nickel 1,4-cyclohexanedicarboxylate coordination polymers – synthesis, characterization, phase...
TRANSCRIPT
![Page 1: Nickel 1,4-cyclohexanedicarboxylate coordination polymers – Synthesis, Characterization, Phase study, and Magnetic Properties Prashant Jain @, Russel K](https://reader036.vdocuments.net/reader036/viewer/2022062423/5697c0011a28abf838cc24b6/html5/thumbnails/1.jpg)
Nickel 1,4-cyclohexanedicarboxylate coordination polymers – Synthesis, Characterization, Phase study, and Magnetic PropertiesPrashant Jain@, Russel K Feller#, Naresh Dalal@, Tony Cheetham#, and Harold W. Kroto@
@ Dept. of Chemistry & Biochemistry, Florida State University, # Materials Research Laboratory, University of California, Santa Barbara
Overview
Coordination polymers or metal organic frameworks are of great recent research interest due to their interesting topologies and potential applications as functional materials. Hydrothermal chemistry has been widely used for preparation of these compounds. Control of products in the hydrothermal reactions is still an exciting challenge for the chemists. Here we report the synthesis of five nickel complexes starting from identical reaction mixture. A detailed study was conducted to determine the way in which reaction conditions governed the resulting phases. Temperature and concentration were found to be the two main determining factors.
Products
Five nickel complexes were observed. Structures of three complexes were solved by single crystal XRD.
For complex 4 (space group R3-c) the temperature dependence of reciprocal of the susceptibility is linear above 60 K and obeys the Curie-Weiss law with a Weiss constant θ = -146.89 K and C = 9.43 cm3 K mol-1. The C value correspond to the six non-interacting Ni II ions (S=1) with g = 2.21. χT value at room temperature (6.33 cm3 K mol-1) is lower then an expected value (7.33 cm3 K mol-1).
Effect of reaction conditions
As shown in the reaction condition diagram, it was possible to synthesize pure complexes. Other variables (eg. solvent volume, fill volume, stirring etc.) do not affect the products though they have an effect on crystal size. Compound 4 has a unique structure with hexanuclear nickel cluster forming 2-D layers. Magnetic measurement for 4, suggest that there are competing ferromagnetic and anti-ferromagnetic behavior with complex being anti-ferromagnetic at lower temperatures. Reaction time was reduced to less then 2 hours in microwave synthesis with higher yield. Magnetic studies are underway to understand interactions within these complexes .
Observations
[Ni6(OH)6(trans-1,4-CHDC)3(H2O)6].2H2O
Space Group: R3-c
[Ni3(OH)2(trans-1,4-CHDC)2(H2O)4].4H2O
Space Group: C2/m
[Ni3(OH)2(cis-1,4-CHDC)2(H2O)4].2H2O
Space Group: P21/c
Crystal Structures Magnetic Measurements
X-r
ay D
iffr
acti
on
Dat
a
Synthesis
Products were characterized by single crystal and powder XRD.
NiAc + CHDC (Hydrothermal reaction for 2 Days)
Nickel 1,4 cyclohexanedicarboxylate
![Page 2: Nickel 1,4-cyclohexanedicarboxylate coordination polymers – Synthesis, Characterization, Phase study, and Magnetic Properties Prashant Jain @, Russel K](https://reader036.vdocuments.net/reader036/viewer/2022062423/5697c0011a28abf838cc24b6/html5/thumbnails/2.jpg)
Nickel 1,4-cyclohexanedicarboxylate coordination polymers –
Prashant Jain@, Russel K Feller#, Naresh Dalal@, Tony Cheetham#, and Harold W. Kroto@
@ Dept. of Chemistry & Biochemistry, Florida State University, # Materials Research Laboratory, University of California, Santa
Barbara
Synthesis, Characterization, Phase study, and Magnetic Properties
![Page 3: Nickel 1,4-cyclohexanedicarboxylate coordination polymers – Synthesis, Characterization, Phase study, and Magnetic Properties Prashant Jain @, Russel K](https://reader036.vdocuments.net/reader036/viewer/2022062423/5697c0011a28abf838cc24b6/html5/thumbnails/3.jpg)
Coordination polymers or metal organic frameworks (MOFs) have very interesting topologies and important
potential applications as functional materials.
