsten(VI) chloride

B

molybdenum(IV) chloride
13320-71-3

molybdenum(IV) chloride

Conditions
ConditionsYield
In neat (no solvent)
molybdenum(III) chloride
13478-18-7

molybdenum(III) chloride

A

molybdenum(II) chloride

molybdenum(II) chloride

B

molybdenum(IV) chloride
13320-71-3

molybdenum(IV) chloride

Conditions
ConditionsYield
With carbon dioxide In neat (no solvent) heating of MoCl3 in a stream of CO2 at weak red heat;; condensation of the volatile MoCl4;;
With carbon dioxide In neat (no solvent) heating of MoCl3 in CO2;;
With CO2 In neat (no solvent) heating of MoCl3 in a stream of CO2 at weak red heat;; condensation of the volatile MoCl4;;
With CO2 In neat (no solvent) heating of MoCl3 in CO2;;
molybdenum dichloride

molybdenum dichloride

molybdenum(III) chloride
13478-18-7

molybdenum(III) chloride

molybdenum(IV) chloride
13320-71-3

molybdenum(IV) chloride

Conditions
ConditionsYield
In neat (no solvent) react. in a quartz optical cell;
molybdenum(VI) oxychloride

molybdenum(VI) oxychloride

molybdenum(V) chloride
10241-05-1

molybdenum(V) chloride

A

molybdenum(VI) oxide chloride

molybdenum(VI) oxide chloride

B

Mo2O3Cl4

Mo2O3Cl4

C

molybdenum(IV) chloride
13320-71-3

molybdenum(IV) chloride

Conditions
ConditionsYield
In melt melting of MoCl5 and MoO2Cl2 in a closed tube;; sublimation in a stream of dry CO2; Mo2O3Cl6 as residue; volatile MoCl4;;
In melt melting of MoCl5 and MoO2Cl2 in a closed tube;; sublimation in a stream of dry CO2; Mo2O3Cl6 as residue; volatile MoCl4;;
molybdenum(V) chloride
10241-05-1

molybdenum(V) chloride

molybdenum(IV) chloride
13320-71-3

molybdenum(IV) chloride

Conditions
ConditionsYield
In 1,1,2,2-tetrachloroethylene MoCl5 refluxed in tetrachloroethylene in evacuated and sealed vessel for 3 d; washed with CCl4;
In 1,1,2,2-tetrachloroethylene MoCl5 refluxed in tetrachloroethylene in evacuated, sealed vessel 3 d; washed with CCl4 in inert-atmosphere glove-box;
trans-Co2[Mo(CN)2(C2H8N2)2(OH)2]Cl4*4H2O

trans-Co2[Mo(CN)2(C2H8N2)2(OH)2]Cl4*4H2O

A

cobalt
7440-48-4

cobalt

B

molybdenum(IV) chloride
13320-71-3

molybdenum(IV) chloride

Conditions
ConditionsYield
In neat (no solvent) Kinetics; byproducts: H2O, ethylenediamine; sample heating in N2 flow (60 ml/min) at 10 K/min up to 550°C; TG, DTG, DSC;
2Cu(2+)*Mo(4+)*2CN(1-)*2OH(1-)*H2NC2H4NH2*2H2O*4Cl(1-)=Cu2[Mo(CN)2(OH)2(C2H8N2)(H2O)2]Cl4

2Cu(2+)*Mo(4+)*2CN(1-)*2OH(1-)*H2NC2H4NH2*2H2O*4Cl(1-)=Cu2[Mo(CN)2(OH)2(C2H8N2)(H2O)2]Cl4

A

copper(l) cyanide

copper(l) cyanide

B

molybdenum(IV) chloride
13320-71-3

molybdenum(IV) chloride

C

copper(II) oxide

copper(II) oxide

Conditions
ConditionsYield
In neat (no solvent) Kinetics; byproducts: H2O, ethylenediamine; sample heating in N2 flow (50 ml/min) at 10 K/min between 30-800°C; TG, DTG, DSC;
diethyl ether
60-29-7

diethyl ether

molybdenum(V) chloride
10241-05-1

molybdenum(V) chloride

molybdenum(IV) chloride
13320-71-3

molybdenum(IV) chloride

Conditions
ConditionsYield
With Sn according to P. Stoffelbach, D. Saurenz, R. Poli, Eur. J. Inorg. Chem. (2007) 2699-2703; MoCl4(OEt2)2 dried under reduced pressure at 0°C, transferred to Schlenk flask heated for 1 h at 80°C;
trans-[MoCl4(nBu2S)2]

