Synthesis and structure characterization of two cadmium coordination polymers based on μ 2 -bridging bidentate hydrazine ligand
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1 Electronic Supplementary Data Synthesis and structure characterization of two cadmium coordination polymers based on μ 2 -bridging bidentate hydrazine ligand D Santhosh Shanthakumar a, R Pradeep b, B Subramani c & B N Sivasankar b, * a Department of Chemistry, Sri Krishna College of Technology, Kovaipudur, Coimbatore , Tamilnadu, India b Department of Chemistry, Government Arts College, Udhagamandalam, The Nilgiris , Tamilnadu, India c Department of Chemistry, Crescent School, Vandalur, Chennai , Tamil Nadu, India sivabickol@yahoo.com No. Contents Pg No. 1 Fig. S1 Infrared spectrum of Fig. S2 Infrared spectrum of Fig. S3 Simultaneous TG-DTA of Fig. S4 Simultaneous TG-DTA of Fig. S5 Bridging binding modes of the unique ligands in Fig. S6 Coordination geometry of the Cd(II) ion of Fig. S7 Bridging binding mode of hydrazine ligand in Fig. S8 Linkage of three different malonate ligands. 5 9 Fig. S9 The μ 3 -bridging pentadentate binding mode of the malonate ligand Table S1 Bond angles of 1 and Table S2 Hydrogen bonding data for 1 and 2 7 1
2 Fig. S1 - Infrared spectrum of 1. Fig. S2 - Infrared spectrum of 2. 2
3 Fig. S3 - Simultaneous TG-DTA of 1. Fig. S4 - Simultaneous TG-DTA of 2. 3
4 Fig. S5a Bridging binding mode mode of the hydrazine ligand (N3N4) in 1. The bidentate bridging binding mode of the first unique hydrazine (N3N4) ligand resulting in a Cd Cd separation of The O1 (or O6) is the terminal oxygen of the nitro group. For clarity the N5 and N6 from the second unique hydrazine on each Cd is not displayed. Fig. S5b Bridging binding mode of the hydrazine ligand (N5N6) in 1. The bidentate bridging binding mode of the second unique hydrazine (N5N6) ligand resulting in a Cd Cd separation of The O1 (or O6) is the terminal oxygen of the nitro group. For clarity the N3 and N4 atoms on each Cd is not displayed. Fig. S6 Coordination geometry of the Cd(II) ion of 2. 4
5 Fig. S7 Bridging binding mode of the hydrazine ligand (N1N2) in 2. The μ 2 -bridging bidentate binding mode of the unique hydrazine ligand in 2 results in a Cd Cd separation of Å. A pair of unique ligands (N1-N2) link a pair of Cd(II) ions. This feature ({Cd 2 N 4 } six membered ring) is same as in 1. Fig. S8 Each malonate is linked to three Cd(II). Alternatively each Cd(II) is linked to three different malonate ligands. Fig. S9 The μ 3 -bridging pentadentate binding mode, leads to three different Cd Cd separations of 3.755, and Å respectively. 5
6 Table S1 - Bond angles for [Cd(NO 3 ) 2 (N 2 H 4 ) 2 ] (1) and Cd(C 3 H 2 O 4 )(N 2 H 4 ) (2) Bond angles (deg.) N(2)-O(6)-Cd(1) 109.5(4) O(1)-C(1)-Cd(1) 66.10(13) N(2')-O(8')-Cd(1) 105.4(16) O(2)-C(1)-Cd(1) 56.81(13) N(4)-N(3)-Cd(1) (9) C(2)-C(1)-Cd(1) (18) Cd(1)-N(3)-H(3A) 109.0(16) N(2)-N(1)-Cd(1) (15) N(3)-N(4)-Cd(1)# (9) Cd(1)-N(1)-H(1A) 110(2) Cd(1)#1-N(4)-H(4B) 109.1(15) Cd(1)-N(1)-H(1B) 107.2(18) Cd(1)#1-N(4)-H(4A) 105.4(15) N(1)-N(2)-Cd(1)# (15) N(1)-O(1)-Cd(1) (9) Cd(1)#3-N(2)-H(2D) 