# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry A.
# This journal is © The Royal Society of Chemistry 2015

 
data_x 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C240 H288 N36 O90 Tb6' 
_chemical_formula_weight          6070.58 
 
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' 
 'O'  'O'   0.0106   0.0060 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Tb'  'Tb'  -0.1723   4.1537 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            CUBIC 
_symmetry_space_group_name_H-M    Im-3 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, -y, z' 
 '-x, y, -z' 
 'x, -y, -z' 
 'z, x, y' 
 'z, -x, -y' 
 '-z, -x, y' 
 '-z, x, -y' 
 'y, z, x' 
 '-y, z, -x' 
 'y, -z, -x' 
 '-y, -z, x' 
 'x+1/2, y+1/2, z+1/2' 
 '-x+1/2, -y+1/2, z+1/2' 
 '-x+1/2, y+1/2, -z+1/2' 
 'x+1/2, -y+1/2, -z+1/2' 
 'z+1/2, x+1/2, y+1/2' 
 'z+1/2, -x+1/2, -y+1/2' 
 '-z+1/2, -x+1/2, y+1/2' 
 '-z+1/2, x+1/2, -y+1/2' 
 'y+1/2, z+1/2, x+1/2' 
 '-y+1/2, z+1/2, -x+1/2' 
 'y+1/2, -z+1/2, -x+1/2' 
 '-y+1/2, -z+1/2, x+1/2' 
 '-x, -y, -z' 
 'x, y, -z' 
 'x, -y, z' 
 '-x, y, z' 
 '-z, -x, -y' 
 '-z, x, y' 
 'z, x, -y' 
 'z, -x, y' 
 '-y, -z, -x' 
 'y, -z, x' 
 '-y, z, x' 
 'y, z, -x' 
 '-x+1/2, -y+1/2, -z+1/2' 
 'x+1/2, y+1/2, -z+1/2' 
 'x+1/2, -y+1/2, z+1/2' 
 '-x+1/2, y+1/2, z+1/2' 
 '-z+1/2, -x+1/2, -y+1/2' 
 '-z+1/2, x+1/2, y+1/2' 
 'z+1/2, x+1/2, -y+1/2' 
 'z+1/2, -x+1/2, y+1/2' 
 '-y+1/2, -z+1/2, -x+1/2' 
 'y+1/2, -z+1/2, x+1/2' 
 '-y+1/2, z+1/2, x+1/2' 
 'y+1/2, z+1/2, -x+1/2' 
 
_cell_length_a                    26.7264(13) 
_cell_length_b                    26.7264(13) 
_cell_length_c                    26.7264(13) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      19090.7(16) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     24310 
_cell_measurement_theta_min       2.1536 
_cell_measurement_theta_max       27.4816 
 
_exptl_crystal_description        'Prism' 
_exptl_crystal_colour             'Colorless' 
_exptl_crystal_size_max           0.2000 
_exptl_crystal_size_mid           0.2000 
_exptl_crystal_size_min           0.2000 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.056 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              6180 
_exptl_absorpt_coefficient_mu     1.163 
_exptl_absorpt_correction_type    'Multi-scan' 
_exptl_absorpt_correction_T_min   0.6254 
_exptl_absorpt_correction_T_max   1.0000 
_exptl_absorpt_process_details    ? 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       293(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   Saturn724+ 
_diffrn_measurement_method        'CCD_Profile_fitting'
_diffrn_detector_area_resol_mean  28.5714 
_diffrn_standards_number          3873 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             80259 
_diffrn_reflns_av_R_equivalents   0.0697 
_diffrn_reflns_av_sigmaI/netI     0.0361 
_diffrn_reflns_limit_h_min        -34 
_diffrn_reflns_limit_h_max        30 
_diffrn_reflns_limit_k_min        -34 
_diffrn_reflns_limit_k_max        33 
_diffrn_reflns_limit_l_min        -34 
_diffrn_reflns_limit_l_max        34 
_diffrn_reflns_theta_min          2.64 
_diffrn_reflns_theta_max          27.48 
_reflns_number_total              3867 
_reflns_number_gt                 3259 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 
 