trans-[MoCl4(nBu2S)2]

molybdenum(IV) chloride
13320-71-3

molybdenum(IV) chloride

Conditions
ConditionsYield
In neat (no solvent) at 25 - 300℃; under 760.051 Torr; Inert atmosphere;
molybdenum(IV) chloride
13320-71-3

molybdenum(IV) chloride

acetonitrile
75-05-8

acetonitrile

bis(acetonitrile)tetrachloromolybdenum(IV)
56613-96-8, 77210-60-7, 15584-93-7, 19187-82-7

bis(acetonitrile)tetrachloromolybdenum(IV)

Conditions
ConditionsYield
In acetonitrile stirring (2 days); solvent removal (vac.);100%
phosphorus pentachloride
10026-13-8, 874483-75-7

phosphorus pentachloride

molybdenum(IV) chloride
13320-71-3

molybdenum(IV) chloride

2PCl4(1+)*[Mo2Cl10](2-)=[PCl4]2[Mo2Cl10]

2PCl4(1+)*[Mo2Cl10](2-)=[PCl4]2[Mo2Cl10]

Conditions
ConditionsYield
In neat (no solvent) vac.; equimolar amts., heating (temp. gradient 250-220°C);100%
molybdenum(IV) chloride
13320-71-3

molybdenum(IV) chloride

lithium tert-butoxide
1907-33-1

lithium tert-butoxide

Tetrakis(tert-butoxy)molybdaen(IV)
60624-53-5

Tetrakis(tert-butoxy)molybdaen(IV)

Conditions
ConditionsYield
In tetrahydrofuran; hexane under Ar; THF added to MoCl4, suspn. cooled (ice bath), soln. of LiOtBu in THF/hexane added with syringe, mixt. stirred for 1 h at 0°C, slowly warmed to room temp., stirred overnight; THF removed (vac.), residue extd. with pentane, then with CH2Cl2, filtered, combined extracts evapd. in vac., recrystd. from cold pentane (low yield); elem. anal.;99%
tetrahydrofuran
109-99-9

tetrahydrofuran

molybdenum(IV) chloride
13320-71-3

molybdenum(IV) chloride

[MoCl4(tetrahydrofuran)2]
16998-75-7

[MoCl4(tetrahydrofuran)2]

Conditions
ConditionsYield
In tetrahydrofuran; pentane under Ar; MoCl5 suspd. in pentane, THF added, mixt. stirred for 2 min; liquid removed via cannula, residue dried;99%
tellurium tetrachloride
10026-07-0

tellurium tetrachloride

molybdenum(IV) chloride
13320-71-3

molybdenum(IV) chloride

2TeCl3(1+)*MoCl6(2-) = (TeCl3)2MoCl6

2TeCl3(1+)*MoCl6(2-) = (TeCl3)2MoCl6

Conditions
ConditionsYield
In melt evacuated glass ampoule: heating to 300°C for melting, after solidifying the ampoule is brought into a temp. gradient from 195 to 180°C; crystn. within some d;99%
tetraethylammonium trichloro-stannate(II)
7781-71-7

tetraethylammonium trichloro-stannate(II)

molybdenum(IV) chloride
13320-71-3

molybdenum(IV) chloride

2N(C2H5)4(1+)*MoCl4(SnCl3)2(2-)=[N(C2H5)4]2[MoCl4(SnCl3)2]
78004-09-8

2N(C2H5)4(1+)*MoCl4(SnCl3)2(2-)=[N(C2H5)4]2[MoCl4(SnCl3)2]

Conditions
ConditionsYield
In dichloromethane CH2Cl2 soln. of Sn-salt was added to suspn. of MoCl4 in CH2Cl2, mixt. was stirred for a few d under N2; filtered off, washed with CH2Cl2, dried in vac.; elem. anal.;98%
2-Picolinic acid
98-98-6

