# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2015

 
data_complex_1
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C18 H54 Cl N3 Si6 Th' 
_chemical_formula_weight          748.67 
 
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' 
 'Si'  'Si'   0.0817   0.0704 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Cl'  'Cl'   0.1484   0.1585 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Th'  'Th'  -7.2400   8.8979 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            Hexagonal 
_symmetry_space_group_name_H-M    R3c 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-y, x-y, z' 
 '-x+y, -x, z' 
 '-y, -x, z+1/2' 
 '-x+y, y, z+1/2' 
 'x, x-y, z+1/2' 
 'x+2/3, y+1/3, z+1/3' 
 '-y+2/3, x-y+1/3, z+1/3' 
 '-x+y+2/3, -x+1/3, z+1/3' 
 '-y+2/3, -x+1/3, z+5/6' 
 '-x+y+2/3, y+1/3, z+5/6' 
 'x+2/3, x-y+1/3, z+5/6' 
 'x+1/3, y+2/3, z+2/3' 
 '-y+1/3, x-y+2/3, z+2/3' 
 '-x+y+1/3, -x+2/3, z+2/3' 
 '-y+1/3, -x+2/3, z+7/6' 
 '-x+y+1/3, y+2/3, z+7/6' 
 'x+1/3, x-y+2/3, z+7/6' 
 
_cell_length_a                    18.4298(12) 
_cell_length_b                    18.4298(12) 
_cell_length_c                    16.8400(11) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 120.00 
_cell_volume                      4953.5(6) 
_cell_formula_units_Z             6 
_cell_measurement_temperature     100(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        block 
_exptl_crystal_colour             colorless 
_exptl_crystal_size_max           0.1 
_exptl_crystal_size_mid           0.1 
_exptl_crystal_size_min           0.1 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.506 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              2244 
_exptl_absorpt_coefficient_mu     4.825 
_exptl_absorpt_correction_type    'multi-scan' 
_exptl_absorpt_correction_T_min   0.5441 
_exptl_absorpt_correction_T_max   0.7461 
_exptl_absorpt_process_details    SADABS 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       100(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   ? 
_diffrn_measurement_method        ? 
_diffrn_detector_area_resol_mean  ? 
_diffrn_reflns_number             20265 
_diffrn_reflns_av_R_equivalents   0.0485 
_diffrn_reflns_av_sigmaI/netI     0.0388 
_diffrn_reflns_limit_h_min        -24 
_diffrn_reflns_limit_h_max        26 
_diffrn_reflns_limit_k_min        -26 
_diffrn_reflns_limit_k_max        26 
_diffrn_reflns_limit_l_min        -24 
_diffrn_reflns_limit_l_max        24 
_diffrn_reflns_theta_min          2.21 
_diffrn_reflns_theta_max          30.64 
_reflns_number_total              3383 
_reflns_number_gt                 3095 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 2008)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 2008)' 
_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)+(0.0000P)²+0.0000P] 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      none 
_refine_ls_extinction_coef        ? 
_refine_ls_abs_structure_details 
 'Flack H D (1983), Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack    -0.002(5) 
_refine_ls_number_reflns          3383 
_refine_ls_number_parameters      94 
_refine_ls_number_restraints      1 
_refine_ls_R_factor_all           0.0213 
_refine_ls_R_factor_gt            0.0176 
_refine_ls_wR_factor_ref          0.0437 
_refine_ls_wR_factor_gt           0.0417 
_refine_ls_goodness_of_fit_ref    1.047 
_refine_ls_restrained_S_all       1.047 
_refine_ls_shift/su_max           0.001 
_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 
Th1 Th 0.3333 0.6667 0.846643(19) 0.01272(4) Uani 1 3 d S . . 
Cl1 Cl 0.3333 0.6667 1.00383(8) 0.0233(2) Uani 1 3 d S . . 
N1 N 0.19756(9) 0.63251(9) 0.82176(10) 0.0124(3) Uani 1 1 d . . . 
Si2 Si 0.13938(5) 0.56306(3) 0.74629(4) 0.01298(13) Uani 1 1 d . . . 
Si1 Si 0.15364(3) 0.67658(3) 0.88232(4) 0.01383(10) Uani 1 1 d . . . 
C1 C 0.07451(13) 0.69449(14) 0.83030(13) 0.0205(4) Uani 1 1 d . . . 
H1A H 0.0999 0.7287 0.7829 0.031 Uiso 1 1 calc R . . 
H1B H 0.0555 0.7236 0.8660 0.031 Uiso 1 1 calc R . . 
H1C H 0.0266 0.6405 0.8147 0.031 Uiso 1 1 calc R . . 
C2 C 0.10175(15) 0.61037(15) 0.97116(14) 0.0243(4) Uani 1 1 d . . . 
H2A H 0.0541 0.5568 0.9542 0.036 Uiso 1 1 calc R . . 
H2B H 0.0819 0.6394 1.0060 0.036 Uiso 1 1 calc R . . 
H2C H 0.1420 0.6001 1.0000 0.036 Uiso 1 1 calc R . . 
C3 C 0.23824(15) 0.78145(17) 0.9176(2) 0.0216(5) Uani 1 1 d . . . 
H3A H 0.2869 0.7772 0.9347 0.032 Uiso 1 1 calc R . . 
H3B H 0.2174 0.7998 0.9625 0.032 Uiso 1 1 calc R . . 
H3C H 0.2547 0.8222 0.8743 0.032 Uiso 1 1 calc R . . 
C4 C 0.10781(13) 0.60970(13) 0.66443(13) 0.0195(4) Uani 1 1 d . . . 
H4A H 0.0699 0.6280 0.6853 0.029 Uiso 1 1 calc R . . 
H4B H 0.0792 0.5677 0.6228 0.029 Uiso 1 1 calc R . . 
H4C H 0.1578 0.6580 0.6421 0.029 Uiso 1 1 calc R . . 
C6 C 0.20523(14) 0.52516(15) 0.69676(13) 0.0215(4) Uani 1 1 d . . . 
H6A H 0.2573 0.5733 0.6776 0.032 Uiso 1 1 calc R . . 
H6B H 0.1744 0.4891 0.6518 0.032 Uiso 1 1 calc R . . 
H6C H 0.2185 0.4933 0.7349 0.032 Uiso 1 1 calc R . . 
C5 C 0.04234(13) 0.47093(14) 0.78475(14) 0.0220(4) Uani 1 1 d . . . 
H5A H 0.0571 0.4428 0.8257 0.033 Uiso 1 1 calc R . . 
H5B H 0.0132 0.4318 0.7411 0.033 Uiso 1 1 calc R . . 
H5C H 0.0056 0.4897 0.8077 0.033 Uiso 1 1 calc R . . 
 
 
_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 
Th1 N1 2.2931(15) 3_565 ? 
Th1 N1 2.2931(15) . ? 
Th1 N1 2.2932(15) 2_665 ? 
Th1 Cl1 2.6470(13) . ? 
Th1 Si1 3.4593(6) 3_565 ? 
Th1 Si1 3.4594(6) 2_665 ? 
N1 Si1 1.7355(16) . ? 
N1 Si2 1.7410(18) . ? 
Si2 C4 1.865(2) . ? 
Si2 C5 1.861(2) . ? 
Si2 C6 1.872(2) . ? 
Si1 C2 1.864(2) . ? 
Si1 C1 1.867(2) . ? 
Si1 C3 1.873(2) . ? 
 
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 
N1 Th1 N1 116.74(3) 3_565 . ? 
N1 Th1 N1 116.74(3) 3_565 2_665 ? 
N1 Th1 N1 116.74(3) . 2_665 ? 
N1 Th1 Cl1 100.53(4) 3_565 . ? 
N1 Th1 Cl1 100.53(4) . . ? 
N1 Th1 Cl1 100.53(4) 2_665 . ? 
N1 Th1 Si1 26.38(4) 3_565 3_565 ? 
N1 Th1 Si1 137.38(4) . 3_565 ? 
N1 Th1 Si1 104.78(4) 2_665 3_565 ? 
Cl1 Th1 Si1 79.998(14) . 3_565 ? 
N1 Th1 Si1 137.38(4) 3_565 2_665 ? 
N1 Th1 Si1 104.79(4) . 2_665 ? 
N1 Th1 Si1 26.38(4) 2_665 2_665 ? 
Cl1 Th1 Si1 79.998(14) . 2_665 ? 
Si1 Th1 Si1 117.047(8) 3_565 2_665 ? 
Si1 N1 Si2 120.88(9) . . ? 
Si1 N1 Th1 117.67(8) . . ? 
Si2 N1 Th1 121.44(8) . . ? 
N1 Si2 C4 114.84(9) . . ? 
N1 Si2 C5 111.97(10) . . ? 
C4 Si2 C5 107.39(10) . . ? 
N1 Si2 C6 108.89(9) . . ? 
C4 Si2 C6 104.63(10) . . ? 
C5 Si2 C6 108.74(11) . . ? 
N1 Si1 C2 111.84(9) . . ? 
N1 Si1 C1 113.29(9) . . ? 
C2 Si1 C1 107.57(10) . . ? 
N1 Si1 C3 109.10(11) . . ? 
C2 Si1 C3 108.09(14) . . ? 
C1 Si1 C3 106.71(13) . . ? 
 
_diffrn_measured_fraction_theta_max    0.999 
_diffrn_reflns_theta_full              30.64 
_diffrn_measured_fraction_theta_full   0.999 
_refine_diff_density_max    0.531 
_refine_diff_density_min   -0.634 
_refine_diff_density_rms    0.068 


###END###


 
data_Th-Cl2-'ate'
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C36 H82 Cl2 N3 Na O4.50 Si6 Th' 
_chemical_formula_weight          1123.52 
 
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' 
 'Na'  'Na'   0.0362   0.0249 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Si'  'Si'   0.0817   0.0704 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Cl'  'Cl'   0.1484   0.1585 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Th'  'Th'  -7.2400   8.8979 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            hexagonal 
_symmetry_space_group_name_H-M    R-3 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-y, x-y, z' 
 '-x+y, -x, z' 
 'x+2/3, y+1/3, z+1/3' 
 '-y+2/3, x-y+1/3, z+1/3' 
 '-x+y+2/3, -x+1/3, z+1/3' 
 'x+1/3, y+2/3, z+2/3' 
 '-y+1/3, x-y+2/3, z+2/3' 
 '-x+y+1/3, -x+2/3, z+2/3' 
 '-x, -y, -z' 
 'y, -x+y, -z' 
 'x-y, x, -z' 
 '-x+2/3, -y+1/3, -z+1/3' 
 'y+2/3, -x+y+1/3, -z+1/3' 
 'x-y+2/3, x+1/3, -z+1/3' 
 '-x+1/3, -y+2/3, -z+2/3' 
 'y+1/3, -x+y+2/3, -z+2/3' 
 'x-y+1/3, x+2/3, -z+2/3' 
 
_cell_length_a                    18.404(4) 
_cell_length_b                    18.404(4) 
_cell_length_c                    29.626(7) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 120.00 
_cell_volume                      8690(3) 
_cell_formula_units_Z             6 
_cell_measurement_temperature     100(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        needle 
_exptl_crystal_colour             colorless 
_exptl_crystal_size_max           0.2 
_exptl_crystal_size_mid           0.05 
_exptl_crystal_size_min           0.02 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.288 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              3444 
_exptl_absorpt_coefficient_mu     2.831 
_exptl_absorpt_correction_type    'multi-scan' 
_exptl_absorpt_correction_T_min   0.5782 
_exptl_absorpt_correction_T_max   0.7455 
_exptl_absorpt_process_details    SADABS 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       100(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   ? 
_diffrn_measurement_method        ? 
_diffrn_detector_area_resol_mean  ? 
_diffrn_reflns_number             8328 
_diffrn_reflns_av_R_equivalents   0.0316 
_diffrn_reflns_av_sigmaI/netI     0.0775 
_diffrn_reflns_limit_h_min        -24 
_diffrn_reflns_limit_h_max        16 
_diffrn_reflns_limit_k_min        -3 
_diffrn_reflns_limit_k_max        26 
_diffrn_reflns_limit_l_min        -24 
_diffrn_reflns_limit_l_max        42 
_diffrn_reflns_theta_min          2.06 
_diffrn_reflns_theta_max          30.64 
_reflns_number_total              5914 
_reflns_number_gt                 4570 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 2008)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 2008)' 
_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)+(0.0683P)²+0.0000P] 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      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          5914 
_refine_ls_number_parameters      167 
_refine_ls_number_restraints      8 
_refine_ls_R_factor_all           0.0745 
_refine_ls_R_factor_gt            0.0503 
_refine_ls_wR_factor_ref          0.1272 
_refine_ls_wR_factor_gt           0.1166 
_refine_ls_goodness_of_fit_ref    1.000 
_refine_ls_restrained_S_all       1.002 
_refine_ls_shift/su_max           0.036 
_refine_ls_shift/su_mean          0.004 
 
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 
Th1 Th 0.3333 0.6667 0.381498(10) 0.02280(9) Uani 1 3 d S . . 
Cl1 Cl 0.3333 0.6667 0.47348(9) 0.0587(7) Uani 1 3 d S . . 
Cl2 Cl 0.3333 0.6667 0.28893(9) 0.0663(8) Uani 1 3 d S . . 
Si1 Si 0.41163(11) 0.53797(11) 0.42223(6) 0.0454(4) Uani 1 1 d . . . 
Si2 Si 0.51242(14) 0.65715(14) 0.34891(9) 0.0731(7) Uani 1 1 d . . . 
N1 N 0.4265(3) 0.6157(3) 0.38364(15) 0.0338(9) Uani 1 1 d . . . 
C1 C 0.3003(5) 0.4721(5) 0.4394(3) 0.082(3) Uani 1 1 d . . . 
H1A H 0.2974 0.4448 0.4682 0.123 Uiso 1 1 calc R . . 
H1B H 0.2700 0.4293 0.4163 0.123 Uiso 1 1 calc R . . 
H1C H 0.2747 0.5074 0.4426 0.123 Uiso 1 1 calc R . . 
C2 C 0.4369(5) 0.4587(4) 0.3989(3) 0.072(2) Uani 1 1 d . . . 
H2A H 0.4213 0.4135 0.4210 0.107 Uiso 1 1 calc R . . 
H2B H 0.4972 0.4857 0.3927 0.107 Uiso 1 1 calc R . . 
H2C H 0.4055 0.4353 0.3709 0.107 Uiso 1 1 calc R . . 
C3 C 0.4784(6) 0.5831(5) 0.4729(3) 0.088(3) Uani 1 1 d . . . 
H3A H 0.5376 0.6097 0.4642 0.132 Uiso 1 1 calc R . . 
H3B H 0.4656 0.5384 0.4948 0.132 Uiso 1 1 calc R . . 
H3C H 0.4673 0.6251 0.4865 0.132 Uiso 1 1 calc R . . 
Na1 Na 0.3333 0.6667 0.6667 0.0293(10) Uani 1 6 d S . . 
O1 O 0.4535(2) 0.7323(2) 0.62127(12) 0.0390(8) Uani 1 1 d . . . 
C10 C 0.4679(4) 0.6949(4) 0.58176(19) 0.0439(13) Uani 1 1 d . . . 
H10A H 0.4243 0.6825 0.5587 0.053 Uiso 1 1 calc R . . 
H10B H 0.4661 0.6419 0.5899 0.053 Uiso 1 1 calc R . . 
C7 C 0.5179(4) 0.8179(4) 0.6245(2) 0.0446(13) Uani 1 1 d . . . 
H7A H 0.5579 0.8254 0.6489 0.053 Uiso 1 1 calc R . . 
H7B H 0.4936 0.8542 0.6309 0.053 Uiso 1 1 calc R . . 
C9 C 0.5520(4) 0.7567(4) 0.5641(2) 0.0507(15) Uani 1 1 d . . . 
H9A H 0.5541 0.7537 0.5308 0.061 Uiso 1 1 calc R . . 
H9B H 0.5963 0.7477 0.5774 0.061 Uiso 1 1 calc R . . 
C8 C 0.5615(4) 0.8395(4) 0.5791(2) 0.0529(16) Uani 1 1 d . . . 
H8A H 0.5339 0.8594 0.5577 0.063 Uiso 1 1 calc R . . 
H8B H 0.6214 0.8829 0.5821 0.063 Uiso 1 1 calc R . . 
C4 C 0.5392(5) 0.7636(5) 0.3281(3) 0.075(2) Uani 1 1 d . . . 
H4A H 0.4923 0.7594 0.3104 0.112 Uiso 1 1 calc R . . 
H4B H 0.5895 0.7863 0.3092 0.112 Uiso 1 1 calc R . . 
H4C H 0.5499 0.8010 0.3540 0.112 Uiso 1 1 calc R . . 
C5 C 0.4941(8) 0.5875(7) 0.2994(4) 0.134(5) Uani 1 1 d . . . 
H5A H 0.4375 0.5674 0.2876 0.202 Uiso 1 1 calc R . . 
H5B H 0.4997 0.5395 0.3088 0.202 Uiso 1 1 calc R . . 
H5C H 0.5354 0.6190 0.2759 0.202 Uiso 1 1 calc R . . 
C6 C 0.6112(5) 0.6768(6) 0.3784(5) 0.145(6) Uani 1 1 d . . . 
H6A H 0.6018 0.6250 0.3929 0.217 Uiso 1 1 calc R . . 
H6B H 0.6266 0.7205 0.4013 0.217 Uiso 1 1 calc R . . 
H6C H 0.6568 0.6952 0.3563 0.217 Uiso 1 1 calc R . . 
Na2 Na 0.3333 0.6667 0.1981(4) 0.083(3) Uani 0.50 3 d SP . . 
O2 O 0.3377(18) 0.5384(18) 0.1760(10) 0.228(11) Uiso 0.50 1 d PD . . 
C11 C 0.4061(19) 0.5577(15) 0.1462(9) 0.178(13) Uiso 0.50 1 d PD . . 
C13 C 0.3310(16) 0.4206(13) 0.1671(8) 0.121(8) Uiso 0.50 1 d PD . . 
C14 C 0.3328(19) 0.4756(19) 0.2030(8) 0.189(14) Uiso 0.50 1 d PD . . 
C12 C 0.412(2) 0.483(2) 0.1464(12) 0.25(2) Uiso 0.50 1 d PD . . 
 
 
_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 
Th1 N1 2.332(4) 2_665 ? 
Th1 N1 2.332(4) 3_565 ? 
Th1 N1 2.332(4) . ? 
Th1 Cl1 2.725(3) . ? 
Th1 Cl2 2.743(3) . ? 
Cl2 Na2 2.691(11) . ? 
Si1 N1 1.742(5) . ? 
Si1 C3 1.854(7) . ? 
Si1 C1 1.855(8) . ? 
Si1 C2 1.871(7) . ? 
Si2 N1 1.712(5) . ? 
Si2 C5 1.864(10) . ? 
Si2 C4 1.870(7) . ? 
Si2 C6 1.883(10) . ? 
Na1 O1 2.343(4) 2_665 ? 
Na1 O1 2.343(4) 3_565 ? 
Na1 O1 2.343(4) . ? 
Na1 O1 2.343(4) 14_456 ? 
Na1 O1 2.343(4) 13_566 ? 
Na1 O1 2.343(4) 15_556 ? 
O1 C7 1.425(6) . ? 
O1 C10 1.448(6) . ? 
C10 C9 1.485(8) . ? 
C7 C8 1.513(8) . ? 
C9 C8 1.510(9) . ? 
Na2 Na2 1.86(2) 13_565 ? 
Na2 O2 2.49(3) 3_565 ? 
Na2 O2 2.49(3) 2_665 ? 
Na2 O2 2.49(3) . ? 
Na2 O2 2.69(3) 15 ? 
Na2 O2 2.69(3) 14_455 ? 
Na2 O2 2.69(3) 13_565 ? 
Na2 C11 2.93(3) 15 ? 
Na2 C11 2.93(3) 14_455 ? 
Na2 C11 2.93(3) 13_565 ? 
O2 C14 1.370(18) . ? 
O2 C11 1.429(18) . ? 
O2 C11 1.84(4) 14_455 ? 
O2 Na2 2.69(3) 13_565 ? 
C11 C12 1.440(19) . ? 
C11 O2 1.84(4) 15 ? 
C11 Na2 2.93(3) 13_565 ? 
C13 C14 1.457(18) . ? 
C13 C12 1.489(18) . ? 
 