_refine_special_details 
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
; 
 
_refine_ls_structure_factor_coef  Fsqd  
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc  
_refine_ls_weighting_details 
 'calc w=1/[σ²(Fo²)+(0.0400P)²+98.0000P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     mixed 
_refine_ls_extinction_method      SHELXL 
_refine_ls_extinction_coef        0.00136(10) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^' 
_refine_ls_number_reflns          3867 
_refine_ls_number_parameters      184 
_refine_ls_number_restraints      45 
_refine_ls_R_factor_all           0.0715 
_refine_ls_R_factor_gt            0.0628 
_refine_ls_wR_factor_ref          0.1521 
_refine_ls_wR_factor_gt           0.1466 
_refine_ls_goodness_of_fit_ref    1.196 
_refine_ls_restrained_S_all       1.203 
_refine_ls_shift/su_max           0.002 
_refine_ls_shift/su_mean          0.000 
 
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_adp_type 
 _atom_site_occupancy 
 _atom_site_symmetry_multiplicity 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
Tb1 Tb 0.0000 0.5000 0.372971(15) 0.0411(2) Uani 1 4 d S . . 
O1 O 0.0573(5) 0.4281(5) 0.3938(3) 0.065(3) Uani 0.502(9) 1 d PDU A 1 
O2 O 0.0369(3) 0.4318(3) 0.3202(3) 0.067(2) Uani 0.502(9) 1 d PDU A 1 
O1B O 0.0679(6) 0.4453(4) 0.3940(2) 0.068(3) Uani 0.498(9) 1 d PDU A 2 
O2B O 0.0668(3) 0.4674(3) 0.3205(3) 0.063(2) Uani 0.498(9) 1 d PDU . 2 
N1 N 0.2734(2) 0.3279(2) 0.2588(2) 0.0896(19) Uani 1 1 d . . . 
C1 C 0.0741(2) 0.4303(2) 0.3505(2) 0.0749(17) Uani 1 1 d D . . 
C2 C 0.1190(2) 0.3984(2) 0.3383(2) 0.0748(17) Uani 1 1 d . A . 
C3 C 0.1378(3) 0.3994(3) 0.2905(3) 0.121(3) Uani 1 1 d . . . 
H3A H 0.1218 0.4182 0.2660 0.145 Uiso 1 1 calc R A . 
C4 C 0.1802(3) 0.3725(3) 0.2785(3) 0.118(3) Uani 1 1 d . A . 
H4A H 0.1932 0.3745 0.2463 0.141 Uiso 1 1 calc R . . 
C5 C 0.2032(2) 0.3431(3) 0.3128(2) 0.085(2) Uani 1 1 d . . . 
C6 C 0.1839(3) 0.3404(3) 0.3611(2) 0.090(2) Uani 1 1 d . A . 
H6A H 0.1987 0.3199 0.3850 0.108 Uiso 1 1 calc R . . 
C7 C 0.1420(2) 0.3689(3) 0.3728(2) 0.081(2) Uani 1 1 d . . . 
H7A H 0.1292 0.3677 0.4052 0.097 Uiso 1 1 calc R A . 
C8 C 0.2471(2) 0.3131(3) 0.2989(2) 0.086(2) Uani 1 1 d . A . 
O3 O 0.0000 0.5000 0.4577(2) 0.073(2) Uani 1 4 d SD . . 
C9 C 0.0175(7) 0.5000 0.5000 0.066(6) Uani 0.50 4 d SPD . . 
N2 N 0.0000 0.3275(5) 0.5000 0.098(4) Uani 1 4 d S . . 
C10 C 0.0392(14) 0.3677(9) 0.5000 0.160(13) Uani 0.50 2 d SP . . 
C11 C 0.0000 0.2997(11) 0.4538(11) 0.148(12) Uani 0.50 2 d SP . . 
O1W O 0.3726(2) 0.3726(2) 0.3726(2) 0.046(2) Uiso 0.50 3 d SP . . 
O7W O 0.2549(16) 0.5000 0.3669(15) 0.145(13) Uiso 0.25 2 d SP . . 
N3 N 0.1612(11) 0.5000 0.5000 0.147(14) Uani 0.50 4 d SP . . 
C12 C 0.1285(14) 0.4507(16) 0.5000 0.087(12) Uani 0.25 2 d SP . . 
C13 C 0.186(2) 0.5000 0.449(2) 0.14(2) Uani 0.25 2 d SP . . 
O4 O 0.1625(10) 0.3197(11) 0.5000 0.185(9) Uiso 0.50 2 d SPD . . 
N5 N 0.1916(10) 0.2394(10) 0.5000 0.136(8) Uiso 0.50 2 d SPD . . 
C14 C 0.1541(12) 0.2731(10) 0.5000 0.191(16) Uiso 0.50 2 d SPD . . 
C15 C 0.1912(15) 0.1862(10) 0.5000 0.188(15) Uiso 0.50 2 d SPD . . 
C16 C 0.2393(13) 0.2629(16) 0.5000 0.222(19) Uiso 0.50 2 d SPD . . 
 
