Supporting Information
Assembly of Robust and Porous Hydrogen-Bonded Coordination Frameworks: Isomorphism, Polymorphism and Selective Adsorption Ji-Jun Jiang, Mei Pan, Jun-Min Liu, Wei Wang, and Cheng-Yong Su*
MOE Laboratory of Bioinorganic and Synthetic Chemistry, State Key Laboratory of Optoelectronic Materials and Technologies, School of Chemistry and Chemical Engineering, Sun Yat-Sen University, Guangzhou 510275, China, and State Key Laboratory of Applied Organic Chemistry, Lanzhou University, Lanzhou 730000, China.
E-mail:
[email protected] Simulation of complex 1-Gd.2H2O Complex of 1-Gd.2H2O Complex of 1-Yb.2H2O
c b a 10
20
30 2θ (°)
40
50
60
Figure S1. Powder XRD patterns of bulk sample at room temperature. a) simulation of 1-Gd.2H2O; b), 1-Gd.2H2O; c) 1-Yb.2H2O. Complex 2-Nd.3H2O Complex 2-Er.H2O Complex 2-Eu Complex 2-Gd.2H2O Simulation of 2-Gd.2H2O
e d c b a 10
20
30
2θ (°)
40
50
60
Figure S2. Powder XRD patterns of bulk sample at room temperature. a), simulation of 2-Gd; b), 2-Gd.2H2O; c), 2-Eu; d), 2-Er.H2O; e), 2-Nd.3H2O.
Figure S3. Powder XRD patterns of bulk sample at room temperature. a) simulation of 3-Gd; b), 3-Gd·1.5MeOH; c) 3-Er·1.5MeOH.
a
b
c
Figure S4. Hydrogen-binding 3D frameworks in 1-Gd⋅2H2O (upper), 2Gd⋅2H2O (middle) and 3-Gd⋅1.5CH3OH (lower): a) hydrogen bonds formed by each [Ln(ntb)(NO3)3] coordination motif shown in dash lines, b) hydrogen bonds formed between 2D layers shown in dash lines, c) cylindrical and triangular channels and lattice cavities represented in ball-and-stick modes for the frameworks and space-filling modes for the guest molecules.
100
100
Complex 2-Gd Complex 2-Gd-H2O
90
Complex 1-Gd Complex 1-Yb
90
80
80
TG %
TG %
70
70 60
60 50
50
40
40
30
30
20 100
100
200
300 400 Temperature / °C
500
600
200
700
300
400
500
600
700
Temperature / °C
a
b
100 Complex 3-Gd Complex 3-Er
90 80
TG %
70 60 50 40 30 20 100
200
300 400 500 Temperature / °C
600
700
c
Figure S5. Thermogravimetric curves: a) black line, 1-Gd•2H2O; red line, 1-Yb•2H2O; b) black line, 2-Gd; blue line, 2-Gd•2H2O; c), black line: 3-Gd·1.5MeOH, red line, 3-Er·1.5MeOH.
3000
613.5
30000
2700
25000
2400
Intensity(a. u)
Intensity(a.u)
35000
20000 622.2
15000
592.8
10000
2100 1800 1500
5000 0 550
1060
1200
600
650 λ / nm
a
700
900 800
920
900
1000
1100
1200
λ / nm
b
Figure S6. a) Solid-state luminescence spectra of 2-Eu at 298 K show the emission peak at 592, 613 and 622 nm. b) The near infrared and visible region emission of 2-Nd.3H2O scanned from 800 to 1500 nm showing peaks at 920 and 1060 nm attributable to 4F3/2 →4I9/2 and 4F3/2→4I11/2.