2-Picolinic acid

molybdenum(IV) chloride
13320-71-3

molybdenum(IV) chloride

A

Mo(pic)2Cl2

Mo(pic)2Cl2

B

Mo(NC5H4COO)3Cl
87739-32-0

Mo(NC5H4COO)3Cl

Conditions
ConditionsYield
In toluene under N2 atm. MoCl4 and picolinic acid (molar ratio 1:3) in toluene heated with stirring under reflux conditions for 22 h; slurry allowed to cool and filtered, solid washed with toluene and dried in vacuo at 150°C for 20 h; elem. anal.;A 10%
B 90%
In toluene under N2 atm. MoCl4 and picolinic acid (molar ratio 1:3) in toluene heated with stirring under reflux conditions for 5 h; slurry allowed to cool and filtered, solid washed with toluene and dried in vacuo at 150°C for 20 h; elem. anal.;A 30%
B 70%
2-Picolinic acid
98-98-6

2-Picolinic acid

molybdenum(IV) chloride
13320-71-3

molybdenum(IV) chloride

B

Mo(NC5H4COO)3Cl
87739-32-0

Mo(NC5H4COO)3Cl

Conditions
ConditionsYield
In toluene under N2 atm. MoCl4 and picolinic acid (molar ratio 1:4) in toluene heated with stirring under reflux conditions for 65 h; slurry allowed to cool and filtered, solid washed with toluene and dried in vacuo at 150°C for 20 h - Mo(pic)3Cl; filtrate reduced in volume and allowed to sit at room temp. for 24 h, ppt. collected and washed with toluene; elem. anal.;A 2%
B 88%
diethyl sulphide
352-93-2

diethyl sulphide

molybdenum(IV) chloride
13320-71-3

molybdenum(IV) chloride

trans-[MoCl4(SEt2)2]
162763-29-3

trans-[MoCl4(SEt2)2]

Conditions
ConditionsYield
In neat (no solvent) absence of moisture; stirring (12 h, 20°C); filtn., crystn. (-30°C), drying (vac.), recrystn. (toluene); elem. anal.;82%
dimethylacetylene
503-17-3

dimethylacetylene

diethyl ether
60-29-7

diethyl ether

molybdenum(IV) chloride
13320-71-3

molybdenum(IV) chloride

Mo(C2(CH3)2)Cl4(C2H5OC2H5)
107847-83-6

Mo(C2(CH3)2)Cl4(C2H5OC2H5)

Conditions
ConditionsYield
In diethyl ether under N2; slow addn. of MoCl4 to ether, addn. of alkyne, stirred for 12-16 h; filtered, dried (vac.);80%
diethyl ether
60-29-7

diethyl ether

hex-3-yne
928-49-4

hex-3-yne

molybdenum(IV) chloride
13320-71-3

molybdenum(IV) chloride

Mo(C2(C2H5)2)Cl4(C2H5OC2H5)
107847-76-7

Mo(C2(C2H5)2)Cl4(C2H5OC2H5)

Conditions
ConditionsYield
In diethyl ether MoCl4 slowly added to Et2O, 2 equiv. of 3-hexyne added, stirred overnight; pptn.;80%
In diethyl ether under N2; slow addn. of MoCl4 to ether, addn. of alkyne, stirred for 12-16 h; filtered, dried (vac.);80%
diethyl ether
60-29-7

diethyl ether

diphenyl acetylene
501-65-5

diphenyl acetylene

molybdenum(IV) chloride
13320-71-3

molybdenum(IV) chloride

Mo(C2(C6H5)2)Cl4(C2H5OC2H5)

Mo(C2(C6H5)2)Cl4(C2H5OC2H5)

Conditions
ConditionsYield
In diethyl ether under N2; slow addn. of MoCl4 to ether, addn. of alkyne, stirred for 12-16 h; filtered, dried (vac.);80%
chloroxine
773-76-2

chloroxine

molybdenum(IV) chloride
13320-71-3

molybdenum(IV) chloride

A

chlorotris(5,7-dichloro-8-quinolinolato)molybdenum(IV)
74620-90-9

chlorotris(5,7-dichloro-8-quinolinolato)molybdenum(IV)

B

dichlorobis(5,7-dichloro-8-quinolinolato)molybdenum(IV)
74594-57-3

dichlorobis(5,7-dichloro-8-quinolinolato)molybdenum(IV)