 
_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 
Tb1 O3 2.264(7) . ? 
Tb1 O1B 2.397(13) 2_565 ? 
Tb1 O1B 2.397(13) 27_565 ? 
Tb1 O1B 2.397(13) 28 ? 
Tb1 O1B 2.397(13) . ? 
Tb1 O2B 2.431(6) 2_565 ? 
Tb1 O2B 2.431(6) 27_565 ? 
Tb1 O2B 2.431(6) 28 ? 
Tb1 O2B 2.431(6) . ? 
Tb1 O2 2.505(7) 2_565 ? 
Tb1 O2 2.505(7) 27_565 ? 
Tb1 O2 2.505(7) 28 ? 
O1 C1 1.243(8) . ? 
O2 C1 1.282(7) . ? 
O1B C1 1.240(9) . ? 
O2B C1 1.290(7) . ? 
O2B O2B 1.740(15) 27_565 ? 
N1 C8 1.343(7) . ? 
N1 C8 1.350(7) 9 ? 
C1 C2 1.510(7) . ? 
C2 C7 1.361(8) . ? 
C2 C3 1.373(8) . ? 
C3 C4 1.380(8) . ? 
C3 H3A 0.9300 . ? 
C4 C5 1.355(8) . ? 
C4 H4A 0.9300 . ? 
C5 C6 1.392(8) . ? 
C5 C8 1.469(7) . ? 
C6 C7 1.391(8) . ? 
C6 H6A 0.9300 . ? 
C7 H7A 0.9300 . ? 
C8 N1 1.350(7) 5 ? 
O3 C9 1.223(7) 25_566 ? 
O3 C9 1.223(7) . ? 
C9 C9 0.93(4) 25_566 ? 
C9 O3 1.223(7) 25_566 ? 
N2 C11 1.44(2) . ? 
N2 C11 1.44(2) 26_556 ? 
N2 C10 1.50(2) 3_556 ? 
N2 C10 1.50(2) . ? 
N3 C13 1.52(5) 26_556 ? 
N3 C13 1.52(5) . ? 
N3 C12 1.58(4) 27_565 ? 
N3 C12 1.58(4) . ? 
O4 C14 1.266(10) . ? 
N5 C14 1.350(10) . ? 
N5 C16 1.419(10) . ? 
N5 C15 1.422(10) . ? 
 