Table S1 Crystallographic data for 1-Gd·2H2O, 1-Yb·2H2O, 2-Eu, 2-Gd (473K) and 2-Gd·2H2O 1-Gd·2H2O
1-Yb·2H2O
2-Eu
2-Gd (473K)
2-Gd·2H2O
empirical formula
C24H25GdN10O11
formula weight
786.79
C24H25N10O11Yb
C24H21EuN10O9
C24H21GdN7O9
C24H25GdN10O11
802.58
745.47
750.76
786.79
space group crystal system
C2/c
C2/c
P31c
P31c
P31c
a [Å ]
Monoclinic
Monoclinic
Hexagonal
Hexagonal
Hexagonal
26.2558(12)
26.5349(18)
12.0855(7)
12.0415(7)
11.800(1)
b [Å ]
14.3119(7)
14.2013(12)
12.0855(7)
12.0415(7)
11.800(1)
c [Å ]
16.9588(8)
17.1284(8)
14.0024(10)
14.1138(10)
14.033(2)
γ [deg]
99.501(4)
97.984(5)
120
120
120
V [Å3]
6285.2(5)
6391.9(8)
1771.18(19)
1772.29(19)
1692.2
Z
8
8
2
2
2
ρcalcd [g cm-3]
1.663
1.668
1.398
1.407
1.544
T [K]
293(2)
293(2)
293(2)
293(2)
293(2)
μ
[mm-1]
14.287
2.997
1.827
1.927
2.026
GOF
1.091
1.037
1.053
1.074
1.064
Rint
0.0527
0.0393
0.0618
0.0728
0.0268
R1 [I > 2σ(I)]
0.0987
0.0388
0.0586
0.0668
0.0222
wR2 (all data)
0.2353
0.1155
0.1579
0.1996
0.0614
Table S2 Crystallographic data for 2-Gd·H2O (473K-air), 2-Er·H2O , 2- Nd·3H2O, 3-Gd·1.5MeOH and 3-Er·1.5MeOH 2-Gd·H2O (473K-air)
2-Er·H2O
2-Nd·3H2O
3-Gd·1.5MeOH
3-Er·1.5MeOH
empirical formula
C24H23GdN10O10
C24H23ErN10O10
C24H27N10O12Nd
C51H54Gd2N20O21
C51H54Er2N20O21
formula weight
768.77
778.78
791.80
1597.64
1617.66
space group
P31c
P31c
P31c
Pa-3
Pa-3
crystal system
Hexagonal
Hexagonal
Hexagonal
Cubic
Cubic
a [Å ]
11.9067(4)
12.0072(4)
11.9877(4)
18.24120(10)
18.3775(12)
b [Å ]
11.9067(4)
12.0072(4)
11.9877(4)
18.24120(10)
18.3775(12)
c [Å ]
14.1230(5)
14.1282(6)
14.2824(5)
18.24120(10)
18.3775(12)
γ [deg]
120
120
120
90
90
V [Å3]
1733.96(10)
1764.01(11)
1777.47(10)
6069.60(6)
6206.7(7)
Z
2
2
2
4
4
ρcalcd [g cm-3]
1.472
1.466
1.479
1.748
1.731
T [K]
293(2)
293(2)
293(2)
293(2)
293(2)
μ
1.974