Conditions
ConditionsYield
In toluene under N2 atm. MoCl4 and 5,7-dichloro-8-quinolinol (molar ratio 1:3) in toluene heated with stirring under reflux conditions for 1 h; solvent removed under vac., residue dissolved in toluene, volume reduced and soln. allowed to sit at room temp. for 24 h, soln. filtered, ppt. washed with toluene, product dried in vacuo at 160°C for 36 h; elem. anal.;A 80%
B 1%
In dichloromethane under N2 atm. MoCl4 and 5,7-dichloro-8-quinolinol (molar ratio 1:3) in CH2Cl2 heated with stirring under reflux conditions for 5 h; soln. filtered, ppt. extd. in Soxhlet extractor with CH2Cl2 for 18 h, residue dried in vacuo at 150°C for 20 h; elem. anal.;A 71%
B 3%
In toluene under N2 atm. MoCl4 and 5,7-dichloro-8-quinolinol (molar ratio 1:2.7) in toluene heated with stirring under reflux conditions for 4 h; solvent removed under vac., residue dissolved in toluene, volume reduced and soln. allowed to sit at room temp. for 24 h, soln. filtered, ppt. washed with toluene, product dried in vacuo at 160°C for 36 h; elem. anal.;A 60%
B 10%
In dichloromethane under N2 atm. MoCl4 and 5,7-dichloro-8-quinolinol (molar ratio 1:2) in CH2Cl2 heated with stirring under reflux conditions for 3 h; soln. filtered, ppt. extd. in Soxhlet extractor with CH2Cl2 for 18 h, residue dried in vacuo at 150°C for 20 h; elem. anal.;A 18%
B 46%
In dichloromethane under N2 atm. MoCl4 and 5,7-dichloro-8-quinolinol (molar ratio 1:3) in CH2Cl2 heated with stirring under reflux conditions for 1 h; soln. filtered, ppt. extd. in Soxhlet extractor with CH2Cl2 for 18 h, residue dried in vacuo at 150°C for 20 h; elem. anal.;A 19%
B 28%
5-Chloro-8-hydroxyquinoline
130-16-5

5-Chloro-8-hydroxyquinoline

molybdenum(IV) chloride
13320-71-3

molybdenum(IV) chloride

dichlorobis(5-chloro-8-quinolinolato)molybdenum (IV)
87739-28-4

dichlorobis(5-chloro-8-quinolinolato)molybdenum (IV)

Conditions
ConditionsYield
In toluene under N2 atm. MoCl4 and 5-chloro-8-quinolinol (molar ratio 1:2) in toluene heated with stirring under reflux conditions for 6 h; soln. filtered, solid extd. in Soxhlet extractor with CH2Cl2 for 15 h, residue dried in vacuo for 18 h at 150°C; elem. anal.;78%
In toluene under N2 atm. MoCl4 and 5-chloro-8-quinolinol in toluene heated with stirring under reflux conditions for 5.5 h; soln. filtered, solid extd. in Soxhlet extractor with CH2Cl2 for 15 h, residue dried in vacuo for 18 h at 150°C; elem. anal.;70%
chloroxine
773-76-2

chloroxine

molybdenum(IV) chloride
13320-71-3

molybdenum(IV) chloride

chlorotris(5,7-dichloro-8-quinolinolato)molybdenum(IV)
74620-90-9

chlorotris(5,7-dichloro-8-quinolinolato)molybdenum(IV)

Conditions
ConditionsYield
In toluene under N2 atm. MoCl4 and 5,7-dichloro-8-quinolinol in toluene heated with stirring under reflux conditions for 5 h; solvent removed under vac., residue dissolved in toluene, volume reduced and soln. allowed to sit at room temp. for 24 h, soln. filtered, ppt. washed with toluene, product dried in vacuo at 160°C for 36 h; elem. anal.;74%
LiC5H4CH2C6H2(OCH3)3

