SUPPLEMENTAL MATERIAL FOR REVIEW PURPOSES ONLY. NOT FOR PUBLICATION
Table 1. Crystal data and structure refinement for cdmipise.
Identification code cdmipise
Empirical formula C20 H32 Cd F12 N8 P2 Se4
Formula weight 1102.72
Temperature 158(2) K
Wavelength 0.71073 A
Crystal system, space group Orthorhombic, Pbcn
Unit cell dimensions a = 12.783(3) A alpha = 90 deg.
b = 22.206(4) A beta = 90 deg.
c = 13.153(3) A gamma = 90 deg.
Volume 3733.8(13) A^3
Z, Calculated density 4, 1.962 Mg/m^3
Absorption coefficient 4.656 mm^-1
F(000) 2120
Crystal size 0.50 x 0.05 x 0.02 mm
Theta range for data collection 2.40 to 25.01 deg.
Limiting indices -15<=h<=12, -25<=k<=26, -15<=l<=15
Reflections collected / unique 16141 / 3291 [R(int) = 0.1334]
Completeness to theta = 25.01 99.8 %
Absorption correction REQAB (multi-scan)
Max. and min. transmission 0.9126 and 0.2042
Refinement method Full-matrix least-squares on F^2
Data / restraints / parameters 3291 / 0 / 219
Goodness-of-fit on F^2 1.053
Final R indices [I>2sigma(I)] R1 = 0.0687, wR2 = 0.1494
R indices (all data) R1 = 0.1174, wR2 = 0.1758
Largest diff. peak and hole 1.269 and -0.751 e.A^-3
Table 2. Atomic coordinates ( x 10^4) and equivalent isotropic
displacement parameters (A^2 x 10^3) for cdmipise.
U(eq) is defined as one third of the trace of the orthogonalized
Uij tensor.
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x y z U(eq)
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Cd(1) 0 3705(1) 7500 30(1)
Se(1) 246(1) 4339(1) 9178(1) 38(1)
Se(2) 1798(1) 3172(1) 7236(1) 52(1)
N(1) -1832(7) 4202(4) 10021(6) 35(2)
N(2) -1763(7) 4919(4) 8904(6) 32(2)
N(3) 2990(8) 3545(4) 8981(7) 43(2)
N(4) 1872(8) 2867(4) 9368(6) 40(2)
C(1) -1167(7) 4488(4) 9364(7) 28(2)
C(2) -2813(9) 4461(6) 9964(8) 44(3)
C(3) -2778(9) 4895(6) 9263(8) 43(3)
C(4) -1528(11) 3693(5) 10640(9) 49(3)
C(5) -1378(10) 5359(5) 8186(9) 43(3)
C(6) 2213(9) 3212(5) 8603(7) 35(2)
C(7) 3085(12) 3435(7) 10005(9) 57(4)
C(8) 2406(13) 3005(7) 10258(10) 60(4)
C(9) 3629(13) 3998(7) 8402(13) 69(4)
C(10) 999(11) 2440(7) 9294(12) 64(4)
P(1) 0 814(2) 7500 35(1)
P(2) 0 2631(2) 12500 43(1)
F(1) 0 126(6) 7500 118(6)
F(2) 69(7) 813(6) 6288(6) 91(3)
F(3) 1222(6) 805(6) 7571(7) 103(4)
F(4) 0 1501(6) 7500 157(10)
F(7) 989(7) 2624(4) 13213(7) 79(3)
F(8) 530(8) 3134(4) 11843(9) 89(3)
F(9) 528(8) 2120(4) 11816(7) 76(3)
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Table 3. Bond lengths [A] and angles [deg] for cdmipise.