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 
O3 Tb1 O1B 76.43(16) . 2_565 ? 
O3 Tb1 O1B 76.43(16) . 27_565 ? 
O1B Tb1 O1B 98.4(7) 2_565 27_565 ? 
O3 Tb1 O1B 76.43(16) . 28 ? 
O1B Tb1 O1B 75.1(7) 2_565 28 ? 
O1B Tb1 O1B 152.9(3) 27_565 28 ? 
O3 Tb1 O1B 76.43(16) . . ? 
O1B Tb1 O1B 152.9(3) 2_565 . ? 
O1B Tb1 O1B 75.1(7) 27_565 . ? 
O1B Tb1 O1B 98.4(7) 28 . ? 
O3 Tb1 O2B 125.21(16) . 2_565 ? 
O1B Tb1 O2B 50.3(2) 2_565 2_565 ? 
O1B Tb1 O2B 118.2(4) 27_565 2_565 ? 
O1B Tb1 O2B 78.3(4) 28 2_565 ? 
O1B Tb1 O2B 155.4(3) . 2_565 ? 
O3 Tb1 O2B 125.21(16) . 27_565 ? 
O1B Tb1 O2B 118.2(4) 2_565 27_565 ? 
O1B Tb1 O2B 50.3(2) 27_565 27_565 ? 
O1B Tb1 O2B 155.4(3) 28 27_565 ? 
O1B Tb1 O2B 78.3(4) . 27_565 ? 
O2B Tb1 O2B 94.5(4) 2_565 27_565 ? 
O3 Tb1 O2B 125.21(16) . 28 ? 
O1B Tb1 O2B 78.3(4) 2_565 28 ? 
O1B Tb1 O2B 155.4(3) 27_565 28 ? 
O1B Tb1 O2B 50.3(2) 28 28 ? 
O1B Tb1 O2B 118.2(4) . 28 ? 
O2B Tb1 O2B 41.9(4) 2_565 28 ? 
O2B Tb1 O2B 109.6(3) 27_565 28 ? 
O3 Tb1 O2B 125.21(16) . . ? 
O1B Tb1 O2B 155.4(3) 2_565 . ? 
O1B Tb1 O2B 78.3(4) 27_565 . ? 
O1B Tb1 O2B 118.2(4) 28 . ? 
O1B Tb1 O2B 50.3(2) . . ? 
O2B Tb1 O2B 109.6(3) 2_565 . ? 
O2B Tb1 O2B 41.9(4) 27_565 . ? 
O2B Tb1 O2B 94.5(4) 28 . ? 
O3 Tb1 O2 124.24(17) . 2_565 ? 
O1B Tb1 O2 52.5(3) 2_565 2_565 ? 
O1B Tb1 O2 89.2(4) 27_565 2_565 ? 
O1B Tb1 O2 106.1(4) 28 2_565 ? 
O1B Tb1 O2 150.8(3) . 2_565 ? 
O2B Tb1 O2 29.1(2) 2_565 2_565 ? 
O2B Tb1 O2 72.8(3) 27_565 2_565 ? 
O2B Tb1 O2 69.3(3) 28 2_565 ? 
O2B Tb1 O2 103.0(2) . 2_565 ? 
O3 Tb1 O2 124.24(18) . 27_565 ? 
O1B Tb1 O2 89.2(4) 2_565 27_565 ? 
O1B Tb1 O2 52.5(3) 27_565 27_565 ? 
O1B Tb1 O2 150.8(3) 28 27_565 ? 
O1B Tb1 O2 106.1(4) . 27_565 ? 
O2B Tb1 O2 72.8(3) 2_565 27_565 ? 
O2B Tb1 O2 29.1(2) 27_565 27_565 ? 
O2B Tb1 O2 103.0(2) 28 27_565 ? 
O2B Tb1 O2 69.3(3) . 27_565 ? 
O2 Tb1 O2 46.3(3) 2_565 27_565 ? 
O3 Tb1 O2 124.24(18) . 28 ? 
O1B Tb1 O2 106.1(4) 2_565 28 ? 
O1B Tb1 O2 150.8(3) 27_565 28 ? 
O1B Tb1 O2 52.5(3) 28 28 ? 
O1B Tb1 O2 89.2(4) . 28 ? 
O2B Tb1 O2 69.3(3) 2_565 28 ? 
O2B Tb1 O2 103.0(2) 27_565 28 ? 
O2B Tb1 O2 29.1(2) 28 28 ? 
O2B Tb1 O2 72.8(3) . 28 ? 
O2 Tb1 O2 93.3(4) 2_565 28 ? 
O2 Tb1 O2 111.5(3) 27_565 28 ? 
C1 O1 Tb1 88.7(7) . . ? 