LiC5H4CH2C6H2(OCH3)3

molybdenum(IV) chloride
13320-71-3

molybdenum(IV) chloride

bis-[(3,4,5-trimethoxybenzyl)czclopentadienyl]molybdenum(IV) dichloride
1229643-41-7

bis-[(3,4,5-trimethoxybenzyl)czclopentadienyl]molybdenum(IV) dichloride

Conditions
ConditionsYield
In tetrahydrofuran byproducts: LiCl; in Schlenk flask; Li compd. in THF added via cannula to THF soln. of MoCl4; refluxed for 20 h at 88°C; allowed to cool to room temp.; solvent removed under reduced pressure; washed with pentane, redissolvedin CH2Cl2, allowed to settle for 10 min; filtered through frit; solvent removed under reduced pressure, washed with pentane; elem. anal.;64.8%
molybdenum(IV) chloride
13320-71-3

molybdenum(IV) chloride

riboflavine
53187-51-2

riboflavine

trichlorooxo(riboflavin-1-ium)molybdenum(IV)

trichlorooxo(riboflavin-1-ium)molybdenum(IV)

Conditions
ConditionsYield
In methanol under protective gas, stirred at room temp. for 48 h; filtrated, toluene/cyclohexane added, allowed to stand at 4°C overnight, dried in high vacuum, elem. anal.;58%
8-quinolinol
148-24-3

8-quinolinol

molybdenum(IV) chloride
13320-71-3

molybdenum(IV) chloride

A

dichlorobis(8-quinolinolato)molybdenum (IV)
36470-65-2

dichlorobis(8-quinolinolato)molybdenum (IV)

B

Mo(q)3Cl

Mo(q)3Cl

Conditions
ConditionsYield
In toluene under N2 atm. MoCl4 and 8-quinolinol (molar ratio 1:3) in toluene heated with stirring under reflux conditions for 4 h; soln. allowed to cool, extd. with CH2Cl2 in Soxhlet-type extractor for 144 h, residue washed with hot toluene and CH2Cl2 and dried in vacuo at 150°C for 15 h; elem. anal.;A 51%
B 23%
2-[[(2-hydroxyphenyl)imino]methyl]phenol
1761-56-4

2-[[(2-hydroxyphenyl)imino]methyl]phenol

molybdenum(IV) chloride
13320-71-3

molybdenum(IV) chloride

MoO(2-salicylideneaminophenolate)(DMF)
80630-33-7

MoO(2-salicylideneaminophenolate)(DMF)

Conditions
ConditionsYield
With N,N-dimethyl-formamide In ethanol; N,N-dimethyl-formamide to a slurry of MoCl4 in MeOH was added a soln. of the ligand in DMF, the mixt. was stirred for a few h (N2 atm.); cooled to -20°C, solid was filtered off, washed with MeOH, dried in vac.;48%
n-butyllithium
109-72-8, 29786-93-4

n-butyllithium

2-methylpropan-2-thiol
75-66-1

2-methylpropan-2-thiol

molybdenum(IV) chloride
13320-71-3

molybdenum(IV) chloride

Mo(t-BuS)4

Mo(t-BuS)4

Conditions
ConditionsYield
In tetrahydrofuran; 1,2-dimethoxyethane n-BuLi in hexane added slowly to t-BuSH in THF at 0°C, stirred for 30 min, THF added, then added to MoCl4 in DME at 0°C, stirredfor 4 h; evapd. under vac., extd. with hexane, filtered, recrystd. from hexane at 0°C, elem.anal.;45%
LiC5H4CH2C6H4OCH3

LiC5H4CH2C6H4OCH3

molybdenum(IV) chloride
13320-71-3

molybdenum(IV) chloride

bis-[(p-methoxybenzyl)cyclopentadienyl]molybdenum(IV) dichloride
1229643-39-3

bis-[(p-methoxybenzyl)cyclopentadienyl]molybdenum(IV) dichloride

Conditions
ConditionsYield
In tetrahydrofuran byproducts: LiCl; in Schlenk flask; Li compd. in THF added via cannula to THF soln. of MoCl4; refluxed for 20 h; allowed to cool to room temp.; solvent removed under reduced pressure; washed with pentane, redissolvedin CH2Cl2, allowed to settle for 10 min; filtered through frit; solvent removed under reduced pressure, washed with pentane; elem. anal.;41.5%
nitroxoline
4008-48-4

nitroxoline

molybdenum(IV) chloride
13320-71-3

molybdenum(IV) chloride

A

chlorotris(5-nitro-8-quinolinolato)molybdenum(IV)
87739-30-8

chlorotris(5-nitro-8-quinolinolato)molybdenum(IV)

B

dichlorobis(5-nitro-8-quinolinolato)molybdenum (IV)

dichlorobis(5-nitro-8-quinolinolato)molybdenum (IV)