![Page 4: Nickel 1,4-cyclohexanedicarboxylate coordination polymers – Synthesis, Characterization, Phase study, and Magnetic Properties Prashant Jain @, Russel K](https://reader036.vdocuments.net/reader036/viewer/2022062423/5697c0011a28abf838cc24b6/html5/thumbnails/4.jpg)
Nickel 1,4-cyclohexanedicarboxylate
![Page 5: Nickel 1,4-cyclohexanedicarboxylate coordination polymers – Synthesis, Characterization, Phase study, and Magnetic Properties Prashant Jain @, Russel K](https://reader036.vdocuments.net/reader036/viewer/2022062423/5697c0011a28abf838cc24b6/html5/thumbnails/5.jpg)
Ni6(OH)6(chdcox)3(H2O)6.2H2O
![Page 6: Nickel 1,4-cyclohexanedicarboxylate coordination polymers – Synthesis, Characterization, Phase study, and Magnetic Properties Prashant Jain @, Russel K](https://reader036.vdocuments.net/reader036/viewer/2022062423/5697c0011a28abf838cc24b6/html5/thumbnails/6.jpg)
Ni6(OH)6(chdcox)3(H2O)6.2H2O
![Page 7: Nickel 1,4-cyclohexanedicarboxylate coordination polymers – Synthesis, Characterization, Phase study, and Magnetic Properties Prashant Jain @, Russel K](https://reader036.vdocuments.net/reader036/viewer/2022062423/5697c0011a28abf838cc24b6/html5/thumbnails/7.jpg)
![Page 8: Nickel 1,4-cyclohexanedicarboxylate coordination polymers – Synthesis, Characterization, Phase study, and Magnetic Properties Prashant Jain @, Russel K](https://reader036.vdocuments.net/reader036/viewer/2022062423/5697c0011a28abf838cc24b6/html5/thumbnails/8.jpg)
Nickel 1,4-cyclohexanedicarboxylate coordination polymers – Synthesis, Characterization, Phase study, and Magnetic PropertiesPrashant Jain@, Russel K Feller#, Naresh Dalal@, Tony Cheetham#, and Harold W. Kroto@
@ Dept. of Chemistry & Biochemistry, Florida State University, # Materials Research Laboratory, University of California, Santa Barbara
Overview
Coordination polymers or metal organic frameworks are of great recent research interest due to their interesting topologies and potential applications as functional materials. Hydrothermal chemistry has been widely used for preparation of these compounds. Control of products in the hydrothermal reactions is still an exciting challenge for the chemists. Here we report the synthesis of five nickel complexes starting from identical reaction mixture. A detailed study was conducted to determine the way in which reaction conditions governed the resulting phases. Temperature and concentration were found to be the two main determining factors.
Products
Five nickel complexes were observed. Structures of three complexes were solved by single crystal XRD.
For complex 4 (space group R3-c) the temperature dependence of reciprocal of the susceptibility is linear above 60 K and obeys the Curie-Weiss law with a Weiss constant θ = -146.89 K and C = 9.43 cm3 K mol-1. The C value correspond to the six non-interacting Ni II ions (S=1) with g = 2.21. χT value at room temperature (6.33 cm3 K mol-1) is lower then an expected value (7.33 cm3 K mol-1).
Effect of reaction conditions
As shown in the reaction condition diagram, it was possible to synthesize pure complexes. Other variables (eg. solvent volume, fill volume, stirring etc.) do not affect the products though they have an effect on crystal size. Compound 4 has a unique structure with hexanuclear nickel cluster forming 2-D layers. Magnetic measurement for 4, suggest that there are competing ferromagnetic and anti-ferromagnetic behavior with complex being anti-ferromagnetic at lower temperatures. Reaction time was reduced to less then 2 hours in microwave synthesis with higher yield. Magnetic studies are underway to understand interactions within these complexes .
