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Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2008
1
An array-based study of reactivity under solvent-free mechanochemical
conditions – insights and trends
Anne Pichon and Stuart L. James
Supplementary information: XRPD patterns for products and starting materials of all reactions. Reactions with copper salts Ligand: HINA
0102030405060708090100
5 10 15 20 25 30 35 40 45 50
2θ (deg)
Inte
nsity
(a.u
.)
Cu(OAc)2.H2O+2HINACu(OAc)2.H2OHINA
010
2030
4050
6070
8090
100
5 10 15 20 25 30 35 40 45 502θ (deg)
Inte
nsity
(a.u
.)
Cu(HCO2)2.H2O+2HINA
Cu(HCO2)2.H2O
HINA
Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2008
2
0
20
40
60
80
100
120
5 10 15 20 25 30
2θ (deg)
Inte
nsity
(a.u
.)Cu(O2CCF3)2.H2O+2HINA
Cu(O2CCF3)2.H2O
HINA
0102030405060708090100
5 10 15 20 25 30 35 40 45 50
2θ (deg)
Inte
nsity
(a.u
.)
Cu(acac)2+2HINACu(acac)2HINA
0102030405060708090100
5 10 15 20 25 30 35 40 45 50
2θ (Deg)
Inte
nsity
(a.u
.)
Cu(F6acac)2+2HINACu(F6acac)2HINA
Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2008
3
0102030405060708090100
5 10 15 20 25 30 35 40 45 50
2θ (deg)
Inte
nsity
(a.u
.)Cu(NO3)2.3H2O+2HINA
Cu(NO3)2.3H2OHINA
0102030405060708090100
5 10 15 20 25 30 35 40 45 50
2θ (deg)
Inte
nsity
(a.u
.)
Cu(SO4).5H2O+2HINACu(SO4).5H2OHINA
Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2008
4
Ligand: H3BTC
0
10
20
30
40
50
60
70
80
90
100
5 10 15 20 25 30 35 40 45 50
2θ (deg)
Inte
nsity
(a.u
.)3Cu(OAc)2.H2O+2H3BTC
Cu(OAc)2.H2O
H3BTC
0102030405060708090100
5 10 15 20 25 30 35 40 45 50
2θ (deg)
Inte
nsity
(a.u
.)
3Cu(HCO2)2.H2O+2H3BTC
Cu(HCO2)2.H2O
H3BTC
0
10
20
30
40
50
60
70
80
90
100
5 10 15 20 25 302θ (deg)
Inte
nsity
(a.u
.)
3Cu(O2CCF3)2.H2O+2H3BTCCu(F3OAc)2.H2OH3BTC
Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2008
5
0
10
20
30
40
50
60
70
80
90
100
5 10 15 20 25 30 35 40 45 50
2θ (deg)
Inte
nsity
(a.u
.)3Cu(acac)2+2H3BTCCu(acac)2H3BTC
0
20
40
60
80
100
120
5 10 15 20 25 30 35 40 45 50
2θ (deg)
Inte
nsity
(a.u
.)
3Cu(F6acac)2+2H3BTC
Cu(F6acac)2
H3BTC
0
10
20
30
40
50
60
70
80
90
100
5 10 15 20 25 30 35 40 45 50
2θ (deg)
Inte
nsity
(a.u
.)
3Cu(NO3)2.3H2O+2H3BTC
Cu(NO3)2.3H2O
H3BTC
Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2008
6
0102030405060708090100
5 10 15 20 25 30 35 40 45 50
2θ (deg)
Inte
nsity
(a.u
.)
3Cu(SO4).5H2O+2H3BTCCu(SO4).5H2OH3BTC
Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2008
7
Ligand: H2ADC
0102030405060708090100
5 10 15 20 25 30 35 40 45 50
2θ (deg)
Inte
nsity
(a.u
.)Cu(OAc)2.H2O+2H2ADC
Cu(OAc)2.H2O
H2ADC
0
20
40
60
80
100
120
140
160
5 10 15 20 25 30 35 40 45 50
2θ (deg)
Inte
nsity
(a.u
.)
Cu(HCO2)2.H2O+2H2ADC
Cu(HCO2)2.H2O
H2ADC
0
10
20
30
40
50
60
70
80
90
100
5 10 15 20 25 30 35 40 45 50
2θ (deg)
Inte
nsity
(a.u
.)
Cu(O2CCF3)2.H2O+2H2ADC
Cu(O2CCF3)2.H2O
H2ADC
Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2008
8
0102030405060708090100
5 10 15 20 25 30 35 40 45 502θ (deg)
Inte
nsity
(a.u
.)Cu(acac)2+2H2ADC
Cu(acac)2
H2ADC
0102030405060708090100
5 10 15 20 25 30 35 40 45 50
2θ (deg)
Inte
nsity
(a.u
.)
Cu(F6acac)2+2H2ADC
Cu(F6acac)2
H2ADC
0
10
20
30
40
50
60
70
80
90
100
5 10 15 20 25 30 35 40 45 502θ (deg)
Inte
nsity
(a.u
.)