2.439
1.528
2.260
2.777
GOF
1.066
1.060
1.098
1.017
1.011
Rint
0.0428
0.0566
0.0434
0.0469
0.0645
R1 [I > 2σ(I)]
0.0335
0.0407
0.0357
0.0287
0.0419
wR2 (all data)
0.0657
0.0980
0.0915
0.0784
0.1570
[mm-1]
Table S3. Selected bond lengths (Å) for complexes. 1-Gd•2H2O
1-Yb•2H2O
2-Er•H2O
2-Eu
2-Nd•3H2O
Gd(1)-O(8)
2.484(7)
Gd(1)-O(7')
2.21(3)
Gd(1)-O(2)
2.514(5)
Gd(1)-O(2)#1
2.475(6)
Nd(1)-O(1)
2.552(5)
Gd(1)-O(2)
2.489(9)
Gd(1)-O(2)
2.406(4)
Gd(1)-O(2)#1 2.514(5)
Gd(1)-O(2)#2
2.475(6)
Nd(1)-O(1)#1
2.552(5)
Gd(1)-O(7)
2.505(8)
Gd(1)-O(7)
2.42(3)
Gd(1)-O(2)#2 2.514(5)
Gd(1)-O(2)
2.475(6)
Nd(1)-O(1)#2
2.552(5)
Gd(1)-O(4)
2.510(7)
Gd(1)-O(5)
2.424(4)
Gd(1)-O(1)#1 2.566(5)
Gd(1)-O(1)#1
2.527(6)
Nd(1)-O(2)
2.590(5)
Gd(1)-O(5)
2.511(7)
Gd(1)-N(2)
2.437(5)
Gd(1)-O(1)
Gd(1)-O(1)#2
2.527(6)
Nd(1)-O(2)#1
2.590(5)
Gd(1)-N(3)
2.532(8)
Gd(1)-O(1)
2.461(5)
Gd(1)-O(1)#2 2.566(5)
Gd(1)-O(1)
2.527(6)
Nd(1)-O(2)#2
2.590(5)
Gd(1)-N(4)
2.559(8)
Gd(1)-N(4)
2.480(5)
Gd(1)-N(3)
Gd(1)-N(4)#1
2.528(6)
Nd(1)-N(2)#2
2.595(6)
Gd(1)-O(1)
2.584(8)
Gd(1)-N(3)
2.491(5)
Gd(1)-N(3)#2 2.573(7)
Gd(1)-N(4)
2.528(6)
Nd(1)-(2)#1
2.595(7)
Gd(1)-N(2)
2.583(8)
Gd(1)-O(4)
2.528(4)
Gd(1)-N(3)#1 2.573(7)
Gd(1)-N(4)#2
2.528(6)
Nd(1)-N(2)
2.595(6)
Gd(1)-N(1)
2.746(8)
Gd(1)-N(1)
2.675(4)
Gd(1)-N(1)
Gd(1)-N(1)
2.679(11)
Nd(1)-N(1)
2.742(8)
Gd(1)-N(9)
2.885(11)
Gd(1)-O(8')
2.77(2)
Gd(1)-N(3)#1
2.927(9)
Nd(1)-N(4)
3.004(7)
Gd(1)-N(10)
2.916(11)
Gd(1)-N(8)
2.841(6)
Gd(1)-N(3)#2
2.927(9)
Nd(1)-N(4)#1
3.004(7)
.
2-Gd (473 K)
2-Gd 2H2O
Gd(1)-O(2)#1 2.503(7)
Gd(1)-O(1)
Gd(1)-O(2)#2 2.503(7) Gd(1)-O(2)
2.566(5)
2.573(7)
2.710(8)
.
2-Gd H2O (473 K-air)
3-Gd•1.5CH3OH
3-Er•1.5CH3OH
Gd(1)-O(1)#12.493(4)
Gd(1)-O(1)#1
2.477(3)
Gd(1)-O(1)#1
2.485(5)
Gd(1)-O(1)#1 2.488(3)
Gd(1)-O(1)#2 2.493(4)
Gd(1)-O(1)#2
2.477(3)
Gd(1)-O(1)