Observations
[Ni6(OH)6(trans-1,4-CHDC)3(H2O)6].2H2O
Space Group: R3-c
[Ni3(OH)2(trans-1,4-CHDC)2(H2O)4].4H2O
Space Group: C2/m
[Ni3(OH)2(cis-1,4-CHDC)2(H2O)4].2H2O
Space Group: P21/c
Crystal Structures Magnetic Measurements
X-r
ay D
iffr
acti
on
Dat
a
Synthesis
Products were characterized by single crystal and powder XRD.
NiAc + CHDC (Hydrothermal reaction for 2 Days)
Nickel 1,4 cyclohexanedicarboxylate
![Page 9: Nickel 1,4-cyclohexanedicarboxylate coordination polymers – Synthesis, Characterization, Phase study, and Magnetic Properties Prashant Jain @, Russel K](https://reader036.vdocuments.net/reader036/viewer/2022062423/5697c0011a28abf838cc24b6/html5/thumbnails/9.jpg)
The temperature dependence of reciprocal of the susceptibility is linear above 60 K and
obeys the Curie-Weiss law
![Page 10: Nickel 1,4-cyclohexanedicarboxylate coordination polymers – Synthesis, Characterization, Phase study, and Magnetic Properties Prashant Jain @, Russel K](https://reader036.vdocuments.net/reader036/viewer/2022062423/5697c0011a28abf838cc24b6/html5/thumbnails/10.jpg)
The temperature dependence of reciprocal of the susceptibility is linear above 60 K and
obeys the Curie-Weiss law
![Page 11: Nickel 1,4-cyclohexanedicarboxylate coordination polymers – Synthesis, Characterization, Phase study, and Magnetic Properties Prashant Jain @, Russel K](https://reader036.vdocuments.net/reader036/viewer/2022062423/5697c0011a28abf838cc24b6/html5/thumbnails/11.jpg)
The temperature dependence of reciprocal of the susceptibility is linear above 60 K and
obeys the Curie-Weiss law
![Page 12: Nickel 1,4-cyclohexanedicarboxylate coordination polymers – Synthesis, Characterization, Phase study, and Magnetic Properties Prashant Jain @, Russel K](https://reader036.vdocuments.net/reader036/viewer/2022062423/5697c0011a28abf838cc24b6/html5/thumbnails/12.jpg)
→
1/χM
The temperature dependence of reciprocal of the susceptibility is linear above 60 K and
obeys the Curie-Weiss law
![Page 13: Nickel 1,4-cyclohexanedicarboxylate coordination polymers – Synthesis, Characterization, Phase study, and Magnetic Properties Prashant Jain @, Russel K](https://reader036.vdocuments.net/reader036/viewer/2022062423/5697c0011a28abf838cc24b6/html5/thumbnails/13.jpg)
The temperature dependence of reciprocal of the susceptibility is linear above 60 K and obeys the Curie-Weiss law with a Weiss constant θ = -146.89 K and C = 9.43 cm3 K mol-1.
![Page 14: Nickel 1,4-cyclohexanedicarboxylate coordination polymers – Synthesis, Characterization, Phase study, and Magnetic Properties Prashant Jain @, Russel K](https://reader036.vdocuments.net/reader036/viewer/2022062423/5697c0011a28abf838cc24b6/html5/thumbnails/14.jpg)
The temperature dependence of reciprocal of the susceptibility is linear above 60 K and obeys the Curie-Weiss law with a Weiss constant θ = -146.89 K and C = 9.43 cm3 K mol-1.
→
1/χM
![Page 15: Nickel 1,4-cyclohexanedicarboxylate coordination polymers – Synthesis, Characterization, Phase study, and Magnetic Properties Prashant Jain @, Russel K](https://reader036.vdocuments.net/reader036/viewer/2022062423/5697c0011a28abf838cc24b6/html5/thumbnails/15.jpg)
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Functional materials are an essential part of our everyday lives.
1.silicon chip with its ever-increasing power
2.light-emitting materials at the heart of today’s telecommunications or DVD players
3.liquid crystal displays
4.magnetic materials used in recording devices.