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 
N1 Th1 N1 119.927(11) 2_665 3_565 ? 
N1 Th1 N1 119.928(12) 2_665 . ? 
N1 Th1 N1 119.926(11) 3_565 . ? 
N1 Th1 Cl1 88.44(11) 2_665 . ? 
N1 Th1 Cl1 88.44(11) 3_565 . ? 
N1 Th1 Cl1 88.44(11) . . ? 
N1 Th1 Cl2 91.56(11) 2_665 . ? 
N1 Th1 Cl2 91.56(11) 3_565 . ? 
N1 Th1 Cl2 91.56(11) . . ? 
Cl1 Th1 Cl2 180.000(1) . . ? 
Na2 Cl2 Th1 180.000(1) . . ? 
N1 Si1 C3 111.5(3) . . ? 
N1 Si1 C1 112.6(3) . . ? 
C3 Si1 C1 109.8(5) . . ? 
N1 Si1 C2 113.5(3) . . ? 
C3 Si1 C2 106.3(4) . . ? 
C1 Si1 C2 102.4(4) . . ? 
N1 Si2 C5 110.9(4) . . ? 
N1 Si2 C4 111.4(3) . . ? 
C5 Si2 C4 108.9(5) . . ? 
N1 Si2 C6 113.2(4) . . ? 
C5 Si2 C6 108.8(6) . . ? 
C4 Si2 C6 103.2(4) . . ? 
Si2 N1 Si1 119.4(2) . . ? 
Si2 N1 Th1 120.3(2) . . ? 
Si1 N1 Th1 120.2(2) . . ? 
O1 Na1 O1 90.32(13) 2_665 3_565 ? 
O1 Na1 O1 90.32(13) 2_665 . ? 
O1 Na1 O1 90.32(13) 3_565 . ? 
O1 Na1 O1 179.993(1) 2_665 14_456 ? 
O1 Na1 O1 89.68(13) 3_565 14_456 ? 
O1 Na1 O1 89.69(13) . 14_456 ? 
O1 Na1 O1 89.68(13) 2_665 13_566 ? 
O1 Na1 O1 89.68(13) 3_565 13_566 ? 
O1 Na1 O1 179.996(1) . 13_566 ? 
O1 Na1 O1 90.31(13) 14_456 13_566 ? 
O1 Na1 O1 89.68(13) 2_665 15_556 ? 
O1 Na1 O1 179.994(1) 3_565 15_556 ? 
O1 Na1 O1 89.69(13) . 15_556 ? 
O1 Na1 O1 90.31(13) 14_456 15_556 ? 
O1 Na1 O1 90.31(13) 13_566 15_556 ? 
C7 O1 C10 109.3(4) . . ? 
C7 O1 Na1 125.5(3) . . ? 
C10 O1 Na1 124.7(3) . . ? 
O1 C10 C9 106.8(5) . . ? 
O1 C7 C8 105.6(5) . . ? 
C10 C9 C8 102.7(5) . . ? 
C9 C8 C7 102.6(5) . . ? 
Na2 Na2 O2 74.7(7) 13_565 3_565 ? 
Na2 Na2 O2 74.7(7) 13_565 2_665 ? 
O2 Na2 O2 113.3(6) 3_565 2_665 ? 
Na2 Na2 O2 74.7(7) 13_565 . ? 
O2 Na2 O2 113.3(6) 3_565 . ? 
O2 Na2 O2 113.3(6) 2_665 . ? 
Na2 Na2 O2 63.3(6) 13_565 15 ? 
O2 Na2 O2 138.0(6) 3_565 15 ? 
O2 Na2 O2 56.7(3) 2_665 15 ? 
O2 Na2 O2 56.7(3) . 15 ? 
Na2 Na2 O2 63.3(6) 13_565 14_455 ? 
O2 Na2 O2 56.7(3) 3_565 14_455 ? 
O2 Na2 O2 138.0(6) 2_665 14_455 ? 
O2 Na2 O2 56.7(3) . 14_455 ? 
O2 Na2 O2 101.4(8) 15 14_455 ? 
Na2 Na2 O2 63.3(6) 13_565 13_565 ? 
O2 Na2 O2 56.7(3) 3_565 13_565 ? 
O2 Na2 O2 56.7(3) 2_665 13_565 ? 
O2 Na2 O2 138.0(6) . 13_565 ? 
O2 Na2 O2 101.4(8) 15 13_565 ? 
O2 Na2 O2 101.4(8) 14_455 13_565 ? 
Na2 Na2 Cl2 180.0 13_565 . ? 
O2 Na2 Cl2 105.3(7) 3_565 . ? 
O2 Na2 Cl2 105.3(7) 2_665 . ? 
O2 Na2 Cl2 105.3(7) . . ? 
O2 Na2 Cl2 116.7(6) 15 . ? 
O2 Na2 Cl2 116.7(6) 14_455 . ? 
O2 Na2 Cl2 116.7(6) 13_565 . ? 
Na2 Na2 C11 83.6(6) 13_565 15 ? 
O2 Na2 C11 149.4(9) 3_565 15 ? 
O2 Na2 C11 38.5(8) 2_665 15 ? 
O2 Na2 C11 80.4(6) . 15 ? 
O2 Na2 C11 29.0(4) 15 15 ? 
O2 Na2 C11 130.4(8) 14_455 15 ? 
O2 Na2 C11 94.4(8) 13_565 15 ? 
Cl2 Na2 C11 96.4(6) . 15 ? 
Na2 Na2 C11 83.6(6) 13_565 14_455 ? 
O2 Na2 C11 80.4(6) 3_565 14_455 ? 
O2 Na2 C11 149.4(9) 2_665 14_455 ? 
O2 Na2 C11 38.5(8) . 14_455 ? 
O2 Na2 C11 94.4(8) 15 14_455 ? 
O2 Na2 C11 29.0(4) 14_455 14_455 ? 
O2 Na2 C11 130.4(8) 13_565 14_455 ? 
Cl2 Na2 C11 96.4(6) . 14_455 ? 
C11 Na2 C11 118.8(2) 15 14_455 ? 
Na2 Na2 C11 83.6(6) 13_565 13_565 ? 
O2 Na2 C11 38.5(8) 3_565 13_565 ? 
O2 Na2 C11 80.4(6) 2_665 13_565 ? 
O2 Na2 C11 149.4(9) . 13_565 ? 
O2 Na2 C11 130.4(8) 15 13_565 ? 
O2 Na2 C11 94.4(8) 14_455 13_565 ? 
O2 Na2 C11 29.0(4) 13_565 13_565 ? 
Cl2 Na2 C11 96.4(6) . 13_565 ? 
C11 Na2 C11 118.8(2) 15 13_565 ? 
C11 Na2 C11 118.8(2) 14_455 13_565 ? 
C14 O2 C11 104.4(16) . . ? 
C14 O2 C11 82(3) . 14_455 ? 
C11 O2 C11 150(2) . 14_455 ? 
C14 O2 Na2 129(2) . . ? 
C11 O2 Na2 112(2) . . ? 
C11 O2 Na2 83.9(10) 14_455 . ? 
C14 O2 Na2 169.8(19) . 13_565 ? 
C11 O2 Na2 85.0(18) . 13_565 ? 
C11 O2 Na2 91.5(12) 14_455 13_565 ? 
Na2 O2 Na2 41.9(6) . 13_565 ? 
O2 C11 C12 104.0(14) . . ? 
O2 C11 O2 97(3) . 15 ? 
C12 C11 O2 143(3) . 15 ? 
O2 C11 Na2 65.9(16) . 13_565 ? 
C12 C11 Na2 160(2) . 13_565 ? 
O2 C11 Na2 57.6(11) 15 13_565 ? 
C14 C13 C12 95.8(13) . . ? 
O2 C14 C13 97.4(19) . . ? 
C11 C12 C13 101.8(15) . . ? 
 
_diffrn_measured_fraction_theta_max    0.990 
_diffrn_reflns_theta_full              30.64 
_diffrn_measured_fraction_theta_full   0.990 
_refine_diff_density_max    1.321 
_refine_diff_density_min   -1.575 
_refine_diff_density_rms    0.153 


###END###


data_complex_2 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C18 H54 I N3 Si6 Th' 
_chemical_formula_weight          840.12 
 
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' 
 'Si'  'Si'   0.0817   0.0704 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'I'  'I'  -0.4742   1.8119 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Th'  'Th'  -7.2400   8.8979 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            Hexagonal
_symmetry_space_group_name_H-M    R3c 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-y, x-y, z' 
 '-x+y, -x, z' 
 '-x+y, y, z+1/2' 
 'x, x-y, z+1/2' 
 '-y, -x, z+1/2' 
 'x+2/3, y+1/3, z+1/3' 
 '-y+2/3, x-y+1/3, z+1/3' 
 '-x+y+2/3, -x+1/3, z+1/3' 
 '-x+y+2/3, y+1/3, z+5/6' 
 'x+2/3, x-y+1/3, z+5/6' 
 '-y+2/3, -x+1/3, z+5/6' 
 'x+1/3, y+2/3, z+2/3' 
 '-y+1/3, x-y+2/3, z+2/3' 
 '-x+y+1/3, -x+2/3, z+2/3' 
 '-x+y+1/3, y+2/3, z+7/6' 
 'x+1/3, x-y+2/3, z+7/6' 
 '-y+1/3, -x+2/3, z+7/6' 
 
_cell_length_a                    18.328(5) 
_cell_length_b                    18.328(5) 
_cell_length_c                    17.356(5) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 120.00 
_cell_volume                      5049(3) 
_cell_formula_units_Z             6 
_cell_measurement_temperature     100(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        block 
_exptl_crystal_colour             colorless 
_exptl_crystal_size_max           0.2 
_exptl_crystal_size_mid           0.1 
_exptl_crystal_size_min           0.1 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.658 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              2460 
_exptl_absorpt_coefficient_mu     5.572 
_exptl_absorpt_correction_type    'multi-scan' 
_exptl_absorpt_correction_T_min   0.5789 
_exptl_absorpt_correction_T_max   0.7461 
_exptl_absorpt_process_details    SADABS 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       100(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   ? 
_diffrn_measurement_method        ? 
_diffrn_detector_area_resol_mean  ? 
_diffrn_reflns_number             9620 
_diffrn_reflns_av_R_equivalents   0.0324 
_diffrn_reflns_av_sigmaI/netI     0.0744 
_diffrn_reflns_limit_h_min        -24 
_diffrn_reflns_limit_h_max        25 
_diffrn_reflns_limit_k_min        -26 
_diffrn_reflns_limit_k_max        20 
_diffrn_reflns_limit_l_min        -23 
_diffrn_reflns_limit_l_max        23 
_diffrn_reflns_theta_min          2.22 
_diffrn_reflns_theta_max          30.50 
_reflns_number_total              3344 
_reflns_number_gt                 2546 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 2008)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 2008)' 
_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)+(0.0000P)²+0.0000P] 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      none 
_refine_ls_extinction_coef        ? 
_refine_ls_abs_structure_details 
 'Flack H D (1983), Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack    -0.005(6) 
_refine_ls_number_reflns          3344 
_refine_ls_number_parameters      94 
_refine_ls_number_restraints      1 
_refine_ls_R_factor_all           0.0458 
_refine_ls_R_factor_gt            0.0295 
_refine_ls_wR_factor_ref          0.0772 
_refine_ls_wR_factor_gt           0.0681 
_refine_ls_goodness_of_fit_ref    0.891 
_refine_ls_restrained_S_all       0.891 
_refine_ls_shift/su_max           0.000 
_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 
Th1 Th 0.3333 0.6667 0.255874(5) 0.01289(7) Uani 1 3 d S . . 
I1 I 0.3333 0.6667 0.43173(4) 0.02496(15) Uani 1 3 d S . . 
Si2 Si 0.15205(8) 0.47480(8) 0.28958(9) 0.0146(2) Uani 1 1 d . . . 
N1 N 0.1962(2) 0.5646(2) 0.2320(2) 0.0132(7) Uani 1 1 d . . . 
Si1 Si 0.13700(9) 0.57681(8) 0.15996(9) 0.0138(3) Uani 1 1 d . . . 
C1 C 0.2019(3) 0.6836(3) 0.1148(3) 0.0208(10) Uani 1 1 d . . . 
H2A H 0.2149 0.7273 0.1535 0.031 Uiso 1 1 calc R . . 
H2B H 0.1702 0.6900 0.0724 0.031 Uiso 1 1 calc R . . 
H2C H 0.2545 0.6892 0.0948 0.031 Uiso 1 1 calc R . . 
C6 C 0.2377(3) 0.4544(4) 0.3251(4) 0.0206(11) Uani 1 1 d . . . 
H3A H 0.2440 0.4167 0.2891 0.031 Uiso 1 1 calc R . . 
H3B H 0.2226 0.4281 0.3762 0.031 Uiso 1 1 calc R . . 
H3C H 0.2911 0.5078 0.3285 0.031 Uiso 1 1 calc R . . 
C4 C 0.0741(3) 0.3784(3) 0.2373(3) 0.0200(10) Uani 1 1 d . . . 
H4A H 0.0274 0.3857 0.2195 0.030 Uiso 1 1 calc R . . 
H4B H 0.0525 0.3298 0.2720 0.030 Uiso 1 1 calc R . . 
H4C H 0.1015 0.3690 0.1929 0.030 Uiso 1 1 calc R . . 
C2 C 0.1067(3) 0.5009(3) 0.0782(3) 0.0200(10) Uani 1 1 d . . . 
H5A H 0.1575 0.5051 0.0553 0.030 Uiso 1 1 calc R . . 
H5B H 0.0766 0.5143 0.0392 0.030 Uiso 1 1 calc R . . 
H5C H 0.0702 0.4435 0.0972 0.030 Uiso 1 1 calc R . . 
C3 C 0.0378(3) 0.5691(3) 0.1983(3) 0.0222(11) Uani 1 1 d . . . 
H6A H 0.0017 0.5128 0.2198 0.033 Uiso 1 1 calc R . . 
H6B H 0.0080 0.5790 0.1564 0.033 Uiso 1 1 calc R . . 
H6C H 0.0519 0.6115 0.2386 0.033 Uiso 1 1 calc R . . 
C5 C 0.0964(3) 0.4861(3) 0.3752(3) 0.0243(11) Uani 1 1 d . . . 
H7A H 0.1344 0.5383 0.4027 0.036 Uiso 1 1 calc R . . 
H7B H 0.0792 0.4379 0.4098 0.036 Uiso 1 1 calc R . . 
H7C H 0.0464 0.4880 0.3581 0.036 Uiso 1 1 calc R . . 
 
 
_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 
Th1 N1 2.299(4) 3_565 ? 
Th1 N1 2.299(4) . ? 
Th1 N1 2.299(4) 2_665 ? 
Th1 I1 3.0523(12) . ? 
Th1 Si2 3.4732(16) 3_565 ? 
Th1 Si2 3.4732(17) 2_665 ? 
Si2 N1 1.740(4) . ? 
Si2 C4 1.860(5) . ? 
Si2 C5 1.872(5) . ? 
Si2 C6 1.891(5) . ? 
N1 Si1 1.743(4) . ? 
Si1 C2 1.867(5) . ? 
Si1 C3 1.873(5) . ? 
Si1 C1 1.880(5) . ? 
 
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 
N1 Th1 N1 116.83(6) 3_565 . ? 
N1 Th1 N1 116.83(6) 3_565 2_665 ? 
N1 Th1 N1 116.83(6) . 2_665 ? 
N1 Th1 I1 100.37(9) 3_565 . ? 
N1 Th1 I1 100.37(9) . . ? 
N1 Th1 I1 100.37(9) 2_665 . ? 
N1 Th1 Si2 26.27(10) 3_565 3_565 ? 
N1 Th1 Si2 104.35(9) . 3_565 ? 
N1 Th1 Si2 137.72(10) 2_665 3_565 ? 
I1 Th1 Si2 80.30(3) . 3_565 ? 
N1 Th1 Si2 104.34(9) 3_565 2_665 ? 
N1 Th1 Si2 137.72(9) . 2_665 ? 
N1 Th1 Si2 26.27(10) 2_665 2_665 ? 
I1 Th1 Si2 80.30(3) . 2_665 ? 
Si2 Th1 Si2 117.223(16) 3_565 2_665 ? 
N1 Si2 C4 113.0(2) . . ? 
N1 Si2 C5 111.9(2) . . ? 
C4 Si2 C5 106.9(2) . . ? 
N1 Si2 C6 109.5(2) . . ? 
C4 Si2 C6 106.9(2) . . ? 
C5 Si2 C6 108.4(3) . . ? 
Si2 N1 Si1 120.6(2) . . ? 
Si2 N1 Th1 117.95(19) . . ? 
Si1 N1 Th1 121.5(2) . . ? 
N1 Si1 C2 114.9(2) . . ? 
N1 Si1 C3 112.3(2) . . ? 
C2 Si1 C3 107.3(2) . . ? 
N1 Si1 C1 108.8(2) . . ? 
C2 Si1 C1 104.9(2) . . ? 
C3 Si1 C1 108.2(2) . . ? 
 
_diffrn_measured_fraction_theta_max    0.988 
_diffrn_reflns_theta_full              30.50 
_diffrn_measured_fraction_theta_full   0.988 
_refine_diff_density_max    5.273 
_refine_diff_density_min   -0.996 
_refine_diff_density_rms    0.154 


###END###

 
data_complex_5
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C53 H73 N2 O2 Si4 Th' 
_chemical_formula_weight          1114.53 
 
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' 
 'Si'  'Si'   0.0817   0.0704 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Th'  'Th'  -7.2400   8.8979 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            Triclinic 
_symmetry_space_group_name_H-M    P-1 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, -y, -z' 
 
