Selected crystallographic data for structures discussed in the text.
Table A1.1 Crystal data and structure refinement for 117.
Identification code js9822
Empirical formula C60 H78 N4
Formula weight 855.26
Temperature 210(2) K
Wavelength 0.71073 Ć
Crystal system Triclinic
Space group P-1
Unit cell dimensions a = 10.974(2) Ć a = 99.730(10)°.
b = 17.163(3) Ć b = 92.87(2)°.
c = 6.895(2) Ć g = 87.860(10)°.
Volume 1277.8(5) Ć3
Z 1
Density (calculated) 1.111 Mg/m3
Absorption coefficient 0.064 mm-1
F(000) 466
Crystal size 0.20 x 0.12 x 0.02 mm3
Theta range for data collection 1.86 to 22.49°.
Index ranges 0<=h<=11, -18<=k<=18, -7<=l<=7
Reflections collected 4861
Independent reflections 2962 [R(int) = 0.1006]
Absorption correction None
Refinement method Full-matrix least-squares on F2
Data / restraints / parameters 2962 / 18 / 273
Goodness-of-fit on F2 1.038
Final R indices [I>2sigma(I)] R1 = 0.1087, wR2 = 0.2282
R indices (all data) R1 = 0.1945, wR2 = 0.2688
Largest diff. peak and hole 0.393 and -0.483 e.Ć-3
Table A1.2 Crystal data and structure refinement for 117.
Identification code js9901
Empirical formula C60 H78 N4
Formula weight 855.26
Temperature 180(2) K
Wavelength 0.71073 Ć
Crystal system Triclinic
Space group P-1
Unit cell dimensions a = 10.387(2) Ć a = 93.850(10)°.
b = 14.622(4) Ć b = 105.85(2)°.
c = 8.821(2) Ć g = 94.56(2)°.
Volume 1279.2(5) Ć3
Z 1
Density (calculated) 1.110 Mg/m3
Absorption coefficient 0.064 mm-1
F(000) 466
Crystal size 0.35 x 0.30 x 0.15 mm3
Theta range for data collection 3.53 to 25.19°.
Index ranges 0<=h<=12, -17<=k<=17, -10<=l<=10
Reflections collected 7204
Independent reflections 4215 [R(int) = 0.0588]
Absorption correction None
Refinement method Full-matrix least-squares on F2
Data / restraints / parameters 4215 / 0 / 291
Goodness-of-fit on F2 0.982
Final R indices [I>2sigma(I)] R1 = 0.0606, wR2 = 0.1152
R indices (all data) R1 = 0.1159, wR2 = 0.1323
Extinction coefficient 0.103(6)
Largest diff. peak and hole 0.210 and -0.199 e.Ć-3
Table A1.3 Crystal data and structure refinement for 118.
Identification code js0010
Empirical formula C60 H76 I N4 Rh
Formula weight 1083.06
Temperature 150(2) K
Wavelength 0.6923 Ć
Crystal system Triclinic
Space group P-1
Unit cell dimensions a = 12.833(4) Ć a = 91.099(5)°.
b = 14.638(5) Ć b = 107.205(5)°.
c = 14.986(5) Ć g = 97.343(6)°.
Volume 2662.2(15) Ć3
Z 2
Density (calculated) 1.351 Mg/m3
Absorption coefficient 0.942 mm-1
F(000) 1124
Crystal size 0.10 x 0.08 x 0.04 mm3
Theta range for data collection 1.80 to 22.50°.
Index ranges -14<=h<=14, -16<=k<=16, -16<=l<=16
Reflections collected 16745
Independent reflections 7520 [R(int) = 0.0609]
Max. and min. transmission 0.9633 and 0.9117
Refinement method Full-matrix least-squares on F2
Data / restraints / parameters 7520 / 43 / 294
Goodness-of-fit on F2 1.111
Final R indices [I>2sigma(I)] R1 = 0.1290, wR2 = 0.3187
R indices (all data) R1 = 0.1593, wR2 = 0.3398
Largest diff. peak and hole 2.815 and -3.215 e.Ć-3
Table A1.4 Crystal data and structure refinement for 118·CH3OH.
Identification code js9909
Empirical formula C61 H80 I N4 O Rh
Formula weight 1115.10
Temperature 180(2) K
Wavelength 0.71073 Ć
Crystal system Monoclinic
Space group P2(1)/n
Unit cell dimensions a = 12.3960(10) Ć a = 90°.
b = 8.4420(10) Ć b = 93.540(10)°.
c = 25.574(2) Ć g = 90°.
Volume 2671.1(4) Ć3
Z 2
Density (calculated) 1.386 Mg/m3
Absorption coefficient 0.942 mm-1
F(000) 1160
Crystal size 0.25 x 0.15 x 0.05 mm3
Theta range for data collection 3.57 to 25.20°.