Conditions
ConditionsYield
In dichloromethane under N2 atm. MoCl4 and 5-nitro-8-quinolinol (molar ratio 1:3) in CH2Cl2 heated under reflux conditions with stirring for 16 h; solvent removed under vac., residue washed with hot toluene, washes combined, volume soln. reduced, soln. allowed to sit at room temp. for 24 hand filtered, product dried in vacuo at 150°C for 20 h; elem. anal.;A 6%
B 40%
In toluene under N2 atm. MoCl4 and 5-nitro-8-quinolinol (molar ratio 1:3) in toluene heated under reflux conditions with stirring for 5 h; solvent removed under vac., residue washed with hot toluene, washes combined, volume soln. reduced, soln. allowed to sit at room temp. for 24 hand filtered, product dried in vacuo at 150°C for 20 h; elem. anal.;A 3%
B 20%
LiC5H4CH2C6H3(OCH3)2

LiC5H4CH2C6H3(OCH3)2

molybdenum(IV) chloride
13320-71-3

molybdenum(IV) chloride

bis-[(3,4-dimethoxybenzyl)cyclopentadienyl]molybdenum(IV)dichloride
1229643-40-6

bis-[(3,4-dimethoxybenzyl)cyclopentadienyl]molybdenum(IV)dichloride

Conditions
ConditionsYield
In tetrahydrofuran byproducts: LiCl; in Schlenk flask; Li compd. in THF added via cannula to THF soln. of MoCl4; refluxed for 20 h at 88°C; allowed to cool to room temp.; solvent removed under reduced pressure; washed with pentane, redissolvedin CH2Cl2, allowed to settle for 10 min; filtered through frit; solvent removed under reduced pressure, washed with pentane; elem. anal.;32.3%
2,4,6-Triisopropylthiophenol
22693-41-0

2,4,6-Triisopropylthiophenol

molybdenum(IV) chloride
13320-71-3

molybdenum(IV) chloride

A

hexakis(2,4,6-triisopropylbenzenethiolato)dimolybdenum(III)
97352-51-7

hexakis(2,4,6-triisopropylbenzenethiolato)dimolybdenum(III)

B

MoO(SC6H2(CH(CH3)2)3)4(1-)*P(C6H5)4(1+)={MoO(SC6H2(CH(CH3)2)3)4}{P(C6H5)4}
97352-54-0

MoO(SC6H2(CH(CH3)2)3)4(1-)*P(C6H5)4(1+)={MoO(SC6H2(CH(CH3)2)3)4}{P(C6H5)4}

Conditions
ConditionsYield
With Na In 1,2-dimethoxyethane Schlenk, N2; the thiophenol in DME is treated with Na pieces, stirred at 50°C for 1 h, cooled to room temp., filtered, soln. of MoCl4 in DME is added, mixt. is stirred (room temp., 16 h), filtered (Celite), solid is washed (MeOH), Ph4PBr is added; resulting solid is the oxo product, filtrate is evapd. to dryness, residue is triturated with pentane, solid is filtered off, washed with MeOH, recrystd. (CH2Cl-MeCN); elem. anal.;A 25%
B 30%
mesitylthiol
1541-10-2

mesitylthiol

molybdenum(IV) chloride
13320-71-3

molybdenum(IV) chloride

Mo2(SC6H2(CH3)3)6
86350-27-8

Mo2(SC6H2(CH3)3)6

Conditions
ConditionsYield
With Na In 1,2-dimethoxyethane under N2, Schlenk technique; the thiophenol in DME is treated with Na metal pieces and stirred at 50°C for 1 h, cooled to room temp., filtered, MoCl4 is added, mixt. is stirred for 0.5 h; filtered (Celite), evapd. to dryness, extd. (hexane), recrystd. (THF-hexane); elem. anal.;28%
N,N'-bis(salicylidene)-o-phenylenediamine
3946-91-6

N,N'-bis(salicylidene)-o-phenylenediamine

molybdenum(IV) chloride
13320-71-3

molybdenum(IV) chloride

dichloro(N,N'-disalicylidene-1,2-diaminobenzene)molybdenum(IV)
87739-29-5

dichloro(N,N'-disalicylidene-1,2-diaminobenzene)molybdenum(IV)