Cu(NO3)2.3H2O+2H2ADC
Cu(NO3)2.3H2O
H2ADC
Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2008
9
0
10
20
30
40
50
60
70
80
90
100
5 10 15 20 25 30 35 40 45 50
2θ (deg)
Inte
nsity
(a.u
.)Cu(SO4).5H2O+2H2ADC
Cu(SO4).5H2O
H2ADC
Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2008
10
Ligand: H2BDC
0102030405060708090100
5 10 15 20 25 30 35 40 45 50
2θ (deg)
Inte
nsity
(a.u
.)Cu(OAc)2.H2O+2H2BDC
Cu(OAc)2.H2O
H2BDC
0102030405060708090100
5 10 15 20 25 30 35 40 45 50
2θ (deg)
Inte
nsity
(a.u
.)
Cu(HCO2)2.H2O+2H2BDC
Cu(HCO2)2.H2O
H2BDC
Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2008
11
0
10
20
30
40
50
60
70
80
90
100
5 10 15 20 25 30
2θ (deg)
Inte
nsity
(a.u
.)
Cu(O2CCF3)2.H2O+2H2BDC
Cu(O2CCF3)2.H2O
H2BDC
0102030405060708090100
5 10 15 20 25 30 35 40 45 50
2θ (deg)
Inte
nsity
(a.u
.)
Cu(acac)2+2H2BDCCu(acac)2H2BDC
Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2008
12
0
20
40
60
80
100
5 10 15 20 25 30 35 40 45 50
2θ (deg)
Inte
nsity
(a.u
.)Cu(F6acac)2+2H2BDCCu(F6acac)2H2BDC
0102030405060708090100
5 10 15 20 25 30 35 40 45 502θ (deg)
Inte
nsity
(a.u
.)
Cu(NO3)2.3H2O+2H2BDC
Cu(NO3)2.3H2O
H2BDC
0102030405060708090100
5 10 15 20 25 30 35 40 45 50
2θ (deg)
Inte
nsity
(a.u
.)
Cu(SO4).5H2O+2H2BDC
Cu(SO4).5H2O
H2BDC
Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2008
13
Ligand: BIPY
0
10
20
30
40
50
60
70
80
90
100
5 10 15 20 25 30 35 40 45 502θ (deg)
Inte
nsity
(a.u
.)
Cu(OAc)2.H2O+1.5BIPYCu(OAc)2.H2OBIPY
0
10
20
30
40
50
60
70
80
90
100
5 10 15 20 25 30 35 40 45 50
2θ (deg)
Inte
nsity
(a.u
.)
Cu(HCO2)2.H2O+1.5BIPYCu(HCO2)2.H2OBIPY
0102030405060708090100
5 10 15 20 25 30
2θ (deg)
Inte
nsity
(a.u
.)
Cu(O2CCF3)2.H2O+1.5BIPY
Cu(O2CCF3)2.H2O
BIPY
Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2008
14
0
10
20
3040
50
60
70
80
90
100
5 10 15 20 25 30 35 40 45 50
2θ (deg)
Inte
nsity
(a.u
.)
Cu(acac)2+1.5BIPY
Cu(acac)2
BIPY
0102030405060708090100
5 10 15 20 25 30 35 40 45 50
2θ (deg)
Inte
nsity
(a.u
.)
Cu(F6acac)2+1.5BIPYCu(F6acac)2BIPY
0102030405060708090100
5 10 15 20 25 30 35 40 45 502θ (deg)
Inte
nsity
(a.u
.)
Cu(NO3)2.3H2O+1.5BIPY
Cu(NO3)2.3H2O
BIPY
Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2008
15
01020304050
60708090100
5 10 15 20 25 30 35 40 45 50
2θ (deg)
Inte
nsity
(a.u
.)
Cu(SO4).5H2O+1.5BIPYCu(SO4).5H2OBIPY
Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2008
16
Reactions with nickel and zinc salts Ligand: HINA
0102030405060708090100
5 10 15 20 25 30 35 40 45 50
2θ (deg)
Inte
nsity
(a.u
.)
Ni(OAc)2.4H2O+2HINANi(OAc).4H2OHINA
0102030405060708090100
5 10 15 20 25 30 35 40 45 502θ (deg)
Inte
nsity
(a.u
.)
Ni(NO3)2.6H2O+2HINANi(NO3)2.6H2OHINA
0102030405060708090100
5 10 15 20 25 30 35 40 45 50
2θ (deg)
Inte
nsity
(a.u
.)
Ni(SO4)2.7H2O+2HINA
Ni(SO4)2.7H2O
HINA
Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2008
17
0102030405060708090100
5 10 15 20 25 30 35 40 45 502θ (deg)
Inte
nsity
(a.u
.)Zn(OAc)2.2H2O+2INAZn(OAc)2.2H2OHINA
0
10
20
30
40
50
60
70
80
90
100
5 10 15 20 25 30 35 40 45 50
2θ (deg)
Inte
nsity
(a.u
.)