Index ranges 0<=h<=14, 0<=k<=10, -30<=l<=30
Reflections collected 8140
Independent reflections 4667 [R(int) = 0.0463]
Absorption correction None
Refinement method Full-matrix least-squares on F2
Data / restraints / parameters 4667 / 22 / 322
Goodness-of-fit on F2 1.147
Final R indices [I>2sigma(I)] R1 = 0.0660, wR2 = 0.1698
R indices (all data) R1 = 0.0788, wR2 = 0.1759
Extinction coefficient 0.039(3)
Largest diff. peak and hole 0.690 and -0.828 e.Ć-3
Table A1.5 Crystal
data and structure refinement for 118·2CH3CN.
Identification code js0008
Empirical formula C64 H82 I N6 Rh
Formula weight 1165.17
Temperature 150(2) K
Wavelength 0.6923 Ć
Crystal system Monoclinic
Space group P2(1)/n
Unit cell dimensions a = 14.6530(10) Ć a = 90°.
b = 23.1722(17) Ć b = 96.673(5)°.
c = 34.574(3) Ć g = 90°.
Volume 11659.8(14) Ć3
Z 8
Density (calculated) 1.328 Mg/m3
Absorption coefficient 0.866 mm-1
F(000) 4848
Crystal size 0.10 x 0.06 x 0.02 mm3
Theta range for data collection 3.52 to 22.50°.
Index ranges -14<=h<=15, -24<=k<=24, -37<=l<=36
Reflections collected 47395
Independent reflections 15160 [R(int) = 0.0737]
Absorption correction Multiscans
Max. and min. transmission 0.9829 and 0.9184
Refinement method Full-matrix least-squares on F2
Data / restraints / parameters 15160 / 163 / 657
Goodness-of-fit on F2 1.075
Final R indices [I>2sigma(I)] R1 = 0.1219, wR2 = 0.2761
R indices (all data) R1 = 0.1536, wR2 = 0.2892
Largest diff. peak and hole 1.771 and -3.303 e.Ć-3
Table A1.6Crystal data and structure refinement for 119.
Identification code js9941
Empirical formula C60 H79 I N5 Rh
Formula weight 1100.09
Temperature 150(2) K
Wavelength 0.6884 Ć
Crystal system Monoclinic
Space group P2(1)/c
Unit cell dimensions a = 16.3158(13) Ć a= 90°.
b = 26.431(2) Ć b= 100.830(2)°.
c = 12.7523(10) Ć g = 90°.
Volume 5401.5(8) Ć3
Z 4
Density (calculated) 1.353 Mg/m3
Absorption coefficient 0.930 mm-1
F(000) 2288
Crystal size 0.07 x 0.06 x 0.02 mm3
Theta range for data collection 1.74 to 25.00°.
Index ranges -16<=h<=20, -26<=k<=32, -12<=l<=15
Reflections collected 29666
Independent reflections 10449 [R(int) = 0.0662]
Absorption correction Multiscans
Max. and min. transmission 0.9816 and 0.9378
Refinement method Full-matrix least-squares on F2
Data / restraints / parameters 10449 / 27 / 599
Goodness-of-fit on F2 1.073
Final R indices [I>2sigma(I)] R1 = 0.0632, wR2 = 0.1177
R indices (all data) R1 = 0.0937, wR2 = 0.1251
Largest diff. peak and hole 1.389 and -1.576 e.Ć-3
Table A1.7 Crystal data and
structure refinement for 120·0.5CHCl3.
Identification code js9935
Empirical formula C60.50 H75.50 Cl1.50 I2 N4 O Rh
Formula weight 1284.63
Temperature 180(2) K
Wavelength 0.71069 Ć
Crystal system Triclinic
Space group P-1
Unit cell dimensions a = 14.2562(6) Ć a = 95.905(2)°.
b = 16.0290(6) Ć b = 115.586(2)°.
c = 16.1051(6) Ć g = 110.142(2)°.
Volume 2975.6(2) Ć3
Z 2
Density (calculated) 1.434 Mg/m3
Absorption coefficient 1.433 mm-1
F(000) 1302
Crystal size 0.09 x 0.07 x 0.07 mm3
Theta range for data collection 3.52 to 27.45°.
Index ranges -18<=h<=17, -19<=k<=20, -20<=l<=20
Reflections collected 18093
Independent reflections 13260 [R(int) = 0.0463]
Absorption correction None
Refinement method Full-matrix least-squares on F2
Data / restraints / parameters 13260 / 78 / 526
Goodness-of-fit on F2 1.022
Final R indices [I>2sigma(I)] R1 = 0.0746, wR2 = 0.1993
R indices (all data) R1 = 0.1162, wR2 = 0.2307
Largest diff. peak and hole 1.671 and -1.081 e.Ć-3
Table A1.8Crystal data and structure refinement for 121·2CH2Cl2.
