Reaction Published on 2023-09-07 

SURMOFs

 

Author: Lena Pilz¹

Reaction DOI: 10.14272/reaction/SA-FUHFF-UHFFFADPSC-DBLYDXDFRQ-UHFFFADPSC-NUHFF-FFHMS-NUHFF-ZZZ.29JSON-LD

Reaction ID: CRR-35494

Reference in the Literature:

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Reaction Table  

IUPAC	Formula	Density/Molarity	Amount [mg]	Volume [mL]	Amount [mmol]	Equiv
Starting materials
copper(II) acetate monohydrate	C4H8CuO5	- / -	205.010	-	1.027	5.315
2,2'-Diazido-4,4'-stilbenedicarboxylic acid	C16H10N6O4	- / -	67.680	-	0.193	1.000
C6H12N2	C6H12N2	- / -	31.860	-	0.284	1.470
Reactants
oxidane	H2O	- / -	-	14.630	-	-
Products						YieldConv.
C51H49Cu8N16O16	C51H49Cu8N16O16	- / -	-	-	-	- %
Solvents
Ethanol	C2H6O		-	191.440	-	91%
Methanol	CH4O		-	18.560	-	9%

Description:

Every synthesis is carried out on a TX-60 6-axis robot from Stäubli in a glovebox under nitrogen atmosphere. From every synthesis two samples are produced, each of 40 cycles.

For the synthesis solutions of copper di-acetate monohydrate in 210 mL ethanol and 2,2’-Diazido-4,4’-stilbenedicarboxylic acid in a mixture of methanol and ethanol includng the modulator water (total volume 210 mL) are prepared separately via ultrasonication --> See Tab "SURMOF Reaction". During the synthesis, the functionalized substrates are subsequently immersed in different solutions in a fixed sequence --> see Tab "SURMOF Reaction". 

RInChiKey Table  

RInChI

1.00.1S/2C16H10N6O4.2C6H12N2.4C2H4O2.8Cu/c2*17-21-19-13-7-11(15(23)24)5-3-9(13)1-2-10-4-6-12(16(25)26)8-14(10)20-22-18;2*1-2-8-5-3-7(1)4-6-8;4*1-2(3)4;;;;;;;;/h2*1-8H,(H,23,24)(H,25,26);2*1-6H2;4*1H3,(H,3,4);;;;;;;;/p-8/b2*2-1+;;;;;;;;;;;;;;<>2C2H4O2.Cu.H2O/c2*1-2(3)4;;/h2*1H3,(H,3,4);;1H2/q;;+2;/p-2!C16H10N6O4/c17-21-19-13-7-11(15(23)24)5-3-9(13)1-2-10-4-6-12(16(25)26)8-14(10)20-22-18/h1-8H,(H,23,24)(H,25,26)/b2-1+!C6H12N2/c1-2-8-5-3-7(1)4-6-8/h1-6H2<>C2H6O/c1-2-3/h3H,2H2,1H3!CH4O/c1-2/h2H,1H3!H2O/h1H2/d-

Long-RInChIKey

SA-BUHFF-DBLYDXDFRQUSRQ-QYQCSXRTSA-F--NWFNSTOSIVLCJA-UHFFFAOYSA-L-GPMRCRXJSWELFY-OWOJBTEDSA-N-IMNIMPAHZVJRPE-UHFFFAOYSA-N--LFQSCWFLJHTTHZ-UHFFFAOYSA-N-OKKJLVBELUTLKV-UHFFFAOYSA-N-XLYOFNOQVPJJNP-UHFFFAOYSA-N

Short-RInChIKey

SA-BUHFF-DBLYDXDFRQ-JPAVRTZQTW-UNKQZBOQUU-FFHMS-LCDMU-NUHFF-ZZZ

Web-RInChIKey

ZNSAZUUKZSMPILINE-DJVSDNGXAXSRVSA

Properties  

Status: Done

Temperature: 25 °C

Duration: 24 Hour(s)

TLC-Control  

Solvents (parts)

Rf-Value

0

TLC-Description

(Sur)MOF Reaction  

Type of Metal Organic Framework

SURMOF

General setting for the synthesis of SURMOFs

Reaction techniques

Dipping

Processing type

automated

Device

TX-60

Type of sample holder

4-fold

No of samples

2

Comments and further Details

Preparation of substrate

Substrate

Silicon wafer

Coating

gold

Dimensions

1x3cm

Activation

SAM

Sam type

MHDA (16- Mercaptohexadecanoic acid)