2.485(5)
2.503(7)
Gd(1)-O(1)#2 2.488(3)
Gd(1)-O(1)
2.493(4)
Gd(1)-O(1)
2.477(3)
Gd(1)-O(1)#2
2.485(5)
Gd(1)-O(1)#1 2.540(8)
Gd(1)-N(2)#1 2.523(4)
Gd(1)-N(2)
2.537(4)
Gd(1)-N(2)
2.551(3)
Gd(1)-O(2)
2.543(5)
2.488(3)
Gd(1)-O(1)#2 2.540(8)
Gd(1)-N(2)
2.523(4)
Gd(1)-N(2)#2 2.537(4)
Gd(1)-N(2)#2
2.551(3)
Gd(1)-O(2)#2
2.543(5)
Gd(1)-O(1)
2.540(8)
Gd(1)-N(2)#2 2.523(4)
Gd(1)-N(2)#1 2.537(4)
Gd(1)-N(2)#1
2.551(3)
Gd(1)-O(2)#1
2.543(5)
Gd(1)-N(2)
2.539(9)
Gd(1)-O(2)
2.528(3)
Gd(1)-O(2)#2 2.542(4)
Gd(1)-O(2)#1
2.554(3)
Gd(1)-N(2)#1
2.569(4)
Gd(1)-N(2)#2 2.539(9)
Gd(1)-O(2)#1 2.528(3)
Gd(1)-O(2)#1 2.542(4)
Gd(1)-O(2)#2
2.554(3)
Gd(1)-N(2)
2.569(4)
Gd(1)-N(2)#1 2.539(9)
Gd(1)-O(2)#2 2.528(3)
Gd(1)-O(2)
2.542(4)
Gd(1)-O(2)
2.554(3)
Gd(1)-N(2)#2
2.569(4)
Gd(1)-N(1)
2.734(14)
Gd(1)-N(1)
2.681(5)
Gd(1)-N(1)
2.706(5)
Gd(1)-N(1)
2.702(5)
Gd(1)-N(1)
2.714(7)
Gd(1)-N(4)#1 2.977(10)
Gd(1)-N(4)
2.930(4)
Gd(1)-N(4)#2 2.943(5)
Gd(1)-N(4)#1
2.928(3)
Gd(1)-N(4)
2.916(6)
Gd(1)-N(4)#2 2.977(10)
Gd(1)-N(4)#1 2.930(4)
Gd(1)-N(4)#1 2.943(5)
Gd(1)-N(4)#2
2.928(3)
Gd(1)-N(4)#1
2.916(6)
Table S4. Selected bond Angles (º) for complexes 1-Gd•2H2O, 2-Gd•2H2O and 3-Gd•1.5CH3OH. 1-Gd.2H2O
2-Gd.2H2O
3-Gd. 1.5CH3OH
O(8)-Gd(1)-O(2)
110.6(3)
O(2)#1-Gd(1)-N(2)
76.5(3)
O(1)#1-Gd(1)-O(1)#2
69.40(11)
(8)-Gd(1)-O(7)
51.7(2)
O(2)#2-Gd(1)-N(2)
143.6(2)
O(1)#1-Gd(1)-O(1)
69.40(11)
O(2)-Gd(1)-O(7)
109.7(3)
O(2)-Gd(1)-N(2)
68.0(3)
O(1)#2-Gd(1)-O(1)
69.40(11)
O(8)-Gd(1)-O(4)
68.1(3)
O(1)#1-Gd(1)-N(2)
72.0(3)
O(1)#1-Gd(1)-N(2)
76.83(10)
O(2)-Gd(1)-O(4)
68.7(3)
O(1)#2-Gd(1)-N(2)
165.1(3)
O(1)#2-Gd(1)-N(2)
119.47(9)
O(7)-Gd(1)-O(4)
115.2(2)
O(1)-Gd(1)-N(2)
76.5(3)
O(1)-Gd(1)-N(2)
138.92(9)
O(8)-Gd(1)-O(5)
72.6(2)
O(2)#1-Gd(1)-N(2)#2
143.6(2)
O(1)#1-Gd(1)-N(2)#2
119.47(9)
O(2)-Gd(1)-O(5)
114.1(3)
O(2)#2-Gd(1)-N(2)#2