_cell_length_a                    12.955(2) 
_cell_length_b                    13.0253(19) 
_cell_length_c                    16.867(2) 
_cell_angle_alpha                 85.654(3) 
_cell_angle_beta                  77.178(3) 
_cell_angle_gamma                 79.336(3) 
_cell_volume                      2725.4(7) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     100(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        plate 
_exptl_crystal_colour             colorless 
_exptl_crystal_size_max           0.1 
_exptl_crystal_size_mid           0.1 
_exptl_crystal_size_min           0.05 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.358 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1134 
_exptl_absorpt_coefficient_mu     2.862 
_exptl_absorpt_correction_type    'multi-scan' 
_exptl_absorpt_correction_T_min   0.6341 
_exptl_absorpt_correction_T_max   0.7454 
_exptl_absorpt_process_details    SADABS 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       100(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   ? 
_diffrn_measurement_method        ? 
_diffrn_detector_area_resol_mean  ? 
_diffrn_reflns_number             56153 
_diffrn_reflns_av_R_equivalents   0.0655 
_diffrn_reflns_av_sigmaI/netI     0.0537 
_diffrn_reflns_limit_h_min        -16 
_diffrn_reflns_limit_h_max        16 
_diffrn_reflns_limit_k_min        -16 
_diffrn_reflns_limit_k_max        16 
_diffrn_reflns_limit_l_min        -21 
_diffrn_reflns_limit_l_max        21 
_diffrn_reflns_theta_min          1.24 
_diffrn_reflns_theta_max          26.44 
_reflns_number_total              11192 
_reflns_number_gt                 9507 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 2008)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 2008)' 
_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)+(0.0320P)²+0.0000P] 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      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          11192 
_refine_ls_number_parameters      572 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0452 
_refine_ls_R_factor_gt            0.0310 
_refine_ls_wR_factor_ref          0.0653 
_refine_ls_wR_factor_gt           0.0612 
_refine_ls_goodness_of_fit_ref    1.013 
_refine_ls_restrained_S_all       1.013 
_refine_ls_shift/su_max           0.001 
_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 
Th1 Th 0.319951(10) 0.767930(10) 0.728213(8) 0.01532(4) Uani 1 1 d . . . 
N1 N 0.4904(2) 0.6717(2) 0.67278(17) 0.0209(7) Uani 1 1 d . . . 
N2 N 0.2047(2) 0.8734(2) 0.65189(18) 0.0242(7) Uani 1 1 d . . . 
Si1 Si 0.53784(8) 0.53997(8) 0.68840(6) 0.0250(2) Uani 1 1 d . . . 
Si4 Si 0.14341(9) 1.00083(8) 0.67249(7) 0.0294(3) Uani 1 1 d . . . 
Si2 Si 0.56922(8) 0.74991(8) 0.60797(6) 0.0236(2) Uani 1 1 d . . . 
Si3 Si 0.19087(10) 0.80977(10) 0.57026(7) 0.0351(3) Uani 1 1 d . . . 
O1 O 0.36482(18) 0.85437(17) 0.81363(13) 0.0163(5) Uani 1 1 d . . . 
O2 O 0.21226(18) 0.67533(17) 0.79960(14) 0.0183(5) Uani 1 1 d . . . 
C12 C 0.1229(3) 1.0219(3) 0.7832(3) 0.0340(10) Uani 1 1 d . . . 
H3A H 0.0783 0.9733 0.8142 0.051 Uiso 1 1 calc R . . 
H3B H 0.0870 1.0939 0.7948 0.051 Uiso 1 1 calc R . . 
H3C H 0.1927 1.0096 0.7990 0.051 Uiso 1 1 calc R . . 
C5 C 0.6830(3) 0.7823(3) 0.6474(3) 0.0329(10) Uani 1 1 d . . . 
H1A H 0.6548 0.8169 0.6993 0.049 Uiso 1 1 calc R . . 
H1B H 0.7211 0.8290 0.6080 0.049 Uiso 1 1 calc R . . 
H1C H 0.7327 0.7178 0.6556 0.049 Uiso 1 1 calc R . . 
C6 C 0.4813(3) 0.8799(3) 0.5952(2) 0.0310(9) Uani 1 1 d . . . 
H2A H 0.4193 0.8692 0.5745 0.047 Uiso 1 1 calc R . . 
H2B H 0.5226 0.9250 0.5565 0.047 Uiso 1 1 calc R . . 
H2C H 0.4562 0.9131 0.6478 0.047 Uiso 1 1 calc R . . 
C39 C 0.1761(3) 0.5022(2) 0.8351(2) 0.0181(8) Uani 1 1 d . . . 
C27 C 0.4620(3) 0.8178(3) 1.0041(2) 0.0186(8) Uani 1 1 d . . . 
H15 H 0.4266 0.8806 1.0304 0.022 Uiso 1 1 calc R . . 
C21 C 0.3075(3) 1.0536(3) 0.9619(2) 0.0188(8) Uani 1 1 d . . . 
H8 H 0.3688 1.0862 0.9433 0.023 Uiso 1 1 calc R . . 
C20 C 0.3057(3) 0.9575(2) 0.9329(2) 0.0162(7) Uani 1 1 d . . . 
C13 C 0.4031(3) 0.8969(2) 0.8745(2) 0.0150(7) Uani 1 1 d . . . 
C32 C 0.1394(3) 0.6182(2) 0.8547(2) 0.0173(7) Uani 1 1 d . . . 
C38 C 0.0582(3) 0.6752(3) 1.0016(2) 0.0197(8) Uani 1 1 d . . . 
H25 H -0.0114 0.6872 0.9897 0.024 Uiso 1 1 calc R . . 
C26 C 0.4590(3) 0.8068(3) 0.9234(2) 0.0158(7) Uani 1 1 d . . . 
C30 C 0.5628(3) 0.6334(3) 0.9304(2) 0.0230(8) Uani 1 1 d . . . 
H18 H 0.5957 0.5692 0.9052 0.028 Uiso 1 1 calc R . . 
C14 C 0.4823(3) 0.9687(3) 0.8321(2) 0.0162(7) Uani 1 1 d . . . 
C33 C 0.1469(3) 0.6394(2) 0.9411(2) 0.0188(8) Uani 1 1 d . . . 
C25 C 0.2154(3) 0.9108(3) 0.9621(2) 0.0190(8) Uani 1 1 d . . . 
H13 H 0.2135 0.8444 0.9433 0.023 Uiso 1 1 calc R . . 
C19 C 0.5841(3) 0.9614(3) 0.8476(2) 0.0222(8) Uani 1 1 d . . . 
H7 H 0.6075 0.9098 0.8857 0.027 Uiso 1 1 calc R . . 
C35 C 0.2599(3) 0.6418(3) 1.0381(2) 0.0227(8) Uani 1 1 d . . . 
H23 H 0.3294 0.6304 1.0503 0.027 Uiso 1 1 calc R . . 
C34 C 0.2484(3) 0.6237(3) 0.9613(2) 0.0193(8) Uani 1 1 d . . . 
H24 H 0.3106 0.6001 0.9210 0.023 Uiso 1 1 calc R . . 
C28 C 0.5159(3) 0.7386(3) 1.0467(2) 0.0233(8) Uani 1 1 d . . . 
H12 H 0.5183 0.7480 1.1016 0.028 Uiso 1 1 calc R . . 
C22 C 0.2197(3) 1.1031(3) 1.0186(2) 0.0244(8) Uani 1 1 d . . . 
H10 H 0.2215 1.1690 1.0382 0.029 Uiso 1 1 calc R . . 
C29 C 0.5663(3) 0.6460(3) 1.0101(2) 0.0247(9) Uani 1 1 d . . . 
H17 H 0.6030 0.5916 1.0395 0.030 Uiso 1 1 calc R . . 
C15 C 0.4501(3) 1.0447(3) 0.7754(2) 0.0230(8) Uani 1 1 d . . . 
H6 H 0.3807 1.0506 0.7637 0.028 Uiso 1 1 calc R . . 
C36 C 0.1701(3) 0.6766(3) 1.0975(2) 0.0266(9) Uani 1 1 d . . . 
H28 H 0.1777 0.6888 1.1506 0.032 Uiso 1 1 calc R . . 
C31 C 0.5113(3) 0.7144(3) 0.8866(2) 0.0192(8) Uani 1 1 d . . . 
H16 H 0.5121 0.7061 0.8310 0.023 Uiso 1 1 calc R . . 
C44 C 0.1886(3) 0.4750(3) 0.7549(2) 0.0270(9) Uani 1 1 d . . . 
H21 H 0.1728 0.5277 0.7151 0.032 Uiso 1 1 calc R . . 
C24 C 0.1286(3) 0.9591(3) 1.0178(2) 0.0235(8) Uani 1 1 d . . . 
H11 H 0.0676 0.9263 1.0370 0.028 Uiso 1 1 calc R . . 
C40 C 0.1951(3) 0.4227(3) 0.8923(2) 0.0220(8) Uani 1 1 d . . . 
H22 H 0.1848 0.4389 0.9478 0.026 Uiso 1 1 calc R . . 
C37 C 0.0689(3) 0.6937(3) 1.0791(2) 0.0272(9) Uani 1 1 d . . . 
H27 H 0.0071 0.7180 1.1194 0.033 Uiso 1 1 calc R . . 
C4 C 0.6229(4) 0.6963(3) 0.5048(2) 0.0421(12) Uani 1 1 d . . . 
H29A H 0.6712 0.6297 0.5089 0.063 Uiso 1 1 calc R . . 
H29B H 0.6624 0.7460 0.4697 0.063 Uiso 1 1 calc R . . 
H29C H 0.5631 0.6852 0.4814 0.063 Uiso 1 1 calc R . . 
C1 C 0.4628(3) 0.4876(3) 0.7856(2) 0.0254(9) Uani 1 1 d . . . 
H31A H 0.4816 0.5163 0.8315 0.038 Uiso 1 1 calc R . . 
H31B H 0.4819 0.4112 0.7880 0.038 Uiso 1 1 calc R . . 
H31C H 0.3854 0.5078 0.7884 0.038 Uiso 1 1 calc R . . 
C2 C 0.5193(4) 0.4590(3) 0.6087(3) 0.0445(12) Uani 1 1 d . . . 
H30A H 0.4432 0.4708 0.6061 0.067 Uiso 1 1 calc R . . 
H30B H 0.5429 0.3850 0.6219 0.067 Uiso 1 1 calc R . . 
H30C H 0.5621 0.4784 0.5560 0.067 Uiso 1 1 calc R . . 
C17 C 0.6198(3) 1.1042(3) 0.7520(2) 0.0319(10) Uani 1 1 d . . . 
H33 H 0.6663 1.1503 0.7248 0.038 Uiso 1 1 calc R . . 
C18 C 0.6532(3) 1.0295(3) 0.8075(2) 0.0291(9) Uani 1 1 d . . . 
H32 H 0.7227 1.0239 0.8187 0.035 Uiso 1 1 calc R . . 
C16 C 0.5185(3) 1.1120(3) 0.7359(2) 0.0308(9) Uani 1 1 d . . . 
H34 H 0.4955 1.1636 0.6976 0.037 Uiso 1 1 calc R . . 
C23 C 0.1310(3) 1.0560(3) 1.0457(2) 0.0238(8) Uani 1 1 d . . . 
H35 H 0.0711 1.0899 1.0836 0.029 Uiso 1 1 calc R . . 
C42 C 0.2443(3) 0.2944(3) 0.7897(3) 0.0323(10) Uani 1 1 d . . . 
H37 H 0.2691 0.2239 0.7744 0.039 Uiso 1 1 calc R . . 
C41 C 0.2290(3) 0.3195(3) 0.8693(3) 0.0308(10) Uani 1 1 d . . . 
H36 H 0.2417 0.2660 0.9092 0.037 Uiso 1 1 calc R . . 
C43 C 0.2239(3) 0.3713(3) 0.7318(3) 0.0331(10) Uani 1 1 d . . . 
H38 H 0.2337 0.3540 0.6766 0.040 Uiso 1 1 calc R . . 
C50 C -0.0068(3) 0.7433(3) 0.7986(2) 0.0219(8) Uani 1 1 d . . . 
H39 H 0.0436 0.7883 0.7775 0.026 Uiso 1 1 calc R . . 
C45 C 0.0252(3) 0.6504(3) 0.8403(2) 0.0195(8) Uani 1 1 d . . . 
C46 C -0.0513(3) 0.5877(3) 0.8713(2) 0.0226(8) Uani 1 1 d . . . 
H41 H -0.0312 0.5244 0.9002 0.027 Uiso 1 1 calc R . . 
C7 C 0.2787(4) 0.6767(4) 0.5708(3) 0.0433(12) Uani 1 1 d . . . 
H42A H 0.3540 0.6851 0.5633 0.065 Uiso 1 1 calc R . . 
H42B H 0.2707 0.6364 0.5264 0.065 Uiso 1 1 calc R . . 
H42C H 0.2570 0.6397 0.6229 0.065 Uiso 1 1 calc R . . 
C9 C 0.0533(4) 0.7828(4) 0.5733(3) 0.0515(13) Uani 1 1 d . . . 
H43A H 0.0309 0.7396 0.6220 0.077 Uiso 1 1 calc R . . 
H43B H 0.0542 0.7457 0.5247 0.077 Uiso 1 1 calc R . . 
H43C H 0.0027 0.8490 0.5749 0.077 Uiso 1 1 calc R . . 
C3 C 0.6834(3) 0.5120(3) 0.6932(3) 0.0481(13) Uani 1 1 d . . . 
H44A H 0.7269 0.5300 0.6404 0.072 Uiso 1 1 calc R . . 
H44B H 0.7043 0.4376 0.7066 0.072 Uiso 1 1 calc R . . 
H44C H 0.6953 0.5538 0.7353 0.072 Uiso 1 1 calc R . . 
C48 C -0.1866(3) 0.7077(3) 0.8200(2) 0.0272(9) Uani 1 1 d . . . 
H46 H -0.2589 0.7277 0.8140 0.033 Uiso 1 1 calc R . . 
C47 C -0.1551(3) 0.6149(3) 0.8612(2) 0.0280(9) Uani 1 1 d . . . 
H47 H -0.2056 0.5701 0.8825 0.034 Uiso 1 1 calc R . . 
C49 C -0.1114(3) 0.7706(3) 0.7877(2) 0.0280(9) Uani 1 1 d . . . 
H45 H -0.1316 0.8331 0.7579 0.034 Uiso 1 1 calc R . . 
C10 C 0.2279(4) 1.0955(3) 0.6157(3) 0.0473(12) Uani 1 1 d . . . 
H48A H 0.2979 1.0824 0.6312 0.071 Uiso 1 1 calc R . . 
H48B H 0.1918 1.1670 0.6290 0.071 Uiso 1 1 calc R . . 
H48C H 0.2383 1.0868 0.5570 0.071 Uiso 1 1 calc R . . 
C11 C 0.0083(4) 1.0374(4) 0.6449(3) 0.0559(14) Uani 1 1 d . . . 
H49A H 0.0157 1.0270 0.5869 0.084 Uiso 1 1 calc R . . 
H49B H -0.0206 1.1110 0.6566 0.084 Uiso 1 1 calc R . . 
H49C H -0.0408 0.9934 0.6770 0.084 Uiso 1 1 calc R . . 
C8 C 0.2372(4) 0.8774(5) 0.4703(3) 0.0622(16) Uani 1 1 d . . . 
H50A H 0.1941 0.9476 0.4687 0.093 Uiso 1 1 calc R . . 
H50B H 0.2287 0.8372 0.4261 0.093 Uiso 1 1 calc R . . 
H50C H 0.3131 0.8831 0.4636 0.093 Uiso 1 1 calc R . . 
C51 C 0.9700(4) 0.4830(4) 0.5405(3) 0.0519(13) Uani 1 1 d . . . 
H51A H 0.9087 0.4527 0.5321 0.062 Uiso 1 1 calc R . . 
H51B H 0.9400 0.5455 0.5735 0.062 Uiso 1 1 calc R . . 
C52 C 1.0349(4) 0.4046(5) 0.5881(3) 0.0648(16) Uani 1 1 d . . . 
H52A H 1.0959 0.4351 0.5967 0.078 Uiso 1 1 calc R . . 
H52B H 1.0652 0.3423 0.5549 0.078 Uiso 1 1 calc R . . 
C53 C 0.9735(4) 0.3688(5) 0.6712(3) 0.0729(18) Uani 1 1 d . . . 
H53A H 0.9428 0.4296 0.7049 0.109 Uiso 1 1 calc R . . 
H53B H 1.0229 0.3197 0.6982 0.109 Uiso 1 1 calc R . . 
H53C H 0.9155 0.3342 0.6635 0.109 Uiso 1 1 calc R . . 
 
 
_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 
Th1 O2 2.123(2) . ? 
Th1 O1 2.131(2) . ? 
Th1 N1 2.358(3) . ? 
Th1 N2 2.367(3) . ? 
N1 Si2 1.731(3) . ? 
N1 Si1 1.733(3) . ? 
N2 Si3 1.718(3) . ? 
N2 Si4 1.727(3) . ? 
Si1 C2 1.852(4) . ? 
Si1 C1 1.862(4) . ? 
Si1 C3 1.872(4) . ? 
Si4 C12 1.862(4) . ? 
Si4 C10 1.869(4) . ? 
Si4 C11 1.878(4) . ? 
Si2 C4 1.862(4) . ? 
Si2 C5 1.871(4) . ? 
Si2 C6 1.884(4) . ? 
Si3 C9 1.868(5) . ? 
Si3 C8 1.872(4) . ? 
Si3 C7 1.889(5) . ? 
O1 C13 1.421(4) . ? 
O2 C32 1.440(4) . ? 
C39 C40 1.387(5) . ? 
C39 C44 1.392(5) . ? 
C39 C32 1.536(5) . ? 
C27 C28 1.383(5) . ? 
C27 C26 1.390(5) . ? 
C21 C20 1.385(5) . ? 
C21 C22 1.400(5) . ? 
C20 C25 1.394(5) . ? 
C20 C13 1.543(4) . ? 
C13 C14 1.540(4) . ? 
C13 C26 1.544(4) . ? 
C32 C45 1.530(5) . ? 
C32 C33 1.531(5) . ? 
C38 C37 1.387(5) . ? 
C38 C33 1.390(5) . ? 
C26 C31 1.386(5) . ? 
C30 C29 1.378(5) . ? 
C30 C31 1.394(5) . ? 
C14 C19 1.385(5) . ? 
C14 C15 1.396(5) . ? 
C33 C34 1.405(5) . ? 
C25 C24 1.379(5) . ? 
C19 C18 1.406(5) . ? 
C35 C34 1.379(5) . ? 
C35 C36 1.385(5) . ? 
C28 C29 1.380(5) . ? 
C22 C23 1.375(5) . ? 
C15 C16 1.390(5) . ? 
C36 C37 1.388(5) . ? 
C44 C43 1.399(5) . ? 
C24 C23 1.387(5) . ? 
C40 C41 1.391(5) . ? 
C17 C18 1.377(6) . ? 
C17 C16 1.382(6) . ? 
C42 C41 1.368(6) . ? 
C42 C43 1.377(6) . ? 
C50 C49 1.385(5) . ? 
C50 C45 1.395(5) . ? 
C45 C46 1.387(5) . ? 
C46 C47 1.370(5) . ? 
C48 C49 1.382(5) . ? 
C48 C47 1.389(5) . ? 
C51 C51 1.495(9) 2_766 ? 
C51 C52 1.500(7) . ? 
C52 C53 1.535(7) . ? 
 
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 
O2 Th1 O1 105.05(9) . . ? 
O2 Th1 N1 113.70(9) . . ? 
O1 Th1 N1 98.95(9) . . ? 
O2 Th1 N2 100.35(9) . . ? 
O1 Th1 N2 112.65(10) . . ? 
N1 Th1 N2 125.06(10) . . ? 
Si2 N1 Si1 120.97(17) . . ? 
Si2 N1 Th1 110.99(14) . . ? 
Si1 N1 Th1 128.02(15) . . ? 
Si3 N2 Si4 122.91(18) . . ? 
Si3 N2 Th1 112.08(15) . . ? 
Si4 N2 Th1 124.99(16) . . ? 
N1 Si1 C2 112.34(18) . . ? 
N1 Si1 C1 111.36(15) . . ? 
C2 Si1 C1 104.97(19) . . ? 
N1 Si1 C3 113.02(18) . . ? 
C2 Si1 C3 107.9(2) . . ? 
C1 Si1 C3 106.75(19) . . ? 
N2 Si4 C12 109.74(16) . . ? 
N2 Si4 C10 111.18(19) . . ? 
C12 Si4 C10 108.1(2) . . ? 
N2 Si4 C11 113.9(2) . . ? 
C12 Si4 C11 107.1(2) . . ? 
C10 Si4 C11 106.6(2) . . ? 
N1 Si2 C4 113.02(17) . . ? 
N1 Si2 C5 115.11(17) . . ? 
C4 Si2 C5 108.8(2) . . ? 
N1 Si2 C6 107.37(16) . . ? 
C4 Si2 C6 107.2(2) . . ? 
C5 Si2 C6 104.73(18) . . ? 
N2 Si3 C9 115.84(18) . . ? 
N2 Si3 C8 113.1(2) . . ? 
C9 Si3 C8 107.9(2) . . ? 
N2 Si3 C7 106.76(17) . . ? 
C9 Si3 C7 105.1(2) . . ? 
C8 Si3 C7 107.6(2) . . ? 
C13 O1 Th1 171.13(19) . . ? 
C32 O2 Th1 174.4(2) . . ? 
C40 C39 C44 118.0(3) . . ? 
C40 C39 C32 124.4(3) . . ? 
C44 C39 C32 117.6(3) . . ? 
C28 C27 C26 120.9(3) . . ? 
C20 C21 C22 120.4(3) . . ? 
C21 C20 C25 118.6(3) . . ? 
C21 C20 C13 122.3(3) . . ? 
C25 C20 C13 119.0(3) . . ? 
O1 C13 C14 108.1(3) . . ? 
O1 C13 C20 108.3(3) . . ? 
C14 C13 C20 111.7(3) . . ? 
O1 C13 C26 109.2(3) . . ? 
C14 C13 C26 110.8(3) . . ? 
C20 C13 C26 108.6(3) . . ? 
O2 C32 C45 110.7(3) . . ? 
O2 C32 C33 107.1(3) . . ? 
C45 C32 C33 112.4(3) . . ? 
O2 C32 C39 107.0(3) . . ? 
C45 C32 C39 107.5(3) . . ? 
C33 C32 C39 112.0(3) . . ? 
C37 C38 C33 121.6(3) . . ? 
C31 C26 C27 118.3(3) . . ? 
C31 C26 C13 120.5(3) . . ? 
C27 C26 C13 121.1(3) . . ? 
C29 C30 C31 120.3(3) . . ? 
C19 C14 C15 118.5(3) . . ? 
C19 C14 C13 123.0(3) . . ? 
C15 C14 C13 118.5(3) . . ? 
C38 C33 C34 117.3(3) . . ? 
C38 C33 C32 123.6(3) . . ? 
C34 C33 C32 119.1(3) . . ? 
C24 C25 C20 121.3(3) . . ? 
C14 C19 C18 120.8(3) . . ? 
C34 C35 C36 120.0(3) . . ? 
C35 C34 C33 121.6(3) . . ? 
C29 C28 C27 120.4(3) . . ? 
C23 C22 C21 119.9(3) . . ? 
C30 C29 C28 119.4(3) . . ? 
C16 C15 C14 120.6(4) . . ? 
C35 C36 C37 119.6(4) . . ? 
C26 C31 C30 120.6(3) . . ? 
C39 C44 C43 121.1(4) . . ? 
C25 C24 C23 119.6(3) . . ? 
C39 C40 C41 120.6(4) . . ? 
C38 C37 C36 119.9(3) . . ? 
C18 C17 C16 119.8(3) . . ? 
C17 C18 C19 119.9(4) . . ? 
C17 C16 C15 120.4(4) . . ? 
C22 C23 C24 120.2(3) . . ? 
C41 C42 C43 120.0(4) . . ? 
C42 C41 C40 120.7(4) . . ? 
C42 C43 C44 119.5(4) . . ? 
C49 C50 C45 120.6(3) . . ? 
C46 C45 C50 117.9(3) . . ? 
C46 C45 C32 119.9(3) . . ? 
C50 C45 C32 122.1(3) . . ? 
C47 C46 C45 121.7(3) . . ? 
C49 C48 C47 119.1(4) . . ? 
C46 C47 C48 120.2(4) . . ? 
C48 C49 C50 120.5(3) . . ? 
C51 C51 C52 115.3(5) 2_766 . ? 
C51 C52 C53 115.5(4) . . ? 
 
