Appendix 1.

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

 


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