114.9(3)
O(1)#2-Gd(1)-N(2)#2
138.92(9)
O(7)-Gd(1)-O(5)
118.0(2)
O(2)-Gd(1)-N(2)#2
72.0(3)
O(1)-Gd(1)-N(2)#2
76.83(10)
O(4)-Gd(1)-O(5)
51.4(2)
O(1)#1-Gd(1)-N(2)#2
165.1(3)
N(2)-Gd(1)-N(2)#2
101.30(8)
O(8)-Gd(1)-N(3)
123.1(3)
O(1)#2-Gd(1)-N(2)#2
68.0(3)
O(1)#1-Gd(1)-N(2)#1
138.92(9)
O(2)-Gd(1)-N(3)
72.2(3)
O(1)-Gd(1)-N(2)#2
101.3(3)
O(1)#2-Gd(1)-N(2)#1
76.83(10)
O(7)-Gd(1)-N(3)
73.3(3)
N(2)-Gd(1)-N(2)#2
143.6(2)
O(1)-Gd(1)-N(2)#1
119.47(9)
O(4)-Gd(1)-N(3)
140.5(3)
O(2)#1-Gd(1)-N(2)#1
114.9(3)
N(2)-Gd(1)-N(2)#1
101.30(9)
O(5)-Gd(1)-N(3)
161.1(2)
O(2)#2-Gd(1)-N(2)#1
76.5(3)
N(2)#2-Gd(1)-N(2)#1
101.30(8)
O(8)-Gd(1)-N(4)
77.7(3)
O(2)-Gd(1)-N(2)#1
165.1(3)
O(1)#1-Gd(1)-O(2)#1
50.66(9)
O(2)-Gd(1)-N(4)
171.3(3)
O(1)#1-Gd(1)-N(2)#1
68.0(3)
O(1)#2-Gd(1)-O(2)#1
115.70(9)
O(7)-Gd(1)-N(4)
73.1(3)
O(1)#2-Gd(1)-N(2)#1
72.0(3)
O(1)-Gd(1)-O(2)#1
69.75(9)
O(4)-Gd(1)-N(4)
118.1(2)
O(1)-Gd(1)-N(2)#1
101.3(3)
N(2)-Gd(1)-O(2)#1
70.93(9)
O(5)-Gd(1)-N(4)
70.1(3)
N(2)-Gd(1)-N(2)#1
101.3(3)
N(2)#2-Gd(1)-O(2)#1
71.21(9)
N(3)-Gd(1)-N(4)
101.4(3)
N(2)#2-Gd(1)-N(2)#1
137.22(17)
N(2)#1-Gd(1)-O(2)#1
167.23(10)
O(8)-Gd(1)-O(1)
64.9(3)
O(2)#1-Gd(1)-N(1)
137.22(17)
O(1)#1-Gd(1)-O(2)#2
69.75(9)
O(2)-Gd(1)-O(1)
49.2(3)
O(2)#2-Gd(1)-N(1)
137.22(17)
O(1)#2-Gd(1)-O(2)#2
50.66(9)
O(7)-Gd(1)-O(1)
67.9(3)
O(2)-Gd(1)-N(1)
102.11(19)
O(1)-Gd(1)-O(2)#2
115.70(9)
O(4)-Gd(1)-O(1)
66.8(3)
O(1)#1-Gd(1)-N(1)
102.11(19)
N(2)-Gd(1)-O(2)#2
71.21(9)
O(5)-Gd(1)-O(1)
114.2(3)
O(1)#2-Gd(1)-N(1)
102.11(19)
N(2)#2-Gd(1)-O(2)#2
167.23(10)
N(3)-Gd(1)-O(1)
83.7(3)
O(1)-Gd(1)-N(1)
63.2(2)
N(2)#1-Gd(1)-O(2)#2
70.93(9)
N(4)-Gd(1)-O(1)
137.2(3)
N(2)-Gd(1)-N(1)
63.2(2)
O(2)#1-Gd(1)-O(2)#2
114.35(5)
O(8)-Gd(1)-N(2)
138.2(3)
N(2)#2-Gd(1)-N(1)
63.2(2)
O(1)#1-Gd(1)-O(2)
115.70(9)
O(2)-Gd(1)-N(2)
69.0(3)
N(2)#1-Gd(1)-N(1)