![Page 18: Nickel 1,4-cyclohexanedicarboxylate coordination polymers – Synthesis, Characterization, Phase study, and Magnetic Properties Prashant Jain @, Russel K](https://reader036.vdocuments.net/reader036/viewer/2022062423/5697c0011a28abf838cc24b6/html5/thumbnails/18.jpg)
For complex 4 (space group R3-c) the temperature dependence of reciprocal of the susceptibility is linear above 60 K and obeys the Curie-Weiss law with a Weiss constant θ = -146.89 K and C = 9.43 cm3 K mol-1. The C value correspond to the six non-interacting NiII ions (S=1) with g = 2.21. χT value at room temperature (6.33 cm3 K mol-1) is lower then an expected value (7.33 cm3 K mol-1).
![Page 19: Nickel 1,4-cyclohexanedicarboxylate coordination polymers – Synthesis, Characterization, Phase study, and Magnetic Properties Prashant Jain @, Russel K](https://reader036.vdocuments.net/reader036/viewer/2022062423/5697c0011a28abf838cc24b6/html5/thumbnails/19.jpg)
Functional materials are an essential part of our everyday lives.
![Page 20: Nickel 1,4-cyclohexanedicarboxylate coordination polymers – Synthesis, Characterization, Phase study, and Magnetic Properties Prashant Jain @, Russel K](https://reader036.vdocuments.net/reader036/viewer/2022062423/5697c0011a28abf838cc24b6/html5/thumbnails/20.jpg)
Functional materials are an essential part of our everyday lives.
1.silicon chip with its ever-increasing power
![Page 21: Nickel 1,4-cyclohexanedicarboxylate coordination polymers – Synthesis, Characterization, Phase study, and Magnetic Properties Prashant Jain @, Russel K](https://reader036.vdocuments.net/reader036/viewer/2022062423/5697c0011a28abf838cc24b6/html5/thumbnails/21.jpg)
![Page 22: Nickel 1,4-cyclohexanedicarboxylate coordination polymers – Synthesis, Characterization, Phase study, and Magnetic Properties Prashant Jain @, Russel K](https://reader036.vdocuments.net/reader036/viewer/2022062423/5697c0011a28abf838cc24b6/html5/thumbnails/22.jpg)
Functional materials are an essential part of our everyday lives.
1.silicon chip with its ever-increasing power
2.light-emitting materials at the heart of today’s telecommunications or DVD players
![Page 23: Nickel 1,4-cyclohexanedicarboxylate coordination polymers – Synthesis, Characterization, Phase study, and Magnetic Properties Prashant Jain @, Russel K](https://reader036.vdocuments.net/reader036/viewer/2022062423/5697c0011a28abf838cc24b6/html5/thumbnails/23.jpg)
![Page 24: Nickel 1,4-cyclohexanedicarboxylate coordination polymers – Synthesis, Characterization, Phase study, and Magnetic Properties Prashant Jain @, Russel K](https://reader036.vdocuments.net/reader036/viewer/2022062423/5697c0011a28abf838cc24b6/html5/thumbnails/24.jpg)
Functional materials are an essential part of our everyday lives.
1.silicon chip with its ever-increasing power
2.light-emitting materials at the heart of today’s telecommunications or DVD players
3.liquid crystal displays
![Page 25: Nickel 1,4-cyclohexanedicarboxylate coordination polymers – Synthesis, Characterization, Phase study, and Magnetic Properties Prashant Jain @, Russel K](https://reader036.vdocuments.net/reader036/viewer/2022062423/5697c0011a28abf838cc24b6/html5/thumbnails/25.jpg)
![Page 26: Nickel 1,4-cyclohexanedicarboxylate coordination polymers – Synthesis, Characterization, Phase study, and Magnetic Properties Prashant Jain @, Russel K](https://reader036.vdocuments.net/reader036/viewer/2022062423/5697c0011a28abf838cc24b6/html5/thumbnails/26.jpg)
Functional materials are an essential part of our everyday lives.
1.silicon chip with its ever-increasing power
2.light-emitting materials at the heart of today’s telecommunications or DVD players
3.liquid crystal displays
4.magnetic materials used in recording devices.