_diffrn_measured_fraction_theta_max    0.997 
_diffrn_reflns_theta_full              26.44 
_diffrn_measured_fraction_theta_full   0.997 
_refine_diff_density_max    1.598 
_refine_diff_density_min   -0.757 
_refine_diff_density_rms    0.110 


###END###

 
data_complex_4
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C37 H69 N3 S Si6 Th' 
_chemical_formula_weight          988.59 
 
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' 
 'Si'  'Si'   0.0817   0.0704 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'S'  'S'   0.1246   0.1234 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Th'  'Th'  -7.2400   8.8979 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            Triclinic 
_symmetry_space_group_name_H-M    P-1 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, -y, -z' 
 
_cell_length_a                    10.5938(10) 
_cell_length_b                    11.5867(11) 
_cell_length_c                    19.5950(19) 
_cell_angle_alpha                 96.883(2) 
_cell_angle_beta                  91.006(2) 
_cell_angle_gamma                 96.270(2) 
_cell_volume                      2372.5(4) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     100(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        needle 
_exptl_crystal_colour             colorless 
_exptl_crystal_size_max           0.1 
_exptl_crystal_size_mid           0.05 
_exptl_crystal_size_min           0.05 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.388 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1010 
_exptl_absorpt_coefficient_mu     3.365 
_exptl_absorpt_correction_type    'multi-scan' 
_exptl_absorpt_correction_T_min   0.4291 
_exptl_absorpt_correction_T_max   0.7456 
_exptl_absorpt_process_details    SADABS 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       100(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   ? 
_diffrn_measurement_method        ? 
_diffrn_detector_area_resol_mean  ? 
_diffrn_reflns_number             19192 
_diffrn_reflns_av_R_equivalents   0.0440 
_diffrn_reflns_av_sigmaI/netI     0.0752 
_diffrn_reflns_limit_h_min        -13 
_diffrn_reflns_limit_h_max        8 
_diffrn_reflns_limit_k_min        -14 
_diffrn_reflns_limit_k_max        14 
_diffrn_reflns_limit_l_min        -24 
_diffrn_reflns_limit_l_max        25 
_diffrn_reflns_theta_min          1.05 
_diffrn_reflns_theta_max          27.10 
_reflns_number_total              10322 
_reflns_number_gt                 8443 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 2008)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 2008)' 
_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)+(0.0283P)²+0.3959P] 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      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          10322 
_refine_ls_number_parameters      451 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0518 
_refine_ls_R_factor_gt            0.0350 
_refine_ls_wR_factor_ref          0.0750 
_refine_ls_wR_factor_gt           0.0702 
_refine_ls_goodness_of_fit_ref    0.957 
_refine_ls_restrained_S_all       0.957 
_refine_ls_shift/su_max           0.001 
_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 
Th1 Th 0.195611(15) 0.239833(13) 0.281375(9) 0.01288(5) Uani 1 1 d . . . 
S1 S 0.39587(11) 0.29123(10) 0.20240(6) 0.0234(3) Uani 1 1 d . . . 
Si1 Si 0.42167(12) 0.09023(10) 0.34477(7) 0.0198(3) Uani 1 1 d . . . 
Si2 Si 0.28713(12) 0.21431(11) 0.45951(7) 0.0205(3) Uani 1 1 d . . . 
Si3 Si -0.02498(11) 0.01418(10) 0.30633(7) 0.0170(3) Uani 1 1 d . . . 
Si4 Si 0.04366(12) 0.00257(10) 0.15852(7) 0.0195(3) Uani 1 1 d . . . 
Si5 Si 0.20452(11) 0.53388(10) 0.33737(7) 0.0181(3) Uani 1 1 d . . . 
Si6 Si -0.05263(11) 0.42808(10) 0.27731(7) 0.0185(3) Uani 1 1 d . . . 
N1 N 0.3027(3) 0.1778(3) 0.37155(18) 0.0155(8) Uani 1 1 d . . . 
N2 N 0.0594(3) 0.0753(3) 0.24158(18) 0.0157(8) Uani 1 1 d . . . 
N3 N 0.1036(3) 0.4110(3) 0.30053(18) 0.0158(8) Uani 1 1 d . . . 
C1 C 0.1798(5) 0.3324(4) 0.4784(3) 0.0282(11) Uani 1 1 d . . . 
H1A H 0.1426 0.3500 0.4352 0.042 Uiso 1 1 calc R . . 
H1B H 0.2290 0.4030 0.5018 0.042 Uiso 1 1 calc R . . 
H1C H 0.1118 0.3056 0.5080 0.042 Uiso 1 1 calc R . . 
C2 C 0.4430(5) 0.2706(4) 0.5043(3) 0.0328(12) Uani 1 1 d . . . 
H2A H 0.4990 0.2083 0.5008 0.049 Uiso 1 1 calc R . . 
H2B H 0.4292 0.2959 0.5529 0.049 Uiso 1 1 calc R . . 
H2C H 0.4825 0.3370 0.4827 0.049 Uiso 1 1 calc R . . 
C3 C 0.2169(5) 0.0883(4) 0.5036(3) 0.0296(11) Uani 1 1 d . . . 
H3A H 0.1314 0.0609 0.4842 0.044 Uiso 1 1 calc R . . 
H3B H 0.2119 0.1136 0.5530 0.044 Uiso 1 1 calc R . . 
H3C H 0.2706 0.0244 0.4967 0.044 Uiso 1 1 calc R . . 
C4 C 0.4432(5) -0.0300(4) 0.3978(3) 0.0314(12) Uani 1 1 d . . . 
H4A H 0.4674 0.0035 0.4451 0.047 Uiso 1 1 calc R . . 
H4B H 0.5102 -0.0750 0.3785 0.047 Uiso 1 1 calc R . . 
H4C H 0.3635 -0.0816 0.3975 0.047 Uiso 1 1 calc R . . 
C5 C 0.5790(4) 0.1801(4) 0.3428(3) 0.0328(12) Uani 1 1 d . . . 
H5A H 0.5723 0.2406 0.3124 0.049 Uiso 1 1 calc R . . 
H5B H 0.6429 0.1297 0.3256 0.049 Uiso 1 1 calc R . . 
H5C H 0.6042 0.2172 0.3894 0.049 Uiso 1 1 calc R . . 
C6 C 0.3799(4) 0.0120(4) 0.2569(2) 0.0238(10) Uani 1 1 d . . . 
H6A H 0.2951 -0.0313 0.2568 0.036 Uiso 1 1 calc R . . 
H6B H 0.4423 -0.0426 0.2440 0.036 Uiso 1 1 calc R . . 
H6C H 0.3804 0.0691 0.2237 0.036 Uiso 1 1 calc R . . 
C7 C 0.0606(4) -0.0957(4) 0.3459(2) 0.0240(10) Uani 1 1 d . . . 
H7A H 0.0729 -0.1608 0.3107 0.036 Uiso 1 1 calc R . . 
H7B H 0.0102 -0.1253 0.3828 0.036 Uiso 1 1 calc R . . 
H7C H 0.1435 -0.0585 0.3647 0.036 Uiso 1 1 calc R . . 
C8 C -0.0506(4) 0.1349(4) 0.3755(2) 0.0217(10) Uani 1 1 d . . . 
H8A H 0.0313 0.1793 0.3904 0.033 Uiso 1 1 calc R . . 
H8B H -0.0899 0.1015 0.4147 0.033 Uiso 1 1 calc R . . 
H8C H -0.1065 0.1870 0.3576 0.033 Uiso 1 1 calc R . . 
C9 C -0.1870(4) -0.0584(4) 0.2785(3) 0.0310(12) Uani 1 1 d . . . 
H9A H -0.2341 -0.0037 0.2567 0.047 Uiso 1 1 calc R . . 
H9B H -0.2325 -0.0817 0.3187 0.047 Uiso 1 1 calc R . . 
H9C H -0.1795 -0.1278 0.2456 0.047 Uiso 1 1 calc R . . 
C10 C 0.1598(5) 0.0721(4) 0.1010(3) 0.0376(14) Uani 1 1 d . . . 
H10A H 0.1509 0.1559 0.1037 0.056 Uiso 1 1 calc R . . 
H10B H 0.1431 0.0355 0.0536 0.056 Uiso 1 1 calc R . . 
H10C H 0.2463 0.0616 0.1157 0.056 Uiso 1 1 calc R . . 
C11 C 0.0737(4) -0.1538(3) 0.1563(2) 0.0221(10) Uani 1 1 d . . . 
H11A H 0.1590 -0.1576 0.1755 0.033 Uiso 1 1 calc R . . 
H11B H 0.0674 -0.1914 0.1087 0.033 Uiso 1 1 calc R . . 
H11C H 0.0105 -0.1944 0.1836 0.033 Uiso 1 1 calc R . . 
C12 C -0.1164(5) 0.0039(4) 0.1169(3) 0.0360(13) Uani 1 1 d . . . 
H12A H -0.1808 -0.0400 0.1419 0.054 Uiso 1 1 calc R . . 
H12B H -0.1164 -0.0323 0.0691 0.054 Uiso 1 1 calc R . . 
H12C H -0.1359 0.0849 0.1180 0.054 Uiso 1 1 calc R . . 
C13 C 0.1358(5) 0.6152(4) 0.4136(3) 0.0278(11) Uani 1 1 d . . . 
H13A H 0.0669 0.6568 0.3981 0.042 Uiso 1 1 calc R . . 
H13B H 0.2021 0.6716 0.4378 0.042 Uiso 1 1 calc R . . 
H13C H 0.1023 0.5598 0.4446 0.042 Uiso 1 1 calc R . . 
C14 C -0.0649(5) 0.5590(4) 0.2307(3) 0.0285(11) Uani 1 1 d . . . 
H14A H -0.0464 0.6305 0.2630 0.043 Uiso 1 1 calc R . . 
H14B H -0.1511 0.5556 0.2110 0.043 Uiso 1 1 calc R . . 
H14C H -0.0037 0.5592 0.1938 0.043 Uiso 1 1 calc R . . 
C15 C -0.1565(4) 0.4445(4) 0.3532(3) 0.0279(11) Uani 1 1 d . . . 
H15A H -0.1530 0.3777 0.3792 0.042 Uiso 1 1 calc R . . 
H15B H -0.2442 0.4475 0.3373 0.042 Uiso 1 1 calc R . . 
H15C H -0.1268 0.5170 0.3828 0.042 Uiso 1 1 calc R . . 
C16 C -0.1212(4) 0.2990(4) 0.2172(2) 0.0217(10) Uani 1 1 d . . . 
H16A H -0.0658 0.2875 0.1781 0.033 Uiso 1 1 calc R . . 
H16B H -0.2057 0.3123 0.2008 0.033 Uiso 1 1 calc R . . 
H16C H -0.1283 0.2292 0.2413 0.033 Uiso 1 1 calc R . . 
C17 C 0.3589(4) 0.4862(4) 0.3658(3) 0.0253(11) Uani 1 1 d . . . 
H17A H 0.3421 0.4271 0.3973 0.038 Uiso 1 1 calc R . . 
H17B H 0.4129 0.5538 0.3893 0.038 Uiso 1 1 calc R . . 
H17C H 0.4021 0.4528 0.3255 0.038 Uiso 1 1 calc R . . 
C18 C 0.2504(4) 0.6415(4) 0.2763(3) 0.0245(11) Uani 1 1 d . . . 
H18A H 0.2933 0.6033 0.2374 0.037 Uiso 1 1 calc R . . 
H18B H 0.3079 0.7067 0.2999 0.037 Uiso 1 1 calc R . . 
H18C H 0.1740 0.6713 0.2595 0.037 Uiso 1 1 calc R . . 
C19 C 0.4283(4) 0.3746(3) 0.1276(2) 0.0149(9) Uani 1 1 d . . . 
C20 C 0.5365(4) 0.3190(4) 0.0894(2) 0.0173(9) Uani 1 1 d . . . 
C21 C 0.5324(4) 0.1975(4) 0.0743(2) 0.0244(11) Uani 1 1 d . . . 
H21 H 0.4630 0.1487 0.0892 0.029 Uiso 1 1 calc R . . 
C22 C 0.6270(5) 0.1470(4) 0.0382(3) 0.0287(11) Uani 1 1 d . . . 
H22 H 0.6221 0.0643 0.0285 0.034 Uiso 1 1 calc R . . 
C23 C 0.7293(4) 0.2166(4) 0.0161(3) 0.0287(11) Uani 1 1 d . . . 
H23 H 0.7947 0.1818 -0.0087 0.034 Uiso 1 1 calc R . . 
C24 C 0.7355(4) 0.3363(4) 0.0303(2) 0.0246(11) Uani 1 1 d . . . 
H24 H 0.8054 0.3845 0.0154 0.030 Uiso 1 1 calc R . . 
C25 C 0.6395(4) 0.3867(4) 0.0664(2) 0.0199(10) Uani 1 1 d . . . 
H25 H 0.6445 0.4695 0.0755 0.024 Uiso 1 1 calc R . . 
C26 C 0.4718(4) 0.5034(4) 0.1534(2) 0.0171(9) Uani 1 1 d . . . 
C27 C 0.4357(4) 0.5926(3) 0.1181(2) 0.0190(10) Uani 1 1 d . . . 
H27 H 0.3803 0.5736 0.0787 0.023 Uiso 1 1 calc R . . 
C28 C 0.4798(4) 0.7089(4) 0.1396(3) 0.0250(11) Uani 1 1 d . . . 
H28 H 0.4540 0.7687 0.1150 0.030 Uiso 1 1 calc R . . 
C29 C 0.5601(4) 0.7375(4) 0.1960(3) 0.0314(12) Uani 1 1 d . . . 
H29 H 0.5894 0.8171 0.2109 0.038 Uiso 1 1 calc R . . 
C30 C 0.5985(4) 0.6503(4) 0.2314(3) 0.0290(12) Uani 1 1 d . . . 
H30 H 0.6552 0.6698 0.2703 0.035 Uiso 1 1 calc R . . 
C31 C 0.5540(4) 0.5343(4) 0.2100(2) 0.0233(10) Uani 1 1 d . . . 
H31 H 0.5804 0.4748 0.2346 0.028 Uiso 1 1 calc R . . 
C32 C 0.3085(4) 0.3636(3) 0.0813(2) 0.0148(9) Uani 1 1 d . . . 
C33 C 0.3074(4) 0.3259(3) 0.0115(2) 0.0174(9) Uani 1 1 d . . . 
H33 H 0.3826 0.3016 -0.0085 0.021 Uiso 1 1 calc R . . 
C34 C 0.1997(4) 0.3227(4) -0.0296(2) 0.0208(10) Uani 1 1 d . . . 
H34 H 0.2014 0.2957 -0.0773 0.025 Uiso 1 1 calc R . . 
C35 C 0.0892(4) 0.3587(4) -0.0018(2) 0.0205(10) Uani 1 1 d . . . 
H35 H 0.0149 0.3569 -0.0300 0.025 Uiso 1 1 calc R . . 
C36 C 0.0892(4) 0.3975(3) 0.0679(2) 0.0196(10) Uani 1 1 d . . . 
H36 H 0.0139 0.4224 0.0877 0.024 Uiso 1 1 calc R . . 
C37 C 0.1967(4) 0.4006(3) 0.1090(2) 0.0180(9) Uani 1 1 d . . . 
H37 H 0.1949 0.4281 0.1566 0.022 Uiso 1 1 calc R . . 
 
 
_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 
Th1 N3 2.299(3) . ? 
Th1 N2 2.308(3) . ? 
Th1 N1 2.311(4) . ? 
Th1 S1 2.7038(11) . ? 
S1 C19 1.866(4) . ? 
Si1 N1 1.751(3) . ? 
Si1 C4 1.865(5) . ? 
Si1 C6 1.869(5) . ? 
Si1 C5 1.870(5) . ? 
Si2 N1 1.740(4) . ? 
Si2 C2 1.870(5) . ? 
Si2 C3 1.877(5) . ? 
Si2 C1 1.880(5) . ? 
Si3 N2 1.740(4) . ? 
Si3 C9 1.869(5) . ? 
Si3 C7 1.872(5) . ? 
Si3 C8 1.873(4) . ? 
Si4 N2 1.737(4) . ? 
Si4 C10 1.866(5) . ? 
Si4 C11 1.869(4) . ? 
Si4 C12 1.871(5) . ? 
Si5 N3 1.756(3) . ? 
Si5 C18 1.863(5) . ? 
Si5 C13 1.870(4) . ? 
Si5 C17 1.878(5) . ? 
Si6 N3 1.747(4) . ? 
Si6 C16 1.860(4) . ? 
Si6 C15 1.869(5) . ? 
Si6 C14 1.877(5) . ? 
C1 H1A 0.9800 . ? 
C1 H1B 0.9800 . ? 
C1 H1C 0.9800 . ? 
C2 H2A 0.9800 . ? 
C2 H2B 0.9800 . ? 
C2 H2C 0.9800 . ? 
C3 H3A 0.9800 . ? 
C3 H3B 0.9800 . ? 
C3 H3C 0.9800 . ? 
C4 H4A 0.9800 . ? 
C4 H4B 0.9800 . ? 
C4 H4C 0.9800 . ? 
C5 H5A 0.9800 . ? 
C5 H5B 0.9800 . ? 
C5 H5C 0.9800 . ? 
C6 H6A 0.9800 . ? 
C6 H6B 0.9800 . ? 
C6 H6C 0.9800 . ? 
C7 H7A 0.9800 . ? 
C7 H7B 0.9800 . ? 
C7 H7C 0.9800 . ? 
C8 H8A 0.9800 . ? 
C8 H8B 0.9800 . ? 
C8 H8C 0.9800 . ? 
C9 H9A 0.9800 . ? 
C9 H9B 0.9800 . ? 
C9 H9C 0.9800 . ? 
C10 H10A 0.9800 . ? 
C10 H10B 0.9800 . ? 
C10 H10C 0.9800 . ? 
C11 H11A 0.9800 . ? 
C11 H11B 0.9800 . ? 
C11 H11C 0.9800 . ? 
C12 H12A 0.9800 . ? 
C12 H12B 0.9800 . ? 
C12 H12C 0.9800 . ? 
C13 H13A 0.9800 . ? 
C13 H13B 0.9800 . ? 
C13 H13C 0.9800 . ? 
C14 H14A 0.9800 . ? 
C14 H14B 0.9800 . ? 
C14 H14C 0.9800 . ? 
C15 H15A 0.9800 . ? 
C15 H15B 0.9800 . ? 
C15 H15C 0.9800 . ? 
C16 H16A 0.9800 . ? 
C16 H16B 0.9800 . ? 
C16 H16C 0.9800 . ? 
C17 H17A 0.9800 . ? 
C17 H17B 0.9800 . ? 
C17 H17C 0.9800 . ? 
C18 H18A 0.9800 . ? 
C18 H18B 0.9800 . ? 
C18 H18C 0.9800 . ? 
C19 C32 1.532(6) . ? 
C19 C26 1.535(5) . ? 
C19 C20 1.538(6) . ? 
C20 C25 1.388(6) . ? 
C20 C21 1.399(6) . ? 
C21 C22 1.378(6) . ? 
C21 H21 0.9500 . ? 
C22 C23 1.386(7) . ? 
C22 H22 0.9500 . ? 
C23 C24 1.376(6) . ? 
C23 H23 0.9500 . ? 
C24 C25 1.390(6) . ? 
C24 H24 0.9500 . ? 
C25 H25 0.9500 . ? 
C26 C31 1.384(6) . ? 
C26 C27 1.394(6) . ? 
C27 C28 1.390(6) . ? 
C27 H27 0.9500 . ? 
C28 C29 1.369(7) . ? 
C28 H28 0.9500 . ? 
C29 C30 1.384(7) . ? 
C29 H29 0.9500 . ? 
C30 C31 1.387(6) . ? 
C30 H30 0.9500 . ? 
C31 H31 0.9500 . ? 
C32 C33 1.384(6) . ? 
C32 C37 1.399(6) . ? 
C33 C34 1.380(6) . ? 
C33 H33 0.9500 . ? 
C34 C35 1.384(6) . ? 
C34 H34 0.9500 . ? 
C35 C36 1.386(6) . ? 
C35 H35 0.9500 . ? 
C36 C37 1.378(6) . ? 
C36 H36 0.9500 . ? 
C37 H37 0.9500 . ? 
 
