Supplementary Material (ESI) for Dalton Transactions
This journal is © The Royal Society of Chemistry 2003

data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222
_journal_volume                  ?
_journal_year                    ?
_journal_page_first              ?

loop_
_publ_author_name
'Dmitri Konarev'
'Rimma N. Lyubovskaya'
'I. S. Neretin'
'Akihiro Otsuka'
'Gunzi Saito'
;
Y.L.Slovokhotov
;

_publ_contact_author_name        'Dmitri Konarev'
_publ_contact_author_address     
;
Dr Dmitri Konarev
Institute of problems of Chemical Physics RAS
Institutski, 18
Chernogolovka
Moscow region
142432
RUSSIAN FEDERATION
;

_publ_contact_author_email       KONAREV@ICP.AC.RU

_publ_section_title              
;
Ionic multi-component complexes containing TDAE+
and C60- radical ions and neutral D1 molecules: D1.TDAE.C60.
;

data_tbpd
_database_code_CSD               211611

_audit_creation_method           SHELXL
_chemical_name_systematic        
;
?
;
_chemical_name_common            C60*2TBPD*TDAE
_chemical_formula_moiety         'C60, 2(C34 H32 N2), C10 H24 N4'
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_sum            'C138 H88 N8'
_chemical_formula_weight         1858.16
_chemical_melting_point          ?
_chemical_compound_source        ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Tetragonal
_symmetry_space_group_name_H-M   I4/m

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'

_cell_length_a                   13.627(2)
_cell_length_b                   13.627(2)
_cell_length_c                   24.662(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4579.3(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    110(1)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       plate
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.1
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1944
_exptl_absorpt_coefficient_mu    0.079
_exptl_absorpt_correction_type   SADABS
_exptl_absorpt_correction_T_min  0.620190
_exptl_absorpt_correction_T_max  0.928022