Identification code js9813
Empirical formula C132 H164 Cl4 I2 N10 Rh2
Formula weight 2492.15
Temperature 180(2) K
Wavelength 0.71073 Ć
Crystal system Triclinic
Space group P-1
Unit cell dimensions a = 15.207(2) Ć a = 110.27(2)°.
b = 17.479(2) Ć b = 90.74(2)°.
c = 12.347(2) Ć g = 95.93(2)°.
Volume 3058.0(7) Ć3
Z 1
Density (calculated) 1.353 Mg/m3
Absorption coefficient 0.915 mm-1
F(000) 1290
Crystal size 0.30 x 0.25 x 0.20 mm3
Theta range for data collection 1.35 to 25.13°.
Index ranges 0<=h<=18, -20<=k<=20, -14<=l<=14
Reflections collected 18022
Independent reflections 10216 [R(int) = 0.0449]
Absorption correction None
Refinement method Full-matrix least-squares on F2
Data / restraints / parameters 10216 / 12 / 656
Goodness-of-fit on F2 1.102
Final R indices [I>2sigma(I)] R1 = 0.0476, wR2 = 0.1179
R indices (all data) R1 = 0.0643, wR2 = 0.1296
Extinction coefficient 0.0258(9)
Largest diff. peak and hole 0.973 and -0.836 e.Ć-3
Table A1.9Crystal data and structure refinement for 123.
Identification code js9906
Empirical formula C61 H79 N4 Rh
Formula weight 971.19
Temperature 180(2) K
Wavelength 0.71073 Ć
Crystal system Triclinic
Space group P-1
Unit cell dimensions a = 14.963(2) Ć a = 97.580(10)°.
b = 19.046(2) Ć b = 107.461(10)°.
c = 10.191(2) Ć g = 71.330(10)°.
Volume 2622.6(7) Ć3
Z 2
Density (calculated) 1.230 Mg/m3
Absorption coefficient 0.368 mm-1
F(000) 1036
Crystal size 0.30 x 0.18 x 0.03 mm3
Theta range for data collection 1.49 to 25.29°.
Index ranges 0<=h<=17, -21<=k<=22, -12<=l<=11
Reflections collected 12194
Independent reflections 8123 [R(int) = 0.0719]
Absorption correction None
Refinement method Full-matrix least-squares on F2
Data / restraints / parameters 8123 / 24 / 596
Goodness-of-fit on F2 1.025
Final R indices [I>2sigma(I)] R1 = 0.0668, wR2 = 0.1584
R indices (all data) R1 = 0.0925, wR2 = 0.1736
Extinction coefficient 0.0282(18)
Largest diff. peak and hole 0.730 and -0.972 e.Ć-3
Table A1.10Crystal data and structure refinement for 124.
Identification code js9824
Empirical formula C65 H81 I N5 Rh
Formula weight 1162.16
Temperature 180(2) K
Wavelength 0.71073 Ć
Crystal system Triclinic
Space group P-1
Unit cell dimensions a = 15.280(2) Ć a = 108.480(10)°.
b = 16.062(2) Ć b = 93.770(10)°.
c = 12.583(2) Ć g = 99.220(10)°.
Volume 2868.6(7) Ć3
Z 2
Density (calculated) 1.345 Mg/m3
Absorption coefficient 0.880 mm-1
F(000) 1208
Crystal size 0.25 x 0.20 x 0.15 mm3
Theta range for data collection 1.36 to 25.16°.
Index ranges 0<=h<=18, -19<=k<=18, -15<=l<=14
Reflections collected 17110
Independent reflections 9758 [R(int) = 0.0451]
Absorption correction None
Refinement method Full-matrix least-squares on F2
Data / restraints / parameters 9758 / 2 / 685
Goodness-of-fit on F2 1.045
Final R indices [I>2sigma(I)] R1 = 0.0410, wR2 = 0.0927
R indices (all data) R1 = 0.0606, wR2 = 0.0984
Largest diff. peak and hole 0.527 and -1.059 e.Ć-3
Table A1.11 Crystal data and structure refinement for 126·2CH2Cl2.
Identification code js9918
Empirical formula C130 H162 Cl4 I2 N12 Rh2
Formula weight 2494.14
Temperature 150(2) K
Wavelength 0.6884 Ć
Crystal system Triclinic
Space group P-1
Unit cell dimensions a = 12.2300(10) Ć a = 96.060(10)°.
b = 15.2190(10) Ć b = 110.390(10)°.
c = 17.2930(10) Ć g = 90.530(10)°.