![Page 27: Nickel 1,4-cyclohexanedicarboxylate coordination polymers – Synthesis, Characterization, Phase study, and Magnetic Properties Prashant Jain @, Russel K](https://reader036.vdocuments.net/reader036/viewer/2022062423/5697c0011a28abf838cc24b6/html5/thumbnails/27.jpg)
As shown in the reaction condition diagram, it was possible to synthesize pure complexes. Other variables (eg. solvent volume, fill volume, stirring etc.) do not affect the products though they have an effect on crystal size. Compound 4 has a unique structure with hexanuclear nickel cluster forming 2-D layers. Magnetic measurement for 4, suggest that there are competing ferromagnetic and anti-ferromagnetic behavior with complex being anti-ferromagnetic at lower temperatures. Reaction time was reduced to less then 2 hours in microwave synthesis with higher yield. Magnetic studies are underway to understand interactions within these complexes .
![Page 28: Nickel 1,4-cyclohexanedicarboxylate coordination polymers – Synthesis, Characterization, Phase study, and Magnetic Properties Prashant Jain @, Russel K](https://reader036.vdocuments.net/reader036/viewer/2022062423/5697c0011a28abf838cc24b6/html5/thumbnails/28.jpg)
Functional materials are ubiquitous. New materials with improved functionality will be in demand in the marketplace and materials exhibiting more than one degree of functionality will appear to provide even more applications
![Page 29: Nickel 1,4-cyclohexanedicarboxylate coordination polymers – Synthesis, Characterization, Phase study, and Magnetic Properties Prashant Jain @, Russel K](https://reader036.vdocuments.net/reader036/viewer/2022062423/5697c0011a28abf838cc24b6/html5/thumbnails/29.jpg)
2 D oligomer self-assembly
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Hydrothermal chemistry has been widely used for preparation of these compounds. Control of products in the hydrothermal reactions is still an exciting challenge for the chemists. Here we report the synthesis of five nickel complexes starting from identical reaction mixture.
![Page 32: Nickel 1,4-cyclohexanedicarboxylate coordination polymers – Synthesis, Characterization, Phase study, and Magnetic Properties Prashant Jain @, Russel K](https://reader036.vdocuments.net/reader036/viewer/2022062423/5697c0011a28abf838cc24b6/html5/thumbnails/32.jpg)
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Effect of reaction conditions
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100 125 150 175 200
Temperature
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100 125 150 175 200
Temperature
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©
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©Pile of flat sheets
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Nickel 1,4-cyclohexanedicarboxylate coordination polymers – Synthesis, Characterization, Phase study, and Magnetic PropertiesPrashant Jain@, Russel K Feller#, Naresh Dalal@, Tony Cheetham#, and Harold W. Kroto@
@ Dept. of Chemistry & Biochemistry, Florida State University, # Materials Research Laboratory, University of California, Santa Barbara
Overview
Coordination polymers or metal organic frameworks are of great recent research interest due to their interesting topologies and potential applications as functional materials. Hydrothermal chemistry has been widely used for preparation of these compounds. Control of products in the hydrothermal reactions is still an exciting challenge for the chemists. Here we report the synthesis of five nickel complexes starting from identical reaction mixture. A detailed study was conducted to determine the way in which reaction conditions governed the resulting phases. Temperature and concentration were found to be the two main determining factors.
Products
Five nickel complexes were observed. Structures of three complexes were solved by single crystal XRD.
For complex 4 (space group R3-c) the temperature dependence of reciprocal of the susceptibility is linear above 60 K and obeys the Curie-Weiss law with a Weiss constant θ = -146.89 K and C = 9.43 cm3 K mol-1. The C value correspond to the six non-interacting Ni II ions (S=1) with g = 2.21. χT value at room temperature (6.33 cm3 K mol-1) is lower then an expected value (7.33 cm3 K mol-1).
Effect of reaction conditions
As shown in the reaction condition diagram, it was possible to synthesize pure complexes. Other variables (eg. solvent volume, fill volume, stirring etc.) do not affect the products though they have an effect on crystal size. Compound 4 has a unique structure with hexanuclear nickel cluster forming 2-D layers. Magnetic measurement for 4, suggest that there are competing ferromagnetic and anti-ferromagnetic behavior with complex being anti-ferromagnetic at lower temperatures. Reaction time was reduced to less then 2 hours in microwave synthesis with higher yield. Magnetic studies are underway to understand interactions within these complexes .