C1 O2 Tb1 88.4(4) . . ? 
C1 O1B Tb1 94.4(7) . . ? 
C1 O2B O2B 140.2(5) . 27_565 ? 
C1 O2B Tb1 91.5(4) . . ? 
O2B O2B Tb1 69.03(18) 27_565 . ? 
C8 N1 C8 115.2(6) . 9 ? 
O1B C1 O1 25.2(8) . . ? 
O1B C1 O2 118.6(9) . . ? 
O1 C1 O2 108.1(7) . . ? 
O1B C1 O2B 108.4(7) . . ? 
O1 C1 O2B 124.2(9) . . ? 
O2 C1 O2B 57.8(5) . . ? 
O1B C1 C2 119.4(8) . . ? 
O1 C1 C2 117.5(8) . . ? 
O2 C1 C2 119.8(6) . . ? 
O2B C1 C2 114.8(6) . . ? 
O1B C1 Tb1 59.2(6) . . ? 
O1 C1 Tb1 64.8(7) . . ? 
O2 C1 Tb1 64.2(4) . . ? 
O2B C1 Tb1 60.9(4) . . ? 
C2 C1 Tb1 172.3(5) . . ? 
C7 C2 C3 118.5(5) . . ? 
C7 C2 C1 122.7(5) . . ? 
C3 C2 C1 118.8(5) . . ? 
C2 C3 C4 120.4(6) . . ? 
C2 C3 H3A 119.8 . . ? 
C4 C3 H3A 119.8 . . ? 
C5 C4 C3 121.2(6) . . ? 
C5 C4 H4A 119.4 . . ? 
C3 C4 H4A 119.4 . . ? 
C4 C5 C6 119.3(5) . . ? 
C4 C5 C8 120.5(5) . . ? 
C6 C5 C8 120.1(5) . . ? 
C7 C6 C5 118.6(6) . . ? 
C7 C6 H6A 120.7 . . ? 
C5 C6 H6A 120.7 . . ? 
C2 C7 C6 121.9(5) . . ? 
C2 C7 H7A 119.0 . . ? 
C6 C7 H7A 119.0 . . ? 
N1 C8 N1 124.8(6) . 5 ? 
N1 C8 C5 117.3(5) . . ? 
N1 C8 C5 117.9(5) 5 . ? 
C9 O3 C9 44.8(17) 25_566 . ? 
C9 O3 Tb1 157.6(8) 25_566 . ? 
C9 O3 Tb1 157.6(8) . . ? 
C9 C9 O3 67.6(8) 25_566 . ? 
C9 C9 O3 67.6(8) 25_566 25_566 ? 
O3 C9 O3 135.2(17) . 25_566 ? 
C11 N2 C11 118(3) . 26_556 ? 
C11 N2 C10 111.6(11) . 3_556 ? 
C11 N2 C10 111.6(11) 26_556 3_556 ? 
C11 N2 C10 111.6(11) . . ? 
C11 N2 C10 111.6(11) 26_556 . ? 
C10 N2 C10 89(3) 3_556 . ? 
C13 N3 C13 128(5) 26_556 . ? 
C13 N3 C12 104.0(14) 26_556 27_565 ? 
C13 N3 C12 104.0(14) . 27_565 ? 
C13 N3 C12 104.0(14) 26_556 . ? 
C13 N3 C12 104.0(14) . . ? 
C12 N3 C12 113(4) 27_565 . ? 
C14 N5 C16 112(3) . . ? 
C14 N5 C15 131(3) . . ? 
C16 N5 C15 117(3) . . ? 
O4 C14 N5 122(3) . . ? 
 
_diffrn_measured_fraction_theta_max    0.994 
_diffrn_reflns_theta_full              27.48 
_diffrn_measured_fraction_theta_full   0.994 
_refine_diff_density_max    1.449 
_refine_diff_density_min   -1.076 
_refine_diff_density_rms    0.144 
# SQUEEZE RESULTS (APPEND TO CIF)
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
         1     0.000     0.000     0.000    2078.9      22.6
         2     0.500     0.500     0.500    2079.1      22.6
_platon_squeeze_details
;
;