Volume 2996.5(4) Ć3
Z 1
Density (calculated) 1.382 Mg/m3
Absorption coefficient 0.934 mm-1
F(000) 1290
Crystal size 0.14 x 0.08 x 0.04 mm3
Theta range for data collection 2.21 to 29.41°.
Index ranges -17<=h<=8, -18<=k<=20, -23<=l<=22
Reflections collected 11438
Independent reflections 9678 [R(int) = 0.0284]
Absorption correction Sadabs
Max. and min. transmission 0.9636 and 0.8804
Refinement method Full-matrix least-squares on F2
Data / restraints / parameters 9678 / 23 / 674
Goodness-of-fit on F2 1.565
Final R indices [I>2sigma(I)] R1 = 0.0738, wR2 = 0.2056
R indices (all data) R1 = 0.0811, wR2 = 0.2098
Largest diff. peak and hole 2.280 and -1.954 e.Ć-3
Table A1.12Crystal data and structure refinement for 132·0.5 CHCl3.
Identification code js0013
Empirical formula C134.50 H160.50 Cl1.50 I2 N10 Rh2
Formula weight 2430.02
Temperature 150(2) K
Wavelength 0.69230 Ć
Crystal system Monoclinic
Space group Cc
Unit cell dimensions a = 15.0183(2) Ć a = 90°.
b = 29.6207(5) Ć b = 102.350(5)°.
c = 29.2941(5) Ć g = 90°.
Volume 12730.0(3) Ć3
Z 4
Density (calculated) 1.268 Mg/m3
Absorption coefficient 0.826 mm-1
F(000) 5036
Crystal size 0.14 x 0.14 x 0.10 mm3
Theta range for data collection 1.78 to 29.09°.
Index ranges -20<=h<=20, -40<=k<=39, -38<=l<=39
Reflections collected 61395
Independent reflections 31771 [R(int) = 0.0442]
Absorption correction Multiscans
Max. and min. transmission 0.9219 and 0.8931
Refinement method Full-matrix least-squares on F2
Data / restraints / parameters 31771 / 90 / 1337
Goodness-of-fit on F2 1.053
Final R indices [I>2sigma(I)] R1 = 0.0440, wR2 = 0.1146
R indices (all data) R1 = 0.0600, wR2 = 0.1209
Absolute structure parameter 0.028(13)
Largest diff. peak and hole 0.964 and -1.136 e.Ć-3
Table A1.13Crystal data and structure refinement for 138.
Identification code js0006
Empirical formula C144 H182 I2 N12 Rh2
Formula weight 2540.64
Temperature 150(2) K
Wavelength 0.6923 Ć
Crystal system Triclinic
Space group P-1
Unit cell dimensions a = 14.4222(10) Ć a = 93.492(2)°.
b = 14.6677(10) Ć b = 110.978(2)°.
c = 16.5079(11) Ć g = 93.249(2)°.
Volume 3243.0(4) Ć3
Z 1
Density (calculated) 1.301 Mg/m3
Absorption coefficient 0.785 mm-1
F(000) 1326
Crystal size 0.06 x 0.06 x 0.02 mm3
Theta range for data collection 1.79 to 29.25°.
Index ranges -20<=h<=19, -20<=k<=20, -23<=l<=22
Reflections collected 29749
Independent reflections 16508 [R(int) = 0.0294]
Absorption correction Multiscans
Max. and min. transmission 0.9845 and 0.9544
Refinement method Full-matrix least-squares on F2
Data / restraints / parameters 16508 / 12 / 695
Goodness-of-fit on F2 1.017
Final R indices [I>2sigma(I)] R1 = 0.0420, wR2 = 0.0978
R indices (all data) R1 = 0.0619, wR2 = 0.1019
Largest diff. peak and hole 0.967 and -0.784 e.Ć-3
Table A1.14 Crystal data and structure refinement for 139·CH2Cl2.
Identification code js0009
Empirical formula C127 H166 Cl2 I2 N10 Rh2
Formula weight 2363.22
Temperature 150(2) K
Wavelength 0.6923 Ć
Crystal system Monoclinic
Space group P2(1)/c
Unit cell dimensions a = 14.8653(8) Ć a = 90°.
b = 34.7225(18) Ć b = 108.140(2)°.
c = 23.6103(12) Ć g = 90°.
Volume 11581.0(10) Ć3
Z 4
Density (calculated) 1.355 Mg/m3
Absorption coefficient 0.917 mm-1
F(000) 4912
Crystal size 0.16 x 0.08 x 0.02 mm3
Theta range for data collection 1.81 to 25.00°.