23.5(2)
O(1)#2-Gd(1)-O(2)
69.75(9)
O(7)-Gd(1)-N(2)
170.1(3)
O(2)#1-Gd(1)-N(4)#1
71.1(2)
O(1)-Gd(1)-O(2)
50.66(9)
O(4)-Gd(1)-N(2)
73.9(2)
O(2)#2-Gd(1)-N(4)#1
94.2(2)
N(2)-Gd(1)-O(2)
167.23(10)
O(5)-Gd(1)-N(2)
70.4(3)
O(2)-Gd(1)-N(4)#1
25.6(2)
N(2)#2-Gd(1)-O(2)
70.93(9)
N(3)-Gd(1)-N(2)
97.2(3)
O(1)#1-Gd(1)-N(4)#1
120.0(3)
N(2)#1-Gd(1)-O(2)
71.21(9)
N(4)-Gd(1)-N(2)
106.7(3)
O(1)#2-Gd(1)-N(4)#1
93.9(3)
O(2)#1-Gd(1)-O(2)
114.35(5)
O(1)-Gd(1)-N(2)
114.8(3)
O(1)-Gd(1)-N(4)#1
92.5(3)
O(2)#2-Gd(1)-O(2)
114.35(5)
O(8)-Gd(1)-N(1)
141.6(2)
N(2)-Gd(1)-N(4)#1
72.7(3)
O(1)#1-Gd(1)-N(1)
138.90(7)
O(2)-Gd(1)-N(1)
107.3(3)
N(2)#2-Gd(1)-N(4)#1
165.9(2)
O(1)#2-Gd(1)-N(1)
138.90(7)
O(7)-Gd(1)-N(1)
109.1(3)
N(2)#1-Gd(1)-N(4)#1
122.02(19)
O(1)-Gd(1)-N(1)
138.90(7)
O(4)-Gd(1)-N(1)
134.1(3)
N(1)-Gd(1)-N(4)#1
94.2(2)
N(2)-Gd(1)-N(1)
63.24(7)
O(5)-Gd(1)-N(1)
97.4(2)
O(2)#1-Gd(1)-N(4)#2
23.5(2)
N(2)#2-Gd(1)-N(1)
63.24(7)
N(3)-Gd(1)-N(1)
63.9(3)
O(2)#2-Gd(1)-N(4)#2
71.1(2)
N(2)#1-Gd(1)-N(1)
63.24(7)
N(4)-Gd(1)-N(1)
64.2(3)
O(2)-Gd(1)-N(4)#2
93.9(3)
O(2)#1-Gd(1)-N(1)
103.99(7)
O(1)-Gd(1)-N(1)
146.0(2)
O(1)#1-Gd(1)-N(4)#2
25.6(2)
O(2)#2-Gd(1)-N(1)
103.99(7)
N(2)-Gd(1)-N(1)
63.0(3)
O(1)#2-Gd(1)-N(4)#2
120.0(3)
O(2)-Gd(1)-N(1)
103.99(7)
O(8)-Gd(1)-N(9)
70.1(3)
O(1)-Gd(1)-N(4)#2
72.7(3)
O(1)#1-Gd(1)-N(4)#1
25.39(9)
O(2)-Gd(1)-N(9)
90.4(3)
N(2)-Gd(1)-N(4)#2
165.9(2)
O(1)#2-Gd(1)-N(4)#1
92.26(10)
O(7)-Gd(1)-N(9)
121.8(3)
N(2)#2-Gd(1)-N(4)#2
92.5(3)
O(1)-Gd(1)-N(4)#1
66.34(9)
O(4)-Gd(1)-N(9)
25.7(2)
N(2)#1-Gd(1)-N(4)#2
122.02(19)
N(2)-Gd(1)-N(4)#1
73.07(9)
O(5)-Gd(1)-N(9)
25.8(2)
N(1)-Gd(1)-N(4)#2
94.5(3)
N(2)#2-Gd(1)-N(4)#1
95.07(10)
N(3)-Gd(1)-N(9)
160.8(3)
N(4)#1-Gd(1)-N(4)#2
116.95(9)
N(2)#1-Gd(1)-N(4)#1
163.49(10)
N(4)-Gd(1)-N(9)
94.9(3)
O(2)#1-Gd(1)-N(4)#1
25.30(9)
O(1)-Gd(1)-N(9)