Conditions
ConditionsYield
In toluene under N2 atm. MoCl4 and N,N'-disalicylidene-1,2-diaminobenzene in toluene heated with stirring under reflux conditions for 2 h; solvent removed under vac., residue extd. with CH2Cl2 in Soxhlet-type extractor for 24 h, residue dried in vacuo at 150°C for 24 h; elem. anal.;24%
5-Chloro-8-hydroxyquinoline
130-16-5

5-Chloro-8-hydroxyquinoline

molybdenum(IV) chloride
13320-71-3

molybdenum(IV) chloride

A

dichlorobis(5-chloro-8-quinolinolato)molybdenum (IV)
87739-28-4

dichlorobis(5-chloro-8-quinolinolato)molybdenum (IV)

B

Mo(cq)3Cl

Mo(cq)3Cl

Conditions
ConditionsYield
In dichloromethane under N2 atm. MoCl4 and 5-chloro-8-quinolinol (molar ratio 1:2) in CH2Cl2 heated with stirring under reflux conditions for 3 h; soln. filtered, solid extd. in Soxhlet extractor with CH2Cl2 for 15 h, residue dried in vacuo for 18 h at 150°C; elem. anal.;A 20%
B 5%
broxyquinoline
521-74-4

broxyquinoline

molybdenum(IV) chloride
13320-71-3

molybdenum(IV) chloride

chlorotris(5,7-dibromo-8-quinolinolato)molybdenum(IV)
87739-31-9

chlorotris(5,7-dibromo-8-quinolinolato)molybdenum(IV)

Conditions
ConditionsYield
In toluene under N2 atm. MoCl4 and 5,7-dibromo-8-quinolinol in toluene heated withstirring under reflux conditions for 5 h; solvent removed under vac., residue dissolved in toluene, volume reduced and soln. allowed to sit at room temp. for 24 h, soln. filtered, ppt. washed with toluene, product dried in vacuo at 160°C for 36 h; elem. anal.;20%
trithiazyl trichloride
105454-00-0, 105453-99-4, 5964-00-1

trithiazyl trichloride

molybdenum(IV) chloride
13320-71-3

molybdenum(IV) chloride

A

{(chlorothionitreno)pentachloromolybdenum(VI)}={(Chlorthionitreno)pentachloromolybdaen(VI)}

{(chlorothionitreno)pentachloromolybdenum(VI)}={(Chlorthionitreno)pentachloromolybdaen(VI)}

B

Mo(6+)*3Cl(1-)*N3S2(3-)=Mo(N3S2)Cl3

Mo(6+)*3Cl(1-)*N3S2(3-)=Mo(N3S2)Cl3

Conditions
ConditionsYield
In dichloromethane byproducts: Cl2; (exclusion of moisture); addn. of (NSCl)3 to MoCl4 in CH2Cl2 at 0-degree.C with stirring, stirring for 30 h at room temp.; filtn., cooling of the filtrate to -10°C, filtn. of the obtained crystals, washing (CH2Cl2/CCl4), drying in vac., elem. anal.;A 9%
B n/a

13320-71-3Relevant articles and documents

Snythesis, characterization and thermal dissociation of cobalt(II) complexes of the photoproducts of octacyanomolybdate(IV) and -tungstate(IV) with ethylenediamine

Ali,Majid, Kowsar

, p. 141 - 149 (1998)

Photosubstituted mixed ligand complexes of Co(II) with irradiated solutions of Mo(CN)84- and W(CN)84- with ethylenediamine have been synthesized. The complexes have been isolated and characterized by their elemental analysis and IR spectroscopy. The assigned formulae are Co2[Mo(CN)2(C2H8N2) 2(OH)2]Cl4.2H2O I and Co[W(CN)2(C2H8N2) 2(OH)2]Cl2.2H2O II for Mo(IV) and W(IV) complexes, respectively. The IR peaks observed for both the complexes show N-H stretching, H-N-H bending and stretching vibrations of the C-N and C-C bonds. Depending on the nature of the absorption bands, complex I is assigned as -trans and complex II as -cis configuration. The thermal decomposition of these complexes has been studied by TG and DSC techniques. The reaction scheme for decomposition of each complex has been proposed. The activation energy (Ea), pre-exponential factor (A) and entropy of activation (ΔS#) have been calculated by employing the integral methods like Arrhenius, Coats-Redfern and Doyle. Enthalpy (ΔH) values for each transition are obtained from DSC data.