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 
N3 Th1 N2 115.58(12) . . ? 
N3 Th1 N1 118.77(12) . . ? 
N2 Th1 N1 102.19(12) . . ? 
N3 Th1 S1 104.57(9) . . ? 
N2 Th1 S1 116.27(9) . . ? 
N1 Th1 S1 98.81(9) . . ? 
C19 S1 Th1 136.72(14) . . ? 
N1 Si1 C4 115.2(2) . . ? 
N1 Si1 C6 109.81(19) . . ? 
C4 Si1 C6 103.8(2) . . ? 
N1 Si1 C5 111.14(19) . . ? 
C4 Si1 C5 107.5(2) . . ? 
C6 Si1 C5 109.0(2) . . ? 
N1 Si2 C2 112.1(2) . . ? 
N1 Si2 C3 113.2(2) . . ? 
C2 Si2 C3 107.1(2) . . ? 
N1 Si2 C1 111.8(2) . . ? 
C2 Si2 C1 106.4(2) . . ? 
C3 Si2 C1 105.7(2) . . ? 
N2 Si3 C9 114.3(2) . . ? 
N2 Si3 C7 112.95(19) . . ? 
C9 Si3 C7 107.2(2) . . ? 
N2 Si3 C8 108.16(18) . . ? 
C9 Si3 C8 105.7(2) . . ? 
C7 Si3 C8 108.2(2) . . ? 
N2 Si4 C10 110.8(2) . . ? 
N2 Si4 C11 111.53(19) . . ? 
C10 Si4 C11 107.3(2) . . ? 
N2 Si4 C12 113.8(2) . . ? 
C10 Si4 C12 105.7(3) . . ? 
C11 Si4 C12 107.4(2) . . ? 
N3 Si5 C18 113.8(2) . . ? 
N3 Si5 C13 113.10(19) . . ? 
C18 Si5 C13 107.2(2) . . ? 
N3 Si5 C17 109.40(19) . . ? 
C18 Si5 C17 104.7(2) . . ? 
C13 Si5 C17 108.1(2) . . ? 
N3 Si6 C16 109.68(18) . . ? 
N3 Si6 C15 112.5(2) . . ? 
C16 Si6 C15 108.6(2) . . ? 
N3 Si6 C14 113.06(19) . . ? 
C16 Si6 C14 106.0(2) . . ? 
C15 Si6 C14 106.6(2) . . ? 
Si2 N1 Si1 117.8(2) . . ? 
Si2 N1 Th1 128.78(18) . . ? 
Si1 N1 Th1 113.25(18) . . ? 
Si4 N2 Si3 118.56(19) . . ? 
Si4 N2 Th1 127.76(18) . . ? 
Si3 N2 Th1 113.43(17) . . ? 
Si6 N3 Si5 119.11(19) . . ? 
Si6 N3 Th1 125.24(17) . . ? 
Si5 N3 Th1 115.55(18) . . ? 
Si2 C1 H1A 109.5 . . ? 
Si2 C1 H1B 109.5 . . ? 
H1A C1 H1B 109.5 . . ? 
Si2 C1 H1C 109.5 . . ? 
H1A C1 H1C 109.5 . . ? 
H1B C1 H1C 109.5 . . ? 
Si2 C2 H2A 109.5 . . ? 
Si2 C2 H2B 109.5 . . ? 
H2A C2 H2B 109.5 . . ? 
Si2 C2 H2C 109.5 . . ? 
H2A C2 H2C 109.5 . . ? 
H2B C2 H2C 109.5 . . ? 
Si2 C3 H3A 109.5 . . ? 
Si2 C3 H3B 109.5 . . ? 
H3A C3 H3B 109.5 . . ? 
Si2 C3 H3C 109.5 . . ? 
H3A C3 H3C 109.5 . . ? 
H3B C3 H3C 109.5 . . ? 
Si1 C4 H4A 109.5 . . ? 
Si1 C4 H4B 109.5 . . ? 
H4A C4 H4B 109.5 . . ? 
Si1 C4 H4C 109.5 . . ? 
H4A C4 H4C 109.5 . . ? 
H4B C4 H4C 109.5 . . ? 
Si1 C5 H5A 109.5 . . ? 
Si1 C5 H5B 109.5 . . ? 
H5A C5 H5B 109.5 . . ? 
Si1 C5 H5C 109.5 . . ? 
H5A C5 H5C 109.5 . . ? 
H5B C5 H5C 109.5 . . ? 
Si1 C6 H6A 109.5 . . ? 
Si1 C6 H6B 109.5 . . ? 
H6A C6 H6B 109.5 . . ? 
Si1 C6 H6C 109.5 . . ? 
H6A C6 H6C 109.5 . . ? 
H6B C6 H6C 109.5 . . ? 
Si3 C7 H7A 109.5 . . ? 
Si3 C7 H7B 109.5 . . ? 
H7A C7 H7B 109.5 . . ? 
Si3 C7 H7C 109.5 . . ? 
H7A C7 H7C 109.5 . . ? 
H7B C7 H7C 109.5 . . ? 
Si3 C8 H8A 109.5 . . ? 
Si3 C8 H8B 109.5 . . ? 
H8A C8 H8B 109.5 . . ? 
Si3 C8 H8C 109.5 . . ? 
H8A C8 H8C 109.5 . . ? 
H8B C8 H8C 109.5 . . ? 
Si3 C9 H9A 109.5 . . ? 
Si3 C9 H9B 109.5 . . ? 
H9A C9 H9B 109.5 . . ? 
Si3 C9 H9C 109.5 . . ? 
H9A C9 H9C 109.5 . . ? 
H9B C9 H9C 109.5 . . ? 
Si4 C10 H10A 109.5 . . ? 
Si4 C10 H10B 109.5 . . ? 
H10A C10 H10B 109.5 . . ? 
Si4 C10 H10C 109.5 . . ? 
H10A C10 H10C 109.5 . . ? 
H10B C10 H10C 109.5 . . ? 
Si4 C11 H11A 109.5 . . ? 
Si4 C11 H11B 109.5 . . ? 
H11A C11 H11B 109.5 . . ? 
Si4 C11 H11C 109.5 . . ? 
H11A C11 H11C 109.5 . . ? 
H11B C11 H11C 109.5 . . ? 
Si4 C12 H12A 109.5 . . ? 
Si4 C12 H12B 109.5 . . ? 
H12A C12 H12B 109.5 . . ? 
Si4 C12 H12C 109.5 . . ? 
H12A C12 H12C 109.5 . . ? 
H12B C12 H12C 109.5 . . ? 
Si5 C13 H13A 109.5 . . ? 
Si5 C13 H13B 109.5 . . ? 
H13A C13 H13B 109.5 . . ? 
Si5 C13 H13C 109.5 . . ? 
H13A C13 H13C 109.5 . . ? 
H13B C13 H13C 109.5 . . ? 
Si6 C14 H14A 109.5 . . ? 
Si6 C14 H14B 109.5 . . ? 
H14A C14 H14B 109.5 . . ? 
Si6 C14 H14C 109.5 . . ? 
H14A C14 H14C 109.5 . . ? 
H14B C14 H14C 109.5 . . ? 
Si6 C15 H15A 109.5 . . ? 
Si6 C15 H15B 109.5 . . ? 
H15A C15 H15B 109.5 . . ? 
Si6 C15 H15C 109.5 . . ? 
H15A C15 H15C 109.5 . . ? 
H15B C15 H15C 109.5 . . ? 
Si6 C16 H16A 109.5 . . ? 
Si6 C16 H16B 109.5 . . ? 
H16A C16 H16B 109.5 . . ? 
Si6 C16 H16C 109.5 . . ? 
H16A C16 H16C 109.5 . . ? 
H16B C16 H16C 109.5 . . ? 
Si5 C17 H17A 109.5 . . ? 
Si5 C17 H17B 109.5 . . ? 
H17A C17 H17B 109.5 . . ? 
Si5 C17 H17C 109.5 . . ? 
H17A C17 H17C 109.5 . . ? 
H17B C17 H17C 109.5 . . ? 
Si5 C18 H18A 109.5 . . ? 
Si5 C18 H18B 109.5 . . ? 
H18A C18 H18B 109.5 . . ? 
Si5 C18 H18C 109.5 . . ? 
H18A C18 H18C 109.5 . . ? 
H18B C18 H18C 109.5 . . ? 
C32 C19 C26 110.7(3) . . ? 
C32 C19 C20 111.1(4) . . ? 
C26 C19 C20 109.8(3) . . ? 
C32 C19 S1 109.7(3) . . ? 
C26 C19 S1 109.7(3) . . ? 
C20 C19 S1 105.7(3) . . ? 
C25 C20 C21 117.2(4) . . ? 
C25 C20 C19 121.7(4) . . ? 
C21 C20 C19 121.1(4) . . ? 
C22 C21 C20 121.5(4) . . ? 
C22 C21 H21 119.3 . . ? 
C20 C21 H21 119.3 . . ? 
C21 C22 C23 120.2(4) . . ? 
C21 C22 H22 119.9 . . ? 
C23 C22 H22 119.9 . . ? 
C24 C23 C22 119.5(4) . . ? 
C24 C23 H23 120.2 . . ? 
C22 C23 H23 120.2 . . ? 
C23 C24 C25 120.0(4) . . ? 
C23 C24 H24 120.0 . . ? 
C25 C24 H24 120.0 . . ? 
C20 C25 C24 121.6(4) . . ? 
C20 C25 H25 119.2 . . ? 
C24 C25 H25 119.2 . . ? 
C31 C26 C27 117.9(4) . . ? 
C31 C26 C19 121.2(4) . . ? 
C27 C26 C19 120.8(4) . . ? 
C28 C27 C26 120.9(4) . . ? 
C28 C27 H27 119.6 . . ? 
C26 C27 H27 119.6 . . ? 
C29 C28 C27 120.2(5) . . ? 
C29 C28 H28 119.9 . . ? 
C27 C28 H28 119.9 . . ? 
C28 C29 C30 120.0(4) . . ? 
C28 C29 H29 120.0 . . ? 
C30 C29 H29 120.0 . . ? 
C29 C30 C31 119.7(5) . . ? 
C29 C30 H30 120.2 . . ? 
C31 C30 H30 120.2 . . ? 
C26 C31 C30 121.4(5) . . ? 
C26 C31 H31 119.3 . . ? 
C30 C31 H31 119.3 . . ? 
C33 C32 C37 117.7(4) . . ? 
C33 C32 C19 122.9(4) . . ? 
C37 C32 C19 119.3(4) . . ? 
C34 C33 C32 121.6(4) . . ? 
C34 C33 H33 119.2 . . ? 
C32 C33 H33 119.2 . . ? 
C33 C34 C35 120.4(4) . . ? 
C33 C34 H34 119.8 . . ? 
C35 C34 H34 119.8 . . ? 
C34 C35 C36 118.6(4) . . ? 
C34 C35 H35 120.7 . . ? 
C36 C35 H35 120.7 . . ? 
C37 C36 C35 121.0(4) . . ? 
C37 C36 H36 119.5 . . ? 
C35 C36 H36 119.5 . . ? 
C36 C37 C32 120.7(4) . . ? 
C36 C37 H37 119.7 . . ? 
C32 C37 H37 119.7 . . ? 
 
_diffrn_measured_fraction_theta_max    0.986 
_diffrn_reflns_theta_full              27.10 
_diffrn_measured_fraction_theta_full   0.986 
_refine_diff_density_max    1.992 
_refine_diff_density_min   -1.407 
_refine_diff_density_rms    0.145 


###END###

 
data_complex_6 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C32 H83 K N3 O7.50 Si6 Th' 
_chemical_formula_weight          1069.69 
 
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' 
 'Si'  'Si'   0.0817   0.0704 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'K'  'K'   0.2009   0.2494 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Th'  'Th'  -7.2400   8.8979 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            Orthorhombic 
_symmetry_space_group_name_H-M    Pbca 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 'x+1/2, -y+1/2, -z' 
 '-x, y+1/2, -z+1/2' 
 '-x+1/2, -y, z+1/2' 
 '-x, -y, -z' 
 '-x-1/2, y-1/2, z' 
 'x, -y-1/2, z-1/2' 
 'x-1/2, y, -z-1/2' 
 