Observations
[Ni6(OH)6(trans-1,4-CHDC)3(H2O)6].2H2O
Space Group: R3-c
[Ni3(OH)2(trans-1,4-CHDC)2(H2O)4].4H2O
Space Group: C2/m
[Ni3(OH)2(cis-1,4-CHDC)2(H2O)4].2H2O
Space Group: P21/c
Crystal Structures Magnetic Measurements
X-r
ay D
iffr
acti
on
Dat
a
Synthesis
Products were characterized by single crystal and powder XRD.
NiAc + CHDC (Hydrothermal reaction for 2 Days)
Nickel 1,4 cyclohexanedicarboxylate
![Page 41: Nickel 1,4-cyclohexanedicarboxylate coordination polymers – Synthesis, Characterization, Phase study, and Magnetic Properties Prashant Jain @, Russel K](https://reader036.vdocuments.net/reader036/viewer/2022062423/5697c0011a28abf838cc24b6/html5/thumbnails/41.jpg)
Functional materials are ubiquitous. New materials with improved functionality will be in demand in the marketplace and materials exhibiting more than one degree of functionality will appear to provide even more applications
![Page 42: Nickel 1,4-cyclohexanedicarboxylate coordination polymers – Synthesis, Characterization, Phase study, and Magnetic Properties Prashant Jain @, Russel K](https://reader036.vdocuments.net/reader036/viewer/2022062423/5697c0011a28abf838cc24b6/html5/thumbnails/42.jpg)
![Page 43: Nickel 1,4-cyclohexanedicarboxylate coordination polymers – Synthesis, Characterization, Phase study, and Magnetic Properties Prashant Jain @, Russel K](https://reader036.vdocuments.net/reader036/viewer/2022062423/5697c0011a28abf838cc24b6/html5/thumbnails/43.jpg)
As shown in the reaction condition diagram, it was possible to synthesize pure complexes. Other variables (eg. solvent volume, fill volume, stirring etc.) do not affect the products though they have an effect on crystal size. Compound 4 has a unique structure with hexanuclear nickel cluster forming 2-D layers. Magnetic measurement for 4, suggest that there are competing ferromagnetic and anti-ferromagnetic behavior with complex being anti-ferromagnetic at lower temperatures. Reaction time was reduced to less then 2 hours in microwave synthesis with higher yield. Magnetic studies are underway to understand interactions within these complexes .
Observations
![Page 44: Nickel 1,4-cyclohexanedicarboxylate coordination polymers – Synthesis, Characterization, Phase study, and Magnetic Properties Prashant Jain @, Russel K](https://reader036.vdocuments.net/reader036/viewer/2022062423/5697c0011a28abf838cc24b6/html5/thumbnails/44.jpg)
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Hydrothermal chemistry has been widely used for preparation of these compounds. Control of products in the hydrothermal reactions is still an exciting challenge for the chemists. Here we report the synthesis of five nickel complexes starting from identical reaction mixture.
A detailed study was conducted to determine the way in which reaction conditions governed the resulting phases. Temperature and concentration were found to be the two main determining factors.
![Page 47: Nickel 1,4-cyclohexanedicarboxylate coordination polymers – Synthesis, Characterization, Phase study, and Magnetic Properties Prashant Jain @, Russel K](https://reader036.vdocuments.net/reader036/viewer/2022062423/5697c0011a28abf838cc24b6/html5/thumbnails/47.jpg)
OverviewCoordination polymers or metal organic frameworks (MOFs) are of great recent research interest due to their interesting topologies and potential applications as functional materials.
Hydrothermal chemistry has been widely used for preparation of these compounds. Control of products in the hydrothermal reactions is still an exciting challenge for the chemists. Here we report the synthesis of five nickel complexes starting from identical reaction mixture. A detailed study was conducted to determine the way in which reaction conditions governed the resulting phases. Temperature and concentration were found to be the two main determining factors.