Thermal, spectroscopic and kinetic characterization of reaction products of copper(II) chloride with photoproducts of octacyanocomplexes of Molybdenum(IV) and Tungsten(IV) with ethylenediamine

Ali,Majid, Kowsar

, p. 173 - 181 (1998)

The thermal dissociation of complexes formed by copper(II) chloride with photoproducts of M(CN)4-8 [where M=Mo or W] and ethylenediamine has been studied by thermogravimetry (TG), differential scanning calorimetry (DSC) and IR spectroscopy. The observed IR bands for different groups support the assigned composition. Both Mo(IV) and W(IV) show the same stoichiometric behaviour towards complex formation but a different decomposition behaviour. In case of Mo(IV) decomposition takes place in four steps with cyanide and oxide of copper and tetrachloro molybdenum(IV) as residue, while in case of W(IV) the decomposition occurs only in three steps up to 298°C. The copper cyanide along with tetrachloro tungstate(IV) is found as residue. DSC for Mo complex displays four transitions, two exothermic and two endothermic. In case of W, DSC displays three endothermic transitions corresponding to three decomposition steps with three different ΔH values. On the basis of TG and DSC, mechanism for decomposition of each complex has been proposed. Kinetic parameters like activation energy (Ea), frequency factor (A), entropy of activation (ΔS#) for each step has been calculated involving differential methods like Doyle, Coats and Redfern and Arrhenius. The heat of the reaction is obtained from DSC curves.

Size-dependent spectroscopy of MoS2 nanoclusters

Chikan,Kelley

, p. 3794 - 3804 (2002)

The synthesis and characterization of 3.5, 4.5, and 8 nm diameter MoS2 nanoclusters are described. Each size is characterized by TEM images, electron diffraction, and optical spectroscopy. These nanoclusters can be synthesized directly or may be synthesized from samples of polydisperse nanoclusters. Obtaining larger or smaller discrete sizes from polydisperse samples indicates that these nanocluster sizes are thermodynamically favored, that is, these sizes correspond to free-energy minima. Electron diffraction and static spectroscopic results indicate that the particles are three atoms thick, specifically, single S-Mo-S trilayer disks. Static and time-resolved absorption and emission spectroscopy were used to determine the polarizations of the lowest energy allowed transitions in each case. We find that the 8 nm particles have a lowest energy absorption maximum at 473 nm that has mixed x - y and z polarizations, 4.5 nm particles have absorption maxima at 400 and 440 nm that are x - y and z polarized, respectively, and 3.5 nm particles have an absorption maximum at 362 nm that is z polarized. These results indicate that the polarization of the lowest observed transition is size-dependent and that the ordering of the lowest excited states changes as the particle size decreases.

Novel benzyl-substituted molybdocene anticancer drugs

Gleeson, Brendan,Claffey, James,Deally, Anthony,Hogan, Megan,Méndez, Luis Miguel Menéndez,Müller-Bunz, Helge,Patil, Siddappa,Tacke, Matthias

, p. 1831 - 1836 (2010/09/04)

From the reaction of 6-(p-methoxyphenyl) fulvene (1a), 6-(3,4-dimethoxyphenyl) fulvene (1b) and 6-(3,4,5-trimethoxyphenyl) fulvene (1c) with LiBEt3H, lithiated cyclopentadienide intermediates (2a-c) were synthesised. These intermediates were then transmetallated to molybdocene using MoCl4 (synthesized in situ) to yield the benzyl-substituted molybdocenes bis-[(p-methoxybenzyl)cyclopentadienyl] molybdenum (IV) dichloride (3a), bis-[(3,4-dimethoxybenzyl)cyclopentadienyl] molybdenum (IV) dichloride (3b), and bis-[(3,4,5-trimethoxybenzyl)cyclopentadienyl] molybdenum (IV) dichloride (3c). The molybdocene 3a was characterised by single crystal X-ray diffraction. All three molybdocenes had their cytotoxicity investigated through MTT based preliminary in vitro testing on the human renal cell line Caki-1 in order to determine their IC50 values and compare them with the corresponding titanocene and vanadocene dichloride derivatives. Molybdocenes 3b-c were found to have the same IC50 values of 290 μM, while 3a yielded a value of 84 μM, respectively.

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