_cell_length_a                    20.457(3) 
_cell_length_b                    20.307(3) 
_cell_length_c                    25.358(3) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      10534(2) 
_cell_formula_units_Z             8 
_cell_measurement_temperature     105(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        block 
_exptl_crystal_colour             colorless 
_exptl_crystal_size_max           0.1 
_exptl_crystal_size_mid           0.1 
_exptl_crystal_size_min           0.1 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.349 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              4392 
_exptl_absorpt_coefficient_mu     3.086 
_exptl_absorpt_correction_type    'multi-scan' 
_exptl_absorpt_correction_T_min   0.6265 
_exptl_absorpt_correction_T_max   0.7457 
_exptl_absorpt_process_details    SADABS 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       105(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   ? 
_diffrn_measurement_method        ? 
_diffrn_detector_area_resol_mean  ? 
_diffrn_reflns_number             51408 
_diffrn_reflns_av_R_equivalents   0.1158 
_diffrn_reflns_av_sigmaI/netI     0.1018 
_diffrn_reflns_limit_h_min        -18 
_diffrn_reflns_limit_h_max        27 
_diffrn_reflns_limit_k_min        -25 
_diffrn_reflns_limit_k_max        27 
_diffrn_reflns_limit_l_min        -34 
_diffrn_reflns_limit_l_max        32 
_diffrn_reflns_theta_min          1.61 
_diffrn_reflns_theta_max          28.80 
_reflns_number_total              13650 
_reflns_number_gt                 9004 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 2008)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 2008)' 
_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)+(0.0001P)²+257.5260P] 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      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          13650 
_refine_ls_number_parameters      472 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.1507 
_refine_ls_R_factor_gt            0.1001 
_refine_ls_wR_factor_ref          0.2046 
_refine_ls_wR_factor_gt           0.1885 
_refine_ls_goodness_of_fit_ref    1.207 
_refine_ls_restrained_S_all       1.207 
_refine_ls_shift/su_max           0.001 
_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 
Th1 Th 0.09861(2) 0.899359(19) 0.329974(16) 0.02294(11) Uani 1 1 d . . . 
O1 O 0.1754(3) 0.9025(4) 0.3776(3) 0.0243(16) Uani 1 1 d . . . 
N2 N 0.1420(4) 0.8415(4) 0.2540(3) 0.0191(19) Uani 1 1 d . . . 
N1 N 0.0197(4) 0.8383(5) 0.3813(4) 0.021(2) Uani 1 1 d . . . 
Si4 Si 0.19655(16) 0.78035(16) 0.26775(12) 0.0223(6) Uani 1 1 d . . . 
Si2 Si -0.03334(15) 0.78584(16) 0.35140(12) 0.0211(6) Uani 1 1 d . . . 
Si3 Si 0.12678(16) 0.86830(19) 0.19147(13) 0.0288(7) Uani 1 1 d . . . 
Si1 Si 0.02493(17) 0.8484(2) 0.44850(13) 0.0308(8) Uani 1 1 d . . . 
K1 K 0.26986(12) 0.93369(13) 0.44432(10) 0.0274(5) Uani 1 1 d . . . 
N3 N 0.0736(5) 1.0147(5) 0.3175(4) 0.027(2) Uani 1 1 d . . . 
Si5 Si -0.00372(16) 1.04562(16) 0.31643(12) 0.0254(7) Uani 1 1 d . . . 
Si6 Si 0.14099(19) 1.06419(19) 0.3162(2) 0.0567(15) Uani 1 1 d . . . 
O3 O 0.2488(4) 1.0198(5) 0.5378(3) 0.036(2) Uani 1 1 d . . . 
O6 O 0.3615(4) 0.8581(5) 0.3911(3) 0.034(2) Uani 1 1 d . . . 
O5 O 0.3125(5) 0.8066(4) 0.4864(3) 0.038(2) Uani 1 1 d . . . 
O2 O 0.3129(5) 1.0709(5) 0.4526(4) 0.040(2) Uani 1 1 d . . . 
O4 O 0.2319(5) 0.8848(5) 0.5478(4) 0.053(3) Uani 1 1 d . . . 
O7 O 0.3792(6) 0.9913(5) 0.3848(4) 0.054(3) Uani 1 1 d . . . 
C1 C -0.0535(7) 0.8367(9) 0.4841(5) 0.052(4) Uani 1 1 d . . . 
H1A H -0.0822 0.8744 0.4774 0.077 Uiso 1 1 calc R . . 
H1B H -0.0450 0.8333 0.5220 0.077 Uiso 1 1 calc R . . 
H1C H -0.0747 0.7963 0.4717 0.077 Uiso 1 1 calc R . . 
C2 C 0.0527(7) 0.9340(8) 0.4639(5) 0.046(4) Uani 1 1 d . . . 
H2A H 0.0834 0.9329 0.4935 0.069 Uiso 1 1 calc R . . 
H2B H 0.0148 0.9611 0.4734 0.069 Uiso 1 1 calc R . . 
H2C H 0.0744 0.9529 0.4329 0.069 Uiso 1 1 calc R . . 
C3 C 0.0864(10) 0.7908(10) 0.4775(6) 0.079(7) Uani 1 1 d . . . 
H3A H 0.0705 0.7454 0.4745 0.119 Uiso 1 1 calc R . . 
H3B H 0.0930 0.8015 0.5148 0.119 Uiso 1 1 calc R . . 
H3C H 0.1279 0.7951 0.4586 0.119 Uiso 1 1 calc R . . 
C5 C -0.0208(7) 0.6985(7) 0.3731(5) 0.036(3) Uani 1 1 d . . . 
H5A H 0.0251 0.6861 0.3677 0.054 Uiso 1 1 calc R . . 
H5B H -0.0490 0.6694 0.3524 0.054 Uiso 1 1 calc R . . 
H5C H -0.0318 0.6944 0.4106 0.054 Uiso 1 1 calc R . . 
C4 C -0.0192(6) 0.7897(6) 0.2787(4) 0.028(3) Uani 1 1 d . . . 
H4A H -0.0298 0.8340 0.2659 0.042 Uiso 1 1 calc R . . 
H4B H -0.0470 0.7573 0.2610 0.042 Uiso 1 1 calc R . . 
H4C H 0.0268 0.7800 0.2712 0.042 Uiso 1 1 calc R . . 
C6 C -0.1226(6) 0.8043(7) 0.3619(5) 0.036(3) Uani 1 1 d . . . 
H6A H -0.1333 0.7991 0.3993 0.054 Uiso 1 1 calc R . . 
H6B H -0.1491 0.7738 0.3409 0.054 Uiso 1 1 calc R . . 
H6C H -0.1318 0.8497 0.3510 0.054 Uiso 1 1 calc R . . 
C7 C 0.2039(6) 0.8981(9) 0.1519(5) 0.047(3) Uani 1 1 d . . . 
H7A H 0.2297 0.9280 0.1740 0.070 Uiso 1 1 calc R . . 
H7B H 0.1898 0.9211 0.1199 0.070 Uiso 1 1 calc R . . 
H7C H 0.2306 0.8599 0.1422 0.070 Uiso 1 1 calc R . . 
C8 C 0.0705(7) 0.9405(9) 0.1939(5) 0.047(3) Uani 1 1 d . . . 
H8A H 0.0286 0.9271 0.2093 0.070 Uiso 1 1 calc R . . 
H8B H 0.0633 0.9572 0.1581 0.070 Uiso 1 1 calc R . . 
H8C H 0.0900 0.9753 0.2157 0.070 Uiso 1 1 calc R . . 
C9 C 0.0847(7) 0.8059(8) 0.1477(5) 0.049(4) Uani 1 1 d . . . 
H9A H 0.1154 0.7704 0.1391 0.073 Uiso 1 1 calc R . . 
H9B H 0.0702 0.8274 0.1152 0.073 Uiso 1 1 calc R . . 
H9C H 0.0468 0.7875 0.1662 0.073 Uiso 1 1 calc R . . 
C12 C 0.1730(7) 0.7394(6) 0.3302(5) 0.037(3) Uani 1 1 d . . . 
H12A H 0.1645 0.7728 0.3572 0.055 Uiso 1 1 calc R . . 
H12B H 0.2086 0.7106 0.3419 0.055 Uiso 1 1 calc R . . 
H12C H 0.1334 0.7131 0.3245 0.055 Uiso 1 1 calc R . . 
C11 C 0.2808(6) 0.8138(7) 0.2761(5) 0.032(3) Uani 1 1 d . . . 
H11A H 0.2924 0.8403 0.2452 0.048 Uiso 1 1 calc R . . 
H11B H 0.3118 0.7773 0.2797 0.048 Uiso 1 1 calc R . . 
H11C H 0.2824 0.8414 0.3078 0.048 Uiso 1 1 calc R . . 
C10 C 0.1994(9) 0.7128(7) 0.2169(6) 0.054(4) Uani 1 1 d . . . 
H10A H 0.1562 0.6925 0.2138 0.080 Uiso 1 1 calc R . . 
H10B H 0.2314 0.6795 0.2276 0.080 Uiso 1 1 calc R . . 
H10C H 0.2123 0.7314 0.1827 0.080 Uiso 1 1 calc R . . 
C15 C -0.0224(9) 1.1043(8) 0.3720(6) 0.057(5) Uani 1 1 d . . . 
H15A H -0.0200 1.0808 0.4057 0.086 Uiso 1 1 calc R . . 
H15B H -0.0664 1.1224 0.3674 0.086 Uiso 1 1 calc R . . 
H15C H 0.0096 1.1403 0.3719 0.086 Uiso 1 1 calc R . . 
C14 C -0.0253(6) 1.0909(6) 0.2546(5) 0.034(3) Uani 1 1 d . . . 
H14A H -0.0037 1.1340 0.2545 0.050 Uiso 1 1 calc R . . 
H14B H -0.0728 1.0970 0.2529 0.050 Uiso 1 1 calc R . . 
H14C H -0.0107 1.0654 0.2240 0.050 Uiso 1 1 calc R . . 
C13 C -0.0636(6) 0.9755(7) 0.3216(5) 0.038(3) Uani 1 1 d . . . 
H13A H -0.0549 0.9434 0.2936 0.057 Uiso 1 1 calc R . . 
H13B H -0.1082 0.9924 0.3180 0.057 Uiso 1 1 calc R . . 
H13C H -0.0588 0.9540 0.3560 0.057 Uiso 1 1 calc R . . 
C17 C 0.2120(6) 1.0207(8) 0.2861(6) 0.043(4) Uani 1 1 d . . . 
H17A H 0.2236 0.9825 0.3079 0.065 Uiso 1 1 calc R . . 
H17B H 0.2493 1.0508 0.2841 0.065 Uiso 1 1 calc R . . 
H17C H 0.2004 1.0058 0.2506 0.065 Uiso 1 1 calc R . . 
C16 C 0.1281(9) 1.1416(10) 0.2797(12) 0.125(12) Uani 1 1 d . . . 
H16A H 0.1275 1.1325 0.2418 0.187 Uiso 1 1 calc R . . 
H16B H 0.1636 1.1724 0.2878 0.187 Uiso 1 1 calc R . . 
H16C H 0.0862 1.1611 0.2902 0.187 Uiso 1 1 calc R . . 
C18 C 0.1663(9) 1.0895(12) 0.3848(10) 0.116(11) Uani 1 1 d . . . 
H18A H 0.1280 1.1053 0.4042 0.174 Uiso 1 1 calc R . . 
H18B H 0.1989 1.1249 0.3825 0.174 Uiso 1 1 calc R . . 
H18C H 0.1853 1.0516 0.4032 0.174 Uiso 1 1 calc R . . 
C27 C 0.4101(6) 0.8859(7) 0.3578(5) 0.041(3) Uani 1 1 d . . . 
H27A H 0.4185 0.8563 0.3275 0.049 Uiso 1 1 calc R . . 
H27B H 0.4514 0.8914 0.3776 0.049 Uiso 1 1 calc R . . 
C30 C 0.3689(7) 1.0923(6) 0.4250(5) 0.040(3) Uani 1 1 d . . . 
H30A H 0.4080 1.0866 0.4475 0.048 Uiso 1 1 calc R . . 
H30B H 0.3646 1.1398 0.4167 0.048 Uiso 1 1 calc R . . 
C26 C 0.3781(7) 0.7943(7) 0.4096(6) 0.046(4) Uani 1 1 d . . . 
H26A H 0.4180 0.7967 0.4316 0.055 Uiso 1 1 calc R . . 
H26B H 0.3872 0.7649 0.3792 0.055 Uiso 1 1 calc R . . 
C28 C 0.3861(6) 0.9522(7) 0.3382(5) 0.041(3) Uani 1 1 d . . . 
H28A H 0.4181 0.9721 0.3137 0.049 Uiso 1 1 calc R . . 
H28B H 0.3436 0.9476 0.3199 0.049 Uiso 1 1 calc R . . 
C21 C 0.1974(7) 0.9936(10) 0.5683(6) 0.058(5) Uani 1 1 d . . . 
H21A H 0.1582 0.9870 0.5461 0.069 Uiso 1 1 calc R . . 
H21B H 0.1860 1.0244 0.5972 0.069 Uiso 1 1 calc R . . 
C24 C 0.2673(9) 0.7804(8) 0.5200(7) 0.062(5) Uani 1 1 d . . . 
H24A H 0.2818 0.7363 0.5319 0.074 Uiso 1 1 calc R . . 
H24B H 0.2249 0.7755 0.5016 0.074 Uiso 1 1 calc R . . 
C25 C 0.3238(8) 0.7674(7) 0.4408(6) 0.046(4) Uani 1 1 d . . . 
H25A H 0.2837 0.7662 0.4190 0.055 Uiso 1 1 calc R . . 
H25B H 0.3342 0.7218 0.4517 0.055 Uiso 1 1 calc R . . 
C20 C 0.2373(8) 1.0861(8) 0.5203(6) 0.055(5) Uani 1 1 d . . . 
H20A H 0.2243 1.1142 0.5505 0.066 Uiso 1 1 calc R . . 
H20B H 0.2017 1.0870 0.4938 0.066 Uiso 1 1 calc R . . 
C29 C 0.3769(9) 1.0557(8) 0.3772(7) 0.057(5) Uani 1 1 d . . . 
H29A H 0.3401 1.0659 0.3532 0.068 Uiso 1 1 calc R . . 
H29B H 0.4177 1.0700 0.3596 0.068 Uiso 1 1 calc R . . 
C19 C 0.2990(9) 1.1108(7) 0.4967(6) 0.052(4) Uani 1 1 d . . . 
H19A H 0.2940 1.1573 0.4857 0.063 Uiso 1 1 calc R . . 
H19B H 0.3350 1.1081 0.5227 0.063 Uiso 1 1 calc R . . 
C22 C 0.2195(9) 0.9300(9) 0.5904(6) 0.064(5) Uani 1 1 d . . . 
H22A H 0.2598 0.9365 0.6113 0.077 Uiso 1 1 calc R . . 
H22B H 0.1854 0.9118 0.6139 0.077 Uiso 1 1 calc R . . 
C23 C 0.2597(11) 0.8249(9) 0.5662(7) 0.071(6) Uani 1 1 d . . . 
H23A H 0.2307 0.8044 0.5928 0.086 Uiso 1 1 calc R . . 
H23B H 0.3027 0.8333 0.5827 0.086 Uiso 1 1 calc R . . 
O8 O 0.5000 1.0000 0.5000 0.062(5) Uani 1 2 d S . . 
C31 C 0.4115(11) 0.9424(10) 0.5412(12) 0.104(10) Uani 1 1 d . . . 
C32 C 0.4533(15) 0.9403(16) 0.5084(12) 0.042(5) Uani 0.50 1 d P . . 
C33 C 0.4653(14) 1.0014(16) 0.5353(12) 0.042(5) Uani 0.50 1 d P . . 
 
 
_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 
Th1 O1 1.983(7) . ? 
Th1 N1 2.416(9) . ? 
Th1 N3 2.418(10) . ? 
Th1 N2 2.424(8) . ? 
O1 K1 2.645(7) . ? 
N2 Si4 1.705(10) . ? 
N2 Si3 1.706(10) . ? 
N1 Si2 1.699(10) . ? 
N1 Si1 1.720(10) . ? 
Si4 C12 1.853(14) . ? 
Si4 C11 1.865(12) . ? 
Si4 C10 1.884(14) . ? 
Si2 C4 1.867(12) . ? 
Si2 C5 1.874(13) . ? 
Si2 C6 1.883(12) . ? 
Si3 C8 1.866(15) . ? 
Si3 C9 1.891(15) . ? 
Si3 C7 1.965(13) . ? 
Si1 C1 1.857(14) . ? 
Si1 C3 1.869(15) . ? 
Si1 C2 1.871(16) . ? 
K1 O6 2.775(9) . ? 
K1 O4 2.911(10) . ? 
K1 O5 2.925(9) . ? 
K1 O2 2.929(10) . ? 
K1 O7 2.942(10) . ? 
K1 O3 2.976(9) . ? 
N3 Si5 1.703(10) . ? 
N3 Si6 1.706(11) . ? 
Si5 C14 1.870(13) . ? 
Si5 C13 1.883(14) . ? 
Si5 C15 1.885(15) . ? 
Si6 C16 1.842(18) . ? 
Si6 C17 1.863(16) . ? 
Si6 C18 1.89(2) . ? 
O3 C21 1.410(17) . ? 
O3 C20 1.438(17) . ? 
O6 C26 1.419(17) . ? 
O6 C27 1.420(16) . ? 
O5 C24 1.366(17) . ? 
O5 C25 1.422(17) . ? 
O2 C30 1.410(16) . ? 
O2 C19 1.411(16) . ? 
O4 C23 1.42(2) . ? 
O4 C22 1.439(18) . ? 
O7 C29 1.322(19) . ? 
O7 C28 1.430(16) . ? 
C27 C28 1.52(2) . ? 
C30 C29 1.43(2) . ? 
C26 C25 1.47(2) . ? 
C21 C22 1.48(3) . ? 
C24 C23 1.49(2) . ? 
C20 C19 1.48(2) . ? 
O8 C33 1.14(3) 5_676 ? 
O8 C33 1.14(3) . ? 
O8 C32 1.56(3) 5_676 ? 
O8 C32 1.56(3) . ? 
C31 C32 1.19(4) . ? 
C31 C33 1.63(4) . ? 
 
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 
O1 Th1 N1 102.5(3) . . ? 
O1 Th1 N3 102.5(3) . . ? 
N1 Th1 N3 115.3(3) . . ? 
O1 Th1 N2 102.1(3) . . ? 
N1 Th1 N2 115.1(3) . . ? 
N3 Th1 N2 116.3(3) . . ? 
Th1 O1 K1 167.5(4) . . ? 
Si4 N2 Si3 122.8(5) . . ? 
Si4 N2 Th1 115.5(5) . . ? 
Si3 N2 Th1 121.1(5) . . ? 
Si2 N1 Si1 123.8(6) . . ? 
Si2 N1 Th1 120.6(5) . . ? 
Si1 N1 Th1 115.5(5) . . ? 
N2 Si4 C12 109.3(5) . . ? 
N2 Si4 C11 111.2(5) . . ? 
C12 Si4 C11 107.9(6) . . ? 
N2 Si4 C10 114.3(6) . . ? 
C12 Si4 C10 105.5(7) . . ? 
C11 Si4 C10 108.3(7) . . ? 
N1 Si2 C4 108.3(5) . . ? 
N1 Si2 C5 112.0(6) . . ? 
C4 Si2 C5 108.0(6) . . ? 
N1 Si2 C6 115.6(5) . . ? 
C4 Si2 C6 106.4(6) . . ? 
C5 Si2 C6 106.3(6) . . ? 
N2 Si3 C8 109.4(5) . . ? 
N2 Si3 C9 114.5(6) . . ? 
C8 Si3 C9 105.4(7) . . ? 
N2 Si3 C7 115.2(5) . . ? 
C8 Si3 C7 105.7(7) . . ? 
C9 Si3 C7 105.8(7) . . ? 
N1 Si1 C1 114.4(6) . . ? 
N1 Si1 C3 110.9(6) . . ? 
C1 Si1 C3 108.1(9) . . ? 
N1 Si1 C2 109.7(6) . . ? 
C1 Si1 C2 106.2(7) . . ? 
C3 Si1 C2 107.2(9) . . ? 
O1 K1 O6 92.9(3) . . ? 
O1 K1 O4 107.4(3) . . ? 
O6 K1 O4 115.5(3) . . ? 
O1 K1 O5 103.9(3) . . ? 
O6 K1 O5 59.2(3) . . ? 
O4 K1 O5 56.6(3) . . ? 
O1 K1 O2 119.5(3) . . ? 
O6 K1 O2 111.0(3) . . ? 
O4 K1 O2 109.9(3) . . ? 
O5 K1 O2 136.3(3) . . ? 
O1 K1 O7 108.8(3) . . ? 
O6 K1 O7 57.1(3) . . ? 
O4 K1 O7 143.2(3) . . ? 
O5 K1 O7 108.1(3) . . ? 
O2 K1 O7 55.2(3) . . ? 
O1 K1 O3 123.0(3) . . ? 
O6 K1 O3 144.1(3) . . ? 
O4 K1 O3 56.2(3) . . ? 
O5 K1 O3 105.7(3) . . ? 
O2 K1 O3 55.1(3) . . ? 
O7 K1 O3 106.6(3) . . ? 
Si5 N3 Si6 122.2(6) . . ? 
Si5 N3 Th1 123.7(5) . . ? 
Si6 N3 Th1 113.7(5) . . ? 
N3 Si5 C14 114.4(6) . . ? 
N3 Si5 C13 108.9(5) . . ? 
C14 Si5 C13 106.1(6) . . ? 
N3 Si5 C15 114.2(6) . . ? 
C14 Si5 C15 105.6(6) . . ? 
C13 Si5 C15 107.1(8) . . ? 
N3 Si6 C16 113.3(7) . . ? 
N3 Si6 C17 111.0(6) . . ? 
C16 Si6 C17 108.1(10) . . ? 
N3 Si6 C18 111.4(9) . . ? 
C16 Si6 C18 105.6(13) . . ? 
C17 Si6 C18 107.0(7) . . ? 
C21 O3 C20 113.6(12) . . ? 
C21 O3 K1 108.9(8) . . ? 
C20 O3 K1 109.2(8) . . ? 
C26 O6 C27 113.1(10) . . ? 
C26 O6 K1 120.4(8) . . ? 
C27 O6 K1 122.8(8) . . ? 
C24 O5 C25 113.4(11) . . ? 
C24 O5 K1 111.7(10) . . ? 
C25 O5 K1 104.2(7) . . ? 
C30 O2 C19 112.3(11) . . ? 
C30 O2 K1 120.2(7) . . ? 
C19 O2 K1 122.9(8) . . ? 
C23 O4 C22 111.7(13) . . ? 
C23 O4 K1 118.8(9) . . ? 
C22 O4 K1 120.4(9) . . ? 
C29 O7 C28 115.6(12) . . ? 
C29 O7 K1 116.2(9) . . ? 
C28 O7 K1 106.1(8) . . ? 
O6 C27 C28 108.7(10) . . ? 
O2 C30 C29 110.6(12) . . ? 
O6 C26 C25 109.6(11) . . ? 
O7 C28 C27 104.8(11) . . ? 
O3 C21 C22 108.0(13) . . ? 
O5 C24 C23 109.0(13) . . ? 
O5 C25 C26 110.6(12) . . ? 
O3 C20 C19 107.5(11) . . ? 
O7 C29 C30 113.2(14) . . ? 
O2 C19 C20 107.3(14) . . ? 
O4 C22 C21 109.1(13) . . ? 
O4 C23 C24 107.6(14) . . ? 
C33 O8 C33 179.996(13) 5_676 . ? 
C33 O8 C32 62.0(19) 5_676 5_676 ? 
C33 O8 C32 118.0(19) . 5_676 ? 
C33 O8 C32 118.0(19) 5_676 . ? 
C33 O8 C32 62.0(19) . . ? 
C32 O8 C32 179.996(7) 5_676 . ? 
C32 C31 C33 59(2) . . ? 
C31 C32 O8 120(3) . . ? 
O8 C33 C31 118(3) . . ? 
 
_diffrn_measured_fraction_theta_max    0.994 
_diffrn_reflns_theta_full              28.80 
_diffrn_measured_fraction_theta_full   0.994 
_refine_diff_density_max    6.017 
_refine_diff_density_min   -3.222 
_refine_diff_density_rms    0.205 


###END###

  
data_complex_7
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C30 H78 K N3 O6 S Si6 Th' 
_chemical_formula_weight          1048.69 
 
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' 
 'Si'  'Si'   0.0817   0.0704 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'S'  'S'   0.1246   0.1234 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'K'  'K'   0.2009   0.2494 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Th'  'Th'  -7.2400   8.8979 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            Triclinic 
_symmetry_space_group_name_H-M    P-1 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, -y, -z' 
 