91.2(3)
O(2)#2-Gd(1)-N(4)#1
92.58(9)
N(2)-Gd(1)-N(9)
68.1(3)
O(2)-Gd(1)-N(4)#1
116.95(9)
N(1)-Gd(1)-N(9)
115.9(3)
N(1)-Gd(1)-N(4)#1
124.03(7)
O(8)-Gd(1)-N(10)
25.7(3)
O(1)#1-Gd(1)-N(4)#2
66.34(9)
O(2)-Gd(1)-N(10)
110.5(3)
O(1)#2-Gd(1)-N(4)#2
25.39(9)
O(7)-Gd(1)-N(10)
26.1(3)
O(1)-Gd(1)-N(4)#2
92.26(10)
O(4)-Gd(1)-N(10)
90.7(3)
N(2)-Gd(1)-N(4)#2
95.07(10)
O(5)-Gd(1)-N(10)
96.2(3)
N(2)#2-Gd(1)-N(4)#2
163.49(10)
N(3)-Gd(1)-N(10)
97.9(3)
N(2)#1-Gd(1)-N(4)#2
73.07(9)
N(4)-Gd(1)-N(10)
75.8(3)
O(2)#1-Gd(1)-N(4)#2
116.95(9)
O(1)-Gd(1)-N(10)
61.5(3)
O(2)#2-Gd(1)-N(4)#2
25.30(9)
N(2)-Gd(1)-N(10)
163.8(3)
O(2)-Gd(1)-N(4)#2
92.58(9)
N(1)-Gd(1)-N(10)
129.8(3)
N(1)-Gd(1)-N(4)#2
124.03(7)
N(9)-Gd(1)-N(10)
95.8(3)
N(4)#1-Gd(1)-N(4)#2
91.73(10)
Symmetry codes for 2-Er•H2O: #1 -x+y+1,-x+1, z, #2 -y+1, x-y, z . 2-Eu: #1 -x+y-1,-x-1,z, #2 -y-1,x-y, z. 2-Gd (473 K): #1 -x+y,-x+1,z, #2 y+1,x-y+1,z. 2-Gd•2H2O: #1 -y+1,x-y, z, #2 -x+y+1,-x+1,z. 2-Gd•H2O (473 K - air): #1 -x+y+1,-x+1,z, #2 -y+1,x-y, z. 2-Nd :#1 -y+1,x-y+1,z, #2 -x+y,-x+1,z. 3-Gd• 1.5CH3OH: #1 -z+1,x-1/2,-y+1/2, #2 y+1/2,-z+1/2,-x+1, #3 -x+2,-y+1,-z , #4 -y+3/2,z+1/2,x-1, #5 z+1,-x+3/2,y-1/2. 3-Er•1.5CH3OH: #1 y, z, x, #2 z, x, y.
Table S5.
Hydrogen Bond Lengths (Å) and Bond Angles (º) in complexes for complexes 1-Gd•2H2O, 2-Gd•2H2O and
3-Gd•1.5CH3OH.
Donor -H... Acceptor
D-H
D...A
D - H...A
1-Gd⋅2H2O ...
0.86
3.062(17)
118
...
0.86
2.936(18)
166
...
0.86
2.800(18)
159
0.86
2.85(3)
146
N(5)-H(5A) O(5) N(5)-H(5A) O(6) N(6)-H(6A) O(3) ...
N(7)-H(7A) O(1W)
2-Gd⋅2H2O ...
N(3)-H(3A) O(2)
0.86
2.9860
163
N(3)-H(3A) ... O(3)
0.86
3.0159
128
2.9406
133
3-Gd⋅1.5CH3OH N(3)-H(3A) ... O(3)
0.86
Symmetry codes for 1-Gd⋅2H2O: 1/2-x, 1/2-y, 1-z. For 1-Gd⋅2H2O: x, 1-y, 1/2+z; 1-x, -x+y, -1/2+z. For 3-Gd⋅1.5CH3OH: -1/2+x, y, 1/2-z.