Zn(NO3)2.6H2O+2HINA
Zn(NO3)2.6H2O
HINA
Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2008
18
Ligand: H3BTC
0102030405060708090100
5 10 15 20 25 30 35 40 45 50
2θ (deg)
Inte
nsity
(a.u
.)3Ni(OAc)2.4H2O+2H3BTC
Ni(OAc)2.4H2O
H3BTC
0102030405060708090100
5 10 15 20 25 30 35 40 45 50
2θ (deg)
Inte
nsity
(a.u
.)
3Ni(NO3)2.6H2O+2H3BTC
Ni(NO3)2.6H2O
H3BTC
0
10
20
30
40
50
60
70
80
90
100
5 10 15 20 25 30 35 40 45 50
2θ (deg)
Inte
nsity
(a.u
.)
3Ni(SO4).7H2O+2H3BTCNi(SO4).7H2OH3BTC
Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2008
19
0
10
20
30
40
50
60
70
80
90
100
5 10 15 20 25 30 35 40 45 50
2θ (deg)
Inte
nsity
(a.u
.)
3Zn(OAc)2.2H2O+2H3BTC
Zn(OAc)2.2H2O
H3BTC
0
20
40
60
80
100
120
5 10 15 20 25 30
2θ (deg)
Inte
nsity
(a.u
.)
3Zn(NO3)2.6H2O+2H3BTCZn(NO3)2.6H2OH3BTC
Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2008
20
Ligand: H2ADC
0
10
20
30
40
50
60
70
80
90
100
5 10 15 20 25 30 35 40 45 50
2θ (deg)
Inte
nsity
(a.u
.)Ni(OAc)2.4H2O+2H2ADC
Ni(OAc)2.4H2O
H2ADC
01020304050
60708090100
5 10 15 20 25 30 35 40 45 50
2θ (deg)
Inte
nsity
(a.u
.)
Ni(NO3)2.6H2O+2H2ADC
Ni(NO3)2.6H2O
H2ADC
0102030405060708090100
5 10 15 20 25 30 35 40 45 50
2θ (deg)
Inte
nsity
(a.u
.)
Ni(SO4).7H2O+2H2ADC
Ni(SO4).7H2O
H2ADC
Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2008
21
0102030405060708090100
5 10 15 20 25 30 35 40 45 50
2θ (deg)
Inte
nsity
(a.u
.)
Zn(OAc)2.2H2O+2H2ADCZn(OAc)2.2H2OH2ADC
0102030405060708090100
5 10 15 20 25 30
2θ (deg)
Inte
nsity
(a.u
.)
Zn(NO3)2.6H2O+2H2ADC
Zn(NO3)2.6H2O
H2ADC
Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2008
22
Ligand: BIPY
0102030405060708090100
5 10 15 20 25 30 35 40 45 502θ (deg)
Inte
nsity
(a.u
.)Ni(OAc)2.4H2O+1.5BIPY
Ni(OAc)2.4H2O
BIPY
0
20
40
60
80
100
120
5 10 15 20 25 30 35 40 45 502θ (deg)
Inte
nsity
(a.u
.)
Ni(NO3)2.6H2O+1.5BIPYNi(NO3)2.6H2OBIPY
0102030405060708090100
5 10 15 20 25 30 35 40 45 50
2θ (deg)
Inte
nsity
(a.u
.)
Ni(SO4).7H2O+1.5BIPYNi(SO4).7H2OBIPY
Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2008
23
0102030405060708090100
5 10 15 20 25 30
2θ (deg)
Inte
nsity
(a.u
.)Zn(OAc)2.2H2O+1.5BIPY
Zn(OAc)2.2H2O
BIPY
0102030405060708090100
10 15 20 25 30 35 402θ (deg)
Inte
nsity
(a.u
.)
Zn(NO3)2.6H2O+1.5BIPYZn(NO3)2.6H2OBIPY
Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2008
24
Ligand: H2BDC
0102030405060708090100
5 10 15 20 25 30 35 40 45 50
2θ (deg)
Inte
nsity
(a.u
.)Ni(OAc)2.4H2O+2H2BDC
Ni(OAc)2.4H2O
H2BDC
0102030405060708090100
5 10 15 20 25 30 35 40 45 50
2θ (deg)
Inte
nsity
(a.u
.)
Ni(NO3)2.6H2O+2H2BDC
Ni(NO3)2.6H2O
H2BDC
0102030405060708090100
5 10 15 20 25 30 35 40 45 50
2θ (deg)
Inte
nsity
(a.u
.)
Ni(SO4).7H2O+2H2BDCNi(SO4).7H2OH2BDC
Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2008
25
0102030405060708090100
5 10 15 20 25 30 35 40 45 502θ (deg)
Inte
nsity
(a.u
.)Zn(OAc)2.2H2O+2H2BDCZn(OAc)2.2H2OH2BDC
0102030405060708090100
10 15 20 25 30 35 402θ (deg)
Inte
nsity
(a.u
.)
Zn(NO3)2.6H2O+2H2BDCZn(NO3)2.6H2OH2BDC
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