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Cd(1)-Se(2)#1 2.6090(13)
Cd(1)-Se(2) 2.6090(13)
Cd(1)-Se(1) 2.6364(12)
Cd(1)-Se(1)#1 2.6364(12)
Se(1)-C(1) 1.852(10)
Se(2)-C(6) 1.876(9)
N(1)-C(1) 1.368(13)
N(1)-C(2) 1.382(14)
N(1)-C(4) 1.446(14)
N(2)-C(1) 1.365(12)
N(2)-C(3) 1.381(14)
N(2)-C(5) 1.446(14)
N(3)-C(6) 1.334(15)
N(3)-C(7) 1.374(15)
N(3)-C(9) 1.503(17)
N(4)-C(6) 1.339(14)
N(4)-C(8) 1.390(15)
N(4)-C(10) 1.468(16)
C(2)-C(3) 1.335(17)
C(2)-H(2) 0.9600
C(3)-H(3) 0.9600
C(4)-H(4A) 0.9599
C(4)-H(4B) 0.9599
C(4)-H(4C) 0.9599
C(5)-H(5A) 0.9599
C(5)-H(5B) 0.9599
C(5)-H(5C) 0.9599
C(7)-C(8) 1.33(2)
C(7)-H(7) 0.9600
C(8)-H(8) 0.9600
C(9)-H(9A) 0.9599
C(9)-H(9B) 0.9599
C(9)-H(9C) 0.9599
C(10)-H(10A) 0.9599
C(10)-H(10B) 0.9599
C(10)-H(10C) 0.9599
P(1)-F(4) 1.526(14)
P(1)-F(1) 1.526(13)
P(1)-F(3) 1.565(8)
P(1)-F(3)#1 1.565(8)
P(1)-F(2) 1.597(7)
P(1)-F(2)#1 1.597(7)
P(2)-F(8) 1.567(9)
P(2)-F(8)#2 1.567(9)
P(2)-F(7)#2 1.574(8)
P(2)-F(7) 1.574(8)
P(2)-F(9)#2 1.598(8)
P(2)-F(9) 1.598(8)
Se(2)#1-Cd(1)-Se(2) 125.96(8)
Se(2)#1-Cd(1)-Se(1) 103.65(4)
Se(2)-Cd(1)-Se(1) 104.41(4)
Se(2)#1-Cd(1)-Se(1)#1 104.41(4)
Se(2)-Cd(1)-Se(1)#1 103.65(4)
Se(1)-Cd(1)-Se(1)#1 115.51(7)
C(1)-Se(1)-Cd(1) 95.1(3)
C(6)-Se(2)-Cd(1) 95.7(3)
C(1)-N(1)-C(2) 109.7(9)
C(1)-N(1)-C(4) 123.5(9)
C(2)-N(1)-C(4) 126.8(10)
C(1)-N(2)-C(3) 110.2(9)
C(1)-N(2)-C(5) 125.0(9)
C(3)-N(2)-C(5) 124.7(9)
C(6)-N(3)-C(7) 109.5(11)
C(6)-N(3)-C(9) 125.9(11)
C(7)-N(3)-C(9) 124.6(12)
C(6)-N(4)-C(8) 110.3(11)
C(6)-N(4)-C(10) 124.6(10)
C(8)-N(4)-C(10) 124.9(11)
N(2)-C(1)-N(1) 105.0(8)
N(2)-C(1)-Se(1) 127.7(8)
N(1)-C(1)-Se(1) 127.3(7)
C(3)-C(2)-N(1) 107.9(10)
C(3)-C(2)-H(2) 126.1
N(1)-C(2)-H(2) 126.1
C(2)-C(3)-N(2) 107.2(10)
C(2)-C(3)-H(3) 126.4
N(2)-C(3)-H(3) 126.4
N(1)-C(4)-H(4A) 109.5
N(1)-C(4)-H(4B) 109.5
H(4A)-C(4)-H(4B) 109.5
N(1)-C(4)-H(4C) 109.5
H(4A)-C(4)-H(4C) 109.5
H(4B)-C(4)-H(4C) 109.5
N(2)-C(5)-H(5A) 109.5
N(2)-C(5)-H(5B) 109.5
H(5A)-C(5)-H(5B) 109.5
N(2)-C(5)-H(5C) 109.5
H(5A)-C(5)-H(5C) 109.5
H(5B)-C(5)-H(5C) 109.5
N(3)-C(6)-N(4) 106.2(9)
N(3)-C(6)-Se(2) 126.5(8)
N(4)-C(6)-Se(2) 126.9(9)
C(8)-C(7)-N(3) 108.4(12)
C(8)-C(7)-H(7) 125.8
N(3)-C(7)-H(7) 125.8
C(7)-C(8)-N(4) 105.5(11)
C(7)-C(8)-H(8) 127.2
N(4)-C(8)-H(8) 127.2
N(3)-C(9)-H(9A) 109.5
N(3)-C(9)-H(9B) 109.5
H(9A)-C(9)-H(9B) 109.5
N(3)-C(9)-H(9C) 109.5
H(9A)-C(9)-H(9C) 109.5
H(9B)-C(9)-H(9C) 109.5
N(4)-C(10)-H(10A) 109.5
N(4)-C(10)-H(10B) 109.5
H(10A)-C(10)-H(10B) 109.5
N(4)-C(10)-H(10C) 109.5
H(10A)-C(10)-H(10C) 109.5
H(10B)-C(10)-H(10C) 109.5
F(4)-P(1)-F(1) 180.000(2)
F(4)-P(1)-F(3) 90.7(5)
F(1)-P(1)-F(3) 89.3(5)
F(4)-P(1)-F(3)#1 90.7(5)
F(1)-P(1)-F(3)#1 89.3(5)
F(3)-P(1)-F(3)#1 178.6(10)
F(4)-P(1)-F(2) 90.0(5)
F(1)-P(1)-F(2) 90.0(5)
F(3)-P(1)-F(2) 90.3(5)
F(3)#1-P(1)-F(2) 89.7(5)