105(2) N(5)#2-N(6)-Cd(1) (9) Cd(1)#3-N(2)-H(2C) 108(2) Cd(1)-N(6)-H(6B) 109.7(14) C(1)-O(1)-Cd(1) 87.10(15) Cd(1)-N(6)-H(6A) 106.1(14) C(1)-O(2)-Cd(1) 95.97(15) N(6)#2-N(5)-Cd(1) (8) C(3)-O(3)-Cd(1) (16) Cd(1)-N(5)-H(5A) 109.6(14) C(3)-O(3)-Cd(1)# (17) Cd(1)-N(5)-H(5B) 109.6(15) Cd(1)-O(3)-Cd(1)# (7) N(4)#1-Cd(1)-N(5) 88.59(4) C(3)-O(4)-Cd(1) 86.52(15) N(4)#1-Cd(1)-N(6) (4) N(1)-Cd(1)-O(2) (7) N(5)-Cd(1)-N(6) 90.90(4) N(1)-Cd(1)-O(3) (7) N(4)#1-Cd(1)-N(3) 91.91(4) O(2)-Cd(1)-O(3) 88.72(7) N(5)-Cd(1)-N(3) (4) N(1)-Cd(1)-N(2)# (8) N(6)-Cd(1)-N(3) 88.14(4) O(2)-Cd(1)-N(2)# (8) N(4)#1-Cd(1)-O(6) (14) O(3)-Cd(1)-N(2)# (8) N(5)-Cd(1)-O(6) 83.61(12) N(1)-Cd(1)-O(3)# (7) N(6)-Cd(1)-O(6) 81.63(14) O(2)-Cd(1)-O(3)# (7) N(3)-Cd(1)-O(6) (11) O(3)-Cd(1)-O(3)# (7) N(4)#1-Cd(1)-O(1) 99.27(4) N(2)#3-Cd(1)-O(3)# (8) N(5)-Cd(1)-O(1) 92.85(4) N(1)-Cd(1)-O(1) 83.23(7) N(6)-Cd(1)-O(1) 77.71(4) O(2)-Cd(1)-O(1) 53.97(6) N(3)-Cd(1)-O(1) 78.42(4) O(3)-Cd(1)-O(1) (7) O(6)-Cd(1)-O(1) (15) N(2)#3-Cd(1)-O(1) (7) N(4)#1-Cd(1)-O(8') 74.2(3) O(3)#4-Cd(1)-O(1) 81.00(7) N(5)-Cd(1)-O(8') 112.3(4) N(1)-Cd(1)-O(4) 80.31(7) N(6)-Cd(1)-O(8') 108.8(3) O(2)-Cd(1)-O(4) 90.98(7) N(3)-Cd(1)-O(8') 76.2(4) O(3)-Cd(1)-O(4) 51.84(6) O(6)-Cd(1)-O(8') 40.6(3) N(2)#3-Cd(1)-O(4) 93.31(7) O(1)-Cd(1)-O(8') 153.5(4) O(3)#4-Cd(1)-O(4) (6) O(1)-Cd(1)-O(4) (6) N(1)-Cd(1)-C(1) 93.51(7) O(2)-Cd(1)-C(1) 27.22(7) O(3)-Cd(1)-C(1) (7) N(2)#3-Cd(1)-C(1) (8) O(3)#4-Cd(1)-C(1) 81.92(7) O(1)-Cd(1)-C(1) 26.80(7) O(4)-Cd(1)-C(1) (7) Symmetry transformations used to generate equivalent atoms: #1 -x,-y,-z; #3 -x,-y,-z+1; #4 -x,-y,-z. 6
7 Table S2 - Hydrogen bonds [Å and deg.] Compound 1 D-H... A d(d-h) d(h...a) d(d...a) <(DHA) N(3)-H(3B)...O(8) 0.876(14) 2.64(2) 3.141(5) 117.5(16) N(3)-H(3B)...O(2)# (14) 2.302(15) (18) 151.5(18) N(6)-H(6B)...O(7)# (14) 2.45(2) 3.083(8) 129.2(17) N(6)-H(6B)...O(3)# (14) 2.279(14) (19) 155.7(18) N(4)-H(4B)...O(7)# (14) 2.365(17) 3.106(8) 146.1(18) N(4)-H(4B)...O(3)# (14) 2.484(19) (18) 136.1(18) N(3)-H(3A)...O(7)# (14) 2.492(19) 3.128(9) 132.0(18) N(6)-H(6A)...O(6)# (14) 2.315(17) 2.977(4) 131.5(17) N(6)-H(6A)...O(6')# (14) 2.25(2) 2.971(15) 138.7(19) N(4)-H(4A)...O(8)# (14) 2.53(2) 3.086(5) 123.6(19) N(4)-H(4A)...O(8')# (14) 2.50(3) 2.942(14) 112.9(19) N(4)-H(4A)...O(1) 0.858(14) 2.292(17) (17) 138(2) N(5)-H(5A)...O(6)# (14) 2.226(17) 2.916(5) 133.2(17) N(5)-H(5A)...O(6')# (14) 2.109(19) 2.863(14) 140.8(19) N(5)-H(5B)...O(7)# (14) 2.297(18) 3.150(10) 161(2) N(5)-H(5B)...O(3)# (14) 2.488(18) (18) 120.3(16) Symmetry transformations used to generate equivalent atoms: #1 -x,-y,-z; #2 -x,-y,-z-1; #3 x,y+1,z; #4 x-1,y,z; #5 -x-1,-y,-z; #6 -x,-y+1,-z; #7 x+1,y,z #8 x,y-1,z. Compound 2 N(1)-H(1A)...O(1)# (17) 2.26(2) 3.082(3) 162(3) N(1)-H(1B)...O(2)# (16) 2.186(18) 2.955(3) 149(2) N(2)-H(2D)...O(2)# (17) 2.401(18) 3.193(3) 158(3) N(2)-H(2D)...O(3)# (17) 2.66(3) 2.995(3) 106(2) N(2)-H(2C)...O(4) 0.835(17) 2.24(2) 2.951(3) 143(3) Symmetry transformations used to generate equivalent atoms: #5 -x+1,-y,-z+1; #6 x,-y+1/2,z+1/2; #7 x,y,z+1. 7
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