Index ranges -18<=h<=18, -42<=k<=42, -28<=l<=28
Reflections collected 88740
Independent reflections 22006 [R(int) = 0.0727]
Absorption correction Multiscans
Max. and min. transmission 0.9819 and 0.8671
Refinement method Full-matrix least-squares on F2
Data / restraints / parameters 22006 / 95 / 606
Goodness-of-fit on F2 1.214
Final R indices [I>2sigma(I)] R1 = 0.1373, wR2 = 0.2755
R indices (all data) R1 = 0.1561, wR2 = 0.2816
Largest diff. peak and hole 2.350 and -3.980 e.Ć-3
Table A1.15 Crystal data and structure refinement for 141.
Identification code js0017
Empirical formula C66 H81 I N5 O2 Rh
Formula weight 1206.17
Temperature 220(2) K
Wavelength 0.71070 Ć
Crystal system Triclinic
Space group P-1
Unit cell dimensions a = 12.3970(4) Ć a = 94.7580(18)°.
b = 14.8480(3) Ć b= 109.8380(13)°.
c = 17.2500(6) Ć g = 90.4860(18)°.
Volume 2974.22(15) Ć3
Z 2
Density (calculated) 1.347 Mg/m3
Absorption coefficient 0.854 mm-1
F(000) 1252
Crystal size 0.16 x 0.13 x 0.12 mm3
Theta range for data collection 2.92 to 25.04°.
Index ranges 0<=h<=14, -17<=k<=17, -20<=l<=19
Reflections collected 16463
Independent reflections 10433 [R(int) = 0.0284]
Absorption correction None
Refinement method Full-matrix least-squares on F2
Data / restraints / parameters 10433 / 34 / 680
Goodness-of-fit on F2 1.075
Final R indices [I>2sigma(I)] R1 = 0.0397, wR2 = 0.0984
R indices (all data) R1 = 0.0557, wR2 = 0.1113
Largest diff. peak and hole 0.930 and -0.752 e.Ć-3
Table A1.16Crystal data and structure refinement for 146.
Identification code js0004
Empirical formula C192 H236 I2 N14 O4 Rh2 Sn
Formula weight 3382.26
Temperature 150(2) K
Wavelength 0.6923 Ć
Crystal system Triclinic
Space group P-1
Unit cell dimensions a = 16.6542(5) Ć a= 117.1100(10)°.
b = 17.7629(6) Ć b= 94.2950(10)°.
c = 17.8328(6) Ć g= 109.7730(10)°.
Volume 4250.5(2) Ć3
Z 1
Density (calculated) 1.321 Mg/m3
Absorption coefficient 0.760 mm-1
F(000) 1764
Crystal size 0.18 x 0.06 x 0.01 mm3
Theta range for data collection 2.02 to 29.35°.
Index ranges -22<=h<=22, -24<=k<=24, -24<=l<=24
Reflections collected 42943
Independent reflections 22479 [R(int) = 0.0316]
Absorption correction Multiscans
Max. and min. transmission 0.9924 and 0.8753
Refinement method Full-matrix least-squares on F2
Data / restraints / parameters 22479 / 66 / 822
Goodness-of-fit on F2 1.083
Final R indices [I>2sigma(I)] R1 = 0.0591, wR2 = 0.1788
R indices (all data) R1 = 0.0828, wR2 = 0.1865
Largest diff. peak and hole 2.219 and -1.370 e.Ć-3
Table A1.17 Crystal data and structure refinement for 151·CH3OH.
Identification code js0011
Empirical formula C121 H154 I N9 O3 Rh
Formula weight 2012.34
Temperature 150(2) K
Wavelength 0.6923 Ć
Crystal system Triclinic
Space group P-1
Unit cell dimensions a = 11.9139(5) Ć a= 104.2840(10)°.
b = 16.7586(7) Ć b= 98.3090(10)°.
c = 28.6361(11) Ć g = 91.6610(10)°.
Volume 5470.1(4) Ć3
Z 2
Density (calculated) 1.222 Mg/m3
Absorption coefficient 0.493 mm-1
F(000) 2130
Crystal size 0.16 x 0.06 x 0.06 mm3
Theta range for data collection 2.02 to 29.37°.
Index ranges -16<=h<=16, -23<=k<=23, -40<=l<=40
Reflections collected 54140
Independent reflections 28580 [R(int) = 0.0282]
Absorption correction Multiscans
Max. and min. transmission 0.9710 and 0.9253
Refinement method Full-matrix least-squares on F2
Data / restraints / parameters 28580 / 53 / 1201
Goodness-of-fit on F2 1.029
Final R indices [I>2sigma(I)] R1 = 0.0467, wR2 = 0.1249
R indices (all data) R1 = 0.0617, wR2 = 0.1303
Largest diff. peak and hole 2.530 and -0.983 e.Ć-3
Table A1.18 Crystal data and structure refinement for 166.