Duration

72 h

Preparation of the used chemicals/materials in detail

Table 1: Listing of solvents and definition of solvent mixtures

Solvent label

Solvent A

Volume A

Solvent B

Volume B

Solvent C

Volume C

Ratio [A:B:C]

sol mix 1

EtOH

1340.05 ml

MeOH

129.95 ml

-

10,3:1

sol mix 2

EtOH

178.1 ml

MeOH

17.27 ml

-

10,3:1

Table 2: Preparation of materials

Vessel No

Vessel Part

Function

Molecule

Method

Solvent label

Volume

Duration

Temperature [°C]

V1

A

metal

sonication

sol mix 1

210 ml

20 m

25

V2

A

cleaning agent

none

sol mix 1

210 ml

-

25

V3

A

cleaning agent

none

sol mix 1

210 ml

-

25

V4

A

cleaning agent

none

sol mix 1

210 ml

-

25

V5

A

linker

sonication

sol mix 2

195.37 ml

20 m

25

V5

B

modulators

sonication

sol mix 2

195.37 ml

20 m

25

V5

C

modulators

sonication

sol mix 2

195.37 ml

20 m

25

V6

A

cleaning agent

none

sol mix 1

210 ml

-

25

V7

A

cleaning agent

none

sol mix 1

210 ml

-

25

V8

A

cleaning agent

none

sol mix 1

210 ml

-

25

Comments and observations

Definition of synthesis cycle

Number of cycles

40

Table 3: Setting referring to materials and their conditions

Step number

Vessel number

Step type

Duration

Temperature [°C]

1

V1

metal installation

10 m

25

2

V2

rinsing

2 m

25

3

V3

rinsing

2 m

25

4

V4

rinsing

2 m

25

5

V5

linker installation

15 m

25

6

V6

rinsing

2 m

25

7

V7

rinsing

2 m

25

8

V8

rinsing

2 m

25

Humidity [% rel.]

12 %

Atmosphere requirements

protective N2

Other conditions

Termination type

storage in solution

Solvent of termination

EtOH/MeOH

Duration of termination step

3 h

Comments and Observations

10-GA2

Analyses  

XRD

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 Product  

Formula: C₅₁H₄₉Cu₈N₁₆O₁₆

Canonical SMILES:

C1CN2CCN1CC2.C1CN2CCN1CC2.[O-]C(=O)C.[O-]C(=O)C.[O-]C(=O)C.[O-]C(=O)C.[N-]=[N+]=Nc1cc(ccc1/C=C/c1ccc(cc1N=[N+]=[N-])C(=O)[O-])C(=O)[O-].[N-]=[N+]=Nc1cc(ccc1/C=C/c1ccc(cc1N=[N+]=[N-])C(=O)[O-])C(=O)[O-].[Cu][Cu].[Cu][Cu].[Cu][Cu].[Cu][Cu]

InChI:

InChI=1S/2C16H10N6O4.2C6H12N2.4C2H4O2.8Cu/c2*17-21-19-13-7-11(15(23)24)5-3-9(13)1-2-10-4-6-12(16(25)26)8-14(10)20-22-18;2*1-2-8-5-3-7(1)4-6-8;4*1-2(3)4;;;;;;;;/h2*1-8H,(H,23,24)(H,25,26);2*1-6H2;4*1H3,(H,3,4);;;;;;;;/p-8/b2*2-1+;;;;;;;;;;;;;;

InChIKey:

DBLYDXDFRQUSRQ-QYQCSXRTSA-F

Exact Mass: 1644.776980 g⋅mol^-1

Sample DOI: 10.14272/DBLYDXDFRQUSRQ-QYQCSXRTSA-F.29JSON-LD

Sample ID: CRS-35862

Reference in the Literature:

(Sur) MOF Details  

(SUR)MOF configuration

List of (ionic) (SUR)MOF fragments

SURMOF

substrate

Silicon

coating

Gold

dimensions

1x3cm

Format ID

MOFid-v1

Format Key

MOFkey-v1

Topology Code(s)

pcu

Catenation

cat0

Comments

https://doi.org/10.1021/acs.cgd.9b01050

CCDC No

MOF identifier

C1CN2CCN1CC2.[Cu][Cu].[N]=[N]=Nc1cc(ccc1C=Cc1ccc(cc1N=[N]=[N])C(=O)[O-])C(=O)[O-]

MOF key

Cu.GPMRCRXJSWELFY.IMNIMPAHZVJRPE

X-ray diffraction (XRD)  View in 3D 

Analysis DOI:10.14272/DBLYDXDFRQUSRQ-QYQCSXRTSA-F/CHMO0000156.29JSON-LD

Analysis ID:CRD-35863

Datasets

• 10-GA2-DASBDC-XRD

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