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      110(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'Bruker SMART'
_diffrn_measurement_method       '\w scan'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13250
_diffrn_reflns_av_R_equivalents  0.0445
_diffrn_reflns_av_sigmaI/netI    0.0404
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.71
_diffrn_reflns_theta_max         25.06
_reflns_number_total             2094
_reflns_number_observed          1150
_reflns_observed_criterion       >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^
or flagged by the user for potential systematic errors.  Weighted R-factors
wR and all goodnesses of fit S are based on F^2^, conventional R-factors R
are based on F, with F set to zero for negative F^2^. The observed criterion
of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
C60 fullerene and TDAE molecules are disordered.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      
'calc w=1/[\s^2^(Fo^2^)+(0.2256P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    ?
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2094
_refine_ls_number_parameters     213
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.1476
_refine_ls_R_factor_obs          0.1002
_refine_ls_wR_factor_all         0.3300
_refine_ls_wR_factor_obs         0.2839
_refine_ls_goodness_of_fit_all   1.040
_refine_ls_goodness_of_fit_obs   1.248
_refine_ls_restrained_S_all      1.037
_refine_ls_restrained_S_obs      1.238
_refine_ls_shift/esd_max         0.010
_refine_ls_shift/esd_mean        0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
N1 N 0.0000 0.5000 0.1139(2) 0.0531(12) Uani 1 d S .
C1 C 0.0000 0.5000 0.0572(2) 0.0493(14) Uani 1 d S .
C2 C -0.0097(3) 0.4132(3) 0.02811(15) 0.0480(10) Uani 1 d . .
C3 C 0.0511(3) 0.5736(3) 0.1456(2) 0.0560(11) Uani 1 d . .
C4 C -0.0119(3) 0.6474(3) 0.17401(14) 0.0497(11) Uani 1 d . .
C5 C -0.1033(3) 0.6741(3) 0.1535(2) 0.0569(11) Uani 1 d . .
C6 C -0.1600(3) 0.7431(3) 0.1805(2) 0.0629(12) Uani 1 d . .
C7 C -0.1258(3) 0.7867(3) 0.2271(2) 0.0592(12) Uani 1 d . .
C8 C -0.0359(3) 0.7592(3) 0.2478(2) 0.0569(12) Uani 1 d . .
C9 C 0.0201(3) 0.6907(3) 0.22152(15) 0.0496(10) Uani 1 d . .
C61 C 0.5000 0.5000 0.4748(4) 0.082(3) Uiso 1 d S .
N11 N 0.4937(15) 0.4201(12) 0.4447(7) 0.180(6) Uiso 0.50 d P .
C62 C 0.3780(14) 0.3717(16) 0.4646(7) 0.181(7) Uiso 0.50 d P .
H62A H 0.3706(14) 0.3909(16) 0.5000(7) 0.271 Uiso 1 d SR .
H62B H 0.3275(14) 0.4020(16) 0.4432(7) 0.271 Uiso 0.50 d PR .
H62C H 0.3727(14) 0.3017(16) 0.4618(7) 0.271 Uiso 0.50 d PR .
C63 C 0.5110(21) 0.4023(18) 0.3893(9) 0.216(10) Uiso 0.50 d P .
H63A H 0.5757(21) 0.4292(18) 0.3857(9) 0.325 Uiso 0.50 d PR .
H63B H 0.5129(21) 0.3330(18) 0.3823(9) 0.325 Uiso 0.50 d PR .
H63C H 0.4678(21) 0.4333(18) 0.3638(9) 0.325 Uiso 0.50 d PR .
H4 H 0.0962(26) 0.5439(24) 0.1736(16) 0.046(9) Uiso 1 d . .
H2 H -0.0161(25) 0.3590(26) 0.0457(15) 0.041(10) Uiso 1 d . .
H8 H -0.0104(32) 0.7880(31) 0.2783(18) 0.068(13) Uiso 1 d . .
H3 H 0.0999(28) 0.6093(28) 0.1172(16) 0.059(11) Uiso 1 d . .
H7 H -0.1662(35) 0.8332(33) 0.2464(19) 0.079(14) Uiso 1 d . .
H9 H 0.0769(29) 0.6682(25) 0.2374(15) 0.046(10) Uiso 1 d . .
H5 H -0.1327(27) 0.6368(26) 0.1198(16) 0.053(10) Uiso 1 d . .
H6 H -0.2263(35) 0.7742(34) 0.1648(19) 0.085(14) Uiso 1 d . .
C31 C 0.0517(6) -0.0079(28) 0.3598(3) 0.067(3) Uani 0.50 d P .
C32 C 0.0757(6) -0.1072(5) 0.3772(2) 0.084(2) Uani 1 d . .
C33 C 0.0128(12) -0.1812(7) 0.3999(3) 0.157(4) Uani 1 d . .
C34 C 0.1619(7) -0.0971(7) 0.4034(3) 0.121(3) Uani 1 d . .
C35 C 0.1796(7) -0.1618(9) 0.4506(3) 0.118(3) Uani 1 d . .
C36 C 0.1095(13) -0.2235(7) 0.4657(5) 0.157(4) Uani 1 d . .
C37 C 0.0162(12) -0.2366(7) 0.4461(8) 0.190(6) Uani 1 d U .
C38 C -0.0744(14) -0.2389(13) 0.4706(12) 0.138(9) Uani 0.50 d PU .
C39 C 0.2515(13) -0.0099(49) 0.5000 0.143(14) Uani 0.50 d SPU .
C40 C 0.2252(14) -0.1232(21) 0.5000 0.106(7) Uani 0.50 d SPU .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
N1 0.056(3) 0.072(3) 0.032(2) 0.000 0.000 0.005(2)