Identification code js9942
Empirical formula C120 H156 I2 N10 Rh2
Formula weight 2198.17
Temperature 150(2) K
Wavelength 0.6884 Ć
Crystal system Triclinic
Space group P-1
Unit cell dimensions a = 16.2361(13) Ć a= 72.554(2)°.
b = 18.6695(15) Ć b= 87.348(2)°.
c = 20.6876(16) Ć g= 67.114(2)°.
Volume 5493.8(8) Ć3
Z 2
Density (calculated) 1.329 Mg/m3
Absorption coefficient 0.914 mm-1
F(000) 2284
Crystal size 0.09 x 0.04 x 0.02 mm3
Theta range for data collection 1.87 to 22.50°.
Index ranges -18<=h<=18, -20<=k<=20, -22<=l<=22
Reflections collected 29031
Independent reflections 15410 [R(int) = 0.0764]
Absorption correction Multiscans
Max. and min. transmission 0.9819 and 0.9222
Refinement method Full-matrix least-squares on F2
Data / restraints / parameters 15410 / 81 / 555
Goodness-of-fit on F2 1.065
Final R indices [I>2sigma(I)] R1 = 0.0895, wR2 = 0.2170
R indices (all data) R1 = 0.1358, wR2 = 0.2322
Largest diff. peak and hole 1.659 and -1.487 e.Ć-3
Table A1.19 Crystal
data and structure refinement for 167·CH2Cl2
Identification code js0015
Empirical formula C123 H162 Cl2 I2 N10 Rh2
Formula weight 2311.15
Temperature 180(2) K
Wavelength 0.71070 Ć
Crystal system Triclinic
Space group P-1
Unit cell dimensions a = 15.1170(4) Ć a= 68.4040(14)°.
b = 18.7980(8) Ć b= 81.457(2)°.
c = 21.9870(9) Ć g= 79.604(2)°.
Volume 5691.0(4) Ć3
Z 2
Density (calculated) 1.349 Mg/m3
Absorption coefficient 0.932 mm-1
F(000) 2400
Crystal size 0.16 x 0.14 x 0.03 mm3
Theta range for data collection 3.53 to 24.99°.
Index ranges 0<=h<=17, -21<=k<=22, -25<=l<=26
Reflections collected 28244
Independent reflections 18890 [R(int) = 0.0481]
Absorption correction None
Refinement method Full-matrix least-squares on F2
Data / restraints / parameters 18890 / 87 / 938
Goodness-of-fit on F2 1.032
Final R indices [I>2sigma(I)] R1 = 0.0863, wR2 = 0.1988
R indices (all data) R1 = 0.1222, wR2 = 0.2219
Largest diff. peak and hole 2.114 and -1.590 e.Ć-3
Table A1.20Crystal data and structure refinement for 169·CH2Cl2.
Identification code js0005
Empirical formula C122 H160 Cl2 I2 N10 Rh2
Formula weight 2297.12
Temperature 150(2) K
Wavelength 0.69230 Ć
Crystal system Triclinic
Space group P-1
Unit cell dimensions a = 15.1665(9) Ć a= 67.709(5)°.
b = 18.7297(11) Ć b= 81.345(5)°.
c = 21.7848(12) Ć g= 79.304(5)°.
Volume 5604.5(6) Ć3
Z 2
Density (calculated) 1.361 Mg/m3
Absorption coefficient 0.945 mm-1
F(000) 2384
Crystal size 0.12 x 0.06 x 0.06 mm3
Theta range for data collection 1.73 to 29.43°.
Index ranges -20<=h<=20, -25<=k<=25, -30<=l<=30
Reflections collected 56372
Independent reflections 29549 [R(int) = 0.0441]
Absorption correction Multiscans
Max. and min. transmission 0.9455 and 0.8950
Refinement method Full-matrix least-squares on F2
Data / restraints / parameters 29549 / 87 / 999
Goodness-of-fit on F2 0.997
Final R indices [I>2sigma(I)] R1 = 0.0702, wR2 = 0.1891
R indices (all data) R1 = 0.1087, wR2 = 0.2013
Largest diff. peak and hole 2.127 and -2.320 e.Ć-3
Table A1.21Crystal data and structure refinement for 170·CH2Cl2.
Identification code js0014
Empirical formula C123 H162 Cl2 I2 N10 Rh2
Formula weight 2311.15
Temperature 200(2) K
Wavelength 0.6923 Ć
Crystal system Triclinic
Space group P-1
Unit cell dimensions a = 15.231(2) Ć a = 65.943(5)°.
b = 18.438(3) Ć b = 83.689(5)°.
c = 22.377(3) Ć g = 81.358(5)°.