F(4)-P(1)-F(2)#1 90.0(5)
F(1)-P(1)-F(2)#1 90.0(5)
F(3)-P(1)-F(2)#1 89.7(5)
F(3)#1-P(1)-F(2)#1 90.3(5)
F(2)-P(1)-F(2)#1 180.0(9)
F(8)-P(2)-F(8)#2 89.0(9)
F(8)-P(2)-F(7)#2 91.4(5)
F(8)#2-P(2)-F(7)#2 89.3(6)
F(8)-P(2)-F(7) 89.3(6)
F(8)#2-P(2)-F(7) 91.4(5)
F(7)#2-P(2)-F(7) 178.9(7)
F(8)-P(2)-F(9)#2 179.1(6)
F(8)#2-P(2)-F(9)#2 90.7(6)
F(7)#2-P(2)-F(9)#2 89.4(5)
F(7)-P(2)-F(9)#2 89.8(6)
F(8)-P(2)-F(9) 90.7(6)
F(8)#2-P(2)-F(9) 179.1(6)
F(7)#2-P(2)-F(9) 89.8(6)
F(7)-P(2)-F(9) 89.4(5)
F(9)#2-P(2)-F(9) 89.5(7)
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Symmetry transformations used to generate equivalent atoms:
#1 -x,y,-z+3/2 #2 -x,y,-z+5/2
Table 4. Anisotropic displacement parameters (A^2 x 10^3) for cdmipise.
The anisotropic displacement factor exponent takes the form:
-2 pi^2 [ h^2 a*^2 U11 + ... + 2 h k a* b* U12 ]
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U11 U22 U33 U23 U13 U12
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Cd(1) 27(1) 37(1) 27(1) 0 -2(1) 0
Se(1) 30(1) 50(1) 33(1) -11(1) -6(1) 7(1)
Se(2) 43(1) 82(1) 31(1) -9(1) -1(1) 28(1)
N(1) 28(5) 44(5) 32(4) 1(4) 8(4) 2(4)
N(2) 32(5) 31(5) 34(4) 4(4) 2(4) 8(4)
N(3) 38(5) 40(5) 51(5) -15(4) -5(5) 12(4)
N(4) 44(6) 47(6) 31(4) 4(4) -6(4) 10(4)
C(1) 19(5) 35(5) 31(5) -1(4) -3(4) 2(4)
C(2) 37(6) 57(8) 38(6) -10(5) 13(5) 12(6)
C(3) 33(6) 56(7) 39(6) -6(5) 2(5) 14(5)
C(4) 56(8) 45(7) 47(6) 11(6) -1(6) 4(6)
C(5) 44(7) 39(7) 45(6) 6(5) 2(5) 7(5)
C(6) 34(6) 49(6) 23(5) -4(5) -1(4) 11(5)
C(7) 65(9) 63(9) 45(7) -14(6) -33(7) 18(7)
C(8) 68(10) 74(10) 38(6) 6(6) -25(6) 15(8)
C(9) 68(10) 54(8) 86(11) -2(8) 30(9) -4(7)
C(10) 50(9) 64(9) 78(10) 24(8) -2(7) -7(7)
P(1) 23(2) 46(2) 35(2) 0 3(2) 0
P(2) 36(2) 42(2) 51(2) 0 -7(2) 0
F(1) 164(17) 50(7) 141(15) 0 -27(14) 0
F(2) 56(5) 188(10) 30(4) 11(5) 2(4) -25(6)
F(3) 23(4) 227(12) 58(5) 10(6) 4(4) 0(6)
F(4) 240(30) 43(7) 190(20) 0 -85(19) 0
F(7) 65(6) 62(5) 110(7) -26(5) -48(5) 19(4)
F(8) 68(6) 74(6) 126(8) 43(6) 2(6) -22(5)
F(9) 86(7) 74(6) 69(5) -23(4) 23(5) 2(5)
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Table 5. Hydrogen coordinates ( x 10^4) and isotropic
displacement parameters (A^2 x 10^3) for cdmipise.
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x y z U(eq)
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H(2) -3414 4348 10358 53
H(3) -3350 5145 9049 51
H(4A) -1718 3326 10301 74
H(4B) -1878 3714 11284 74
H(4C) -785 3701 10745 74
H(5A) -855 5604 8507 64
H(5B) -1946 5610 7963 64
H(5C) -1078 5157 7611 64
H(7) 3560 3634 10460 69
H(8) 2306 2829 10918 72
H(9A) 4354 3887 8429 104
H(9B) 3538 4389 8699 104
H(9C) 3402 4007 7706 104
H(10A) 367 2655 9142 96
H(10B) 920 2232 9929 96
H(10C) 1138 2154 8764 96
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