_cell_length_a                    12.7484(16) 
_cell_length_b                    18.891(2) 
_cell_length_c                    21.817(3) 
_cell_angle_alpha                 91.554(2) 
_cell_angle_beta                  105.863(2) 
_cell_angle_gamma                 92.564(2) 
_cell_volume                      5044.9(11) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     100(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        needle 
_exptl_crystal_colour             colorless 
_exptl_crystal_size_max           0.1 
_exptl_crystal_size_mid           0.02 
_exptl_crystal_size_min           0.02 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.381 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              2144 
_exptl_absorpt_coefficient_mu     3.258 
_exptl_absorpt_correction_type    'multi-scan' 
_exptl_absorpt_correction_T_min   0.5857 
_exptl_absorpt_correction_T_max   0.7457 
_exptl_absorpt_process_details    SADABS 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       100(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   ? 
_diffrn_measurement_method        ? 
_diffrn_detector_area_resol_mean  ? 
_diffrn_reflns_number             63038 
_diffrn_reflns_av_R_equivalents   0.0408 
_diffrn_reflns_av_sigmaI/netI     0.0566 
_diffrn_reflns_limit_h_min        -16 
_diffrn_reflns_limit_h_max        16 
_diffrn_reflns_limit_k_min        -25 
_diffrn_reflns_limit_k_max        25 
_diffrn_reflns_limit_l_min        -27 
_diffrn_reflns_limit_l_max        29 
_diffrn_reflns_theta_min          0.97 
_diffrn_reflns_theta_max          28.25 
_reflns_number_total              24802 
_reflns_number_gt                 18965 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 2008)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 2008)' 
_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)+(0.1000P)²+0.1479P] 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      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          24802 
_refine_ls_number_parameters      901 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0617 
_refine_ls_R_factor_gt            0.0387 
_refine_ls_wR_factor_ref          0.1275 
_refine_ls_wR_factor_gt           0.1126 
_refine_ls_goodness_of_fit_ref    0.870 
_refine_ls_restrained_S_all       0.870 
_refine_ls_shift/su_max           0.003 
_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 
Th1 Th 0.171690(14) 0.731046(9) 0.325433(8) 0.01617(5) Uani 1 1 d . . . 
Th2 Th 0.591113(14) 0.758383(9) 0.843165(8) 0.01498(5) Uani 1 1 d . . . 
N4 N 0.6201(3) 0.7533(2) 0.74120(18) 0.0184(8) Uani 1 1 d . . . 
N2 N 0.1483(3) 0.7300(2) 0.21351(19) 0.0177(8) Uani 1 1 d . . . 
N5 N 0.6509(3) 0.8657(2) 0.90331(19) 0.0164(8) Uani 1 1 d . . . 
N3 N 0.2695(3) 0.6386(2) 0.38023(18) 0.0153(8) Uani 1 1 d . . . 
N1 N 0.1964(3) 0.8432(2) 0.3800(2) 0.0175(8) Uani 1 1 d . . . 
N6 N 0.6115(3) 0.6532(2) 0.90074(18) 0.0160(8) Uani 1 1 d . . . 
S1 S -0.01697(11) 0.69367(7) 0.33198(7) 0.0241(3) Uani 1 1 d . . . 
S2 S 0.38778(11) 0.76899(7) 0.81337(7) 0.0249(3) Uani 1 1 d . . . 
K1 K -0.24687(9) 0.73523(6) 0.34074(5) 0.0203(2) Uani 1 1 d . . . 
K2 K 0.14225(9) 0.78210(6) 0.78237(5) 0.0224(2) Uani 1 1 d . . . 
Si1 Si 0.31212(11) 0.87301(7) 0.43839(7) 0.0188(3) Uani 1 1 d . . . 
Si12 Si 0.52616(12) 0.63980(7) 0.94916(6) 0.0198(3) Uani 1 1 d . . . 
Si11 Si 0.69793(12) 0.58998(7) 0.88959(7) 0.0204(3) Uani 1 1 d . . . 
Si5 Si 0.38452(12) 0.61699(8) 0.35891(7) 0.0211(3) Uani 1 1 d . . . 
Si2 Si 0.08176(12) 0.89219(8) 0.36218(7) 0.0225(3) Uani 1 1 d . . . 
Si6 Si 0.22262(12) 0.58875(8) 0.43374(7) 0.0199(3) Uani 1 1 d . . . 
Si3 Si 0.20417(12) 0.79718(8) 0.17874(7) 0.0209(3) Uani 1 1 d . . . 
Si10 Si 0.76482(12) 0.86670(8) 0.96727(7) 0.0205(3) Uani 1 1 d . . . 
Si4 Si 0.06346(12) 0.66294(8) 0.16832(7) 0.0248(3) Uani 1 1 d . . . 
Si8 Si 0.52133(14) 0.70742(8) 0.68124(7) 0.0260(3) Uani 1 1 d . . . 
Si9 Si 0.57202(12) 0.93821(7) 0.88271(7) 0.0222(3) Uani 1 1 d . . . 
Si7 Si 0.72690(12) 0.79899(8) 0.72346(7) 0.0227(3) Uani 1 1 d . . . 
O4 O -0.2419(3) 0.59557(19) 0.38575(17) 0.0211(7) Uani 1 1 d . . . 
O7 O 0.1214(3) 0.9063(2) 0.70742(17) 0.0257(8) Uani 1 1 d . . . 
O6 O -0.3007(3) 0.8359(2) 0.42552(17) 0.0236(8) Uani 1 1 d . . . 
O12 O 0.1624(3) 0.91482(19) 0.84123(17) 0.0249(8) Uani 1 1 d . . . 
O1 O -0.3315(3) 0.8709(2) 0.29756(17) 0.0251(8) Uani 1 1 d . . . 
O2 O -0.3784(4) 0.7511(2) 0.21430(17) 0.0317(9) Uani 1 1 d . . . 
O5 O -0.1904(3) 0.7151(2) 0.47294(16) 0.0236(8) Uani 1 1 d . . . 
O11 O 0.1131(3) 0.7972(2) 0.90643(17) 0.0284(9) Uani 1 1 d . . . 
O9 O 0.0758(3) 0.6490(2) 0.7168(2) 0.0347(10) Uani 1 1 d . . . 
O3 O -0.3167(4) 0.6191(2) 0.25511(18) 0.0328(9) Uani 1 1 d . . . 
O10 O 0.1233(3) 0.6644(2) 0.8495(2) 0.0336(9) Uani 1 1 d . . . 
O8 O 0.1112(3) 0.7714(2) 0.65153(19) 0.0333(9) Uani 1 1 d . . . 
C3 C 0.2822(5) 0.8989(3) 0.5156(3) 0.0276(12) Uani 1 1 d . . . 
H3A H 0.2303 0.9366 0.5083 0.041 Uiso 1 1 calc R . . 
H3B H 0.3501 0.9161 0.5470 0.041 Uiso 1 1 calc R . . 
H3C H 0.2507 0.8576 0.5319 0.041 Uiso 1 1 calc R . . 
C2 C 0.3865(5) 0.9521(3) 0.4159(3) 0.0277(12) Uani 1 1 d . . . 
H2A H 0.3920 0.9446 0.3723 0.042 Uiso 1 1 calc R . . 
H2B H 0.4600 0.9583 0.4454 0.042 Uiso 1 1 calc R . . 
H2C H 0.3464 0.9947 0.4184 0.042 Uiso 1 1 calc R . . 
C1 C 0.4131(5) 0.8022(3) 0.4553(3) 0.0288(12) Uani 1 1 d . . . 
H1A H 0.3776 0.7584 0.4650 0.043 Uiso 1 1 calc R . . 
H1B H 0.4744 0.8175 0.4920 0.043 Uiso 1 1 calc R . . 
H1C H 0.4400 0.7936 0.4180 0.043 Uiso 1 1 calc R . . 
C5 C -0.0021(4) 0.8730(3) 0.2769(3) 0.0276(12) Uani 1 1 d . . . 
H5A H 0.0350 0.8952 0.2479 0.041 Uiso 1 1 calc R . . 
H5B H -0.0742 0.8922 0.2706 0.041 Uiso 1 1 calc R . . 
H5C H -0.0105 0.8216 0.2680 0.041 Uiso 1 1 calc R . . 
C4 C -0.0065(5) 0.8748(3) 0.4165(3) 0.0356(14) Uani 1 1 d . . . 
H4A H -0.0175 0.8235 0.4198 0.053 Uiso 1 1 calc R . . 
H4B H -0.0773 0.8953 0.3993 0.053 Uiso 1 1 calc R . . 
H4C H 0.0291 0.8963 0.4589 0.053 Uiso 1 1 calc R . . 
C6 C 0.1131(5) 0.9904(3) 0.3667(3) 0.0343(13) Uani 1 1 d . . . 
H6A H 0.1486 1.0060 0.4110 0.052 Uiso 1 1 calc R . . 
H6B H 0.0451 1.0147 0.3511 0.052 Uiso 1 1 calc R . . 
H6C H 0.1620 1.0018 0.3402 0.052 Uiso 1 1 calc R . . 
C8 C 0.2781(5) 0.8655(3) 0.2409(3) 0.0303(13) Uani 1 1 d . . . 
H8A H 0.2260 0.8873 0.2604 0.046 Uiso 1 1 calc R . . 
H8B H 0.3135 0.9021 0.2212 0.046 Uiso 1 1 calc R . . 
H8C H 0.3335 0.8430 0.2738 0.046 Uiso 1 1 calc R . . 
C7 C 0.3086(5) 0.7678(3) 0.1381(3) 0.0283(12) Uani 1 1 d . . . 
H7A H 0.3709 0.7498 0.1698 0.042 Uiso 1 1 calc R . . 
H7B H 0.3336 0.8081 0.1175 0.042 Uiso 1 1 calc R . . 
H7C H 0.2757 0.7301 0.1059 0.042 Uiso 1 1 calc R . . 
C9 C 0.0983(5) 0.8428(3) 0.1187(3) 0.0311(13) Uani 1 1 d . . . 
H9A H 0.0617 0.8092 0.0836 0.047 Uiso 1 1 calc R . . 
H9B H 0.1331 0.8824 0.1020 0.047 Uiso 1 1 calc R . . 
H9C H 0.0445 0.8610 0.1389 0.047 Uiso 1 1 calc R . . 
C10 C 0.0955(5) 0.6378(4) 0.0917(3) 0.0350(14) Uani 1 1 d . . . 
H10A H 0.0914 0.6795 0.0655 0.053 Uiso 1 1 calc R . . 
H10B H 0.0426 0.6005 0.0684 0.053 Uiso 1 1 calc R . . 
H10C H 0.1693 0.6204 0.1012 0.053 Uiso 1 1 calc R . . 
C12 C 0.0774(6) 0.5789(3) 0.2135(3) 0.0387(15) Uani 1 1 d . . . 
H12A H 0.1543 0.5676 0.2270 0.058 Uiso 1 1 calc R . . 
H12B H 0.0345 0.5400 0.1860 0.058 Uiso 1 1 calc R . . 
H12C H 0.0505 0.5855 0.2512 0.058 Uiso 1 1 calc R . . 
C11 C -0.0827(5) 0.6862(4) 0.1469(3) 0.0405(16) Uani 1 1 d . . . 
H11A H -0.1034 0.6984 0.1858 0.061 Uiso 1 1 calc R . . 
H11B H -0.1290 0.6455 0.1243 0.061 Uiso 1 1 calc R . . 
H11C H -0.0925 0.7268 0.1192 0.061 Uiso 1 1 calc R . . 
C14 C 0.5141(4) 0.6246(3) 0.4247(3) 0.0281(12) Uani 1 1 d . . . 
H14A H 0.5137 0.6663 0.4524 0.042 Uiso 1 1 calc R . . 
H14B H 0.5763 0.6296 0.4067 0.042 Uiso 1 1 calc R . . 
H14C H 0.5203 0.5819 0.4498 0.042 Uiso 1 1 calc R . . 
C13 C 0.4071(5) 0.6810(4) 0.2992(3) 0.0386(15) Uani 1 1 d . . . 
H13A H 0.3479 0.6739 0.2596 0.058 Uiso 1 1 calc R . . 
H13B H 0.4771 0.6730 0.2904 0.058 Uiso 1 1 calc R . . 
H13C H 0.4079 0.7296 0.3163 0.058 Uiso 1 1 calc R . . 
C15 C 0.3724(5) 0.5262(4) 0.3211(3) 0.0426(16) Uani 1 1 d . . . 
H15A H 0.3436 0.4925 0.3465 0.064 Uiso 1 1 calc R . . 
H15B H 0.4446 0.5125 0.3188 0.064 Uiso 1 1 calc R . . 
H15C H 0.3228 0.5259 0.2779 0.064 Uiso 1 1 calc R . . 
C17 C 0.1112(4) 0.5215(3) 0.3934(3) 0.0273(12) Uani 1 1 d . . . 
H17A H 0.0531 0.5450 0.3631 0.041 Uiso 1 1 calc R . . 
H17B H 0.0815 0.4989 0.4255 0.041 Uiso 1 1 calc R . . 
H17C H 0.1407 0.4855 0.3706 0.041 Uiso 1 1 calc R . . 
C16 C 0.1713(5) 0.6468(3) 0.4885(3) 0.0332(14) Uani 1 1 d . . . 
H16A H 0.2321 0.6766 0.5155 0.050 Uiso 1 1 calc R . . 
H16B H 0.1384 0.6173 0.5153 0.050 Uiso 1 1 calc R . . 
H16C H 0.1163 0.6770 0.4633 0.050 Uiso 1 1 calc R . . 
C18 C 0.3316(5) 0.5380(4) 0.4878(3) 0.0371(15) Uani 1 1 d . . . 
H18A H 0.3579 0.5029 0.4624 0.056 Uiso 1 1 calc R . . 
H18B H 0.3013 0.5138 0.5188 0.056 Uiso 1 1 calc R . . 
H18C H 0.3924 0.5709 0.5103 0.056 Uiso 1 1 calc R . . 
C26 C -0.1859(4) 0.6433(3) 0.4921(2) 0.0242(11) Uani 1 1 d . . . 
H26A H -0.2582 0.6258 0.4958 0.029 Uiso 1 1 calc R . . 
H26B H -0.1319 0.6401 0.5341 0.029 Uiso 1 1 calc R . . 
C23 C -0.3200(5) 0.5495(3) 0.2801(3) 0.0298(12) Uani 1 1 d . . . 
H23A H -0.3150 0.5129 0.2479 0.036 Uiso 1 1 calc R . . 
H23B H -0.3894 0.5404 0.2915 0.036 Uiso 1 1 calc R . . 
C24 C -0.2247(4) 0.5474(3) 0.3383(3) 0.0252(11) Uani 1 1 d . . . 
H24A H -0.2189 0.4988 0.3543 0.030 Uiso 1 1 calc R . . 
H24B H -0.1561 0.5613 0.3278 0.030 Uiso 1 1 calc R . . 
C27 C -0.2418(5) 0.7573(3) 0.5100(2) 0.0250(11) Uani 1 1 d . . . 
H27A H -0.2033 0.7547 0.5559 0.030 Uiso 1 1 calc R . . 
H27B H -0.3185 0.7394 0.5034 0.030 Uiso 1 1 calc R . . 
C30 C -0.3837(5) 0.9070(3) 0.3392(3) 0.0299(12) Uani 1 1 d . . . 
H30A H -0.4550 0.8824 0.3368 0.036 Uiso 1 1 calc R . . 
H30B H -0.3968 0.9562 0.3259 0.036 Uiso 1 1 calc R . . 
C28 C -0.2386(5) 0.8319(3) 0.4902(2) 0.0252(11) Uani 1 1 d . . . 
H28A H -0.2689 0.8627 0.5179 0.030 Uiso 1 1 calc R . . 
H28B H -0.1620 0.8488 0.4950 0.030 Uiso 1 1 calc R . . 
C25 C -0.1531(4) 0.5989(3) 0.4422(2) 0.0239(11) Uani 1 1 d . . . 
H25A H -0.0869 0.6207 0.4335 0.029 Uiso 1 1 calc R . . 
H25B H -0.1371 0.5506 0.4574 0.029 Uiso 1 1 calc R . . 
C29 C -0.3118(5) 0.9076(3) 0.4061(3) 0.0292(12) Uani 1 1 d . . . 
H29A H -0.2392 0.9302 0.4083 0.035 Uiso 1 1 calc R . . 
H29B H -0.3445 0.9351 0.4348 0.035 Uiso 1 1 calc R . . 
C21 C -0.3694(5) 0.6958(3) 0.1706(3) 0.0301(13) Uani 1 1 d . . . 
H21A H -0.2949 0.6979 0.1649 0.036 Uiso 1 1 calc R . . 
H21B H -0.4221 0.7018 0.1285 0.036 Uiso 1 1 calc R . . 
C20 C -0.3575(5) 0.8187(3) 0.1937(3) 0.0297(12) Uani 1 1 d . . . 
H20A H -0.3964 0.8222 0.1481 0.036 Uiso 1 1 calc R . . 
H20B H -0.2782 0.8271 0.1990 0.036 Uiso 1 1 calc R . . 
C22 C -0.3922(5) 0.6267(3) 0.1953(3) 0.0345(14) Uani 1 1 d . . . 
H22A H -0.4675 0.6240 0.1998 0.041 Uiso 1 1 calc R . . 
H22B H -0.3860 0.5880 0.1653 0.041 Uiso 1 1 calc R . . 
C19 C -0.3959(6) 0.8722(3) 0.2327(3) 0.0362(14) Uani 1 1 d . . . 
H19A H -0.3890 0.9200 0.2162 0.043 Uiso 1 1 calc R . . 
H19B H -0.4738 0.8614 0.2301 0.043 Uiso 1 1 calc R . . 
C31 C 0.6790(5) 0.8580(3) 0.6546(3) 0.0336(14) Uani 1 1 d . . . 
H31A H 0.6406 0.8290 0.6164 0.050 Uiso 1 1 calc R . . 
H31B H 0.7421 0.8839 0.6467 0.050 Uiso 1 1 calc R . . 
H31C H 0.6294 0.8918 0.6646 0.050 Uiso 1 1 calc R . . 
C32 C 0.8319(5) 0.7422(4) 0.7045(3) 0.0416(17) Uani 1 1 d . . . 
H32A H 0.8671 0.7159 0.7420 0.062 Uiso 1 1 calc R . . 
H32B H 0.8871 0.7723 0.6925 0.062 Uiso 1 1 calc R . . 
H32C H 0.7965 0.7087 0.6690 0.062 Uiso 1 1 calc R . . 
C33 C 0.8075(5) 0.8570(4) 0.7927(3) 0.0457(18) Uani 1 1 d . . . 
H33A H 0.7584 0.8879 0.8071 0.069 Uiso 1 1 calc R . . 
H33B H 0.8626 0.8862 0.7796 0.069 Uiso 1 1 calc R . . 
H33C H 0.8438 0.8274 0.8276 0.069 Uiso 1 1 calc R . . 
C36 C 0.4606(5) 0.6298(3) 0.7147(3) 0.0317(13) Uani 1 1 d . . . 
H36A H 0.5187 0.5991 0.7356 0.048 Uiso 1 1 calc R . . 
H36B H 0.4074 0.6028 0.6800 0.048 Uiso 1 1 calc R . . 
H36C H 0.4241 0.6471 0.7458 0.048 Uiso 1 1 calc R . . 
C34 C 0.5779(7) 0.6684(4) 0.6170(3) 0.061(3) Uani 1 1 d . . . 
H34A H 0.6020 0.7068 0.5939 0.092 Uiso 1 1 calc R . . 
H34B H 0.5209 0.6381 0.5873 0.092 Uiso 1 1 calc R . . 
H34C H 0.6399 0.6401 0.6366 0.092 Uiso 1 1 calc R . . 
C35 C 0.4079(5) 0.7647(4) 0.6417(3) 0.0459(17) Uani 1 1 d . . . 
H35A H 0.3786 0.7871 0.6742 0.069 Uiso 1 1 calc R . . 
H35B H 0.3498 0.7355 0.6117 0.069 Uiso 1 1 calc R . . 
H35C H 0.4360 0.8015 0.6186 0.069 Uiso 1 1 calc R . . 
C37 C 0.5269(5) 0.9415(3) 0.7926(3) 0.0323(13) Uani 1 1 d . . . 
H37A H 0.5904 0.9530 0.7769 0.048 Uiso 1 1 calc R . . 
H37B H 0.4736 0.9779 0.7801 0.048 Uiso 1 1 calc R . . 
H37C H 0.4934 0.8952 0.7743 0.048 Uiso 1 1 calc R . . 
C38 C 0.4504(5) 0.9369(3) 0.9153(3) 0.0367(15) Uani 1 1 d . . . 
H38A H 0.4013 0.8958 0.8968 0.055 Uiso 1 1 calc R . . 
H38B H 0.4117 0.9805 0.9045 0.055 Uiso 1 1 calc R . . 
H38C H 0.4746 0.9338 0.9618 0.055 Uiso 1 1 calc R . . 
C39 C 0.6486(6) 1.0260(3) 0.9114(4) 0.0420(16) Uani 1 1 d . . . 
H39A H 0.6803 1.0261 0.9577 0.063 Uiso 1 1 calc R . . 
H39B H 0.5982 1.0644 0.9009 0.063 Uiso 1 1 calc R . . 
H39C H 0.7070 1.0331 0.8905 0.063 Uiso 1 1 calc R . . 
C42 C 0.8763(4) 0.9346(3) 0.9650(3) 0.0294(12) Uani 1 1 d . . . 
H42A H 0.8999 0.9260 0.9264 0.044 Uiso 1 1 calc R . . 
H42B H 0.9383 0.9308 1.0027 0.044 Uiso 1 1 calc R . . 
H42C H 0.8486 0.9822 0.9647 0.044 Uiso 1 1 calc R . . 
C40 C 0.7349(6) 0.8815(4) 1.0463(3) 0.0398(16) Uani 1 1 d . . . 
H40A H 0.7043 0.9280 1.0478 0.060 Uiso 1 1 calc R . . 
H40B H 0.8026 0.8798 1.0808 0.060 Uiso 1 1 calc R . . 
H40C H 0.6821 0.8444 1.0515 0.060 Uiso 1 1 calc R . . 
C41 C 0.8266(5) 0.7785(3) 0.9680(3) 0.0396(15) Uani 1 1 d . . . 
H41A H 0.7720 0.7408 0.9693 0.059 Uiso 1 1 calc R . . 
H41B H 0.8893 0.7769 1.0056 0.059 Uiso 1 1 calc R . . 
H41C H 0.8507 0.7718 0.9294 0.059 Uiso 1 1 calc R . . 
C43 C 0.7659(5) 0.6184(3) 0.8273(3) 0.0289(12) Uani 1 1 d . . . 
H43A H 0.7106 0.6217 0.7864 0.043 Uiso 1 1 calc R . . 
H43B H 0.8183 0.5835 0.8229 0.043 Uiso 1 1 calc R . . 
H43C H 0.8044 0.6648 0.8401 0.043 Uiso 1 1 calc R . . 
C44 C 0.6248(5) 0.5016(3) 0.8615(3) 0.0289(12) Uani 1 1 d . . . 
H44A H 0.5938 0.4829 0.8946 0.043 Uiso 1 1 calc R . . 
H44B H 0.6765 0.4685 0.8526 0.043 Uiso 1 1 calc R . . 
H44C H 0.5660 0.5071 0.8225 0.043 Uiso 1 1 calc R . . 
C45 C 0.8145(5) 0.5750(3) 0.9620(3) 0.0347(14) Uani 1 1 d . . . 
H45A H 0.8482 0.6209 0.9813 0.052 Uiso 1 1 calc R . . 
H45B H 0.8691 0.5476 0.9492 0.052 Uiso 1 1 calc R . . 
H45C H 0.7869 0.5489 0.9930 0.052 Uiso 1 1 calc R . . 
C48 C 0.4990(5) 0.7265(3) 0.9839(3) 0.0264(12) Uani 1 1 d . . . 
H48A H 0.5674 0.7483 1.0115 0.040 Uiso 1 1 calc R . . 
H48B H 0.4468 0.7184 1.0090 0.040 Uiso 1 1 calc R . . 
H48C H 0.4686 0.7581 0.9494 0.040 Uiso 1 1 calc R . . 
C47 C 0.3917(5) 0.5952(3) 0.9054(3) 0.0289(12) Uani 1 1 d . . . 
H47A H 0.3538 0.6252 0.8712 0.043 Uiso 1 1 calc R . . 
H47B H 0.3471 0.5877 0.9350 0.043 Uiso 1 1 calc R . . 
H47C H 0.4037 0.5494 0.8869 0.043 Uiso 1 1 calc R . . 
C46 C 0.5877(5) 0.5854(3) 1.0192(2) 0.0267(12) Uani 1 1 d . . . 
H46A H 0.6114 0.5411 1.0043 0.040 Uiso 1 1 calc R . . 
H46B H 0.5331 0.5746 1.0422 0.040 Uiso 1 1 calc R . . 
H46C H 0.6506 0.6121 1.0478 0.040 Uiso 1 1 calc R . . 
C59 C 0.1452(5) 0.9753(3) 0.8032(3) 0.0312(13) Uani 1 1 d . . . 
H59A H 0.1838 1.0177 0.8283 0.037 Uiso 1 1 calc R . . 
H59B H 0.0662 0.9837 0.7889 0.037 Uiso 1 1 calc R . . 
C58 C 0.1245(5) 0.9221(3) 0.8957(3) 0.0325(13) Uani 1 1 d . . . 
H58A H 0.0437 0.9207 0.8832 0.039 Uiso 1 1 calc R . . 
H58B H 0.1522 0.9681 0.9185 0.039 Uiso 1 1 calc R . . 
C60 C 0.1886(5) 0.9618(3) 0.7457(3) 0.0305(12) Uani 1 1 d . . . 
H60A H 0.1861 1.0053 0.7211 0.037 Uiso 1 1 calc R . . 
H60B H 0.2652 0.9480 0.7598 0.037 Uiso 1 1 calc R . . 
C57 C 0.1645(6) 0.8624(3) 0.9382(3) 0.0382(15) Uani 1 1 d . . . 
H57A H 0.2448 0.8610 0.9474 0.046 Uiso 1 1 calc R . . 
H57B H 0.1461 0.8692 0.9791 0.046 Uiso 1 1 calc R . . 
C49 C 0.1492(5) 0.8938(3) 0.6502(3) 0.0342(14) Uani 1 1 d . . . 
H49A H 0.2275 0.8839 0.6594 0.041 Uiso 1 1 calc R . . 
H49B H 0.1362 0.9361 0.6239 0.041 Uiso 1 1 calc R . . 
C55 C 0.0991(6) 0.6718(4) 0.9086(3) 0.0430(16) Uani 1 1 d . . . 
H55A H 0.1243 0.6307 0.9348 0.052 Uiso 1 1 calc R . . 
H55B H 0.0192 0.6738 0.9017 0.052 Uiso 1 1 calc R . . 
C52 C 0.1046(6) 0.6469(3) 0.6587(3) 0.0418(16) Uani 1 1 d . . . 
H52A H 0.0761 0.6017 0.6347 0.050 Uiso 1 1 calc R . . 
H52B H 0.1851 0.6499 0.6673 0.050 Uiso 1 1 calc R . . 
C53 C 0.1228(5) 0.5946(3) 0.7583(4) 0.0416(16) Uani 1 1 d . . . 
H53A H 0.2034 0.6009 0.7702 0.050 Uiso 1 1 calc R . . 
H53B H 0.1012 0.5476 0.7363 0.050 Uiso 1 1 calc R . . 
C51 C 0.0567(5) 0.7085(3) 0.6201(3) 0.0375(15) Uani 1 1 d . . . 
H51A H 0.0663 0.7040 0.5767 0.045 Uiso 1 1 calc R . . 
H51B H -0.0225 0.7093 0.6163 0.045 Uiso 1 1 calc R . . 
C54 C 0.0841(5) 0.5985(3) 0.8165(4) 0.0424(16) Uani 1 1 d . . . 
H54A H 0.0033 0.5948 0.8047 0.051 Uiso 1 1 calc R . . 
H54B H 0.1118 0.5589 0.8442 0.051 Uiso 1 1 calc R . . 
C50 C 0.0808(5) 0.8318(4) 0.6151(3) 0.0371(15) Uani 1 1 d . . . 
H50A H 0.0025 0.8395 0.6095 0.045 Uiso 1 1 calc R . . 
H50B H 0.0929 0.8250 0.5725 0.045 Uiso 1 1 calc R . . 
C56 C 0.1562(6) 0.7391(4) 0.9421(3) 0.0427(16) Uani 1 1 d . . . 
H56A H 0.1456 0.7435 0.9853 0.051 Uiso 1 1 calc R . . 
H56B H 0.2356 0.7382 0.9466 0.051 Uiso 1 1 calc R . . 
 