Volume 5664.8(14) Ć3
Z 2
Density (calculated) 1.355 Mg/m3
Absorption coefficient 0.936 mm-1
F(000) 2400
Crystal size 0.20 x 0.04 x 0.04 mm3
Theta range for data collection 1.81 to 25.00°.
Index ranges -18<=h<=18, -22<=k<=22, -26<=l<=27
Reflections collected 43952
Independent reflections 21262 [R(int) = 0.0548]
Absorption correction Multiscans
Max. and min. transmission 0.9635 and 0.8349
Refinement method Full-matrix least-squares on F2
Data / restraints / parameters 21262 / 86 / 581
Goodness-of-fit on F2 1.143
Final R indices [I>2sigma(I)] R1 = 0.1544, wR2 = 0.3393
R indices (all data) R1 = 0.1816, wR2 = 0.3509
Largest diff. peak and hole 3.290 and -4.738 e.Ć-3
Table A1.22Crystal data and structure refinement for 172.
Identification code js9920
Empirical formula C62 H82 I N4 O Rh S
Formula weight 1161.19
Temperature 150(2) K
Wavelength 0.50610 Ć
Crystal system Triclinic
Space group P-1
Unit cell dimensions a = 12.2300(10) Ć a = 90.850(10)°.
b = 14.8990(10) Ć b = 91.510(10)°.
c = 16.0430(10) Ć g = 104.420(10)°.
Volume 2829.5(3) Ć3
Z 2
Density (calculated) 1.363 Mg/m3
Absorption coefficient 0.497 mm-1
F(000) 1208
Crystal size 0.10 x 0.06 x 0.02 mm3
Theta range for data collection 2.60 to 19.75°.
Index ranges -15<=h<=9, -17<=k<=19, -20<=l<=21
Reflections collected 39916
Independent reflections 12407 [R(int) = 0.0738]
Absorption correction Multiscans
Max. and min. transmission 0.9901 and 0.9520
Refinement method Full-matrix least-squares on F2
Data / restraints / parameters 12407 / 153 / 721
Goodness-of-fit on F2 0.956
Final R indices [I>2sigma(I)] R1 = 0.0407, wR2 = 0.0951
R indices (all data) R1 = 0.0580, wR2 = 0.1017
Largest diff. peak and hole 1.216 and -1.062 e.Ć-3
Table A1.23Crystal data and structure refinement for 181.
Identification code js9938
Empirical formula C34 H52 N2 O4 S2
Formula weight 616.90
Temperature 180(2) K
Wavelength 0.71069 Ć
Crystal system Triclinic
Space group P1
Unit cell dimensions a = 4.8600(2) Ć a = 87.290(2)°.
b = 5.4270(2) Ć b = 89.477(2)°.
c = 33.5578(13) Ć g = 71.003(2)°.
Volume 835.93(6) Ć3
Z 1
Density (calculated) 1.225 Mg/m3
Absorption coefficient 0.198 mm-1
F(000) 334
Crystal size 0.20 x 0.18 x 0.05 mm3
Theta range for data collection 3.98 to 25.00°.
Index ranges -5<=h<=5, -6<=k<=6, -39<=l<=39
Reflections collected 10836
Independent reflections 5201 [R(int) = 0.0667]
Absorption correction Multi scans
Max. and min. transmission 1.020 and 0.922
Refinement method Full-matrix least-squares on F2
Data / restraints / parameters 5201 / 3 / 380
Goodness-of-fit on F2 1.139
Final R indices [I>2sigma(I)] R1 = 0.1208, wR2 = 0.3123
R indices (all data) R1 = 0.1279, wR2 = 0.3170
Absolute structure parameter 0.1(2)
Extinction coefficient 0.110(16)
Largest diff. peak and hole 1.011 and -0.613 e.Ć-3
Table A1.24Crystal data and structure refinement for 188·2H2O.
Identification code js9928
Empirical formula C12 H12 N2 O6
Formula weight 280.24
Temperature 130(2) K
Wavelength 0.71073 Ć
Crystal system Monoclinic
Space group P2(1)/n
Unit cell dimensions a = 8.5200(10) Ć a = 90°.
b = 15.970(2) Ć b = 110.770(10)°.
c = 9.6700(10) Ć g = 90°.
Volume 1230.2(2) Ć3
Z 4
Density (calculated) 1.513 Mg/m3
Absorption coefficient 0.123 mm-1
F(000) 584
Crystal size 0.15 x 0.15 x 0.10 mm3
Theta range for data collection 2.55 to 25.20°.