C1 0.039(3) 0.076(4) 0.033(3) 0.000 0.000 0.010(2)
C2 0.043(2) 0.064(2) 0.038(2) 0.005(2) 0.002(2) 0.008(2)
C3 0.049(2) 0.083(3) 0.036(2) -0.004(2) -0.005(2) 0.010(2)
C4 0.044(2) 0.068(3) 0.037(2) 0.002(2) 0.004(2) 0.002(2)
C5 0.051(2) 0.076(3) 0.044(2) -0.002(2) -0.007(2) 0.005(2)
C6 0.054(2) 0.073(3) 0.061(3) 0.002(2) 0.000(2) 0.007(2)
C7 0.055(3) 0.060(3) 0.063(3) -0.009(2) 0.012(2) 0.000(2)
C8 0.057(3) 0.065(3) 0.048(2) -0.010(2) 0.002(2) -0.011(2)
C9 0.044(2) 0.064(2) 0.041(2) 0.003(2) -0.002(2) -0.001(2)
C31 0.079(6) 0.091(9) 0.032(3) -0.012(7) 0.010(3) -0.006(17)
C32 0.110(5) 0.098(5) 0.043(3) -0.021(3) 0.011(3) 0.033(4)
C33 0.293(16) 0.087(6) 0.091(5) -0.068(5) 0.020(8) 0.005(8)
C34 0.122(7) 0.137(7) 0.105(6) -0.006(5) 0.062(6) 0.039(5)
C35 0.107(5) 0.152(8) 0.096(5) -0.042(5) -0.008(4) 0.097(6)
C36 0.210(10) 0.062(4) 0.198(10) -0.011(5) 0.082(10) 0.057(6)
C37 0.236(15) 0.070(6) 0.263(19) -0.094(9) 0.081(15) -0.022(8)
C38 0.121(12) 0.087(11) 0.205(21) -0.099(13) 0.105(14) -0.076(11)
C39 0.013(7) 0.305(52) 0.113(21) 0.000 0.000 0.014(16)
C40 0.053(10) 0.160(20) 0.106(15) 0.000 0.000 0.072(12)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix.  The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry.  An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C1 1.399(6) . ?
N1 C3 1.450(5) . ?
N1 C3 1.450(5) 2_565 ?
C1 C2 1.390(5) . ?
C1 C2 1.390(5) 2_565 ?
C2 C2 1.386(7) 10 ?
C3 C4 1.496(5) . ?
C4 C9 1.382(5) . ?
C4 C5 1.394(5) . ?
C5 C6 1.386(6) . ?
C6 C7 1.375(6) . ?
C7 C8 1.378(6) . ?
C8 C9 1.370(6) . ?
C61 C61 1.24(2) 9_666 ?
C61 N11 1.32(2) 4_565 ?
C61 N11 1.32(2) 2_665 ?
C61 N11 1.32(2) . ?
C61 N11 1.32(2) 3_655 ?
N11 C63 1.41(2) . ?
N11 N11 1.54(2) 3_655 ?
N11 N11 1.54(2) 4_565 ?
N11 C62 1.78(2) . ?
C31 C31 1.42(2) 2 ?
C31 C32 1.43(3) 3 ?
C31 C32 1.46(4) . ?
C32 C34 1.348(10) . ?
C32 C31 1.43(3) 4 ?
C32 C33 1.436(13) . ?
C33 C37 1.37(2) . ?
C33 C34 1.523(14) 4 ?
C34 C35 1.480(13) . ?
C34 C33 1.523(14) 3 ?
C35 C36 1.326(13) . ?
C35 C40 1.46(2) . ?
C35 C38 1.52(3) 3 ?
C36 C37 1.37(2) . ?
C36 C36 1.69(2) 10_556 ?
C37 C38 1.38(2) . ?
C37 C39 1.39(2) 11_556 ?
C38 C38 1.45(6) 10_556 ?
C38 C35 1.52(3) 4 ?
C39 C37 1.39(2) 3 ?
C39 C37 1.39(2) 12_556 ?
C39 C40 1.59(6) . ?
C40 C35 1.46(2) 10_556 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 N1 C3 122.6(2) . . ?
C1 N1 C3 122.6(2) . 2_565 ?
C3 N1 C3 114.8(4) . 2_565 ?
C2 C1 C2 117.8(5) . 2_565 ?
C2 C1 N1 121.1(2) . . ?
C2 C1 N1 121.1(2) 2_565 . ?
C2 C2 C1 121.1(2) 10 . ?
N1 C3 C4 116.2(3) . . ?
C9 C4 C5 118.6(3) . . ?
C9 C4 C3 120.2(3) . . ?
C5 C4 C3 121.3(3) . . ?
C6 C5 C4 120.0(4) . . ?
C7 C6 C5 120.4(4) . . ?
C6 C7 C8 119.5(4) . . ?
C9 C8 C7 120.3(4) . . ?
C8 C9 C4 121.1(4) . . ?
C61 C61 N11 124.3(8) 9_666 4_565 ?
N11 C61 N11 111.5(16) 2_665 . ?
C61 N11 C63 132.7(17) . . ?
C61 N11 C62 102.0(13) . . ?
C63 N11 C62 110.7(18) . . ?
C31 C31 C32 113.8(36) 2 3 ?
C31 C31 C32 111.2(35) 2 . ?
C32 C31 C32 122.1(6) 3 . ?
C34 C32 C33 113.9(6) . . ?
C34 C32 C31 104.0(10) . . ?
C33 C32 C31 129.3(8) . . ?
C32 C33 C34 119.2(9) . 4 ?
C32 C34 C35 117.3(9) . . ?
C32 C34 C33 103.0(9) . 3 ?
C35 C34 C33 127.0(10) . 3 ?
C32 C34 C38 151.3(6) . 3 ?
C36 C35 C40 107.4(14) . . ?
C36 C35 C34 118.8(8) . . ?
C40 C35 C34 120.6(14) . . ?
C35 C36 C37 130.6(14) . . ?
C35 C36 C36 106.3(7) . 10_556 ?
C37 C36 C36 110.7(10) . 10_556 ?
C33 C37 C36 104.7(14) . . ?
C33 C37 C38 110.5(21) . . ?
C37 C38 C38 116.1(17) . 10_556 ?
C37 C38 C35 123.2(25) . 4 ?
C38 C38 C35 108.9(11) 10_556 4 ?
C40 C38 C34 113.7(25) 11_556 4 ?
C38 C39 C36 110.4(20) 3 3 ?
C38 C39 C36 110.4(20) 12_556 12_556 ?
C35 C40 C35 112.5(22) . 10_556 ?
C35 C40 C39 116.4(11) . . ?
C35 C40 C39 116.4(11) 10_556 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C3 -23.9(3) . . . . ?
C1 C2 C3 C4 53.7(4) . . . . ?
C2 C3 C4 C5 -8.5(6) . . . . ?
C3 C4 C5 C6 -179.7(4) . . . . ?
C4 C5 C6 C7 1.1(7) . . . . ?
C5 C6 C7 C8 -2.0(7) . . . . ?
C6 C7 C8 C9 1.5(6) . . . . ?

_refine_diff_density_max         0.494
_refine_diff_density_min         -0.994
_refine_diff_density_rms         0.082