 
_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 
Th1 N3 2.351(4) . ? 
Th1 N1 2.368(4) . ? 
Th1 N2 2.377(4) . ? 
Th1 S1 2.5190(13) . ? 
Th2 N4 2.353(4) . ? 
Th2 N5 2.363(4) . ? 
Th2 N6 2.366(4) . ? 
Th2 S2 2.5129(14) . ? 
N4 Si7 1.718(4) . ? 
N4 Si8 1.729(4) . ? 
N2 Si3 1.720(4) . ? 
N2 Si4 1.725(4) . ? 
N5 Si10 1.716(4) . ? 
N5 Si9 1.732(4) . ? 
N3 Si5 1.717(4) . ? 
N3 Si6 1.732(4) . ? 
N1 Si2 1.724(4) . ? 
N1 Si1 1.724(4) . ? 
N6 Si11 1.717(4) . ? 
N6 Si12 1.726(4) . ? 
S1 K1 3.1219(17) . ? 
S2 K2 3.0393(18) . ? 
K1 O3 2.791(4) . ? 
K1 O5 2.816(4) . ? 
K1 O4 2.837(4) . ? 
K1 O2 2.841(4) . ? 
K1 O6 2.852(4) . ? 
K1 O1 2.906(4) . ? 
K2 O10 2.732(4) . ? 
K2 O12 2.755(4) . ? 
K2 O8 2.773(4) . ? 
K2 O9 2.834(4) . ? 
K2 O11 2.839(4) . ? 
K2 O7 2.877(4) . ? 
Si1 C1 1.872(6) . ? 
Si1 C2 1.882(6) . ? 
Si1 C3 1.884(5) . ? 
Si12 C47 1.868(6) . ? 
Si12 C48 1.872(5) . ? 
Si12 C46 1.873(5) . ? 
Si11 C44 1.878(6) . ? 
Si11 C43 1.879(6) . ? 
Si11 C45 1.887(6) . ? 
Si5 C15 1.865(6) . ? 
Si5 C14 1.866(6) . ? 
Si5 C13 1.871(6) . ? 
Si2 C4 1.870(6) . ? 
Si2 C6 1.875(6) . ? 
Si2 C5 1.891(6) . ? 
Si6 C16 1.864(6) . ? 
Si6 C17 1.870(6) . ? 
Si6 C18 1.876(6) . ? 
Si3 C9 1.866(6) . ? 
Si3 C8 1.869(6) . ? 
Si3 C7 1.885(6) . ? 
Si10 C41 1.872(6) . ? 
Si10 C40 1.881(6) . ? 
Si10 C42 1.882(6) . ? 
Si4 C11 1.869(6) . ? 
Si4 C12 1.881(6) . ? 
Si4 C10 1.881(6) . ? 
Si8 C35 1.875(7) . ? 
Si8 C36 1.883(6) . ? 
Si8 C34 1.889(7) . ? 
Si9 C38 1.874(6) . ? 
Si9 C39 1.887(6) . ? 
Si9 C37 1.895(6) . ? 
Si7 C33 1.871(6) . ? 
Si7 C32 1.877(6) . ? 
Si7 C31 1.877(6) . ? 
O4 C25 1.424(6) . ? 
O4 C24 1.428(6) . ? 
O7 C49 1.406(6) . ? 
O7 C60 1.419(7) . ? 
O6 C28 1.424(6) . ? 
O6 C29 1.431(7) . ? 
O12 C58 1.407(6) . ? 
O12 C59 1.420(7) . ? 
O1 C19 1.430(7) . ? 
O1 C30 1.439(6) . ? 
O2 C20 1.403(7) . ? 
O2 C21 1.426(7) . ? 
O5 C27 1.422(6) . ? 
O5 C26 1.430(6) . ? 
O11 C56 1.406(8) . ? 
O11 C57 1.435(7) . ? 
O9 C52 1.413(8) . ? 
O9 C53 1.430(8) . ? 
O3 C22 1.409(7) . ? 
O3 C23 1.440(7) . ? 
O10 C55 1.411(8) . ? 
O10 C54 1.420(7) . ? 
O8 C51 1.410(7) . ? 
O8 C50 1.415(8) . ? 
C26 C25 1.515(8) . ? 
C23 C24 1.501(8) . ? 
C27 C28 1.488(8) . ? 
C30 C29 1.495(8) . ? 
C21 C22 1.472(8) . ? 
C20 C19 1.488(8) . ? 
C59 C60 1.522(8) . ? 
C58 C57 1.497(9) . ? 
C49 C50 1.488(9) . ? 
C55 C56 1.503(10) . ? 
C52 C51 1.508(10) . ? 
C53 C54 1.483(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 
N3 Th1 N1 116.67(14) . . ? 
N3 Th1 N2 116.17(14) . . ? 
N1 Th1 N2 117.12(14) . . ? 
N3 Th1 S1 99.50(10) . . ? 
N1 Th1 S1 100.25(10) . . ? 
N2 Th1 S1 102.26(10) . . ? 
N4 Th2 N5 115.64(14) . . ? 
N4 Th2 N6 117.37(14) . . ? 
N5 Th2 N6 116.47(14) . . ? 
N4 Th2 S2 100.18(11) . . ? 
N5 Th2 S2 100.69(10) . . ? 
N6 Th2 S2 101.89(10) . . ? 
Si7 N4 Si8 119.9(2) . . ? 
Si7 N4 Th2 122.8(2) . . ? 
Si8 N4 Th2 117.0(2) . . ? 
Si3 N2 Si4 121.6(2) . . ? 
Si3 N2 Th1 121.4(2) . . ? 
Si4 N2 Th1 116.8(2) . . ? 
Si10 N5 Si9 123.5(2) . . ? 
Si10 N5 Th2 118.8(2) . . ? 
Si9 N5 Th2 117.6(2) . . ? 
Si5 N3 Si6 120.9(2) . . ? 
Si5 N3 Th1 116.38(19) . . ? 
Si6 N3 Th1 122.4(2) . . ? 
Si2 N1 Si1 120.7(2) . . ? 
Si2 N1 Th1 114.0(2) . . ? 
Si1 N1 Th1 125.0(2) . . ? 
Si11 N6 Si12 121.7(2) . . ? 
Si11 N6 Th2 121.6(2) . . ? 
Si12 N6 Th2 116.4(2) . . ? 
Th1 S1 K1 149.20(6) . . ? 
Th2 S2 K2 177.95(6) . . ? 
O3 K1 O5 119.90(12) . . ? 
O3 K1 O4 59.71(11) . . ? 
O5 K1 O4 60.45(11) . . ? 
O3 K1 O2 58.35(12) . . ? 
O5 K1 O2 159.70(12) . . ? 
O4 K1 O2 115.82(11) . . ? 
O3 K1 O6 147.38(13) . . ? 
O5 K1 O6 59.38(11) . . ? 
O4 K1 O6 112.52(11) . . ? 
O2 K1 O6 110.01(12) . . ? 
O3 K1 O1 116.45(12) . . ? 
O5 K1 O1 117.24(11) . . ? 
O4 K1 O1 159.44(11) . . ? 
O2 K1 O1 58.32(11) . . ? 
O6 K1 O1 58.46(10) . . ? 
O3 K1 S1 82.58(10) . . ? 
O5 K1 S1 91.82(9) . . ? 
O4 K1 S1 79.33(8) . . ? 
O2 K1 S1 107.41(9) . . ? 
O6 K1 S1 128.99(9) . . ? 
O1 K1 S1 121.04(9) . . ? 
O10 K2 O12 119.82(12) . . ? 
O10 K2 O8 120.73(14) . . ? 
O12 K2 O8 118.85(13) . . ? 
O10 K2 O9 60.22(14) . . ? 
O12 K2 O9 168.46(12) . . ? 
O8 K2 O9 60.64(13) . . ? 
O10 K2 O11 60.13(12) . . ? 
O12 K2 O11 60.27(11) . . ? 
O8 K2 O11 164.72(12) . . ? 
O9 K2 O11 116.78(13) . . ? 
O10 K2 O7 169.96(12) . . ? 
O12 K2 O7 60.06(11) . . ? 
O8 K2 O7 58.84(12) . . ? 
O9 K2 O7 117.61(13) . . ? 
O11 K2 O7 117.29(11) . . ? 
O10 K2 S2 90.44(10) . . ? 
O12 K2 S2 93.28(9) . . ? 
O8 K2 S2 94.05(9) . . ? 
O9 K2 S2 98.25(9) . . ? 
O11 K2 S2 101.23(9) . . ? 
O7 K2 S2 99.60(9) . . ? 
N1 Si1 C1 110.2(2) . . ? 
N1 Si1 C2 113.9(2) . . ? 
C1 Si1 C2 105.6(3) . . ? 
N1 Si1 C3 112.6(2) . . ? 
C1 Si1 C3 107.7(3) . . ? 
C2 Si1 C3 106.4(3) . . ? 
N6 Si12 C47 112.5(2) . . ? 
N6 Si12 C48 110.3(2) . . ? 
C47 Si12 C48 107.9(3) . . ? 
N6 Si12 C46 112.7(2) . . ? 
C47 Si12 C46 107.6(3) . . ? 
C48 Si12 C46 105.4(2) . . ? 
N6 Si11 C44 112.6(2) . . ? 
N6 Si11 C43 109.8(2) . . ? 
C44 Si11 C43 107.1(3) . . ? 
N6 Si11 C45 114.8(2) . . ? 
C44 Si11 C45 107.5(3) . . ? 
C43 Si11 C45 104.5(3) . . ? 
N3 Si5 C15 113.0(3) . . ? 
N3 Si5 C14 115.3(2) . . ? 
C15 Si5 C14 107.7(3) . . ? 
N3 Si5 C13 108.5(2) . . ? 
C15 Si5 C13 107.3(3) . . ? 
C14 Si5 C13 104.6(3) . . ? 
N1 Si2 C4 112.3(3) . . ? 
N1 Si2 C6 113.7(2) . . ? 
C4 Si2 C6 106.6(3) . . ? 
N1 Si2 C5 110.8(2) . . ? 
C4 Si2 C5 108.9(3) . . ? 
C6 Si2 C5 104.0(3) . . ? 
N3 Si6 C16 110.9(2) . . ? 
N3 Si6 C17 112.8(2) . . ? 
C16 Si6 C17 108.5(3) . . ? 
N3 Si6 C18 113.4(2) . . ? 
C16 Si6 C18 104.8(3) . . ? 
C17 Si6 C18 106.0(3) . . ? 
N2 Si3 C9 112.2(2) . . ? 
N2 Si3 C8 109.9(2) . . ? 
C9 Si3 C8 107.4(3) . . ? 
N2 Si3 C7 114.1(2) . . ? 
C9 Si3 C7 107.4(3) . . ? 
C8 Si3 C7 105.4(3) . . ? 
N5 Si10 C41 108.1(2) . . ? 
N5 Si10 C40 113.5(3) . . ? 
C41 Si10 C40 107.7(3) . . ? 
N5 Si10 C42 115.0(2) . . ? 
C41 Si10 C42 105.7(3) . . ? 
C40 Si10 C42 106.4(3) . . ? 
N2 Si4 C11 111.7(3) . . ? 
N2 Si4 C12 110.0(2) . . ? 
C11 Si4 C12 108.8(3) . . ? 
N2 Si4 C10 114.6(2) . . ? 
C11 Si4 C10 106.9(3) . . ? 
C12 Si4 C10 104.4(3) . . ? 
N4 Si8 C35 112.1(3) . . ? 
N4 Si8 C36 110.1(2) . . ? 
C35 Si8 C36 108.2(3) . . ? 
N4 Si8 C34 112.8(3) . . ? 
C35 Si8 C34 107.7(4) . . ? 
C36 Si8 C34 105.6(3) . . ? 
N5 Si9 C38 113.2(3) . . ? 
N5 Si9 C39 113.7(3) . . ? 
C38 Si9 C39 105.5(3) . . ? 
N5 Si9 C37 108.6(2) . . ? 
C38 Si9 C37 110.3(3) . . ? 
C39 Si9 C37 105.2(3) . . ? 
N4 Si7 C33 111.5(2) . . ? 
N4 Si7 C32 115.1(3) . . ? 
C33 Si7 C32 103.5(3) . . ? 
N4 Si7 C31 112.0(2) . . ? 
C33 Si7 C31 106.9(3) . . ? 
C32 Si7 C31 107.1(3) . . ? 
C25 O4 C24 111.9(4) . . ? 
C25 O4 K1 104.5(3) . . ? 
C24 O4 K1 109.3(3) . . ? 
C49 O7 C60 111.9(4) . . ? 
C49 O7 K2 111.6(3) . . ? 
C60 O7 K2 107.5(3) . . ? 
C28 O6 C29 112.1(4) . . ? 
C28 O6 K1 113.9(3) . . ? 
C29 O6 K1 117.6(3) . . ? 
C58 O12 C59 112.6(4) . . ? 
C58 O12 K2 117.7(3) . . ? 
C59 O12 K2 119.1(3) . . ? 
C19 O1 C30 110.6(4) . . ? 
C19 O1 K1 116.4(3) . . ? 
C30 O1 K1 115.0(3) . . ? 
C20 O2 C21 112.5(4) . . ? 
C20 O2 K1 110.0(3) . . ? 
C21 O2 K1 113.7(3) . . ? 
C27 O5 C26 111.3(4) . . ? 
C27 O5 K1 117.1(3) . . ? 
C26 O5 K1 116.4(3) . . ? 
C56 O11 C57 110.3(5) . . ? 
C56 O11 K2 109.2(4) . . ? 
C57 O11 K2 111.4(3) . . ? 
C52 O9 C53 112.9(5) . . ? 
C52 O9 K2 110.5(4) . . ? 
C53 O9 K2 108.4(3) . . ? 
C22 O3 C23 114.3(4) . . ? 
C22 O3 K1 120.7(3) . . ? 
C23 O3 K1 118.6(3) . . ? 
C55 O10 C54 113.5(5) . . ? 
C55 O10 K2 119.6(4) . . ? 
C54 O10 K2 119.8(4) . . ? 
C51 O8 C50 112.2(5) . . ? 
C51 O8 K2 116.3(4) . . ? 
C50 O8 K2 119.0(3) . . ? 
O5 C26 C25 108.1(4) . . ? 
O3 C23 C24 107.4(4) . . ? 
O4 C24 C23 108.0(4) . . ? 
O5 C27 C28 108.7(4) . . ? 
O1 C30 C29 109.2(4) . . ? 
O6 C28 C27 109.6(4) . . ? 
O4 C25 C26 107.6(4) . . ? 
O6 C29 C30 108.4(5) . . ? 
O2 C21 C22 109.4(4) . . ? 
O2 C20 C19 108.3(5) . . ? 
O3 C22 C21 109.1(5) . . ? 
O1 C19 C20 109.1(5) . . ? 
O12 C59 C60 108.4(4) . . ? 
O12 C58 C57 108.3(5) . . ? 
O7 C60 C59 107.4(5) . . ? 
O11 C57 C58 108.5(5) . . ? 
O7 C49 C50 108.5(5) . . ? 
O10 C55 C56 108.3(5) . . ? 
O9 C52 C51 108.9(5) . . ? 
O9 C53 C54 109.3(5) . . ? 
O8 C51 C52 108.0(5) . . ? 
O10 C54 C53 108.4(5) . . ? 
O8 C50 C49 107.6(5) . . ? 
O11 C56 C55 109.1(6) . . ? 
 
_diffrn_measured_fraction_theta_max    0.994 
_diffrn_reflns_theta_full              28.25 
_diffrn_measured_fraction_theta_full   0.994 
_refine_diff_density_max    4.482 
_refine_diff_density_min   -1.860 
_refine_diff_density_rms    0.132 