Index ranges 0<=h<=10, 0<=k<=19, -11<=l<=10
Reflections collected 3856
Independent reflections 2126 [R(int) = 0.0427]
Absorption correction None
Refinement method Full-matrix least-squares on F2
Data / restraints / parameters 2126 / 6 / 203
Goodness-of-fit on F2 0.899
Final R indices [I>2sigma(I)] R1 = 0.0535, wR2 = 0.0904
R indices (all data) R1 = 0.1014, wR2 = 0.1052
Extinction coefficient 0.039(2)
Largest diff. peak and hole 0.225 and -0.306 e.Ć-3
Table A1.25Crystal data and structure refinement for 196.
Identification code js9802
Empirical formula C60 H78 N4 O2
Formula weight 887.26
Temperature 180(2) K
Wavelength 0.71069 Ć
Crystal system Triclinic
Space group P-1
Unit cell dimensions a = 10.053 Ć a = 92.80°.
b = 14.640 Ć b = 104.13°.
c = 9.551 Ć g = 72.38°.
Volume 1298.7 Ć3
Z 1
Density (calculated) 1.134 Mg/m3
Absorption coefficient 0.068 mm-1
F(000) 482
Crystal size 0.20 x 0.20 x 0.08 mm3
Theta range for data collection 1.46 to 23.68°.
Index ranges -11<=h<=11, -16<=k<=16, -10<=l<=10
Reflections collected 4948
Independent reflections 2980 [R(int) = 0.0653]
Refinement method Full-matrix least-squares on F2
Data / restraints / parameters 2967 / 0 / 303
Goodness-of-fit on F2 1.260
Final R indices [I>2sigma(I)] R1 = 0.1229, wR2 = 0.2123
R indices (all data) R1 = 0.1545, wR2 = 0.2380
Extinction coefficient 0.0504(43)
Largest diff. peak and hole 0.454 and -0.235 e.Ć-3
Table A1.26Crystal data and structure refinement for 197.
Identification code js9815
Empirical formula C60 H78 N4 O
Formula weight 871.26
Temperature 150(2) K
Wavelength 0.69190 Ć
Crystal system Triclinic
Space group P-1
Unit cell dimensions a = 10.1430(10) Ć a= 92.400(10)°.
b = 14.5410(10) Ć b= 104.210(10)°.
c = 9.357(2) Ć g= 71.630(10)°.
Volume 1268.7(3) Ć3
Z 1
Density (calculated) 1.140 Mg/m3
Absorption coefficient 0.067 mm-1
F(000) 474
Crystal size 0.14 x 0.08 x 0.03 mm3
Theta range for data collection 2.12 to 29.48°.
Index ranges -11<=h<=14, -20<=k<=19, -12<=l<=13
Reflections collected 8848
Independent reflections 6460 [R(int) = 0.0295]
Absorption correction Sadabs
Max. and min. transmission 0.9980 and 0.9907
Refinement method Full-matrix least-squares on F2
Data / restraints / parameters 6460 / 0 / 299
Goodness-of-fit on F2 0.941
Final R indices [I>2sigma(I)] R1 = 0.0591, wR2 = 0.1475
R indices (all data) R1 = 0.0810, wR2 = 0.1582
Largest diff. peak and hole 0.375 and -0.265 e.Ć-3
Table A1.27Crystal data and structure refinement for 217.
Identification code js9944
Empirical formula C86 H126 N4 O4 S2
Formula weight 1344.03
Temperature 150(2) K
Wavelength 0.6893 Ć
Crystal system Triclinic
Space group P-1
Unit cell dimensions a = 8.8191(6) Ć a= 86.111(2)°.
b = 10.2453(7) Ć b= 88.338(2)°.
c = 43.781(3) Ć g= 89.332(2)°.
Volume 3944.9(5) Ć3
Z 2
Density (calculated) 1.132 Mg/m3
Absorption coefficient 0.119 mm-1
F(000) 1468
Crystal size 0.12 x 0.10 x 0.03 mm3
Theta range for data collection 3.44 to 25.00°.
Index ranges -10<=h<=10, -12<=k<=12, -53<=l<=53
Reflections collected 26596
Independent reflections 14557 [R(int) = 0.0473]
Absorption correction Multiscans
Max. and min. transmission 0.9964 and 0.9859
Refinement method Full-matrix least-squares on F2
Data / restraints / parameters 14557 / 155 / 494
Goodness-of-fit on F2 1.824
Final R indices [I>2sigma(I)] R1 = 0.1728, wR2 = 0.4632
R indices (all data) R1 = 0.2103, wR2 = 0.4797
Extinction coefficient 0.080(12)
Largest diff. peak and hole 1.265 and -1.086 e.Ć-3